NC0089109_Renewal (Application)_20221216

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ROY COOPER -
Governor >�
ELIZABETH S.BISER
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Secretary
RICHARD E.ROGERS,JR. NORTH CAROLINA
Director Environmental Quality
December 29, 2022
Befesa Zinc Metal, LLC
Attn: Jan Nedbal, Environmental Manager
484 Hicks Grove Rd
Mooresboro, NC 28114
Subject: Permit Renewal
Application No. NC0089109
Befesa Zinc Metal, LLC
Rutherford County
Dear Applicant:
The Water Quality Permitting Section acknowledges the December 16, 2022, receipt of your permit renewal application
and supporting documentation. Your application will be assigned to a permit writer within the Section's NPDES WW
permitting branch. Per G.S. 150E-3 your current permit does not expire until permit decision on the application is made.
Continuation of the current permit is contingent on timely and sufficient application for renewal of the current permit. The
permit writer will contact you if additional information is required to complete your permit renewal. Please respond in a
timely manner to requests for additional information necessary to allow a complete review of the application and renewal
of the permit.
Information regarding the status of your renewal application can be found online using the Department of Environmental
Quality's Environmental Application Tracker at:
https://deq.nc.gov/permits-regulations/permit-guidance/environmental-application-tracker
If you have any additional questions about the permit, please contact the primary reviewer of the application using the
links available within the Application Tracker.
Sincerely,
Wren Thedford
Administrative Assistant
Water Quality Permitting Section
ec: WQPS Laserfiche File w/application

RECE"JED
14 December 2022 DEC 16 2022
North Carolina Dept. of Environmental Quality NCDEQIDW�NP�ES
Division of Water Resources
Water Quality Permitting Section
512 N Salisbury Street
Raleigh, NC 27604
Subject: NPDES Effluent Permit Renewal Application
Befesa Zinc Metal, LLC
NPDES Individual Permit No. NC0089109
Rutherford County
Dear Sir/Madam:
Enclosed are three (3) copies of the NPDES Effluent Permit Renewal Application and required supplemental
information for the Befesa Zinc Metal, LLC(Befesa) facility located in Mooresboro, Rutherford County, North
Carolina.This is a timely submittal of the permit application due on January 2, 2023 for renewal of the current
NPDES Individual Permit No. NC0089109, which expires on July 31, 2023.
Befesa has been engaged in discussions with representatives from TRC Environmental Corporation (TRC) as their
consultant. After completing a site with TRC and conducting a detailed review of the previous permit, Befesa
proposes and requests several changes to the permit, details of which are outlined in the attached supplemental
information narrative, namely a request for the removal of the Cadmium Compliance Schedule from the permit
with supporting documentation and data.
Please note that all application information should be considered Confidential Business Information. Information
contained in the application is based on recent effluent discharge monitoring information dated back to the
issuance of the previous permit in June 2020.
Please contact us if you have any questions or require additional information.
Sincerely,
Befesa Zinc Metal, LLC
Jan Nedbal
Environmental Manager
Attachments
cc: Dan Curry(TRC)
Scott Menniti (TRC)
Jan Nedbal (Befesa)
William White (Befesa)

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal, LLC OMB No.2040-0004
Form U.S.Environmental Protection Agency
\=/EPA Application for NPDES Permit to Discharge Wastewater
NPDES GENERAL INFORMATION
SECTION 1.ACTIVITIES REQUIRING AN NPDES PERMIT(40 CFR 122.21(f)and(f)(1))
1.1 Applicants Not Required to Submit Form 1
1.1.1 Is the facility a new or existing publicly owned 1 1 2 Is the facility a new or existing treatment works
treatment works? treating domestic sewage?
If yes,STOP. Do NOT complete ❑✓ No If yes, STOP.Do NOT t✓ No
Form 1.Complete Form 2A. complete Form 1.Complete
Form 2S.
1.2 Applicants Required to Submit Form 1
1.2.1 Is the facility a concentrated animal feeding 1.2.2 Is the facility an existing manufacturing,
operation or a concentrated aquatic animal commercial, mining,or silvicultural facility that is
a production facility? currently discharging process wastewater?
oElYes 4 Complete Form 1 ❑✓ No 0✓ Yes 4 Complete Form ❑ No
and Form 2B. 1 and Form 2C.
a 1.2.3 Is the facility a new manufacturing,commercial, 1.2.4 Is the facility a new or existing manufacturing,
cti
mining,or silvicultural facility that has not yet commercial,mining,or silvicultural facility that
commenced to discharge? discharges only nonprocess wastewater?
Yes 4 Complete Form 1 E✓ No EI Yes 4 Complete Form 0✓ No
and Form 2D. 1 and Form 2E.
N
= 1.2.5 Is the facility a new or existing facility whose
discharge is composed entirely of stormwater
associated with industrial activity or whose
discharge is composed of both stormwater and
non-stormwater?
❑ Yes 4 Complete Form 1 0✓ No
and Form 2F
unless exempted by
40 CFR
122.26(b)(14)(x)or
b 15 .
SECTION 2.NAME,MAILING ADDRESS,AND LOCATION(40 CFR 122.21(f)(2))
2.1 Facility Name
Befesa Zinc Metal,LLC
0 2.2 EPA Identification Number
co
J NCR000159038
2.3 Facility Contact
d Name(first and last) Title Phone number
Jan Nedbal Environmental Manager [phone]
Email address
[e-mail]
a
2.4 Facility Mailing Address
Street or P.O.box
484 Hicks Grove Road
City or town State ZIP code
Mooresboro North Carolina 28114
EPA Form 3510-1(revised 3-19) Page 1

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
g 2.5 Facility Location
▪ . Street,route number,or other specific identifier
Q U 484 Hicks Grove Road
• c County name County code(if known)
Rutherford County 161
3 City or town State ZIP code
co z Mooresboro North Carolina 28114
SECTION 3.SIC AND NAICS CODES(40 CFR 122.21(f)(3))
3.1 SIC Code(s) Description(optional)
3341 Secondary Nonferrous Metals
N
N
0
O
V
0
3.2 NAICS Code(s) Description(optional)
U
SECTION 4.OPERATOR INFORMATION(40 CFR 122.21(f)(4))
4.1 Name of Operator
Befesa Zinc Metal,LLC
0 4.2 Is the name you listed in Item 4.1 also the owner?
`o
✓❑ Yes ❑ No
4.3 Operator Status
2 ❑ Public—federal ❑ Public—state 0 Other public(specify)
❑✓ Private 0 Other(specify)
4.4 Phone Number of Operator
[phone]
4.5 Operator Address
Street or P.O. Box
E y 484 Hicks Grove Road
=
• .c City or town State ZIP code
o o Mooresboro North Carolina 28114
R
o Email address of operator
[phone]
SECTION 5.IND AN LAND(40 CFR 122.21(f)(5))
D 5.1 Is the facility located on Indian Land?
J ❑ Yes ❑✓ No
EPA Form 3510-1(revised 3-19) Page 2

•
EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 6.EXISTING ENVIRONMENTAL PERMITS(40 CFR 122.21(f)(6))
6.1 Existing Environmental Permits(check all that apply and print or type the corresponding permit number for each)
Ta
iv ❑ NPDES(discharges to surface ❑ RCRA(hazardous wastes) ❑ UIC(underground injection of
water) fluids)
o NCS000562
w a ❑✓ PSD(air emissions) ElNonattainment program(CAA) ❑ NESHAPs(CAA)
rn
10248R07
❑ Ocean dumping(MPRSA) ❑ Dredge or fill(CWA Section 404) ❑✓ Other(specify)
NCG500000(NC Cooling)
SECTION 7.MAP(40 CFR 122.21(f)(7))
7.1 Have you attached a topographic map containing all required information to this application?(See instructions for
specific requirements.)
❑✓ Yes ❑ No ❑ CAFO—Not Applicable(See requirements in Form 2B.)
SECTION 8.NATURE OF BUSINESS(40 CFR 122.21(f)(8))
8.1 Describe the nature of your business.
This facility processes Waelz Oxide(a.k.a.Crude Zinc Oxide)as its principal raw material to produce Special
High-Grade(SHG)zinc metal and other metals as it's principal product.The manufacturing process consists of an
integrated system of leaching,extraction,stripping,and electrowinning processes.Feed,including metal bearing
oxides(e.g.Walez Oxide)and other raw materials,are managed in solution throughout the process.Metal products
are removed as precipitates,concentrates,SHG zinc metal and CGG alloy.Metal-bearing Waelz Oxide feed is
00 delivered to the subject facility from local and international sources.The specific technologies and configuration of
the operation are confidential business information.
f6
z
SECTION 9.COOLING WATER INTAKE STRUCTURES(40 CFR 122.21(f)(9))
9.1 Does your facility use cooling water?
d ❑✓ Yes ❑ No 4 SKIP to Item 10.1.
9.2 Identify the source of cooling water.(Note that facilities that use a cooling water intake structure as described at
2 40 CFR 125,Subparts I and J may have additional application requirements at 40 CFR 122.21(r).Consult with your
o NPDES permitting authority to determine what specific information needs to be submitted and when.)
o w Forest City,NC Water Supply
U �
SECTION 10.VARIANCE REQUESTS(40 CFR 122.21(f)(10))
10.1 Do you intend to request or renew one or more of the variances authorized at 40 CFR 122.21(m)?(Check all that
apply.Consult with your NPDES permitting authority to determine what information needs to be submitted and
when.)
d ❑ Fundamentally different factors(CWA ❑ Water quality related effluent limitations(CWA Section
ce Section 301(n)) 302(b)(2))
❑ Non-conventional pollutants(CWA ❑ Thermal discharges(CWA Section 316(a))
Section 301(c)and(g))
❑✓ Not applicable
EPA Form 3510-1(revised 3-19) Page 3

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 11.CHECKLIST AND CERTIFICATION STATEMENT(40 CFR 122.22(a)and(d))
11.1 In Column 1 below,mark the sections of Form 1 that you have completed and are submitting with your application.
For each section,specify in Column 2 any attachments that you are enclosing to alert the permitting authority.Note
that not all applicants are required to provide attachments.
Column 1 Column 2
❑✓ Section 1:Activities Requiring an NPDES Permit ❑ w/attachments
❑✓ Section 2:Name, Mailing Address,and Location ❑ w/attachments
❑✓ Section 3: SIC Codes 0 w/attachments
❑✓ Section 4:Operator Information ❑ w/attachments
❑✓ Section 5: Indian Land ❑ w/attachments
❑✓ Section 6: Existing Environmental Permits ❑ w/attachments
❑✓ Section 7:Map ❑✓ matpopographic ❑ w/additional attachments
as o ❑✓ Section 8:Nature of Business ❑ w/attachments
❑✓ Section 9:Cooling Water Intake Structures ❑ w/attachments
c' ❑✓ Section 10:Variance Requests ❑ w/attachments
_y ❑✓ Section 11: Checklist and Certification Statement ❑ w/attachments
Y
11.2 Certification Statement
I certify under penalty of law that this document and all attachments were prepared under my direction or supervision
in accordance with a system designed to assure that qualified personnel properly gather and evaluate the
information submitted.Based on my inquiry of the person or persons who manage the system,or those persons
directly responsible for gathering the information,the information submitted is,to the best of my knowledge and
belief,true,accurate,and complete.I am aware that there are significant penalties for submitting false information,
including the possibility of fine and imprisonment for knowing violations.
Name(print or type first and last name) Official title
Jan Nedbal Environmental Manager
Signature Date signed
(2.14 '2r2Z
EPA Form 3510-1(revised 3-19) Page 4

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
Form U.S.Environmental Protection Agency
2C
3EPA Application for NPDES Permit to Discharge Wastewater
NPDES EXISTING MANUFACTURING,COMMERCIAL,MINING,AND SILVICULTURE OPERATIONS
SECTION 1.OUTFALL LOCATION(40 CFR 122.21(g)(1))
1.1 Provide information on each of the facility's outfalls in the table below.
g Numbelr Receiving Water Name Latitude Longitude
Co
U
J
001 Broad River 35° 12' 2.6" N 81° 51' 3.1" W
to
w ° n o
0
SECTION 2.LINE DRAWING(40 CFR 122.21(g)(2))
a, 2.1 Have you attached a line drawing to this application that shows the water flow through your facility with a water
a .3 balance?(See instructions for drawing requirements.See Exhibit 2C-1 at end of instructions for example.)
o ❑✓ Yes ❑ No
SECTION 3.AVERAGE FLOWS AND TREATMENT(40 CFR 122.21(g)(3))
3.1 For each outfall identified under Item 1.1,provide average flow and treatment information.Add additional sheets if
necessary.
**Outfall Number** 001
Operations Contributing to Flow
Operation Average Flow
Process Water(Average Daily Flow Jan.2021-April 2022) 0.875 mgd
mgd
mgd
mgd
0 Treatment Units
Description Final Disposal of Solid or
07
T. (include size,flow rate through each treatment unit, Code from Liquid Wastes Other Than
retention time,etc.) Table 2C•1 by Discharge
N/A.No wastewater treatment system N/A N/A
See Narrative for details
EPA Form 3510-2C(Revised 3-19) Page 1

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
3.1 **Outfall Number**
cont. Operations Contributing to Flow
Operation Average Flow
mgd
mgd
mgd
mgd
Treatment Units
Description Code from Final Disposal of Solid or
(include size,flow rate through each treatment unit, Table 2C-1 Liquid Wastes Other Than
retention time,etc.) by Discharge
"3
0
U
d
E
I-
**Outfall Number**
a
Operations Contributing to Flow
o Operation Average Flow
rn mgd
C)
mgd
mgd
mgd
Description Code from Final Disposal of Solid or
(include size,flow rate through each treatment unit, Table 2C-1 Liquid Wastes Other Than
retention time,etc.) by Discharge
3.2 Are you applying for an NPDES permit to operate a privately owned treatment works?
E ❑ Yes ❑✓ No 4 SKIP to Section 4.
N 3.3 Have you attached a list that identifies each user of the treatment works?
❑ Yes ❑ No
EPA Form 3510-2C(Revised 3-19) Page 2
L.. -

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 4.INTERMITTENT FLOWS(40 CFR 122.21(g)(4))
4.1 Except for storm runoff,leaks,or spills,are any discharges described in Sections 1 and 3 intermittent or seasonal?
❑✓ Yes ❑ No 4 SKIP to Section 5.
4.2 Provide information on intermittent or seasonal flows for each applicable outfall.Attach additional pages,if necessary.
Outfall Operation Frecuency Flow Rate
Number (list) Average Average Long-Term Maximum Duration
DaysiWeek Months/Year Average Daily
Process Water 7 days/week 12 months/year 0.873 mgd 0.949 mgd 1 days
001 days/week months/year mgd mgd days
days/week months/year mgd mgd days
days/week months/year mgd mgd days
days/week months/year mgd mgd days
days/week months/year mgd mgd days
days/week months/year mgd mgd days
days/week months/year mgd mgd days
days/week months/year mgd mgd days
SECTION 5.PRODUCTION(40 CFR 122.21(g)(5))
5.1 Do any effluent limitation guidelines(ELGs)promulgated by EPA under Section 304 of the CWA apply to your facility?
❑ Yes ❑✓ No 4 SKIP to Section 6.
y 5.2 Provide the following information on applicable ELGs.
(.D ELG Category ELG Subcategory Regulatory Citation
a)
5.3 Are any of the applicable ELGs expressed in terms of production(or other measure of operation)?
❑ Yes ❑ No 4 SKIP to Section 6.
5.4 Provide an actual measure of daily production expressed in terms and units of applicable ELGs.
Outfall Operation,Product,or Material Quantity per Day Unit of
-p Number Measure
f9
m
O
'D
•EPA Form 3510-2C(Revised 3-19) Page 3

•
EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 6.IMPROVEMENTS(40 CFR 122.21(g)(6))
6.1 Are you presently required by any federal,state,or local authority to meet an implementation schedule for constructing,
upgrading,or operating wastewater treatment equipment or practices or any other environmental programs that could
affect the discharges described in this application?
❑✓ Yes ❑ No 4 SKIP to Item 6.3.
6.2 Briefly identify each applicable project in the table below.
Affected Final Compliance Dates
Brief Identification and Description of Outfalls Source(s)of
o Project (list outfall Discharge Required Projected
number)
E
Cadmium Compliance Schedule 001 Process Water 12/01/2027 09/01/2022
N
G)
0.
Q
6.3 Have you attached sheets describing any additional water pollution control programs(or other environmental projects
that may affect your discharges)that you now have underway or planned?(optional item)
❑✓ Yes ❑ No ❑ Not applicable
SECTION 7.EFFLUENT AND INTAKE CHARACTERISTICS(40 CFR 122.21(g)(7))
See the instructions to determine the pollutants and parameters you are required to monitor and,in turn,the tables you must
complete. Not all applicants need to complete each table.
Table A.Conventional and Non-Conventional Pollutants
7.1 Are you requesting a waiver from your NPDES permitting authority for one or more of the Table A pollutants for any of
your outfalls?
❑✓ Yes ❑ No 4 SKIP to Item 7.3.
7.2 If yes,indicate the applicable outfalls below.Attach waiver request and other required information to the application.
Outfall Number ool Outfall Number Outfall Number
cn
7.3 Have you completed monitoring for all Table A pollutants at each of your outfalls for which a waiver has not been
requested and attached the results to this application package?
❑✓ Yes ❑ No;a waiver has been requested from my NPDES
permitting authority for all pollutants at all outfalls.
co
ES Table B.Toxic Metals,Cyanide,Total Phenols,and Organic Toxic Pollutants
. 7.4 Do any of the facility's processes that contribute wastewater fall into one or more of the primary industry categories
listed in Exhibit 2C-3?(See end of instructions for exhibit.)
❑✓ Yes ❑ No 4 SKIP to Item 7.8.
7.5 Have you checked"Testing Required"for all toxic metals,cyanide,and total phenols in Section 1 of Table B?
❑✓ Yes ❑ No
7.6 List the applicable primary industry categories and check the boxes indicating the required GC/MS fraction(s)identified
in Exhibit 2C-3.
Primary Industry Category Required GCIMS Fraction(s)
(Check applicable boxes.)
Nonferrous Metals Manufacturing 0 Volatile 0 Acid 0 Base/Neutral 0 Pesticide
❑Volatile 0 Acid 0 Base/Neutral 0 Pesticide
❑Volatile 0 Acid 0 Base/Neutral 0 Pesticide
EPA Form 3510-2C(Revised 3-19) Page 4

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
7.7 Have you checked"Testing Required"for all required pollutants in Sections 2 through 5 of Table B for each of the
GC/MS fractions checked in Item 7.6?
❑✓ Yes ❑ No
7.8 Have you checked"Believed Present"or"Believed Absent"for all pollutants listed in Sections 1 through 5 of Table B
where testing is not required?
❑✓ Yes 0 No
7.9 Have you provided(1)quantitative data for those Section 1,Table B,pollutants for which you have indicated testing is
required or(2)quantitative data or other required information for those Section 1,Table B,pollutants that you have
indicated are"Believed Present"in your discharge?
✓❑ Yes ❑ No
7.10 Does the applicant qualify for a small business exemption under the criteria specified in the instructions?
❑ Yes 4 Note that you qualify at the top of Table B, ❑✓ No
-o then SKIP to Item 7.12.
w= 7.11 Have you provided(1)quantitative data for those Sections 2 through 5,Table B,pollutants for which you have
o determined testing is required or(2)quantitative data or an explanation for those Sections 2 through 5,Table B,
pollutants you have indicated are"Believed Present"in your discharge?
❑✓ Yes 0 No
w; Table C.Certain Conventional and Non-Conventional Pollutants
m 7.12 Have you indicated whether pollutants are"Believed Present"or"Believed Absent"for all pollutants listed on Table C
s for all outfalls?
U
❑✓ Yes ❑ No
c 7.13 Have you completed Table C by providing(1)quantitative data for those pollutants that are limited either directly or
indirectly in an ELG and/or(2)quantitative data or an explanation for those pollutants for which you have indicated
"Believed Present"?
a) ❑✓ Yes ❑ No
Table D.Certain Hazardous Substances and Asbestos
7.14 Have you indicated whether pollutants are"Believed Present"or"Believed Absent"for all pollutants listed in Table D for
all outfalls?
❑✓ Yes ❑ No
7.15 Have you completed Table D by(1)describing the reasons the applicable pollutants are expected to be discharged
and(2)by providing quantitative data,if available?
❑✓ Yes 0 No
Table E.2,3,7,8-Tetrachlorodibenzo-p-Dioxin(2,3,7,8-TCDD)
7.16 Does the facility use or manufacture one or more of the 2,3,7,8-TCDD congeners listed in the instructions,or do you
know or have reason to believe that TCDD is or may be present in the effluent?
O Yes-4 Complete Table E. ❑✓ No 4 SKIP to Section 8.
7.17 Have you completed Table E by reporting qualitative data for TCDD?
O Yes ❑ No
SECTION 8.USED OR MANUFACTURED TOXICS(40 CFR 122.21(g)(9))
8.1 Is any pollutant listed in Table B a substance or a component of a substance used or manufactured at your facility as
an intermediate or final product or byproduct?
y ❑✓ Yes ❑ No 4 SKIP to Section 9.
0 8.2 List the pollutants below.
0 1. Cadmium 4. 7.
`o
2. Lead 5. 8.
3, Zinc 6. 9.
EPA Form 3510-2C(Revised 3-19) Page 5

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 9.BIOLOGICAL TOXICITY TESTS(40 CFR 122.21(g)(11))
9.1 Do you have any knowledge or reason to believe that any biological test for acute or chronic toxicity has been made
within the last three years on(1)any of your discharges or(2)on a receiving water in relation to your discharge?
❑✓ Yes ❑ No 4 SKIP to Section 10.
ET 9.2 Identify the tests and their.urposes below.
Test(s) Purpose of Test(s) Submitted to NPDES� Date Submitted
Permitting Authority.
Fish Tissue Sampling To Biological,Under NPDES ✓❑ Yes ElNo 12/14/2022
Permit
0
❑ Yes ❑ No
❑ Yes ❑ No
SECTION 10.CONTRACT ANALYSES(40 CFR 122.21(g)(12))
10.1 Were any of the analyses reported in Section 7 performed by a contract laboratory or consulting firm?
❑✓ Yes ❑ No 4 SKIP to Section 11.
10.2 Provide information for each contract laboratory or consulting firm below.
Laboratory Number 1 Laboratory Number 2 Laboratory Number 3
Name of laboratory/firm Pace Analytical Services,LLC ETT Environmental,Inc.
LaboratoryaddressKincey
9800 Ave. Suite 100 4 Craftsman Court
Huntersville,NC 28078 Greer,SC 29650
c
V
0 Phone number
[phone] [phone]
Pollutant(s)analyzed Priority Pollutants DO,Hardness,Phosphorus,
Ammonia-N,TKN
SECTION 11.ADDITIONAL INFORMATION(40 CFR 122.21(g)(13))
11.1 Has the NPDES permitting authority requested additional information?
❑ Yes ❑✓ No 4 SKIP to Section 12.
0
11.2 List the information requested and attach it to this application.
1. 4,
0
47. 2, 5.
3. 6.
EPA Form 3510-2C(Revised 3-19) Page 6

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 12.CHECKLIST AND CERTIFICATION STATEMENT(40 CFR 122.22(a)and(d))
12.1 In Column 1 below,mark the sections of Form 2C that you have completed and are submitting with your application.
For each section,specify in Column 2 any attachments that you are enclosing to alert the permitting authority.Note
that not all applicants are required to complete all sections or provide attachments.
Column 1 Column 2
✓❑ Section 1:Outfall Location ❑ w/attachments
❑✓ Section 2:Line Drawing ✓❑ w/line drawing ❑ w/additional attachments
Section 3:Average Flows and w/list of each user of
❑✓ Treatment ❑ w/attachments ❑ privately owned treatment
works
❑✓ Section 4:Intermittent Flows ❑ w/attachments
❑✓ Section 5:Production ❑ w/attachments
w/optional additional
2Section 6:Improvements 0 w/attachments ❑ sheets describing any
additional pollution control
plans
❑ w/request for a waiver and ❑ w/explanation for identical
supporting information outfalls
d ❑ w/small business exemption ❑ w/other attachments
request
❑ Section 7:Effluent and Intake ❑ w/Table A ✓❑ w/Table B
Characteristics
0
✓❑ w/Table C ❑✓ w/Table D
❑✓ wl Table E 0w/analytical results as an
0 attachment
✓❑ Section 8:Used or Manufactured Li w/attachments
Toxics
•
32 ❑ Section 9:Biological Toxicity ❑✓ w/attachments
Tests
U
❑✓ Section 10:Contract Analyses ❑ wl attachments
✓❑ Section 11:Additional Information ❑ w/attachments
❑✓ Section 12:Checklist and ❑ w/attachments
Certification Statement
12.2 Certification Statement
1 certify under penalty of law that this document and all attachments were prepared under my direction or supervision in
accordance with a system designed to assure that qualified personnel properly gather and evaluate the information
submitted. Based on my inquiry of the person or persons who manage the system,or those persons directly
responsible for gathering the information, the information submitted is,to the best of my knowledge and belief, true,
accurate,and complete.I am aware that there are significant penalties for submitting false information,including the
possibility of fine and imprisonment for knowing violations.
Name(print or type first and last name) Official title
Jan Nedbal Environmental Manager
Signature Date signed
�2• tl.� •202Z
EPA Form 3510-2C(Revised 3-19) Page 7

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE A.CONVENTIONAL AND NON CONVENTIONAL POLLUTANTS(40 CFR 122.21(g)(7)(iii))1
Effluent Intake
(Optional)
Waiver Units Maximum Maximum Long-Term
Pollutant Requested (specify) Daily Monthly Average Daily Number of Long-Term Number of
(if applicable) Discharge Discharge Discharge Analyses Average Value Analyses
(required) (if available) (if available)
0 Check here if you have applied to your NPDES permitting authority for a waiver for all of the pollutants listed on this table for the noted outfall.
-
1 - - -
Biochemical oxygen demand
ElConcentration
(BOD5) Mass - - -
- -
2 -
Chemical oxygen demand ElConcentration
(COD) Mass - - - - - -
Concentration - - - - - - -
3. Total organic carbon(TOC) 0
Mass - - - - - - -
Concentration mg/L 56.7 56.7 20.4 54 - -
4. Total suspended solids(TSS) ❑
Mass lbs 473.1 449.1 149.2 54 - -
Concentration mg/L 0.81 0.81 0.29 9 - -
5. Ammonia(as N) 0
Mass lbs 8.01 6.08 2.13 9 - -
6. Flow ❑ Rate MGD 1.393 0.957 0.875 803/27/27 - -
Temperature(winter) 0 °C °C - - - - - -
7.
Temperature(summer) 0 °C °C - - - - - -
pH(minimum) ❑ Standard units S.U. 6.44 6.44 7.80 27 - -
8.
pH(maximum) 0 Standard units S.U. 8.34 8.34 7.80 27 - -
1 Sampling shall be conducted according to sufficiently sensitive test procedures(i.e.,methods)approved under 40 CFR 136 for the analysis of pollutants or pollutant parameters or
required under 40 CFR chapter I,subchapter N or 0.See instructions and 40 CFR 122.21(e)(3).
EPA Form 3510-2C(Revised 3-19) Page 9

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004 -
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) (if available) Value
0 Check here if you qualify as a small business per the instructions to Form 2C and,therefore,do not need to submit quantitative data for any of the organic toxic pollutants in Sections
2 through 5 of this table.Note,however,that you must still indicate in the appropriate column of this table if you believe any of the pollutants listed are present in your discharge.
Section 1.Toxic Metals,Cyanide,and Total Phenols
1.1 Antimony,total Concentration mg/L 0.149 0.149 0.039 9 - -
(7440-36-0) Mass lbs 1.053 1.120 0.284 9 - -
1.2 Arsenic,total Concentration mg/L 0.013 0.013 <0.01 9 - -
(7440-38-2) Mass lbs 0.091 0.087 <0.073 9 - -
1.3 Beryllium,total Concentration pg/L <1.0 <1.0 - 1 -El El ID
-
(7440-41-7). Mass lbs <0.009 <0.009 - 1 - -
1.4 Cadmium,total Concentration mg/L 0.130 0.130 0.038 54 - -
El El 1:1
(7440-43-9) Mass lbs 0.629 0.890 0.277 54 - -
1.5 Chromium,total Concentration mg/L <0.025 <0.025 <0.01 9ID CI
- -
(7440-47-3) ✓ Mass lbs <0.29 <0.20 <0.07 9 - -
1.6 Copper,total Concentration mg/L 0.048 0.048 0.015 9 - -
l El
(7440-50-8) ✓ ✓ Mass lbs 0.261 0.264 0.112 9 - -
1.7 Lead,total Concentration mg/L 0.39 0.39 0.017 54 - -
El El El
(7439-92-1) Mass lbs 0.329 0.292 0.125 54 - -
1.8 Mercury,total Concentration pg/L <1.0 <1.0 - 1 - -
El El El
(7439-97-6) Mass lbs <0.009 <0.009 - 1 - -
1.9 Nickel,total Concentration mg/L 0.063 0.063 0.019 27 - -
(7440-02-0) Mass lbs .544 0.493 0.141 27 - -
Selenium,total Concentration pg/L 1,040 1,040 967 2 - -
1.10 El El El
(7782-49-2) Mass lbs 8.98 8.98 8.30 2 - -
1.11 Silver,total Concentration pg/L 41.5 41.5 26.6 2 - -
(7440-22-4) Mass lbs 0.353 0.353 0.227 2 - -
EPA Form 3510-2C(Revised 3-19) Page 11

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004 -
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long-Term Number
Present Absent Daily Monthly Daily of of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available)
1.12 Thallium,total ❑ Concentration pg/L 56.5 56.5 42.6 2 - -
0
(7440-28-0) Mass lbs 0.488 0.488 0.366 2 - -
1.13 Zinc,total ❑ ❑ Concentration ma 0.630 0.630 0.145 54 -0 -
(7440-66-6) Mass lbs 3.047 4.311 1.06 54 - -
1.14 Cyanide,total Concentration mg/L 0.038 0.038 - 1 - -
(57-12-5) Mass lbs 0.323 0.323 - 1 - -
Concentration mg/L <2.0 <2.0 - 1 - -
1.15 Phenols,total ❑✓ ❑ ❑✓
Mass lbs <0.17 <0.17 - 1 - -
Section 2.Organic Toxic Pollutants(GCIMS Fraction-Volatile Compounds)
2.1 Acrolein ❑ Concentration µg/L <5.0 <5..0 - 1 - -
(107-02-8) ✓ Mass lbs <0.043 <0.043 - 1 - -
2.2 Acrylonitrile ❑ Concentration µg/L <5.0 <5.0 - 1 - -
(107-13-1) Mass lbs <0.043 <0.043 - 1 - -
2.3 Benzene ElConcentration µg/L <1.0 <1.0 - 1 - -
0(71-43-2) Mass lbs <0.009 <0.009 - 1 - -
2.4 Bromoform Concentration pg/L 85.3 85.3 54.8 2 - -
0
(75-25-2) l El ✓ Mass lbs 0.737 0.737 0.472 2 - -
2.5 Carbon tetrachloride ❑ Concentration µg/L <2.0 <2.0 - 1 - -
El
(56-23-5) Mass lbs <0.017 <0.017 - 1 - -
2.6 Chlorobenzene ElConcentration µg/L <2.0 <2.0 - 1 - -
El
(108-90-7) Mass lbs <0.017 <0.017 - 1 - -
2.7 Chlorodibromomethane ❑ ❑ Concentration µg/L <2.0 <2.0 - 1 - -
El
(124-48-1) Mass lbs <0.017 <0.017 - 1 - -
2.8 Chloroethane Concentration µg/L <2.0 <2.0 - 1 0 El El
- -
(75-00-3) Mass lbs <0.017 <0.017 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 12

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant]Parameter Testing Units Long-Term Long-
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available)
2.9 2-chloroethylvinyl ether El 0
❑ Concentration µg/L <5.0 <5.0 - 1 - -
(110-75-8) Mass lbs <0.043 <0.043 - 1 - -
Concentration u9/L 2.3 2.3 <3.2 2 - -
2.10 Chloroform(67-66-3) ❑✓ ❑✓ 0
Mass ibs 0.020 0.020 <0.027 2
2.11 Dichlorobromomethane ❑ 0
❑ Concentration µg/L <2.0 <2.0 - 1 - 1
(75-27-4) Mass lbs <0.017 <0.017 - 1 - -
212 1,1-dichloroethane Concentration µg/L <2.0 <2.0 - 1 - 1
(75-34-3) ,l D ✓ Mass Ibs <0.017 <0.017 - 1 - -
2.13 1,2-dichloroethane El Concentration µg/L <2.0 <2.0 - 1 - 1
0(107-06-2) ✓ Mass lbs <0.017 <0.017 - 1 - -
2.14 1,1-dichloroethylene ❑ ❑ Concentration µg/L <2.0 <2.0 - 1 - 1
(75-35-4) Mass Ibs <0.017 <0.017 - 1 - -
2.15 12-dichloropropane El El
µg/L <2.0 <2.0 - 1 - 1
0(78-87-5) Mass lbs <0.017 <0.017 - 1 - -
2.16 13-dichloropropylene El El El Concentration - - - - - -
(542-75-6) Mass - - - - - - -
2.17 Ethylbenzene El 0
0
Concentration µg/L <1.0 <1.0 - 1 - 1
(100-41-4) Mass lbs <0.009 <0.009 - 1 - -
2.18 Methyl bromide Concentration µg/L <2.0 <2.0 - 1 - 1
(74-83-9) Mass lbs <0.017 <0.017 - 1 - -
2.19 Methyl chloride 0
Concentration µg/L <2.0 <2.0 - 1 - 1
(74-87-3) Mass Ibs <0.017 <0.017 - 1 - -
Methylene chloride Concentration µg/L <2.0 <2.0 - 1 - 1
2.20 El(75-09-2) 0 El lbs <0.017 <0.017 - 1 - -
221 1,1,2,2-tetrachloroethane El ® Concentration µg/L <2.0 <2.0 - 1 - 1
(79-34-5) Mass lbs <0.017 <0.017 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 13

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004 .
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
PollutantIParameter Testing Units Long-Term Long-
(
and CAS Number,if available) Re uired Believed Believed (specify) Maximum Maximum Average Number Number
( q Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) (if available) Value
2.22 Tetrachloroethylene Concentration µg/L <2.0 <2.0 - 1 - -
(127-18-4) Mass Ibs <0.017 <0.017 - 1 - -
2.23 Toluene Concentration µg/L <1.0 <1.0 1- - -
(108-88-3) Mass lbs <0.009 <0.009 - 1 - -
2.24 1,2-trans-dichloroethylene Concentration µg/L <2.0 <2.0 - 1 - -
CI 0 CI
(156-60-5) Mass lbs <0.017 <0.017 - 1 - -
2.25 1,1,1-trichloroethane Concentration µg/L <2.0 <2.0 - 1 -CI CI I
-
(71-55-6) ✓ Mass lbs <0.017 <0.017 - 1 - -
2.26 1,1,2-trichloroethane Concentration µg/L <2.0 <2.0 - 1 -CI CI CI
-
(79-00-5) Mass lbs <0.017 <0.017 - 1 - -
2.27 Trichloroethylene Concentration µg/L <2.0 <2.0 - 1 -CI 1=1
-
(79-01-6) ✓ Mass lbs <0.017 <0.017 - 1 - -
2.28 Vinyl chloride Concentration µg/L <2.0 <2.0 - 1 - -
CI CI
(75-01-4) ✓ Mass lbs <0.017 <0.017 - 1 - -
Section 3.Organic Toxic Pollutants(GCIMS Fraction-Acid Compounds)
3.1 2-chlorophenol Concentration µg/L <20.8 <20.8 - 1CI 0 CI
- -
(95-57-8) Mass lbs <0.177 <0.177 - 1 - -
3.2 2,4-dichlorophenol Concentration [TA <20.8 <20.8 - 1 - -
CI CI(120-83-2) ✓ Mass lbs <0.177 <0.177 - 1 - -
2,4-dimethylphenol Concentration µg/L <41.7 <41.7 - 1 - -
3.3 0 CI ID
(105-67-9) Mass Ibs <0.355 <0.355 - 1 - -
3.4 4,6-dinitro-o-cresol Concentration µ 1
g/L <41.7 <41.7 - - -
CI CI
(534-52-1) ✓ Mass lbs <0.355 <0.355 - 1 - -
2 4-dinitrophenol Concentration - - - - - - -
3.5 0 CI(51 28 5) ® Mass - - - - - - -
EPA Form 3510-2C(Revised 3-19) Page 14

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004 •
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term Long-
(and
CAS Number,if available) Re uired Believed Believed (specify) Maximum Maximum Average Number Number
q Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available)
3.6 2-nitrophenol Concentration pg/L <20.8 <20.8 - 1 - -
0 El El
(88-75-5) Mass lbs <0.177 <0.177 - 1 - -
3.7 4-nitrophenol Concentration lag/L <41.7 <41.7 - 1 - -
(100-02-7) Mass lbs <0.355 <0.355 - 1 - -
3.8 p-chloro-m-cresol El 0 Concentration tag/L <20.8 <20.8 - 1 - -
(59-50-7) Mass lbs <0.177 <0.177 - 1 - -
3.9 Pentachlorophenol Concentration pg/L <41.7 <41.7 - 1 - -
El 0 El
(87-86-5) Mass lbs <0.355 <0.355 - 1 - -
Phenol Concentration pg/L <20.8 <20.8 - 1 - -
3.10 (108-95-2) Mass lbs <0.177 <0.177 - 1 - -
3.11 2,4,6-trichlorophenol Concentration tag/L <41.7 <41.7 - 1 - -
(88-05-2) Mass lbs <0.355 <0.355 - 1 - -
Section 4.Organic Toxic Pollutants(GC/MS Fraction-Base/Neutral Compounds)
4.1 Acenaphthene ❑ Concentration Ng/L <20.8 <20.8 - 1 - -
El 0
(83-32-9) Mass lbs <0.177 <0.177 - 1 - -
Acenaphthylene Concentration pg/L <20.8 <20.8 - 1 - -
4.2 CI CI 0
(208-96-8) Mass Ibs <0.177 <0.177 - 1 - -
4,3 Anthracene Concentration Ng/L <20.8 <20.8 - 1 - -
0 Ell ID
(120-12-7) Mass lbs <0.177 <0.177 - 1 - -
4.4 Benzidine Concentration pg/L <208 <208 - 1 - -
(92-87-5) Mass lbs <1.77 <1.77 - 1 - -
Benzo(a)anthracene Ei Concentration pg/L <20.8 <20.8 - 1 - -
4.5 El 0
(56-55-3) Mass lbs <0.177 <0.177 - 1 - -
Benzo(a)pyrene Concentration pg/L <20.8 <20.8 - 1 - -
4.6 El 0 El
(50-32-8) Mass lbs <0.177 <0.177 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 15

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v)p
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term Lon -
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number g Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available) _
4.7 3,4-benzofluoranthene Concentration µg/L <20.8 <20.8 - 1 - -
El 0
(205-99-2) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.8 Benzo(ghi)perylene Concentration µg/L <20.8 <20.8 - 1 - -
(191-24-2) Mass lbs <0.177 <0.177 - 1 - -
4.9 Benzo(k)fluoranthene 0 Concentration µg/L <20.8 <20.8 - 1 - -
(207-08-9) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.10 Bis(2-chloroethoxy)methane � Concentration µg/L <41.7 <41.7 - 1 - -
(111-91-1) Mass lbs <0.355 <0.355 - 1 - -
4.11 Bis(2-chloroethyl)ether 0 Concentration µg/L <20.8 <20.8 - 1 - -
(111-44-4) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.12 Bis(2-chloroisopropyl)ether Concentration µg/L <20.8 <20.8 - 1 -El El -
(102-80-1) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.13 Bis(2-ethylhexyl)phthalate Concentration µg/L <20.8 <20.8 - 1 - -
El 0 El
(117-81-7) Mass Ibs <0.177 <0.177 - 1 - -
4-bromophenyl phenyl ether Concentration µg/L <20.8 <20.8 - 1 - -
4.14 (101-55-3) Mass lbs <0.177 <0.177 - 1 - -
4.15 Butyl benzyl phthalate Concentration µg/L <20.8 <20.8 - 1 - -
(85-68-7) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.16 2-chloronaphthalene 0 0 � Concentration µg/L <20.8 <20.8 - 1 - -
(91-58-7) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.17 4-chlorophenyl phenyl ether Concentration µg/L <20.8 <20.8 - 1 -El 0
-
(7005-72-3) 0 Mass Ibs <0.177 <0.177 - 1 - -
Chrysene Concentration µg/L <20.8 <20.8 - 1 - -
4.18 0 0 0 -
(218-01-9) Mass lbs <0.177 <0.177 - 1 - -
Dibenzo(a,h)anthracene Concentration µg/L <20.8 <20.8 - 1 - -
4.19 (53-70-3) Mass lbs <0.177 <0.177 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 16

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004 .
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Daily Monthly Term
Present Absent Daily of of
Discharge Discharged) available) Discharge Analyses Average
Analyses
(if available)
4.20 1,2-dichlorobenzene Concentration µg/L <20.8 <20.8 - 1 - -
(95-50-1) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.21 1,3-dichlorobenzene Concentration µg/L <20.8 <20.8 - 1 - -
0
(541-73-1) ✓ 0 Mass Ibs <0.177 <0.177 - 1 - -
4.22 1,4-dichlorobenzene Concentration µg/L <20.8 <20.8 - 1 - -
(106-46-7) Mass Ibs <0.177 <0.177 - 1 - -
3,3-dichlorobenzidine Concentration µg/L <41.7 <41.7 - 1 - -
4.23 El 0 El
(91-94-1) Mass Ibs <0.355 <0.355 - 1 - -
4.24 Diethyl phthalate 0✓ Concentration µg/L <20.8 <20.8 - 1 - -
(84-66-2) Mass Ibs <0.177 <0.177 - 1 - -
4.25 Dimethyl phthalate Concentration µg/L <20.8 <20.8 - 1 - -
El El 0
(131-11-3) Mass Ibs <0.177 <0.177 - 1 - -
4.26 Di-n-butyl phthalate 0Concentration µg/L <20.8 <20.8 - 1 - -
El 0
(84-74-2) Mass Ibs <0.177 <0.177 - 1 - -
4.27 2,4-dinitrotoluene Concentration µg/L <20.8 <20.8 - 1 - -
El 0 El
(121-14-2) Mass Ibs <0.177 <0.177 - 1 - -
4.28 2 6-dinitrotoluene Concentration µg/L <20.8 <20.8 - 1 - -
0 0 0
(606-20-2) Mass Ibs <0.177 <0.177 - 1 - -
4.29 Di-n-octyl phthalate 0 0 Concentration µg/L <20.8 <20.8 - 1 - -
(117-84-0) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.30 1,2-Diphenylhydrazine Concentration µg/L <20.8 <20.8 - 1 - -
(as azobenzene)(122-66-7) Mass Ibs <0.177 <0.177 - 1 - -
4.31 Fluoranthene Concentration µg/L <20.8 <20.8 - 1 -0 0
-
(206-44-0) 0
Mass Ibs <0.177 <0.177 - 1 - -
Fluorene Concentration µg/L <20.8 <20.8 - 1 - -
4.32 El El 0
(86 73 7) Mass Ibs <0.177 <0.177 1 - -
EPA Form 3510-2C(Revised 3-19) Page 17

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term Long-
(and
CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Number
q Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) (if available) Value
4.33 Hexachlorobenzene Concentration µg/L <20.8 <20.8 - 1 - -
(118-74-1) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.34 Hexachlorobutadiene Concentration µg/L <20.8 <20.8 - 1 - -
(87-68-3) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.35 Hexachlorocyclopentadiene Concentration µg/L <41.7 <41.7 - 1 - -
0 El
(77-47-4) ✓ Mass lbs <0.355 <0.355 - 1 - -
4.36 Hexachloroethane Concentration µg/L <20.8 <20.8 - 1 - -
(67-72-1) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.37 Indeno(1,2,3-cd)pyrene Concentration µg/L <20.8 <20.8 - 1 - -
(193-39-5) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.38 Isophorone Concentration µg/L <41.7 <41.7 - 1 -El El
-
(78-59-1) ✓ Mass lbs <0.355 <0.355 - 1 - -
4.39 Naphthalene Concentration µg/L <20.8 <20.8 - 1 - -
(91-20-3) ✓ Mass Ibs <0.177 <0.177 - 1 - -
4.40 Nitrobenzene Concentration µg/L <20.8 <20.8 - 1 - -
(98-95-3) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.41 N-nitrosodimethylamine Concentration µg/L <20.8 <20.8 - 1 - -
(62-75-9) ✓ Mass Ibs <0.177 <0.177 - 1 - -
4.42 N-nitrosodi-n-propylamine Concentration µg/L <20.8 <20.8 - 1 - -
El 0 El
(621-64-7) Mass lbs <0.177 <0.177 - 1 - -
4.43 N-nitrosodiphenylamine Concentration µg/L <41.7 <41.7 - 1 - -
(86-30-6) ✓ Mass lbs <0.355 <0.355 - 1 - -
Phenanthrene Concentration µg/L <20.8 <20.8 - 1 - -
4.44 (85-01-8) Mass Ibs <0.177 <0.177 - 1 - -
Pyrene Concentration µg/L <20.8 <20.8 - 1 - -
4.45 (129-00-0) Mass Ibs <0.177 <0.177 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 18

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Daily Monthly Term
Present Absent Daily of of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available)
4.46 1,2,4-trichlorobenzene Concentration µg/L <20.8 <20.8 - 1 - 1
(120-82-1) Mass lbs <0.177 <0.177 - 1 - -
Section 5.Organic Toxic Pollutants(GC/MS Fraction—Pesticides)
51 Aldrin Concentration SEE NARRATIVE - - - - -
(309-00-2) Mass - - - - - - -
a-BHC Concentration - - - - - - -
5.2 (319-84-6) Mass - - - - - - -
R_BHC Concentration - - - - - - -
5.3 (319-85-7) Mass - - - - - - -
y-BHC Concentration - - - - - - -
5.4 0 0 0
(58-89-9) Mass - - - - - - -
6-BHC Concentration - - - - - - -
5.5 (319-86-8) Mass - - - - - - -
5.6 Chlordane Concentration - - - - - - -
El 0 El
(57-74-9) Mass - - - - - - -
4 4'-DDT Concentration - - - - - - -
5.7 0 0 0
(50-29-3) Mass - - - - - - -
4,4'-DDE Concentration - - - - - - -
5.8 (72-55-9) Mass - - . - - - - -
5.9 4,4'-DDD Concentration - - - - - - -
(72-54-8) Mass - - - - - - -
5.10 Dieldrin Concentration - - - - - - -
(60-57-1) Mass - - - - - - -
a-endosulfan Concentration - - - - - - -
5.11 (115-29-7) 0 0 0 Mass - - - - - - -
EPA Form 3510-2C(Revised 3-19) Page 19

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term Lon -
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long-
(and
Daily Monthly Term
Present Absent Daily of of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available)
(i-endosulfan ✓ Concentration - - - - - - -
5.12 El 0(115-29-7) Mass - - - - - - -
5.13 Endosulfan sulfate 0 Concentration - -
(1031-07-8) ✓ Mass - - - - - - -
Endrin Concentration - - - - - - -
5.14 (72-20-8) Mass - - - - - - -
5.15 Endrin aldehyde ElConcentration - - - - - - -
(7421-93-4) Mass - - - - - - -
5.16 Heptachlor Concentration - - - - - - -
El 0 El
(76-44-8) Mass - - - - - - -
Heptachlor epoxide Concentration - - - - - - -
5.17 (1024-57-3) 0 El El - - - - - - -
PCB-1242 Concentration - - - - - - -
5.18 (53469-21-9) El El ✓ Mass - - - - - - -
PCB-1254 Concentration - - - - - - -
5.19 (11097-69-1) El El �✓ Mass - - - - - - -
PCB-1221 Concentration - - - - - - -
5.20 (11104-28-2) ID El El Mass - - - - - - -
PCB-1232 Concentration - - - - - - -
5.21 (11141-16-5) El CI ❑ Mass - - - - - - -
PCB-1248 ✓ Concentration - - - - - - -
5.22 (12672-29-6) 0 Mass - - - - - - -
PCB-1260 Concentration - - - - - - -
5.23 (11096-82-5) El 0 ❑ Mass - - - - - - -
PCB-1016 ✓ Concentration - - - - - - -
5.24 (12674-11-2) Mass - - - - - - -
EPA Form 3510-2C(Revised 3-19) Page 20

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Daily of Term of
D(eqh erdge) Df availabe) Discharge Analyses AverageValue Analyses
r (if available)
Toxaphene Concentration - - - - - - -
5.25 (8001-35-2) ❑ 0 ✓❑ - - - - - - -
Mass
1 Sampling shall be conducted according to sufficiently sensitive test procedures(i.e.,methods)approved under 40 CFR 136 for the analysis of pollutants or pollutant parameters or
required under 40 CFR chapter I,subchapter N or 0.See instructions and 40 CFR 122.21(e)(3).
EPA Form 3510-2C(Revised 3-19) Page 21

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004 -
TABLE C.CERTAIN CONVENTIONAL AND NON CONVENTIONAL POLLUTANTS(40 CFR 122.21(g)(7)(vi))1
Presence or Absence Intake
(check one) Effluent (Optional)
Units Maximum Long-Term
PollutantLong-Term
Believed Believed (specify) Maximum Daily Monthly Average Daily Number of Number of
Present Absent Discharge Discharge Discharge Analyses Average Analyses
(required) Value
(if available) (if available)
❑
Check here if you believe all pollutants on Table C to be present in your discharge from the noted outfall.You need not complete the"Presence or Absence"column of Table C for
each pollutant.
❑
Check here if you believe all pollutants on Table C to be absent in your discharge from the noted outfall.You need not complete the"Presence or Absence"column of Table C for
each pollutant.
1. Bromide 0 ❑ Concentration - - - - - - -
(24959-67-9) Mass - - - - - - -
Chlorine,total Concentration ug/L <10 <10 - 1 - -
2' El Elresidual Mass lb 0.086 0.086 - 1 - -
Concentration - - - - - - -
3. Color 0 ❑✓
Mass - - - - - - -
Concentration - - - - - - -
4. Fecal coliform 0 ❑✓ Mass
5 Fluoride ❑ Concentration mg/L 9.2 9.2 <0.1 9 - -
(16984-48-8) ✓ Mass lbs 65.04 69.18 <0.73 9 - -
Concentration mg/L 0.61 0.61 - 1 - -
6 Nitrate-nitrite ❑✓ ❑
Mass lbs 5.19 5.19 - 1 -
Nitrogen,total Concentration mg/L 1.5 1.5 - 1 - -
7. organic(as N) 0El Mass lbs 12.89 12.89 - 1 - -
Concentration mg/L <4.9 <4.9 - 1 - -
8. Oil and grease 0 ✓❑
Mass lbs <41.7 <41.7 - 1 - -
Phosphorus(as Concentration mg/L 19 19 6.6 3 - -
9' P),total(7723-14-0) El lbs 164 164 46.8 3 - -
10. Sulfate(as SO4) 0 ❑ Concentration g/L 12.5 12.5 5.3 740 - -
(14808-79-8) Mass lbs 72,733 72,733 37,265 740 - -
Concentration - N/A See Narrative - - - -
11. Sulfide(as S) ❑✓ 0
Mass - - - - - - -
EPA Form 3510-2C(Revised 3-19) Page 23

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
TABLE C.CERTAIN CONVENTIONAL AND NON CONVENTIONAL POLLUTANTS(40 CFR 122.21(g)(7)(vi))l
Presence or Absence
(check one) Effluent Intake
(Optional)
Pollutant Units Maximum Long-Term Lon Term
Believed Believed (specify) Maximum Daily Monthly Average Daily Number of g- Number of
Present Absent Discharge Average
Discharge Discharge Analyses Analyses
(required) Value
(if available) (if available)
12. Sulfite(as S03) ❑ ❑✓ Concentration - - - - - - -
(14265-45-3) Mass - - - - - - -
Concentration - N/A See Narrative - - - -
13. Surfactants ❑✓ 0 Mass
14. Aluminum,total ❑ ❑ Concentration mg/L 0.276 0.276 0.118 9 - -
(7429-90-5) Mass lbs 2.075 2.075 0.859 9 - -
15. Barium,total ❑ ❑ Concentration - - - - - - -
(7440-39-3) Mass - - - - - - -
16. Boron,total ❑ ❑ Concentration - - - - - - -
(7440-2-8) Mass - - - - - - -
Cobalt,total Concentration mg/L <0.04 <0.04 <0.005 1 - -
17. ❑(7440-48-) Mass lbs <0.46 <0.32 <0.04 1 - -
18 Iron,total ❑✓ ❑ Concentration mg/L 0.154 0.154 0.017 9 - -
(7439-89-0) Mass lbs 1.322 1.197 0.125 9 - -
19 Magnesium,total ❑ 0
Concentration mg/L 1,071 1,071 577 740 - -
(7439-95-) Mass Ibs 8,939 8,938 4,072 740 - -
Molybdenum, Concentration µg/L 949 949 30 740 - -
20. total ❑✓ 0
(7439-98-7) Mass lbs 7.1 7.1 0.2 740 - -
21 Manganese,total ❑ 0 Concentration mg/L 724 724 83 - 740 - -
(7439-96-5) Mass lbs 4,209 4,209 582 740 - -
22 Tin,total ❑ ❑ Concentration mg/L <0.005 <0.005 <0.005 1 - -
(7440-31-5) Mass lbs <0.58 <0.40 <0.04 1 - -
23 Titanium,total 0 ❑ Concentration - - - - - -
(7440-32-6) Mass - - - - - - -
EPA Form 3510-2C(Revised 3-19) Page 24

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
•
TABLE C.CERTAIN CONVENTIONAL AND NON CONVENTIONAL POLLUTANTS(40 CFR 122.21(g)(7)(vi))1
Presence or Absence Intake
(check one) Effluent (Optional)
Pollutant Units Maximum Long-Term
Believed Believed (specify) Maximum Daily Long-Term
Present Absent Discharge Monthly Average Daily Number of Average Number of
Discharge Discharge Analyses Analyses
(required) Value
(if available) (if available)
24. Radioactivity
Concentration - - - - - - -
Alpha,total ❑ 0
Mass - - - - - - -
Concentration - - - - - - -
Beta,total ❑ ❑✓ Mass
Concentration - - - - - -
Radium,total ❑ Cl Mass
Concentration - - - - - - -
Radium 226,total ❑ EMass
1 Sampling shall be conducted according to sufficiently sensitive test procedures(i.e., methods)approved under 40 CFR 136 for the analysis of pollutants or pollutant parameters or
required under 40 CFR chapter I,subchapter N or 0.See instructions and 40 CFR 122.21(e)(3).
EPA Form 3510-2C(Revised 3-19) Page 25

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE D.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))1
Presence or Absence
Pollutant (check one) Reason Pollutant Believed Present in Discharge Available Quantitative Data
Believed Believed (specify units)
Present Absent
1. Asbestos ❑ ❑✓ - -
2. Acetaldehyde 0 ❑✓ - -
3. Allyl alcohol ❑ ❑✓ - -
4. Allyl chloride ❑ ❑✓ - -
5. Amyl acetate 0 ❑✓ - -
6. Aniline 0 ❑✓ - -
7. Benzonitrile 0 ✓❑ - -
8. Benzyl chloride 0 ❑� - -
9. Butyl acetate ❑ ❑✓ - -
10. Butylamine ❑ ❑✓ - -
11. Captan ❑ ❑✓ - -
12. Carbaryl ❑ ❑� - -
13. Carbofuran 0 ❑✓ - -
14. Carbon disulfide ❑ ❑✓ - -
15. Chlorpyrifos ❑ ✓❑ - -
16. Coumaphos ❑ ❑� - -
17. Cresol 0 ❑✓ - -
18. Crotonaldehyde 0 ❑✓ - -
19. Cyclohexane 0 ❑ - -
EPA Form 3510-2C(Revised 3-19) Page 27

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
•
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLED.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))l
Presence or Absence
Pollutant (check one) Reason Pollutant Believed Present in Discharge Available Quantitative Data
Believed Believed (specify units)
Present Absent
20. 2,4-D(2,4-dichlorophenoxyacetic acid) 0 ❑✓ - -
21. Diazinon 0 ❑✓ - -
22. Dicamba ❑ ❑✓ - -
23. Dichlobenil 0 ❑✓ - -
24. Dichlone El ❑✓ - -
25. 2,2-dichloropropionic acid 0 ❑✓ - -
26. Dichlorvos ❑ ❑✓ - -
27. Diethyl amine ❑ ❑✓ - -
28. Dimethyl amine 0 ❑✓ - -
29. Dintrobenzene CI 0 - -
30. Diquat 0 ❑✓ - -
31. Disulfoton ❑ ❑✓ - -
32. Diuron 0 ❑✓ - -
33. Epichlorohydrin 0 ❑✓ - -
34. Ethion 0 ❑✓ -
35. Ethylene diamine 0 ❑✓ - -
36. Ethylene dibromide ❑ ❑✓ - -
37. Formaldehyde 0 ❑✓ - -
38. Furfural 0 0 - -
EPA Form 3510-2C(Revised 3-19) Page 28

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE D.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))1
Presence or Absence
Pollutant (check one) Available Quantitative Data
Believed Believed Reason Pollutant Believed Present in Discharge (specify units)
Present Absent
39. Guthion ❑ ❑✓ - -
40. Isoprene ❑ ❑✓ - -
41. Isopropanolamine ❑ ❑✓ - -
42. Kelthane 0 ❑✓ -
43. Kepone ❑ 0 - -
44. Malathion 0 ❑✓ - -
45. Mercaptodimethur 0 0 -
46. Methoxychlor 0 ❑✓ - -
47. Methyl mercaptan ❑ ❑✓ - -
48. Methyl methacrylate ❑ 0 - -
49. Methyl parathion 0 0 - -
50. Mevinphos 0 0 - -
51. Mexacarbate ❑ ❑✓ - -
52. Monoethyl amine ❑ 0 - -
53. Monomethyl amine ❑ 0 - -
54. Naled ❑ 0 - -
55. Naphthenic acid ❑ 0 - -
56. Nitrotoluene ❑ 0 - -
57. Parathion 0 0 -
EPA Form 3510-2C(Revised 3-19) Page 29

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
•
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE D.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))1
Presence or Absence
Pollutant (check one) Reason Pollutant Believed Present in Discharge Available Quantitative Data
Believed Believed (specify units)
Present Absent
58. Phenolsulfonate 0 ❑✓ - -
59. Phosgene ❑ 0 - -
60. Propargite ❑ ❑✓ - -
61. Propylene oxide ❑ 0 - -
62. Pyrethrins ❑ ❑✓ - -
63. Quinoline ❑ 0 - -
64. Resorcinol 0 0 - -
65. Strontium ❑✓ ❑ Routine in-house analytical data(Max/Avg Daily Dis.:MDD/ADD) MDD:37 mg/L;ADD:3.9 mg/L
66. Strychnine ❑ 0 - -
67. Styrene 0 0 - -
68. 2,4 5-T(2,4,5-trichlorophenoxyacetic ❑ El - -
acid)
69. TDE(tetrachlorodiphenyl ethane) ❑ 0 - -
70. 2,4,5-TP[2-(2,4,5-trichlorophenoxy) El 0 - -
propanoic acid]
71. Trichlorofon ❑ ❑✓ - -
72. Triethanolamine ❑ ❑ - -
73. Triethylamine ❑ 0 - -
74. Trimethylamine ❑ El - -
75. Uranium ❑ 0 - -
76. Vanadium ❑ 0 - -
EPA Form 3510-2C(Revised 3-19) Page 30

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLED.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))1
Presence or Absence
Pollutant (check one) Reason Pollutant Believed Present in Discharge Available Quantitative Data
Believed Believed (specify units)
Present Absent
77. Vinyl acetate ❑ 0 - -
78. Xylene D 0 - -
79. Xylenol ❑ 0 - -
80. Zirconium 0 0 - -
1 Sampling shall be conducted according to sufficiently sensitive test procedures(i.e., methods)approved under 40 CFR 136 for the analysis of pollutants or pollutant parameters or
required under 40 CFR chapter I,subchapter N or 0.See instructions and 40 CFR 122.21(e)(3).
EPA Form 3510-2C(Revised 3-19) Page 31

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE E.2,3,7,8 TETRACHLORODIBENZO P DIOXIN(2,3,7,8 TCDD)(40 CFR 122.21(g)(7)(viii))
TCDD Presence or
Congeners Absence
Pollutant (check one) Results of Screening Procedure
Used or
Manufactured Believed Believed
Present Absent
2,3,7,8-TCDD
EPA Form 3510-2C(Revised 3-19) Page 33

Narrative:Supplemental Information
Befesa Mooresboro, NC Effluent Discharge Permit Renewal Application
Permit NC0089109
This renewal application is submitted to the North Carolina Department of Environmental Quality(NCDEQ) for
timely renewal of the effluent discharge permit (Permit NC0089109) for the Befesa Mooresboro, NC facility
("the facility"), formerly American Zinc Products, LLC. See Form 1 attached for site information.
Information provided in this permit renewal application includes effluent discharge monitoring data collected
for Outfall 001 from June 2020 to August 2022 (See Form 2C—Section 1 Attachments for outfall location).
Monitoring was performed in accordance with permit requirements for analytical monitoringof
Y discharged
effluent. Information provided in this permit renewal application reflects effluent discharge monitoring data
provided in monthly discharge monitoring reports (DMRs) submitted to the Department from June 2020 to
August 2022.This information reflects the nature of effluent discharge water based on current operations.
A summary of effluent flow and characteristic information is provided below. Data from Monthly DMR's for the
past 26 months from June 2020 to August 2022 are provided in the tables in the Form 2C-Section 7
Attachments of this narrative.
Facility Description
The manufacturing process at the facility consists of an integrated system of leaching, solvent extraction, and
electrowinning processes. This facility replaced a former zinc smelter. Feedstock for the Mooresboro facility,
including metal bearing oxides and other raw materials, is managed in solution throughout the process.
Valuable metal products are removed as precipitates,concentrates, and high-grade zinc metal. As detailed on
the water flow line drawing included in the Form 2C—Section 2 Attachments,the facility differs from a
traditional definition of a process facility with wastewater effluent as there is no wastewater treatment system.
Removal from the process streams of what would otherwise be considered pollutants represents the generation
of commercial products for this facility.
Process units described on the line drawing extract valuable metals and products, most of which are listed as
effluent discharge parameters. Once all cost-effective metals extraction is achieved,the resulting process
wastewater stream requires no further treatment to comply with the categorical effluent standards applicable
to the discharge. These process cycles are all inherent to facility operations. The uniqueness of the facility is
made clear in the fact that it is only one of three facilities in the world that performs these processes.
Permit History
NPDES Effluent Discharge Permit No. NC0089109 ("the permit" or"the current permit") was issued to AZP for
the discharge of process water effluent to the Broad River on June 9, 2020, effective July 1, 2020, and expiring
July 31, 2023. On September 20, 2022,the facility's name was changed to Befesa Zinc Metals, LLC.
NCDE DW
Q/ Q was notified of this change via a Name Change Form.
g g
1

In addition to this permit,the plant has two additional NPDES Permits:
■ NCG500677 issued by NCDEQ on January 6, 2021 -Certificate of coverage for discharge of non-contact
cooling water, cooling tower and boiler blowdown, condensate, exempt stormwater, cooling water
associated with hydroelectric operations, and similar wastewaters under the DEQ's General Permit
NCG50000.
Currently this plant continues to route these discharges through the stormwater outlet. Befesa has plans to
reroute this water back into the process where it can be reused. This modification is planned for calendar
year 2023 and is not anticipated to impact the parameters in this permit.
■ NCS000562 Issued by NCDEQ May 2, 2018,for the discharge of stormwater to the Broad River.
Fish Tissue Study
The fish tissue study required by Section A.4 of the permit in the Broad River was performed in the summer of
2022. Results have been reported to NCDEQ electronically. A copy and summary of the results have been
included here for reference in Appendix 2.
Discharge Volume
The current permitted monthly average discharge volume is 980,000 gallons/day (0.980 MGD). As the facility
production has increased over the current permit period,the effluent discharge volume has also increased
accordingly while staying within the 0.98 MGD limit. The reported maximum monthly average discharge volume
is 0.957 MGD with the monthly average for the permit period being 0.875 MGD.
While the monitoring data summarized in Form 2C Section 7 and in this narrative includes data from the start of
the permit period (June 2020)to present,the average monthly discharge of 0.875 MGD is only based on flow
data back to January 2021. It was determined that the lower monthly average flows from the ramp up
production period are not representative of the facility flow (i.e.,flows mostly below 0.80 MGD).
Effluent Limitations and Monitoring Requirements
As is now required by NCDEQ, EPA Forms 1 and 2C were completed for the facility, an existing industrial facility
discharging process wastewater. The facility has met its permit limits for flow, pH, and Total Cadmium. The pH
limits of>_6 SU and 5_9 SU were not exceeded per the daily averages recorded,the minimum daily average being
6.44 and the maximum daily average being 8.34. The Total Cadmium monitoring is discussed in further detail
later in this narrative as it pertains to the Cadmium Compliance Schedule.
The facility is requesting a waiver for the following parameters, as was done for the last permit:
■ Biochemical Oxygen Demand (BOD5)
■ Chemical Oxygen Demand (COD)
■ Total Organic Carbon (TOC)
■ Temperature (winter)
■ Temperature (summer)
2

The facility still has reason to believe that BOD5, COD,TOC, and temperature are not pollutants of concern
significantly present in the effluent because of the nature of the facility operations. There are no sources that
would contribute levels of these parameters with a reasonable potential to exceed water quality standards in
the effluent discharge.
Tables A through E in Form 2C were completed with quantitative results listed for those pollutants/parameters
for which testing is required per the current permit. This includes those listed in the permit requiring quarterly
or more frequent monitoring as well as the Priority Pollutants listed in Section A.5 of the permit. The permit
does list parameters under the Section A.5 Priority Pollutants Analysis corresponding to pollutants/parameters
in Table B Sections 1 "Toxic Metals, Cyanide, and Total Phenols", Section 2 "Organic Toxic Pollutants (GC/MS
Fraction—Volatile Compounds)", Section 3 "Organic Toxic Pollutants (GC/MS Fraction—Acid Compounds)", and
Section 4 "Organic Toxic Pollutants (GC/MS Fraction—Base/Neutral Compounds)". While the facility does fall
into the Nonferrous Metals Manufacturing category and Form 2C indicates that the facility is required to
monitor for pollutants in Table B Section 5 "Organic Toxic Pollutants (GC/MS Fraction—Pesticides)", none of
these parameters were required by the previous permit and have not been analyzed. They are all believed
absent from the facility with no reasonable potential to be present.
There are two pollutants noted in Form 2C as "believed present" where no quantitative data were reported:
Sulfide (as S) and Surfactants in Table C. These are not monitored by the facility currently and were not required
in the previous permit. Sulfide is believed present in the effluent as sodium sulfide is used in the process as
precipitating reagent. Surfactants are believed present in the effluent due to a flocculant is used in final solid-
liquid separation step of the process.
Cadmium Compliance Schedule
The Cadmium Compliance Schedule (CCS) set forth in section A.6 of the current permit has a deadline to achieve
full compliance as December 1, 2027. The compliance limits in the current permit for Cadmium are a monthly
average of 350.0 µg/L and a daily maximum of 2,143 µg/L. The compliance limits for Cadmium at the
completion of the CCS are a monthly average of 90.4 µg/L and a daily maximum of 454.4 µg/L. These CCS
compliance limits have been consistently met by the facility, acknowledging only two exceedances in the last
permit period. Please see Appendix 1 for a detailed compliance evaluation and justification. The facility is
proposing that full compliance has been achieved and,therefore, is requesting the removal of the CCS from the
permit.
3

NPDES Form 1
General Information

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
Form U.S.Environmental Protection Agency
&EPA Application for NPDES Permit to Discharge Wastewater
NPDES GENERAL INFORMATION
SECTION 1.ACTIVITIES REQUIRING AN NPDES PERMIT(40 CFR 122.21(f)and(f)(1))
1.1 Applicants Not Required to Submit Form 1
Is the facility a new or existing publicly owned Is the facility a new or existing treatment works
1.1.1 treatment works? 1.1.2 treating domestic sewage?
If yes,STOP.Do NOT complete 0 No If yes,STOP.Do NOT E No
Form 1.Complete Form 2A. complete Form 1.Complete
Form 2S.
1.2 Applicants Required to Submit Form 1
.• 1.2.1 Is the facility a concentrated animal feeding 1.2.2 Is the facility an existing manufacturing,
operation or a concentrated aquatic animal commercial,mining,or silvicultural facility that is
a production facility? currently discharging process wastewater?
o 0 Yes 4 Complete Form 1 El No El Yes 4 Complete Form 0 No
z and Form 2B. 1 and Form 2C. _
0 1.2.3 Is the facility a new manufacturing,commercial, 1.2.4 Is the facility a new or existing manufacturing,
mining,or silvicultural facility that has not yet commercial,mining,or silvicultural facility that
commenced to discharge? discharges only nonprocess wastewater?
Cr D Yes 4 Complete Form 1 E No Yes 4 Complete Form 0 No
ce and Form 2D. 1 and Form 2E.
°: 1.2.5 Is the facility a new or existing facility whose
discharge is composed entirely of stormwater
associated with industrial activity or whose
discharge is composed of both stormwater and
non-stormwater?
❑ Yes 4 Complete Form 1 E No
and Form 2F
unless exempted by
40 CFR
122.26(b)(14)(x)or
b 15.
SECTION 2.NAME,MAILING ADDRESS,AND LOCATION(40 CFR 122.21(f)(2))
2.1 Facility Name
Befesa Zinc Metal,LLC
0 2.2 EPA Identification Number
U
NCR000159038
v
0 2.3 Facility Contact
Name(first and last) Title Phone number
aJan Nedbal Environmental Manager [phone]
Email address
[e-mail]
z
2.4 Facility Mailing Address
Street or P.O.box
484 Hicks Grove Road
City or town State ZIP code
Mooresboro North Carolina 28114
EPA Form 3510-1(revised 3-19) Pa9 e 1

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
y 2.5 Facility Location
a . Street, route number,or other specific identifier
< o 484 Hicks Grove Road
a U
.s o County name County code(if known)
ns
Rutherford County 161
E -0 City or town State ZIP code
z Mooresboro North Carolina 28114
SECTION 3.SIC AND NAICS CODES(40 CFR 122.21(f)(3))
3.1 SIC Code(s) Description (optional)
3341 Secondary Nonferrous Metals
a)
0
U
3.2 NAICS Code(s) Description (optional)
U
SECTION 4.OPERATOR INFORMATION(40 CFR 122.21(f)(4))
4.1 Name of Operator
Befesa Zinc Metal,LLC
0 4.2 Is the name you listed in Item 4.1 also the owner?
c 0 Yes ❑ No
4.3 Operator Status
❑ Public—federal ❑ Public—state ❑ Other public(specify)
o ❑� Private ❑ Other(specify)
4.4 Phone Number of Operator
[phone]
4.5 Operator Address
Street or P.O. Box
E 484 Hicks Grove Road
ci
• City or town State ZIP code
o Mooresboro North Carolina 28114
tits
Email address of operator
[phone]
SECTION 5.INDIAN LAND(40 CFR 122.21(f)(5))
F o 5.1 Is the facility located on Indian Land?
�' El Yes ❑r No
EPA Form 3510-1(revised 3-19) Page 2

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 6.EXISTING ENVIRONMENTAL PERMITS(40 CFR 122.21(f)(6))
6.1 Existing Environmental Permits(check all that apply and print or type the corresponding permit number for each)
❑✓ NPDES(discharges to surface ❑ RCRA(hazardous wastes) ❑ UIC(underground injection of
water) fluids)
2 E NCS000562
.c
ui n 1=1 PSD(air emissions) ❑ Nonattainment program(CM) ❑ NESHAPs(CM)
102481107
x ❑ Ocean dumping(MPRSA) ❑ Dredge or fill(CWA Section 404) 0 Other(specify)
w
NCG500000(NC Cooling)
SECTION 7.MAP(40 CFR 122.21(f)(7))
7.1 Have you attached a topographic map containing all required information to this application?(See instructions for
specific requirements.)
E Yes ❑ No ❑ CAFO—Not Applicable(See requirements in Form 2B.)
SECTION 8.NATURE OF BUSINESS(40 CFR 122.21(f)(8))
8.1 Describe the nature of your business.
This facility processes Waelz Oxide(a.k.a.Crude Zinc Oxide)as its principal raw material to produce Special
High-Grade(SHG)zinc metal and other metals as it's principal product.The manufacturing process consists of an
integrated system of leaching,extraction,stripping,and electrowinning processes.Feed,including metal bearing
oxides(e.g.Walez Oxide)and other raw materials,are managed in solution throughout the process. Metal products
are removed as precipitates,concentrates,SHG zinc metal and CGG alloy. Metal-bearing Waelz Oxide feed is
delivered to the subject facility from local and international sources.The specific technologies and configuration of
e the operation are confidential business information.
a>
z
SECTION 9.COOLING WATER INTAKE STRUCTURES(40 CFR 122.21(f)(9))
9.1 Does your facility use cooling water?
❑✓ Yes ❑ No 4 SKIP to Item 10.1.
' 9.2 Identify the source of cooling water.(Note that facilities that use a cooling water intake structure as described at
a, 40 CFR 125,Subparts I and J may have additional application requirements at 40 CFR 122.21(r).Consult with your
0
NPDES permitting authority to determine what specific information needs to be submitted and when.)
0 c, Forest City,NC Water Supply
SECTION 10.VARIANCE REQUESTS(40 CFR 122.21(f)(10))
10.1 Do you intend to request or renew one or more of the variances authorized at 40 CFR 122.21(m)?(Check all that
apply. Consult with your NPDES permitting authority to determine what information needs to be submitted and
when.)
CD
❑ Fundamentally different factors(CWA ❑ Water quality related effluent limitations(CWA Section
e Section 301(n)) 302(b)(2))
❑ Non-conventional pollutants(CWA ❑ Thermal discharges(CWA Section 316(a))
•
co Section 301(c)and(g))
❑✓ Not applicable
EPA Form 3510-1(revised 3-19) Page 3

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 11.CHECKLIST AND CERTIFICATION STATEMENT(40 CFR 122.22(a)and(d))
11.1 In Column 1 below, mark the sections of Form 1 that you have completed and are submitting with your application.
For each section,specify in Column 2 any attachments that you are enclosing to alert the permitting authority.Note
that not all applicants are required to provide attachments.
Column 1 Column 2
O Section 1:Activities Requiring an NPDES Permit ❑ w/attachments
❑✓ Section 2:Name,Mailing Address,and Location ❑ w/attachments
O Section 3:SIC Codes ❑ wl attachments
❑✓ Section 4:Operator Information ❑ w/attachments
❑✓ Section 5: Indian Land ❑ w/attachments
❑✓ Section 6:Existing Environmental Permits ❑ w/attachments
w/topographic
Section 7: Map ❑✓ map ❑El Section additional attachments
o ❑✓ Section 8: Nature of Business ❑ w/attachments
a,
0 Section 9:Cooling Water Intake Structures ❑ w/attachments
❑✓ Section 10:Variance Requests ❑ w/attachments
173
VCS
Section 11:Checklist and Certification Statement L14 w/attachments n
I >y
11.2 Certification Statement
I certify under penalty of law that this document and all attachments were prepared under my direction or supervision
in accordance with a system designed to assure that qualified personnel properly gather and evaluate the
information submitted.Based on my inquiry of the person or persons who manage the system, or those persons
directly responsible for gathering the information,the information submitted is,to the best of my knowledge and
belief, true,accurate,and complete.lam aware that there are significant penalties for submitting false information,
including the possibility of fine and imprisonment for knowing violations.
Name(print or type first and last name) Official title
Jan Nedbal Environmental Superintendent
Signature Date signed
a").\ 1'2. .\`t. ?-02,-2-
EPA Form 3510-1 (revised 3-19) Page 4

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 12.CHECKLIST AND CERTIFICATION STATEMENT(40 CFR 122.22(a)and(d))
12.1 In Column 1 below, mark the sections of Form 2C that you have completed and are submitting with your application.
For each section,specify in Column 2 any attachments that you are enclosing to alert the permitting authority.Note
that not all applicants are required to complete all sections or provide attachments.
Column 1 Column 2
O Section 1:Outfall Location ❑ w/attachments
O Section 2: Line Drawing ✓❑ w/line drawing ❑ w/additional attachments
w/list of each user of
Section 3:Average Flows and
Treatment ❑ w/attachments ❑ privately owned treatment
works
Section 4: Intermittent Flows ❑ w/attachments
0 Section 5: Production ❑ w/attachments
w/optional additional
0 Section 6: Improvements ❑ w/attachments ❑ sheets describing any
additional pollution control
plans
• w/request for a waiver and ❑ w/explanation for identical
supporting information outfalls
w/small business exemption
❑ request ❑ w/other attachments
0 Section 7: Effluent and Intake 0 w/Table A ❑✓ w/Table B
Characteristics
0
Ei w/Table C ❑✓ w/Table D
w/Table E w/analytical results as an
'CSattachment
Section 8: Used or Manufactured
rt, 0 Toxics ❑ w/attachments
0 Section 9: Biological Toxicity 0 w/attachments
Tests
U
O Section 10:Contract Analyses ❑ w/attachments
0 Section 11:Additional Information ❑ w/attachments
Section 12:Checklist and ip [21/w/attachments
Certification Statement
12.2 Certification Statement
I certify under penalty of law that this document and all attachments were prepared under my direction or supervision in
accordance with a system designed to assure that qualified personnel properly gather and evaluate the information
submitted.Based on my inquiry of the person or persons who manage the system, or those persons directly
responsible for gathering the information, the information submitted is, to the best of my knowledge and belief, true,
accurate, and complete. I am aware that there are significant penalties for submitting false information,including the
possibility of fine and imprisonment for knowing violations.
Name(print or type first and last name) Official title
<1A)/1 EtwItt-bOtsA.EtZTINL—
n^4,6•S et ER-
Signature Date signed
?%5jk/ ")( t6 .202 -
EPA Form 3510-2C(Revised 3-19) Page 7

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 9.BIOLOGICAL TOXICITY TESTS(40 CFR 122.21(g)(11))
9.1 Do you have any knowledge or reason to believe that any biological test for acute or chronic toxicity has been made
within the last three years on(1)any of your discharges or(2)on a receiving water in relation to your discharge?
❑✓ Yes ❑ No 4 SKIP to Section 10.
cu
cu 9.2 Identify the tests and their purposes below.
Test(s) Purpose of Test(s) Submitted to NPDES Date Submitted
oPermitting Authority?
Fish Tissue Sampling Biological,Under NPDES
❑Permit Yes ❑ No
❑ Yes ❑ No
❑ Yes ❑ No
SECTION 10.CONTRACT ANALYSES(40 CFR 122.21(g)(12))
10.1 Were any of the analyses reported in Section 7 performed by a contract laboratory or consulting firm?
❑ Yes ❑ No 4 SKIP to Section 11.
10.2 Provide information for each contract laboratory or consulting firm below.
Laboratory Number 1 Laboratory Number 2 Laboratory Number 3
Name of laboratory/firm Pace Analytical Services,LLC ETT Environmental,Inc.
N
Laboratory address 9800 Kincey Ave. Suite 100 4 Craftsman Court
c Huntersville,NC 28078 Greer,SC 29650
c0 Phone number
[phone] [phone]
Pollutant(s)analyzed Priority Pollutants DO,Hardness,Phosphorus,
Ammonia-N,TKN
SECTION 11.ADDITIONAL INFORMATION(40 CFR 122.21(g)(13))
11.1 Has the NPDES permitting authority requested additional information?
❑ Yes ❑✓ No 4 SKIP to Section 12.
0
E 11.2 List the information requested and attach it to this application.
1. 4.
Ct
•
3. 6,
EPA Form 3510-2C(Revised 3-19) Page 6

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
7.7 Have you checked"Testing Required"for all required pollutants in Sections 2 through 5 of Table B for each of the
GC/MS fractions checked in Item 7.6?
❑r Yes ❑ No
7.8 Have you checked"Believed Present"or"Believed Absent"for all pollutants listed in Sections 1 through 5 of Table B
where testing is not required?
O Yes ❑ No
7.9 Have you provided (1)quantitative data for those Section 1,Table B, pollutants for which you have indicated testing is
required or(2)quantitative data or other required information for those Section 1,Table B, pollutants that you have
indicated are"Believed Present"in your discharge?
Yes ❑ No
7.10 Does the applicant for a small business exemptionspecified in the instructions?
PP qualify fY under the criteria P❑ Yes 4 Note that you qualify at the top of Table B, ❑ No
0 then SKIP to Item 7.12.
CD
7.11 Have you provided(1)quantitative data for those Sections 2 through 5,Table B, pollutants for which you have
o determined testing is required or(2)quantitative data or an explanation for those Sections 2 through 5,Table B,
N pollutants you have indicated are"Believed Present"in your discharge?
0 Yes ❑ No
a� Table C.Certain Conventional and Non-Conventional Pollutants
• 7.12 Have you indicated whether pollutants are"Believed Present"or"Believed Absent"for all pollutants listed on Table C
s for all outfalls?
U
;� 0 Yes ElNo
c 7.13 Have you completed Table C by providing(1)quantitative data for those pollutants that are limited either directly or
indirectly in an ELG and/or(2)quantitative data or an explanation for those pollutants for which you have indicated
"Believed Present"?
O ❑ Yes ❑ No
▪ Table D.Certain Hazardous Substances and Asbestos
7.14 Have you indicated whether pollutants are'Believed Present"or"Believed Absent"for all pollutants listed in Table D for
all outfalls?
1✓ Yes El No
7.15 Have you completed Table D by(1)describing the reasons the applicable pollutants are expected to be discharged
and(2)by providing quantitative data,if available?
0 Yes ❑ No
Table E.2,3,7,8-Tetrachlorodibenzo-p-Dioxin(2,3,7,8-TCDD)
7.16 Does the facility use or manufacture one or more of the 2,3,7,8-TCDD congeners listed in the instructions,or do you
know or have reason to believe that TCDD is or may be present in the effluent?
❑ Yes 4 Complete Table E. ❑✓ No 4 SKIP to Section 8.
7.17 Have you completed Table E by reporting qualitative data for TCDD?
❑ Yes ❑ No
SECTI0118.USED OR MANUFACTURED TOXICS(40 CFR 122.21(g)(9))
8.1 Is any pollutant listed in Table B a substance or a component of a substance used or manufactured at your facility as
an intermediate or final product or byproduct?
❑ Yes El No 3 SKIP to Section 9.
8.2 List the pollutants below.
1. Cadmium 4, 7. .
0
2. Lead 5. 8.
3, Zinc 6. 9.
II
EPA Form 3510-2C(Revised 3-19) Page 5

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 6.IMPROVEMENTS(40 CFR 122.21(g)(6))
6.1 Are you presently required by any federal,state,or local authority to meet an implementation schedule for constructing,
upgrading,or operating wastewater treatment equipment or practices or any other environmental programs that could
affect the discharges described in this application?
❑✓ Yes ❑ No 4 SKIP to Item 6.3.
6.2 Briefly identify each applicable project in the table below.
Affected Final Compliance Dates
Brief Identification and Description of Outfalls Source(s)of
Project (list outfall Discharge Required Projected
c2number)
a Cadmium Compliance Schedule 001 Process Water 12/01/2027 09/01/2022
U,
m
cc
R
Q
6.3 Have you attached sheets describing any additional water pollution control programs(or other environmental projects
that may affect your discharges)that you now have underway or planned?(optional item)
❑r Yes ❑ No ❑ Not applicable
SECTION 7.EFFLUENT AND INTAKE CHARACTERISTICS(40 CFR 122.21(g)(7))
See the instructions to determine the pollutants and parameters you are required to monitor and, in turn,the tables you must
complete.Not all applicants need to complete each table.
Table A.Conventional and Non-Conventional Pollutants
7.1 Are you requesting a waiver from your NPDES permitting authority for one or more of the Table A pollutants for any of
your outfalls?
El Yes ❑ No SKIP to Item 7.3.
7.2 If yes,indicate the applicable outfalls below.Attach waiver request and other required information to the application.
Outfall Number 001 Outfall Number Outfall Number
7.3 Have you completed monitoring for all Table A pollutants at each of your outfalls for which a waiver has not been
7-7
requested and attached the results to this application package?
0 Yes "I permitting
a waiver has been requested from my NPDES
permitting authority for all pollutants at all outfalls.
iS Table B.Toxic Metals,Cyanide,Total Phenols,and Organic Toxic Pollutants
7.4 Do any of the facility's processes that contribute wastewater fall into one or more of the primary industry categories
to
listed in Exhibit 2C-3?(See end of instructions for exhibit.)
0 Yes ❑ No SKIP to Item 7.8.
7.5 Have you checked"Testing Required"for all toxic metals,cyanide,and total phenols in Section 1 of Table B?
0 Yes ❑ No
7.6 List the applicable primary industry categories and check the boxes indicating the required GC/MS fraction(s)identified
in Exhibit 2C-3.
Primary Industry Category Required GC/MS Fraction(s)
(Check applicable boxes.)
Nonferrous Metals Manufacturing 0 Volatile 0 Acid 0 Base/Neutral 0 Pesticide
0 Volatile 0 Acid ❑ Base/Neutral 0 Pesticide
❑Volatile 0 Acid ❑ Base/Neutral ❑ Pesticide
EPA Form 3510-2C(Revised 3-19) Page 4

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
SECTION 4.INTERMITTENT FLOWS(40 CFR 122.21(g)(4))
4.1 Except for storm runoff,leaks,or spills,are any discharges described in Sections 1 and 3 intermittent or seasonal?
0 Yes ❑ No 4 SKIP to Section 5.
4.2 Provide information on intermittent or seasonal flows for each applicable outfall.Attach additional pages,if necessary.
Outfall Operation Frequency Flow Rate
Number (list) Average Average Long-Term Maximum Duration
Days/Week Months/Year Average Daily
Process Water 7 days/week 12 months/year 0.873 mgd 0.949 mgd 1 days
001 days/week months/year mgd mgd days
days/week months/year mgd mgd days
CD
E days/week months/year mgd mgd days
m
days/week months/year mgd mgd days
days/week months/year mgd mgd days
days/week months/year mgd mgd days
•
days/week months/year mgd mgd days
days/week months/year mgd mgd days
SECTION 5.PRODUCTION(40 CFR 122.21(g)(5))
5.1 Do any effluent limitation guidelines(ELGs)promulgated by EPA under Section 304 of the CWA apply to your facility?
❑ Yes E No 4 SKIP to Section 6.
5.2 Provide the following information on applicable ELGs.
ELG Category ELG Subcategory Regulatory Citation
.a
.Q
5.3 Are any of the applicable ELGs expressed in terms of production(or other measure of operation)?
❑ Yes ❑ No -4 SKIP to Section 6.
0
5.4 Provide an actual measure of daily production expressed in terms and units of applicable ELGs.
Outfall Operation,Product,or Material Quantity per Day Unit of
-0 Number Measure
COCII
0
c.�
0
d
EPA Form 3510-2C(Revised 3-19) Page 3

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
3.1 **Outfall Number**
cont. Operations Contributing to Flow
Operation Average Flow
mgd
mgd
mgd
mgd
Treatment Units
Description Code from Final Disposal of Solid or
(include size,flow rate through each treatment unit, Table 2C-1 Liquid Wastes Other Than
retention time,etc.) by Discharge
0
U
m
E
is
a
I
**Outfall Number**
Operations Contributing to Flow
Operation Average Flow
T.
mgd
R
N
mgd
mgd
mgd
Description Code from Final Disposal of Solid or
(include size,flow rate through each treatment unit, Table 2C-1 Liquid Wastes Other Than
retention time,etc.) by Discharge
3.2 Are you applying for an NPDES permit to operate a privately owned treatment works?
E ❑ Yes ElNo -+SKIP to Section 4.
3.3 Have you attached a list that identifies each user of the treatment works?
❑ Yes ❑ No
EPA Form 3510-2C(Revised 3-19) Page 2

EPA Identification Number NPDES Permit Number Facility Name Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
Form U.S.Environmental Protection Agency
2C `'EPA
�/� Application for NPDES Permit to Discharge Wastewater
NPDES G i"� EXISTING MANUFACTURING, COMMERCIAL, MINING,AND SILVICULTURE OPERATIONS
SECTION 1.OUTFALL LOCATION(40 CFR 122.21(g)(1))
1.1 Provide information on each of the facility's outfalls in the table below.
o Nu bear Receiving Water Name Latitude Longitude
Ce
0 001 Broad River 35° 12' 2.6" N 81° 51' 3.1" W
co
11
0
o » o u
SECTION 2.LINE DRAWING(40 CFR 122.21(g)(2))
2.1 Have you attached a line drawing to this application that shows the water flow through your facility with a water
. balance?(See instructions for drawing requirements.See Exhibit 2C-1 at end of instructions for example.)
J R
❑✓ Yes ❑ No
SECTION 3.AVERAGE FLOWS AND TREATMENT(40 CFR 122.21(g)(3))
3.1 For each outfall identified under Item 1.1,provide average flow and treatment information.Add additional sheets if
necessary.
**Outfall Number** 001
Operations Contributing to Flow
Operation Average Flow
Process Water(Average Daily Flow Jan.2021-April 2022) 0.875 mgd
mgd
mgd
a
mgd
Treatment Units
Description Code from Final Disposal of Solid or
(include size,flow rate through each treatment unit, Table 2C-1 Liquid Wastes Other Than
retention time,etc.) by Discharge
N/A.No wastewater treatment system N/A N/A
See Narrative for details
EPA Form 3510-2C(Revised 3-19) Page 1

NPDES Form 2C
Existing Manufacturing, Commercial, Mining, and
Silvicultural Operations

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE A.CONVENTIONAL AND NON CONVENTIONAL POLLUTANTS(40 CFR 122.21(g)(7)(iii))1
Effluent Intake
(Optional)
Waiver Units Maximum Maximum Long-Term
Pollutant Requested (specify) Daily Monthly Average Daily Number of Long-Term Number of
(if applicable)
Discharge Discharge Discharge Analyses Average Value Analyses
(required) (if available) (if available)
❑ Check here if you have applied to your NPDES permitting authority for a waiver for all of the pollutants listed on this table for the noted outfall.
- - - - - -
Biochemical oxygen demand Concentration
1 El(BOD5) -
-
Mass
Chemical oxygen demand Concentration -
2. (COD)
Mass - - - - -
Concentration - - - - - - -
3. Total organic carbon (TOC) 0
Mass - - - - - - -
Concentration mg/L 56.7 56.7 20.4 54 - -
4. Total suspended solids(TSS) ❑
Mass lbs 473.1 449.1 149.2 54 - -
Concentration mg/L 0.81 0.81 0.29 9 - -
5. Ammonia (as N) ✓❑
Mass lbs 8.01 6.08 2.13 9 - -
6. Flow ❑ Rate MGD 1.393 0.957 0.875 803/27/27 - -
Temperature(winter) ❑✓ °C °C - - - - - -
7.
Temperature(summer) ❑✓ °C °C - - - - - -
pH(minimum) 0 Standard units S.U. 6.44 6.44 7.80 27 - -
8.
pH(maximum) ❑ Standard units S.U. 8.34 8.34 7.80 27 - -
1 Sampling shall be conducted according to sufficiently sensitive test procedures(i.e.,methods)approved under 40 CFR 136 for the analysis of pollutants or pollutant parameters or
required under 40 CFR chapter I,subchapter N or 0.See instructions and 40 CFR 12221(e)(3).
EPA Form 3510-2C(Revised 3-19) Page 9

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term -Long
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Number
Daily Monthly Term
Present Absent Daily of of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) (if available) Value
Check here if you qualify as a small business per the instructions to Form 2C and,therefore,do not need to submit quantitative data for any of the organic toxic pollutants in Sections
2 through 5 of this table.Note,however,that you must still indicate in the appropriate column of this table if you believe any of the pollutants listed are present in your discharge.
Section 1.Toxic Metals,Cyanide,and Total Phenols
1.1 Antimony,total 0 Concentration mg/L 0.149 0.149 0.039 9 - -
Ei CI
(7440-36-0) Mass lbs 1.053 1.120 0.284 9 - -
1.2 Arsenic,total 0 Concentration mg/L 0.013 0.013 <0.01 9 - -
(7440-38-2) ✓ ✓ Mass lbs 0.091 0.087 <0.073 9 - -
1.3 Beryllium,total 0 Concentration µg/L <1.0 <1.0 - 1 - -
(7440-41-7) Mass lbs <0.009 <0.009 - 1 - -
1.4 Cadmium,total 0 Concentration mg/L 0.130 0.130 0.038 54 - -
0 0
(7440-43-9) Mass lbs 0.629 0.890 0.277 54 - -
1.5 Chromium,total 0 Concentration mg/L <0.025 <0.025 <0.01 9 - -
(7440-47-3) Mass lbs <0.29 <0.20 <0.07 9 - -
1.6 Copper,total 0 Concentration mg/L 0.048 0.048 0.015 9 - -
(7440-50-8) Mass lbs 0.261 0.264 0.112 9 - -
1.7 Lead,total 0 Concentration mg/L 0.39 0.39 0.017 54 - -
El 1=1
(7439-92-1) Mass lbs 0.329 0.292 0.125 54 - -
1.8 Mercury,total 0 Concentration µg/L <1.0 <1.0 - 1 - -
El I=1
(7439-97-6) Mass lbs <0.009 <0.009 - 1 - -
1.9 Nickel,total 0 Concentration mg/L 0.063 0.063 0.019 27 - -
(7440-02-0) ✓ ✓ Mass Ibs .544 0.493 0.141 27 - -
1.10 Selenium,total Concentration µg/L 1,040 1,040 967 2 - -
CI
(7782-49-2) ✓ ✓ Mass lbs 8.98 8.98 8.30 2 - -
1.11 Silver,total 0 Concentration µg/L 41.5 41.5 26.6 2 - -
CI 12
(7440-22-4) Mass lbs 0.353 0.353 0.227 2 - -
EPA Form 3510-2C(Revised 3-19) Page 11

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal, LLC 001
OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) (if available) Value
1.12 Thallium,total ❑ ❑ ❑ Concentration ma_ 56.5 56.5 42.6 2 - -
(7440-28-0) Mass lbs 0.488 0.488 0.366 2 - -
1.13 Zinc,total ❑ ❑ Concentration mg/L 0.630 0.630 0.145 54 - -
(7440-66-6) Mass lbs 3.047 4.311 1.06 54 - -
1.14 Cyanide,total CI Concentration mg/L 0.038 0.038 - 1 - -ID
(57-•12-5) Mass lbs 0.323 0.323 - 1 - -
Concentration mg/L <2.0 <2.0 - 1 - -
1.15 Phenols,total ❑✓ CI
Mass lbs <0.17 <0.17 - 1 - -
Section 2.Organic Toxic Pollutants(GC/MS Fraction-Volatile Compounds)
Acrolein Concentration µg/L <5.0 <5..0 - 1 - -
2.1 E CI(107-02-8) CI lbs <0.043 <0.043 - 1 - -
Acrylonitrile Concentration µg/L <5.0 <5.0 - 1 - -
2.2 (107-13-1) ❑ CI ❑ Mass lbs <0.043 <0.043 - 1 - -
2.3 Benzene CIConcentration µg/L <1.0 <1.0 - 1 - -
(71-43-2) Mass Ibs <0.009 <0.009 - 1 - -
2.4 Bromoform ❑ ❑ CIConcentration llg/L 85.3 85.3 54.8 2 - -
(75-25-2) Mass lbs 0.737 0.737 0.472 2 --
-
2.5 Carbon tetrachloride ❑ ❑ ❑ Concentration µg/L <2.0 <2.0 - 1 - -
(56-23-5) Mass lbs <0.017 <0.017 - 1 - -
2.6 Chlorobenzene ❑ ❑ Concentration µg/L <2.0 <2.0 - 1 - -
(108-90-7) Mass lbs <0.017 <0.017 - 1 - -
2.7 Chlorodibromomethane ❑ Concentration µg/L <2.0 <2.0 - 1 - -
(124-48-1) Mass lbs <0.017 <0.017 - 1 - -
2.8 Chloroethane CI ❑ ❑ Concentration µg/L <2.0 <2.0 - 1 - -
(75-00-3) Mass lbs <0.017 <0.017 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 12

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Daily Monthly Term
Present Absent Daily of of
D(equi edge Dischar ifavailabe) Discharge Analyses AValuee Analyses
(if available)
2.9 2-chloroethylvinyl ether ❑ ❑ LiConcentration µg/L <5.0 <5.0 - 1 - -
(110-75-8) Mass lbs <0.043 <0.043 - 1 - -
Concentration µg/L 2.3 2.3 <3.2 2 - -
2.10 Chloroform(67-66-3) 0 0 ❑
Mass Ibs 0.020 0.020 <0.027 2 - -
2.11 Dichlorobromomethane El Concentration µg/L <2.0 <2.0 - 1 - 1
El
(75-27-4) Mass Ibs <0.017 <0.017 - 1 - -
2.12 11-dichloroethane El Concentration µg/L <2.0 <2.0 - 1 - 1
El
(75-34-3) El Mass lbs <0.017 <0.017 - 1 - -
12-dichloroethane Concentration µg/L <2.0 <2.0 - 1 - 1
2.13 El
(107-06-2) El ❑ Mass lbs <0.017 <0.017 - 1 - -
1,1-dichioroethylene 0 ❑ 0 Concentration µg/L <2.0 <2.0 -
2.14 1 - 1
(75-35-4) Mass lbs <0.017 <0.017 - 1 - -
2.15 1,2-dichloropropane ❑ ❑ Concentration µg/L <2.0 <2.0 - 1 - 1
(78-87-5) El Mass Ibs <0.017 <0.017 - 1 - -
1,3-dichloropropylene Concentration - - - - - -
2.16 (542-75-6) ❑ Mass - - - -
2.17 Ethylbenzene El El
❑ Concentration µg/L <1.0 <1.0 - 1 - 1
(100-41-4) Mass Ibs <0.009 <0.009 - 1 - -
Methyl bromide El ❑ 0 Concentration µg/L <2.0 <2.0 -
2181 - 1
(74-83-9) Mass lbs <0.017 <0.017 - 1 - -
Methyl chloride Concentration µg/L <2.0 <2.0 - 1 - 1
2.19 (74-87-3) El El ❑ Mass lbs <0.017 <0.017 - 1 - -
Methylene chloride Ei Concentration µg/L <2.0 <2.0 - 1 - 1
2.20 (75 09 2) Mass Ibs <0.017 <0.017 - 1 - -
1,1,2,2-tetrachloroethane Concentration µg/L <2.0 <2.0 - 1 - 1
2.21 ❑ El(79-34-5) Mass lbs <0.017 <0.017 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 13

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Daily of Term of
D(eq uiced) ifavailabe) Discharge Analyses AValuee Analyses
r (if available)
2.22 Tetrachloroethylene Concentration µg/L <2.0 <2.0 - 1 - -
-
(127-18-4) Mass Ibs <0.017 <0.017 - 1 - -
Toluene Concentration µ 1
g/L <1.0 <1.0 - -
2.23 -
(108-88-3) Mass Ibs <0.009 <0.009 - 1 - -
2 24 1,2-trans-dichloroethylene Concentration µg/L <2.0 <2.0 - 1D CI
- -
(156-60-5) ✓ Mass lbs <0.017 <0.017 - 1 - -
2.25 1,1,1-trichloroethane Concentration p.g/L <2.0 <2.0 - 1 - -
l El
(71-55-6) ✓ ✓ Mass lbs <0.017 <0.017 - 1 - -
2.26 1 1,2-trichloroethane Concentration µg/L <2.0 <2.0 - 1 - -
El 0
(79-00-5) ✓ Mass lbs <0.017 <0.017 - 1 - -
2.27 Trichloroethylene Concentration µg/L <2.0 <2.0 - 1 - -
(79-01-6) Mass lbs <0.017 <0.017 - 1 - -
2.28 Vinyl chloride Concentration µg/L <2.0 <2.0 - 1 -El
-
(75-01-4) ✓ ✓ Mass Ibs <0.017 <0.017 - 1 - -
Section 3.Organic Toxic Pollutants(GCIMS Fraction-Acid Compounds)
3.1 2-chlorophenol Concentration µg/L <20.8 <20.8 - 1 -1 El
-
(95 57 8) ✓ ✓ Mass lbs <0.177 <0.177 - 1 - -
3.2 2,4-dichlorophenol Concentration µg/L <20.8 <20.8 - 1 - -
El El El
(120-83-2) Mass lbs <0.177 <0.177 - 1 - -
2,4-dimethylphenol Concentration µg/L <41.7 <41.7 - 1 - -
3.3 (105 67 9) Mass lbs <0.355 <0.355 - 1 - -
3.4 4,6-dinitro-o-cresol Concentration µg/L <41.7 <41.7 - 1 - -
El El El
(534 52 1) Mass lbs <0.355 <0.355 - 1 - -
3.5 2,4-dinitrophenol ® Concentration - - - - -
III 0
(51 28 5) Mass - - - -
EPA Form 3510-2C(Revised 3-19) Page 14

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) (if available) Value
3.6 2-nitrophenol Concentration µg/L <20.8 <20.8 - 1 - -
(88-75-5) Mass lbs <0.177 <0.177 - 1 - -
4-nitrophenol Concentration µg/L <41.7 <41.7 - 1 - -
3.7 (100-02-7) Mass lbs <0.355 <0.355 - 1 - -
3 8 p-chloro-m-cresol Concentration µg/L <20.8 <20.8 - 1 - -
(59-50-7) Mass lbs <0.177 <0.177 - 1 - -
3 9 Pentachlorophenol Concentration µg/L <41.7 <41.7 - 1 - -
(87-86-5) Mass lbs <0.355 <0.355 - 1 - -
Phenol Concentration µg/L <20.8 <20.8 - 1 - -
3.10 (108-95-2) Mass lbs <0.177 <0.177 - 1 - -
2,4,6-trichlorophenol Concentration µg/L <41.7 <41.7 - 1 - -
3.11 (88 05 2) Mass lbs <0.355 <0.355 - 1 - -
Section 4.Organic Toxic Pollutants(GC/MS Fraction-Base/Neutral Compounds)
Acenaphthene Concentration µg/L <20.8 <20.8 - 1 - -
4.1 (83-32-9) Mass lbs <0.177 <0.177 - 1 - -
4 2 Acenaphthylene L 0 Concentration µg/L <20.8 <20.8 - 1 - -
(208-96-8) Mass lbs <0.177 <0.177 - 1 - -
4.3 Anthracene Concentration µg/L <20.8 <20.8 - 1 - -
(120-12-7) Mass lbs <0.177 <0.177 - 1 - -
4.4 Benzidine Concentration µg/L <208 <208 - 1 - -
(92-87-5) Mass lbs <1.77 <1.77 - 1 - -
Benzo(a)anthracene Concentration µg/L <20.8 <20.8 - 1 - -
4.5 (56-55-3) Mass lbs <0.177 <0.177 - 1 - -
4.6 Benzo(a)pyrene 0 Concentration µg/L <20.8 <20.8 - 1 - -
0 ID
(50-32-8) Mass lbs <0.177 <0.177 - 1 - -
EPA Form 3510-20(Revised 3-19) Page 15

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001
OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) (if available) Value
4.7 3,4-benzofluoranthene ✓ Concentration µg/L <20.8 <20.8 - 1 - -
El
(205-99-2) ✓ Mass lbs <0.177 <0.177 - 1 - -
Benzo(ghi)perylene z Concentration µg/L <20.8 <20.8 - 1 - -
4.8 Ei El
(191-24-2) Mass lbs <0.177 <0.177 - 1 - -
Benzo(k)fluoranthene ri Concentration µg/L <20.8 <20.8 - 1 - -
4.9 El
(207-08-9) El
Mass lbs <0.177 <0.177 1 - -
4.10 Bis(2-chloroethoxy)methane 0 Concentration µg/L <41.7 <41.7 - 1 - -
(111-91-1) ✓ Mass lbs <0.355 <0.355 - 1 - -
4.11 Bis(2-chloroethyl)ether 0 Concentration µg/L <20.8 <20.8 - 1 -El Ill
-
(111-44-4) Mass lbs <0.177 <0.177 - 1 - -
4.12 Bis(2-chloroisopropyl)ether 0 Concentration µg/L <20.8 <20.8 - 1 - -
0 El
(102-80-1) Mass lbs <0.177 <0.177 - 1 - -
4.13 Bis(2-ethyihexyl)phthalate Concentration µg/L <20.8 <20.8 - 1 -El El El
-
(117-81-7) Mass lbs <0.177 <0.177 - 1 - -
4.14 4-bromophenyl phenyl ether Concentration µg/L <20.8 <20.8 - 1 -El El E
-
(101-55-3) Mass lbs <0.177 <0.177 - 1 - -
4.15 Butyl benzyl phthalate Concentration RA <20.8 <20.8 - 1 -E El
-
(85-68-7) Mass lbs <0.177 <0.177 - 1 - -
4.16 2-chloronaphthalene 0 Concentration µg/L <20.8 <20.8 - 1 -E El
-
(91-58-7) Mass lbs <0.177 <0.177 - 1 - -
4-chlorophenyl phenyl ether Concentration µg/L <20.8 <20.8 - 1 - -
4.17 El El E
(7005-72-3) Mass Ibs <0.177 <0.177 - 1 - -
Chrysene Concentration µg/L <20.8 <20.8 - 1 - -
4.18 El El I=1
(218-01-9) Mass lbs <0.177 <0.177 - 1 - -
4.19 Dibenzo(a,h)anthracene El Concentration µg/L <20.8 <20.8 - 1 - -
El El
(53-70-3) Mass lbs <0.177 <0.177 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 16

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05119
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence Intake
(check one) Effluent (optional)
Pollutant/Parameter Testing Units 1 Long-Term Long-
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number g Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available)
4.20 1,2-dichlorobenzene 0 Concentration µg/L <20.8 <20.8 - 1 - -
El
(95-50-1) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.21 1,3-dichlorobenzene ❑ Concentration µg/L <20.8 <20.8 - 1 - -
CI
(541-73-1) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.22 1,4-dichlorobenzene Concentration mil <20.8 <20.8 - 1 - -
0 El
(106-46-7) ✓ Mass Ibs <0.177 <0.177 - 1 - -
3,3-dichlorobenzidine Concentration µg/L <41.7 <41.7 - 1 - -
4.23 (91-94-1) Mass lbs <0.355 <0.355 - 1 - -
4.24 Diethyl phthalate ✓ Concentration µg/L <20.8 <20.8 - 1 - -
(84-66-2) Mass lbs <0.177 <0.177 - 1 - -
4.25 Dimethyl phthalate ✓� Concentration µg/L <20.8 <20.8 - 1 - -
(131-11-3) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.26 Di-n-butyl phthalate 0 Concentration µg/L <20.8 <20.8 - 1 - -
(84-74-2) Mass lbs <0.177 <0.177 - 1 - -
2 4-dinitrotoluene z Concentration µg/L <20.8 <20.8 - 1 - -
4.27 El D
(121-14-2) Mass lbs <0.177 <0.177 - 1 - -
4.28 2,6-dinitrotoluene ❑ Concentration µg/L <20.8 <20.8 - 1 - -
(606-20-2) ✓ Mass Ibs <0.177 <0.177 - 1 - -
Di-n-octyl phthalate z Concentration µg/L <20.8 <20.8 - 1 - -
4.29 (117-84-0) Mass Ibs <0.177 <0.177 - 1 - -
4.30 1,2-Diphenylhydrazine ❑ Concentration µg/L <20.8 <20.8 - 1 - -
(as azobenzene)(122-66-7) Mass Ibs <0.177 <0.177 - 1 - -
4.31 Fluoranthene ❑ Concentration µg/L <20.8 <20.8 - 1 - -
(206-44-0) ✓ Mass lbs <0.177 <0.177 - 1 - -
4.32 Fluorene EI Concentration µg/L <20.8 <20.8 - 1 -1=1 Ell
-
(86-73-7) Mass lbs <0.177 <0.177 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 17

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Daily Monthly Term
Present Absent Daily of of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available)
4.33 Hexachlorobenzene Concentration µg/L <20.8 <20.8 - 1 - -
✓ 0 ✓
(118-74-1) Mass lbs <0.177 <0.177 - 1 - -
Hexachlorobutadiene Concentration Pei- <20.8 <20.8 -
4.34 1 - -
(87-68-3) ✓ ✓ Mass lbs <0.177 <0.177 - 1 - -
4.35 Hexachlorocyclopentadiene ❑✓ ❑ Concentration µg/L <41.7 <41.7 1 - -
(77-47-4) Mass Ibs <0.355 <0.355 - 1 - -
4.36 Hexachloroethane Concentration HA <20.8 <20.8 - 1 - -
El ✓
(67-72-1) Mass lbs <0.177 <0.177 - 1 - -
4.37 Indeno(1,2,3-cd)pyrene � Concentration µg/L <20.8 <20.8 - 1 - -
(193-39-5) ✓ ✓ Mass Ibs <0.177 <0.177 - 1 - -
4.38 lsophorone � ❑ ❑ Concentration µg/L <41.7 <41.7 - 1 - -
(78 59 1) ✓ Mass Ibs <0.355 <0.355 - 1 - -
4.39 Naphthalene Concentration µg/L <20.8 <20.8 - 1 - -
(91-20-3) ✓ ✓ Mass Ibs <0.177 <0.177 - 1 - -
4.40 Nitrobenzene Concentration µg/L <20.8 <20.8 - 1 - -
(98 95 3) ✓ ✓ Mass lbs <0.177 <0.177 - 1 - -
4.41 N-nitrosodimethylamine Concentration µg/L <20.8 <20.8 - 1 -CI
-
(62-75-9) ✓ ✓ Mass lbs <0.177 <0.177 - 1 - -
4.42 N-nitrosodi-n-propylamine Concentration µg/L <20.8 <20.8 - 1 - -
CI
(621-64-7) ✓ ✓ Mass Ibs <0.177 <0.177 - 1 - -
4.43 N-nitrosodiphenylamine Concentration µg/L <41.7 <41.7 - 1 - -
✓ CI ✓
(86-30-6) Mass lbs <0.355 <0.355 - 1 - -
4.44 Phenanthrene Concentration µg/L <20.8 <20.8 - 1 - -
CI
(85-01-8) ✓ ✓ Mass lbs <0.177 <0.177 - 1 - -
4.45 Pyrene ❑ Concentration µg/L <20.8 <20.8 - 1 - -
(129-00-0) ✓ Mass lbs <0.177 <0.177 - 1 - -
EPA Form 3510-2C(Revised 3-19) Page 18

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal, LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))1
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge
Discharge Analyses AverageValue Analyses
(required) ) (if available)
4.46 1 2 4-trichlorobenzene ❑ 0 ❑ Concentration µg/L <20.8 <20.8 - 1 - 1
(120-82-1) Mass lbs <0.177 <0.177 - 1 - -
Section 5.Organic Toxic Pollutants(GC/MS Fraction—Pesticides) _
Aldrin Concentration SEE NARRATIVE - - - - -
5.1 (309-00-2) ❑ ❑ ❑ Mass -- - - - - -
a-BHC Concentration - - - - - - -
5.2 (319-84-6) 0 0 El Mass -
-
Q-BHC Concentration - - - - - - -
5.3 (319-85-7) 0 0 ❑ Mass
-
-
-
y-BHC Concentration - - - - - - -
5.4 (58-89-9) ❑ ❑ Mass - - - - - - -
5-BHC 0
❑ Concentration - - - - - - -
5.5 (319-86-8) El Mass - -
5.6 Chlordane 0
❑ ❑ Concentration - - - - - - -
(57-74-9) Mass - - - - - - -
4 4'-DDT ❑ ❑ ❑ Concentration - - - - - - -
5.7 (50-29-3) Mass - - -
5.8 4,4'-DDE 0 0 0 Concentration - - - - - - -
(72-55-9) Mass - - - - - - -
4,4'-DDD ❑ ❑ ❑ Concentration - - - - - - -
5.9 (72-54-8) Mass - - -
5.10 Dieldrin ❑ ❑ ❑ Concentration - - - - - - -
(60-57-1) Mass - - - - - - -
5.11 a-endosulfan 0 0
0 Concentration - - - - - - -
(115-29-7) Mass - - - - - - -
EPA Form 3510-2C(Revised 3-19) Page 19

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001
OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CF' 122.21(g)(7)(v))1
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Dailischargey of Term of
D(eg fired) (if available) Discharge Analyses AverageValue Analyses
r (if available)
(3-endosulfan Concentration - - - - - - -
5.12 (115-29-7) 0 El 0 Mass - - - - - - -
5.13 Endosulfan sulfate Concentration - - - -
l 0 El
(1031-07-8) ✓ Mass - - - - - - -
5.14 Endrin r� Concentration - - - - - - -
0 El
(72-20-8) Mass - - - - - - -
5.15 Endrin aldehyde 0 Concentration - - - - - -0 El
-
(7421-93-4) Mass - _ - - - - - -
5.16 Heptachlor 0 Concentration - - - - - - -
(76-44-8) Mass - - - - - - -
Heptachlor epoxide 0 Concentration - - - - - - -
5.17 (1024-57-3) ElEl
- - - - - - -
Mass
PCB-1242 Concentration - - - - - - -
5.18 (53469-21-9) 0 Mass - - - - - - -
PCB-1254 Concentration - - - - - - -
5.19 (11097-69-1) ❑ ❑ 0 Mass - - - -
PCB-1221 Concentration - - - - - - -
5.20 (11104-28-2) 0
0 - - - - -
Mass
PCB-1232 Concentration - - - - - - -
5.21 (11141-16-5) Mass
PCB-1248 Concentration - - - - - - -
5.22 (12672-29-6) 0 Mass
PCB-1260 Concentration - - - - - - -
5.23 (11096-82-5) El 0 0 - - _ - - -
Mass
PCB-1016 Concentration - - - - - - -
5.24 (12674-11-2) 0 0 0 Mass - - - - - - -
EPA Form 3510-2C(Revised 3-19) Page 20

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal, LLC 001 OMB No.2040-0004
TABLE B.TOXIC METALS,CYANIDE,TOTAL PHENOLS,AND ORGANIC TOXIC POLLUTANTS(40 CFR 122.21(g)(7)(v))l
Presence or Absence
(check one) Effluent Intake
(optional)
Pollutant/Parameter Testing Units Long-Term
(and CAS Number,if available) Required Believed Believed (specify) Maximum Maximum Average Number Long- Number
Present Absent Daily Monthly Daily of Term of
Discharge Discharge Discharge Analyses Average Analyses
(required) (if available) Value
(if available)
Toxaphene Concentration - - - - - - -
5.25 (8001-35-2) ❑ ❑ E Mass -
-
1 Sampling shall be conducted according to sufficiently sensitive test procedures(i.e.,methods)approved under 40 CFR 136 for the analysis of pollutants or pollutant parameters or
required under 40 CFR chapter I,subchapter N or 0.See instructions and 40 CFR 122.21(e)(3).
EPA Form 3510-2C(Revised 3-19) Page 21

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
TABLE C.CERTAIN CONVENTIONAL AND NON CONVENTIONAL POLLUTANTS(40 CFR 122.21(g)(7)(vi))1
Presence or Absence Intake
(check one) Effluent (Optional)
Units •
Pollutant Maximum Long-Term
Believed Believed (specify) Maximum Daily Long-Term
Present Absent Discharge Monthly Average Daily Number of Average Number of
Discharge Discharge Analyses Analyses
(required) Value
(if available) (if available)
❑ Check here if you believe all pollutants on Table C to be present in your discharge from the noted outfall.You need not complete the"Presence or Absence"column of Table C for
each pollutant.
❑ Check here if you believe all pollutants on Table C to be absent in your discharge from the noted outfall.You need not complete the"Presence or Absence"column of Table C for
each pollutant.
1 Bromide ❑ ✓ Concentration - - - - - -
(24959-67-9) Mass - - - - - - -
Chlorine,total Concentration µ9/L <10 <10 - 1 - -
2. residual Mass lb 0.086 0.086 - 1 - -
Concentration - - - - - - -
3. Color 0 El Mass
Concentration - - - - - - -
4. Fecal coliform ❑ 0 Mass
5 Fluoride El ❑ Concentration mg/L 9.2 9.2 <0.1 9 - -
(16984-48-8) Mass lbs 65.04 69.18 <0.73 9 - -
Concentration mg/L 0.61 0.61 - 1 - -
6 Nitrate-nitrite 0 ❑ Mass lbs 5.19 5.19 1
7 Nitrogen,total ❑ ❑ Concentration mg/L 1.5 1.5 - 1 - -
organic(as N) Mass Ibs 12.89 12.89 - 1 - -
Concentration mg/L <4.9 <4.9 - 1 - -
8. Oil and grease El 0 Mass lbs <41.7 <41.7 - 1 - -
g Phosphorus(as 0 ❑ Concentration mg/L 19 19 6.6 3 - -
P),total(7723-14-0) Mass Ibs 164 164 46.8 3 - -
10. Sulfate(as SO4) 0 0 Concentration g/L 12.5 12.5 5.3 740 - -
(14808-79-8) Mass lbs 72,733 72,733 37,265 740 - -
Concentration - N/A See Narrative - - - -
11. Sulfide(as S) 0 El _Mass
EPA Form 3510-2C(Revised 3-19) Page 23

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
TABLE C.CERTAIN CONVENTIONAL AND NON CONVENTIONAL POLLUTANTS(40 CFR 122.21(g)(7)(vi))1
Presence or Absence
(check one) Effluent Intake
(Optional)
Units
Pollutant Maximum Long-Term
Believed Believed (specify) Maximum Daily Long-Term
Present Absent Discharge Monthly Average Daily Number of Average Number of
Discharge Discharge Analyses Analyses
(required) Value
(if available) (if available)
12. Sulfite(as SO3) ❑ 0 Concentration - - - - - - -
(14265-45-3) Mass - - - - - - -
Concentration - N/A See Narrative - - - -
13. Surfactants El El Mass
14. Aluminum,total ✓ Concentration mg/L 0.276 0.276 0.118 9 - -
(7429-90-5) Mass lbs 2.075 2.075 0.859 9 - -
15. Barium,total Concentration - - - - - - -
(7440-39-3) Mass - - - - - - -
16. Boron,total ❑ 0 Concentration - - - - - - -
(7440-42-8) Mass - - - - - - -
17 Cobalt,total Concentration mg/L <0.04 <0.04 <0.005 1 - -
(7440-48-4) Mass lbs <0.46 <0.32 <0.04 1 - -
18 Iron,total ❑ El
Concentration mg/L 0.154 0.154 0.017 9 - -
(7439-89-6) Mass lbs 1.322 1.197 0.125 9 - -
19. Magnesium,total ❑✓ ❑ Concentration mg/L 1,071 1,071 577 740 - -
(7439-95-4) Mass lbs 8,939 8,938 4,072 740 - -
Molybdenum, Concentration µg/L 949 949 30 740 - -
20. total 0 0(7439 98 7) Mass lbs 7.1 7.1 0.2 740 - -
-
21 Manganese,total 0 0 Concentration mg/L 724 724 83 740 -
(7439-96-5) Mass lbs 4,209 4,209 582 740 - -
22. Tin,totalEl El Concentration mg/L <0.005 - <0.005 <0.005 1
(7440-31-5) Mass lbs <0.58 <0.40 <0.04 1 - -
23. Titanium,total 0 ✓ Concentration - - - - - - -
(7440-32-6) Mass - - - - - - -
EPA Form 3510-2C(Revised 3-19) Page 24

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC OMB No.2040-0004
TABLE C.CERTAIN CONVENTIONAL AND NON CONVENTIONAL POLLUTANTS(40 CFR 122.21(g)(7)(vi))1
Presence or Absence Intake
(check one) Effluent (Optional)
Units
Pollutant Maximum Long-Term Long-Term
Believed Believed (specify) Maximum Daily Monthly Average Daily Number of Number of
Present Absent Discharge Discharge Discharge Analyses Average Analyses
(required) Value
(if available) (if available)
24. Radioactivity
Alpha,total Concentration - - - - - - -
Mass - - - - - - -
Beta,total ❑ ❑ Concentration - - - - - - -
Mass - - - - - - -
Concentration - - - - - - -
Radium,total ❑ 2Mass
-
- - -
Radium 226,total ❑ 0 Concentration
Mass - - - - - - -
1 Sampling shall be conducted according to sufficiently sensitive test procedures(i.e.,methods)approved under 40 CFR 136 for the analysis of pollutants or pollutant parameters or
required under 40 CFR chapter I,subchapter N or 0.See instructions and 40 CFR 122.21(e)(3).
EPA Form 3510-2C(Revised 3-19) Page 25
I

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE D.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))1
Presence or Absence
Pollutant (check one) Reason Pollutant Believed Present in Discharge Available Quantitative Data
Believed Believed (specify units)
Present Absent
1. Asbestos ❑ 0 - -
2. Acetaldehyde 0 0 - -
3. Allyl alcohol 0 0 - -
4. Allyl chloride 0 0 - -
5. Amyl acetate 0 0 -
6. Aniline 0 0 -
7. Benzonitrile ❑ 0 - -
8. Benzyl chloride ❑ 0 - -
9. Butyl acetate 0 0 - -
10. Butylamine 0 0 - -
11. Captan 0 0 -
12. Carbaryl 0 ✓❑ - -
13. Carbofuran ❑ 0 -
14. Carbon disulfide ❑ 0 - -
15. Chlorpyrifos ❑ 0 - -
16. Coumaphos ❑ 0 -
17. Cresol ❑ 0 - -
18. Crotonaldehyde ❑ 0 - -
19. Cyclohexane ❑ 0 - -
EPA Form 3510-2C(Revised 3-19) Page 27

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE D.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))l
Presence or Absence
Pollutant (check one) Available Quantitative Data
Believed Believed Reason Pollutant Believed Present in Discharge (specify units)
Present Absent
20. 2,4-D(2,4-dichlorophenoxyacetic acid) El 0 -
21. Diazinon El ✓❑ - -
22. Dicamba El El - -
23. Dichlobenil ❑ ❑✓ - -
24. Dichlone ❑ ❑✓ - -
25. 2,2-dichloropropionic acid ❑ ❑✓ - -
26. Dichlorvos ❑ ❑✓ - -
27. Diethyl amine ❑ CI - -
28. Dimethyl amine ❑ 0 - -
29. Dintrobenzene ❑ ❑✓ - -
30. Diquat ❑ 0 - -
31. Disulfoton ❑ ✓❑ - -
32. Diuron ❑ ❑✓ - -
33. Epichlorohydrin ❑ ❑✓ - -
34. Ethion ❑ ❑✓ - -
35. Ethylene diamine ❑ ❑✓ - -
36. Ethylene dibromide ❑ ✓❑ - -
37. Formaldehyde ❑ CI - -
38. Furfural ❑ ❑✓ - -
EPA Form 3510-2C(Revised 3-19) Page 28 I
i

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC ow. OMB No.2040-0004
TABLE D.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))1
Presence or Absence
Pollutant (check one) Available Quantitative Data
Believed Believed Reason Pollutant Believed Present in Discharge (specify units)
Present Absent
39. Guthion ❑ 0 - -
40. Isoprene 0 0 - -
41. Isopropanolamine 0 0 - -
42. Kelthane 0 0 - -
43. Kepone 0 El - -
44. Malathion 0 0 - -
45. Mercaptodimethur 0 0 - -
46. Methoxychlor 0 0 - -
47. Methyl mercaptan 0 0 - -
48. Methyl methacrylate 0 0 - -
49. Methyl parathion 0 0 - -
50. Mevinphos 0 0 - -
51. Mexacarbate 0 0 - -
52. Monoethyl amine 0 0 - -
53. Monomethyl amine 0 0 - -
54. Naled 0 0 - -
55. Naphthenic acid 0 0 - -
56. Nitrotoluene 0 0 - -
57. Parathion 0 0 - -
EPA Form 3510-2C(Revised 3-19) Page 29

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE D.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))1
Presence or Absence
Pollutant (check one) Available Quantitative Data
Believed Believed Reason Pollutant Believed Present in Discharge (specify units)
Present Absent
58. Phenolsulfonate ❑ 0 -
59. Phosgene 0 0 -
60. Propargite ❑ El - -
61. Propylene oxide ❑ 0 - -
62. Pyrethrins 0 El - -
63. Quinoline ❑ 0 - -
64. Resorcinol ❑ 0 - -
65. Strontium ❑✓ ❑ Routine in-house analytical data(Max/Avg Daily Dis.:MDD/ADD) MDD:37 mg/L;ADD:3.9 mg/L
66. Strychnine ❑ 0 - -
67. Styrene ❑ 0 - -
68 2,4,5-T(2,4,5-trichlorophenoxyacetic ❑ 0 - -
acid)
69. TDE(tetrachlorodiphenyl ethane) ❑ ❑✓ - -
70. 2,4,5-TP[2-(2,4,5-trichlorophenoxy) ❑ 0 - -
propanoic acid]
71. Trichlorofon ❑ El - -
72. Triethanolamine ❑ 0 - -
73. Triethylamine ❑ 0 - -
74. Trimethylamine 0 0 - -
75. Uranium ❑ 0 - -
76. Vanadium ❑ 0 - -
EPA Form 3510-2C(Revised 3-19) Page 30

EPA Identification Number NPDES Permit Number Facility Name Outfall Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE D.CERTAIN HAZARDOUS SUBSTANCES AND ASBESTOS(40 CFR 12221(g)(7)(vii))l
Presence or Absence
Pollutant (check one) Reason Pollutant Believed Present in Discharge Available Quantitative Data
Believed Believed (specify units)
Present Absent
77. Vinyl acetate ❑ E - -
78. Xylene 0 I - -
79. Xylenol ❑ El -
80. Zirconium ❑ ❑✓ - -
t Sampling shall be conducted according to sufficiently sensitive test procedures(i.e.,methods)approved under 40 CFR 136 for the analysis of pollutants or pollutant parameters or
required under 40 CFR chapter I,subchapter N or 0.See instructions and 40 CFR 122.21(e)(3).
EPA Form 3510-2C(Revised 3-19) Page 31

This page intentionally left blank.

EPA Identification Number NPDES Permit Number Facility Name Duffel'Number Form Approved 03/05/19
NCR000159038 NC0089109 Befesa Zinc Metal,LLC 001 OMB No.2040-0004
TABLE E.2,3,7,8 TETRACHLORODIBENZO P DIOXIN(2,3,7,8 TCDD)(40 CFR 122.21(g)(7)(viii))
TCDD Presence or
Congeners Absence
Pollutant Used or (check one) Results of Screening Procedure
Believed Believed
Manufactured Present Absent
2,3,7,8-TCDD El El
EPA Form 3510-2C(Revised 3-19) Page 33

Form 2C:
Section 1 Attachments
OUTFALL LOCATION MAP

.,.,•\ -, -..• , tIlik,Iii ,.. :;,..--.,e;\ . lb i )16
. 's,''' ','. :0,: k „:„,., -„1, 7). ...v...1...,%:‘, ,,, 6 F .,,,. - i j A
iiii.) . ) E. ,,,:.: A .. . ..,,, L\L-1 x\ - -wir, ,w*::"Sretelt.-W) i
-;‘f--" --'::* ''r' . .1 '‘'T lrctikiget , i., etrirl,\\
1 . \'' .‘ e, ,,, ,:. ,.
,• , . 4 ,,, 4 ,
et,
\\\‘ ', 4' yti, c 1A-iiii,-1-va%ci) ,_,
. ,
4.• .
,,,
.--... .. ' ,1,., . \\,,,, ,s ,\ Ad . rrita
1 tk\ L,„. i ,i° AL.-,,,1-0%.* , - AIIII"`,1 ILLIA•sw)./1 .( N -
-7 '\'.7' .40P. illi •, tr LVI7
- -,_/H- ii...-- ----orra trif __ irkiklk\ii --. ,e_.,
,t,,,.--:- --,,, Ft .ii %iet .-,.,,_ ,11 .„, 1mi '1)
,...,.• , . ip,
. 'ftk N‘ill>6_
N't . /• '-1/ r-c- NS)411. , ,i1P0r71.7,,,\INVYrr Art-t....jItt,47,,w I.
/v `1 �a IQ► — ury off SCALE:1"=3000'
0_. yo.,' i N,y \ 7 i I : -�_k VIA
L'a., 1__L iiitiktianiti ,,7. Pit ‘. ,;;
.0 MN\
$,_\.__ _-7, •.1.... -...;..---.-...,
OU TFALL 001 ) Lr 4 A Arl,i.‘Nc.
jo0Av A-1i).".
, 0
:.-., i‘l,l..m0.m...,1.04.
o WASTEWATER AND , ". )Op
s 0 �.
.\%s--'1z,'iW,,i_:,‘A,,biu-i't',i-.'-„4---.ml'l
.iirC'-i20a,,ire7
,. STORMWATER ` • h �
RGE LOCATION �: ��
DISCHA __ ��>�7
---- ; .,.: (LATITUDE N 35° 12'2.65", � �I����,.,rir„ i; w &Air ,._`�:£LONGITUDE W 81°51'5")
'4/
%-%-imis ,,,„1 ,:i._..-.407A? .. ' AA to,,I..„ , filhs , - ::.1
-------- ----i-t- ----4 . - , e'' AirrIU. 4,--qr . )-p"•- 14.:z--\,-. ? 0,..;.:.4.4&___;;46,...,,..."-'0.
-7-------"----;-----)\ - ' Lc---71111014111111011Ainrsb-allillick-_—_-,‘‘ t i- 0-ii\AWZII„tilhff---iir-- --: diCire-41--1411VT- it4o.:
-.. .)- _--",i ----- 3, 1 VIIP-AairretIVTAIIIVO(44411";;ii(0 a # 8
,, N - LL-.\ pirc‘-,, .._ [ft itrelwa4 0 .,,,infrAto o )4-. ,, it
c„
' ' ' ' ' -IN . .*reirli:' Q\ e.-At\- - • . 4 rfc'\
1 . i'L'-) ' ------.V k(ts a_t?' ).1, 4,, 6) ..-T 7/ .•_,. %I'\5‘k,, 4i (g '4
71(-,,,: :.;.1, .Z,.PrIPIC?'„,--- ..,er(likinii•Arilk glikal'*(iii...°I. '31.*- - ji°' • "2:-* V°A .11, 6:k.:-\ _itt ) i
,, ..ok,_ ,..., .!(_-61-.4-..._
S4 ,, ,,-," . ...,,us- 1. fa S ik - 40" .---.'11.44' / / N \ - aVif ° Ni9 ItAt ql
-.1 - ' ;rd.Lk
\ '''.:‘,0--- ..\r.: - ' -.1! r '!- --(- ,A"-re,yir- 1,',0/0 F.,._, , .,.. , , ... L.
, , 0
,.._,,,„..._____ ,. _, A. .ki..,
• e0,0 _-II ,NORTH CAROLINA ,, I i,:, ► I i' o i'� SOUTH C — --_ -- ,' _ 4
AROLINA ( I
4-1
i,
' ;4001
.I •�I \~o / 1c,\ lay, Y O
4
-"/#1144451
-./, - I ,l-•• ii tioWlf ;Al I. Ili 0,.,,,,,
, ,f., . j Asi, . .. por U---44'1%.iii-\'' _, _A AP: .4
/ ' Y I. ''f-2 ..,,,,,,4_ -P-',.,-,," ),17-,A1 k .).V-- . \ -
rdik ImiN
- ' M fiks%1 Ir441MNiesioa
-----.... :.'1.-'":1'1/4,:,10%.1,1010/
vielivelairagrawNifmik
\ . , •wi-- , p_:,,,,...--ivi 0: .. 1:
FIGURE III-2
`285.6 II �►`A'" 0 DISCHARGE LOCATION MAP
':{ I '"jbII
RODUCTS
. ��:7 ,‘7
� � AMERICAN ZINC P __
�
�' r• - ---
• II pp !;�',:��.� • -I,.q :( I% RUTHERFORD COUNTY, NORTH CAROLINA
Inns orn1

Form 2C:
Section 2 Attachments
WATER PROCESS LINE DRAWING

r
Forest City Process Water
--I Water Suppy } Distribution
964,900 GPD /
/ 76,000 GPO 24,000 GPO 37,000 GPO 110,000 GPO 149,000 GPO
F
SX Reagents
)..
3,000 GPD P 4 LINT Reagents
Y
�5,000 GPD
/
Demin Water n
Distribution 371,000 GPD 1
Y w
194,400 GPD ; Solvent Reagents ,� PLINT �'►uINT Co-products
■ — * Extraction Preparation T— —� \ 18,000 GPD
Y \
A.
) Leaching "
n
Flow Sample point
44
meter
Leach Reagents Y r■■■
15,000 GPD '
Y ) Bleed Treatment •
Effluent to Outfall
A. N 980,000 GPD
■
Discretionary \
Bleed 40Co-products
Stormwater
63, 0 GPD
79,000 GPD}
/Electrowinning
Reagents
11,000 GPD
Admin 'V
Buildings
Y * Electrowinning —
r Utility
}, Wastewater
14,400 GPD
Forest City \
Pores Rutherford County Zinc Refinery —
3,500 GPD Water Balance Line Drawing Note—Units within the dotted line are process units

Form 2C:
Section 7 Attachments
ANALYTICAL MONITORING DATA SUMMARY
(MAXIMUM AND AVERAGE DISCHARGE VALUES HIGHLIGHTED)

TABLE 1: PROCESS EFFLUENT RESULTS SUMMARY (BEFESA MOM"
Daily Semi-Monthly Monthly
50050 50050 00400 01027 01051 01092 00530 01027 01051 10347 01092 00530 ` 00610 32011
FLOW FLOW E E
EFF 111 EFF 9 7 -6 u 2 13 TOu
u.1 INF ❑ INFO E a, E a) u Z �p -6
I- _ -6 _1 RI (I) J Z N N m + 'L
0 >„w dw Q U T 73
1- U @ E- z U 7
a 0 I- r O LL
q O t4 +O F-X 0 +� H
H H
MGD MGD SU mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L ' mg/L 1 mg/L mg/L j mg/L
8/16/2022 1.049 0.957 8.1 0 0 0.0328 6 0.0209 0 0 0.0572 8.8
7/11/2022 0.953 0.820 8.1 0.037 0.0092 0.031 23.4 0.0445 <0.025 <0.02 0.0967 38.4 0.74 <0.01 9.0
6/8/2022 0.806 0.860 7.8 0.036 <0.025 0.0059 22.1 0.052 <0.025 <0.02 0.0327 20.5
5/3/2022 1.009 0.897 7.9 0.09 <0.025 <0.25 12.1 0.042 0.039 0.0099 <0.01 16.0
4/4/2022 0.847 0.901 6.44 0.014 0.03 <0.1 8 0.025 0.0091 0.0161 0.0964 19.2 <0.1 <0.01 9.2
3/1/2022 0.926 0.932 7.90 0.097 0.02 0.319 25.0 0.01 0.025 0.0209 0.0311 23.4
2/8/2022 0.908 0.940 8.34 0.019 0.0096 0.075 26.8 0.015 0.026 0.0088 <0.01 11.6
1/10/2022 1.029 0.931 8.20 0.011 0.028 <0.01 30.4 0.0633 <0.025 0.0634 0.183 29.2 0.27 <0.01 <0.1
12/14/2021 1.000 0.949 8.33 0.094 0.036 0.3 56.7 0.03 0.031 0.0446 0.0823 39.5
11/2/2021 0.769 0.830 8.28 0.0271 0.0097 0.0782 55.0 0.034 0.0084 0.0231 0.239 44
10/4/2021 1.003 0.850 8.00 0.061 0.016 0.25 38.7 0.039 0.024 0.041 0.243 18.7 0.11 <0.010 <0.1C
_ 9/14/2021 1.003 0.850 7.80 0.071 0.024 0.17 29.3 0.0124 0.021 0.029 0.373 30.0
8/15/2021 0.868 0.900 7.50 0.037 0.016 0.091 16.2 0.006 0.027 0.0232 0.442 16.2
7/6/2021 1.185 0.900 7.60 0.029 0.028 0.192 19.2 0.014 0.014 0.0082 0.049 48.7 0.81 <0.01 <0.1
6/3/2021 0.903 0.860 7.10 0.04 0.013 0.13 23.5 0.0148 <0.01 0.0158 <0.1 19
_ 5/4/2021 0.818 0.850 7.60 0.033 0.013 0.0879 41.9 0.065 0.039 0.0061 0.32 8.8
4/5/2021 0.759 0.773 7.20 0.015 0.017 0.108 5.3 0.018 0.016 0.0081 0.081 25.1 <0.1 <0.01 <0.1
3/2/2021 0.975 0.850 7.40 0.029 0.021 0.14 10.2 0.021 0.017 0.0261 0.181 6.7
2/2/2021 0.866 0.820 7.30 0.0914 <0.005 0.155 11 0.038 0.0081 0.0094 0.142 6.3
1/5/2021 0.850 0.830 7.20 0.057 0.0072 0.21 15.3 0.011 0.0055 0.0099 0.0985 4.3 <0.1 <0.01 <0.1
12/2/2020 0.730 0.790 7.20 0.011 0.0064 0.16 _ 9.2 0.048 0.0093 0.01 0.308 5.9
11/5/2020 0.579 0.820 6.90 0.016 0.011 0.089 12.8 0.130 0.017 0.02 0.630 4.7
10/6/2020 0.840 0.800 7.00 0.04 0.0078 0.069 10.6 0.021 0.017 0.022 0.22 20.1 <0.10 <0.01 <0.1C
9/1/2020 0.434 , 0.71 7.3 0.022 0.0088 0.09 11.1 0.041 <0.005 0.033 0.063 28.8
8/5/2020 0.424 0.74 7.2 0.023 <0.005 0.04 _ 6.6 0.03 <0.005 0.013 0.033 16.3
7/6/2020 0.652 0.66 7.4 0.016 <0.005 0.011 19.1 0.09 <0.005 0.009 0.05 11.9 0.7 <0.025 0.3
6/9/2020 0.519 0.60 6.9 0.044 <0.005 0.031 11 0.05 <0.005 0.011 0.048 25.1 ,
Minimum Discharge 0.424 0.773 6.44 0.000 0.000 0.0059 4.3 0.000 0.000 0.000 0.006 4.3 <0.1 <0.01 <0.1

TABLE 2: ROUTINE IN-HOUSE MONITORING
Long-term Long-term
Maximum Daily Average Daily Maximum Daily Average Daily
Effluent Parameter Conc.Units Discharge _ Discharge Mass Units Discharge Discharge
Magnesium,total mg/L 1,071 577 lbs/day 8,938 4,072
Molybdenum,total µg/L 949 30 lbs/day 7.1 0.2
Manganese,total mg/L 724 83 lbs/day 4,209 582
Strontium,total mg/L 37 4 lbs/day 265 27
Sulfate(as SO4) g/L 12.5 5.3 lbs/day 72,723 37,265
Magnesium,total Molybdenum,total Manganese,total Strontium,total Sulfate(as 504) Flow Rate(gpm) Flow Rate(MGD);, Magnesii
5P330 5P330 SP330 SP330 SP330 FIC_3032 FIC_3032 SP;
Effluent Tank Effluent Tank Effluent Tank Effluent Tank Effluent Tank Effluent Flow Effluent Flow Effluer
mg/L µg/L mg/L mg/L g/L gpm MGD MI
Max.Daily Discharge 1,071 949 724 37 12.5 967 1.393 Avg.Daily Discharge

Appendix 1 :
Cadmium Compliance Schedule Removal
COMPLIANCE EVALUATION AND JUSTIFCATION

Cadmium Compliance Schedule
Preliminary Engineering Report - Removal Request
Befesa Zinc Metal, LLC
484 Hicks Grove Road
Mooresboro, North Carolina 28114
November 2022
Prepared For
Befesa Zinc Metal, LLC
laCt/C-Al
Scott Menniti, P.E. `�� D Curry
Senior Project Engineer Project Development Coordinator
TRC Environmental Corporation /Befesa Zinc Metal
Cadmium Compliance Schedule
Preliminary Engineering Report
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50 INTERNATIONAL DRIVE,SUITE 150,GREENVILLE,SC 29615,•864.281.0030 PHONE•864.281.0288 FAx•WWW.TRCCOMPANIES.COM

Table of Contents
1. Introduction and Objectives 1
2. Regulatory and Permitting Overview 3
2.1 Monitoring Requirements and Effluent Limitations 3
2.2 Effluent Flow and Discharge 3
3. Conclusions 6
List of Tables
Table 1 Total Cadmium— Effluent Limits and Monitoring Results 1
Table 2 Total Cadmium— Effluent Limits and Monitoring Results 3
Table 3 Total Cadmium—Effluent Flow Monitoring Results 4
Table 4 Total Cadmium—Monitoring Results 5
TRC Environmental Corporation I Befesa Zinc Metal
Cadmium Compliance Schedule
Preliminary Engineering Report i November 2022
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Section 1
Introduction and Objectives
Befesa Zinc Metal, LLC (Befesa) (FormerlyAmerican Zinc Products as required bythepermit conditions), q
set forth by the North Carolina Department of Environmental Quality (NCDEQ) effluent discharge permit
(Permit NC0089109)for the Befesa Mooresboro, NC facility ("the facility"), is required to meet a
Cadmium Compliance Schedule (CCS)throughout the life of the permit term and beyond. Interim
Cadmium limits were added to the facilities discharge permit upon renewal in 2020 and modifications
included extensions added to the CCS set forth in Table 1 below:
Table 1
Total Cadmium—Effluent Limits and Monitoring Results
Activity Description Deadline
1. Commence production of Zinc at Mooresboro Facility. June 1, 2020
2. Ramp-up production to 75% December 1, 2020
3. Stabilize plant operation and commence evaluation of June 1, 2021
permit compliance.
4. Complete evaluation period. June 1, 2022
5. Prepare a Preliminary Engineering Report (PER) of process December 1, 2022
alternatives and/or pollution prevention/waste minimization (parallel with
alternatives designed to achieve compliance.This report activity 4)
would include the results of the compliance evaluation.
Submit to DWR for review and comment.
6. Agency review and addressing comments February 1, 2023
7. Bench scale test work of process alternatives (start in April 1, 2023
parallel with Activity 6).
8. Evaluate business case and funding requirements for April 1, 2023
technically suitable alternative(s). (parallel with
activity 7)
9. Complete pilot test work for selected technology option(s) August 1, 2023
and final technology selection. Develop a summary of the
results of this evaluation. Submit summary to DWR for
review.
10. Agency review and addressing comments October 1, 2023
11. Detailed engineering and design of selection option. Submit February 1, 2024
to DWR for comment
12. Agency review and addressing comments. April 1, 2024
TRC Environmental Corporation I Befesa Zinc Metal
Cadmium Compliance Schedule
Preliminary Engineering Report 1 November 2022
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Table 1
Total Cadmium—Effluent Limits and Monitoring Results
Activity Description Deadline
13. Prepare capital project application and secure funding for June 1, 2024
selected option, obtain building permits and all needed (much of this work
approvals for implementation. will be done in
parallel with
activities 11, 12)
14. Project implementation, including design completion, June 1, 2025
procurement, and construction.
15. Commission and ramp up. June 1, 2026
16. Stabilize operation and evaluate performance. December 1, 2026
17. Make necessary final modifications to optimize and obtain August 1, 2027
full operational status.
18. Achieve full compliance. December 1, 2027
The facility was approved in June 2020 to commence production of Zinc at the Mooresboro facility with
an initial ramp up in production expected to be 75% production capacity by December 2020. Following
the initial ramp up, Befesa was to begin an evaluation period for permit compliance with the cadmium
discharge limits through June 2022. The CCS evaluation period ended on June 1, 2022, with additional
activities required to be performed through December 1, 2027, as stated within the CCS. The next step
of the CCS, as required by the permit, is for the facility to prepare and submit for review and comment a
Preliminary Engineering Report (PER) of process alternatives and/or pollution prevention/waste
minimization alternatives to achieve future compliance standards. The PER is required to be completed
by December 2022.
Information provided within this permit renewal application includes effluent discharge monitoring data
provided in monthly discharge monitoring reports (DMRs) submitted to the Department for Outfall 001
since June 2020 (See Form 2C—Section 7 Attachments). Monitoring was performed in accordance with
permit requirements for analytical and monitoring of discharged effluent. This information reflects the
nature of effluent discharge water based on current operations and flows relating to the Total Cadmium
present in the discharge.
TRC Environmental Corporation I Befesa Zinc Metal
Cadmium Compliance Schedule
Preliminary Engineering Report 2 November 2022
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Section 2
Regulatory and Permitting Overview
2.1 Monitoring Requirements and Effluent Limitations
The next required step of the CCS is to prepare a Preliminary Engineering Report(PER) of process
alternatives and/or pollution prevention/waste minimization alternatives to achieve future compliance
standards. Under the current permit,the facility has an interim monthly average discharge limit for
Total Cadmium of 350.0 µg/L with a daily maximum of 2,143.00 µg/L. Final limits established by the
permit indicate that concentration limits are to be reduced to a monthly average of 90.4 µg/L with a
daily maximum of 454.4 µg/L when ramp up of production is complete.
Table 2
Total Cadmium—Effluent Limits and Monitoring Results
Effluent Characteristics Monthly Average Daily Maximum Measurement Frequency
Interim
350.0 pg/L 2,143.00 pg/L BI-WEEKLY
Total Cadmium Limit
Final
90.4 pg/L 454.4 pg/L BI-WEEKLY
Total Cadmium Limit
Monitoring results
Total Cadmium 37.9 pg/L 130.0 pg/L BI-WEEKLY
As shown on Table 2 above, monitoring results indicate that the facility is meeting not only the current
interim effluent discharge limits, but also the final limits proposed for a 75% production rate (per
activity 2 of the CCS). The facility has attained this discharge while at a 97%total production rate. The
effluent discharge monitoring data represents Outfall 001 since June 2020. Additional monitoring data
may be reviewed within Form 2C—Section 7 Attachments of the permit application.
2.2 Effluent Flow and Discharge
Currently,the facility has reached 97%of its production capacity. The permit limits process flow to a
monthly average of 0.98 MGD. The daily maximum flow to date has been 1.393 million gallons a day
(MGD). The facility is currently experiencing an average monthly discharge 0.875 MGD, 89% of the
permitted limit.
TRC Environmental Corporation /Befesa Zinc Metal
Cadmium Compliance Schedule
Preliminary Engineering Report 3 November 2022
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Table 3
Total Cadmium—Effluent Flow Monitoring Results
Effluent Characteristics Monthly Average Daily Maximum Measurement Frequency
Flow Limit 0.98 MGD N/A Continuous
Flow Monitoring Results 0.875 MGD 1.393 MGD Continuous
There are two additional process flow ramp ups activities scheduled as part of the CCS, however the
facility has limited capacity for further ramp up of its production process. Flow data indicates that the
facility now averages less than the permitted flow requirements, at cadmium concentrations lower than
required and is near maximum production capacity, with limited production increases planned in the
future.
As expressed in the NPDES permit issued on June 9, 2020, Permit No. NC0089109,the facility is required
to meet interim Total Cadmium limits with final limits expressed in the permit as ramp up of the facility
occurs over the permit term, see Table 2 above. As part of the permit,the facility is required to meet a
CCS in order to achieve compliance with final limits. The facility monitoring results, since June 2020,
indicate monthly averages and daily maximum levels of total cadmium in the discharge are consistently
below the final effluent limits. See Table 4 on the following page for sampling results over the permit
term.
TRC Environmental Corporation /Refesa Zinc Metal
Cadmium Compliance Schedule
Preliminary Engineering Report 4 November 2022
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Table 4
Total Cadmium-Monitoring Results
Sample Period* Semi-monthly Sample Resultsl Monthly Average
Results'
Total Cadmium Daily Total Cadmium DAILY Cadmium Monthly Avg.
(mg/L) (mg/L) (mg/L)
Final Limit 0.4544 0.4544 .0904
Aug-22 0 0.021 0.021
Jul-22 0.037 0.045 0.041
Jun-22 0.036 0.052 0.044
May-22 0.09 0.042 0.066
Apr-22 0.014 0.025 0.0195
Mar-22 0.097 0.01 0.0535
Feb-22 0.019 0.015 0.0170
Jan-22 0.011 0.0633 0.0372
Dec-21 0.094 0.03 0.0620
Nov-21 0.0271 0.034 0.0306
Oct-21 0.061 0.039 0.0500
Sep-21 0.071 0.0124 0.0417
Aug-21 0.029 0.014 0.0215
Jul-21 0.029 0.014 0.0215
Jun-21 0.04 0.0148 0.0274
May-21 0.033 0.065 0.0490
Apr-21 0.015 0.018 0.0165
Mar-21 0.029 0.021 0.0250
Feb-21 0.0914 0.038 0.0647
Jan-21 0.057 0.011 0.0340
Dec-20 0.011 0.048 0.0295
Nov-20 0.016 0.13 0.0730
Oct-20 0.04 0.021 0.0305
Sep-20 0.022 0.041 0.0315
Aug-20 0.023 0.03 0.0265
Jul-20 0.016 0.09 0.0530
Jun-20 0.044 0.05 0.0470
Total Cadmium Min 0.0010 mg/L
Total Cadmium Average 0.0379 mg/L
Total Cadmium Max 0.1300 mg/L
Notes:
1. Cadmium Sample Results are taken on a semi-monthly basis
2. Total min/max/average values shown are based respectively for both monthly samples
TRC Environmental Corporation l Befesa Zinc Metal
Cadmium Compliance Schedule
Preliminary Engineering Report 5 November 2022
\tGREENVILLE-FPI\WPGVLIPJT21488144100001ATTACHMENTS FOR NARRATIVE\APPENDIX 2 CD COMPLIANCE COMPLIANCE SCHEDULE 2022-11-17 SGM DAC.DOCX

Section 3
Conclusions
As described within the CCS,the facility shall evaluate process alternatives to achieve compliance with
permit limits. The facility is currently achieving compliance with the final effluent limits at current
production rates and is requesting removal of the future CCS requirements and removal of the CCS from
the renewed permit.
The daily maximum and monthly average of cadmium in the facility's discharge indicate a daily
maximum of 130 µg/L, well below final effluent limits daily maximum of 454.4 µg/L. The facility under
current operating conditions has an allowable discharge rate of 3.716 lbs/day of Cadmium utilizing its
maximum average monthly flow and future effluent limits. Considering the facility's current average
monthly discharge rate of 0.875 MGD and the lower average monthly cadmium discharge
concentrations of 90.4 µg/L, operations indicate that it may be feasible to request either a flow increase
to allow for further production or a release from additional compliance schedule requirements since
these parameters have routinely been achieved since the effective date of the current permit in 2020.
The facility process is a refining process where treatment units are inherent to its process and intended
for recovery of product rather than wastewater treatment intended to meet effluent guidelines. As part
of the CCS,the Preliminary Engineering Report is required to provide process alternatives or waste
minimization to achieve compliance while the facility increases flow to full production capacity. The
facility effluent monitoring indicates that additional process or minimization is not necessary to meet
permit requirements. Befesa is therefore requesting that no further action be required related to the
CCS and that it be removed from the permit upon renewal.
TRC Environmental Corporation l Befesa Zinc Metal
Cadmium Compliance Schedule
Preliminary Engineering Report 6 November 2022
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Appendix 2:
Fish Tissue Study
REPORT AND RESULTS

t 4
;,.„, c
Broad River NPDES Fish Tissue
Study Summary
American Zinc Products, LLC
Mooresboro, North Carolina
October 2022
111( (-21204g,
Heather Smith Robert W. Hanley, Ph.D.
Senior Biological Scientist Senior Consultant
TRC Environmental Corporation/American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary
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50 INTERNATIONAL DRIVE,SUITE 150,GREENVILLE,SC 29615,•864.281.0030 PHONE•864.281.0288 FAx•WWW.TR000MPANIES.COM

Table of Contents
1. Introduction
1
2. NPDES Permit Requirements 3
3. Project Overview 4
4. Summary of Fish Tissue Collection Efforts 5
5. Summary of Analytical Results 7
5.1 Upstream 7
5.2 Downstream 7
6. Conclusions 15
List of Tables
Table 1 Summary of Analytical Results for Fish Tissue Samples (Upstream) -- May 2022 9
Table 2 Summary of Analytical Results for Fish Tissue Samples (Downstream) -- May 2022 12
List of Figures
Figure 1 Site Location Map 2
Figure 2 Sample Location Map 6
List of Appendices
Appendix A AZR Revised Fish Sampling Plan 2020
Appendix B Broad River SOP—EA
Appendix C Broad River 2022 Technical Memorandum - EA
TRC Environmental Corporation I American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary i
\\GREENVILLE-FPI\WPGVL\PJT2\479013\DDOD\R4790130000-001_FINAL.DOCX October 2022

Section I
Introduction
Part 1, Condition A.(4) of National Pollutant Discharge Elimination System (NPDES) Permit NC0089109
issued to American Zinc Products (AZP), LLC, requires AZP to conduct fish tissue monitoring once during
the current permit cycle.. In response, AZP developed a fish sampling plan for their facility located in
Mooresboro, Rutherford County, North Carolina (Figure 1). The sampling plan was submitted to the
North Carolina Division of Water Resources (NCDWR) Water Quality Permitting Section and Water
Sciences Section for review and comment. Comments were addressed in a Revised Fish Tissue
Monitoring Plan (Plan) submitted to NCDWR on April 16, 2020, and approved on May 5, 2020. The
approved Plan is included as Attachment A to this report. The primary component of the Plan requires
collection of fish tissue for evaluation of arsenic, cadmium and zinc(i.e.,target metal) concentrations.
TRC Environmental Corporation (TRC) was contracted by AZP to advise, coordinate, and oversee
implementation of the Plan in accordance with the permit requirements. EA Engineering, Science, and
Technology, Inc., PBC (EA) performed the in-stream fish tissue collection efforts.
This report presents-results of the fish tissue sampling effort and the fish tissue analytical results to
satisfy requirements of the NPDES permit. Fish tissue sample collection efforts were conducted in the
Broad River, Rutherford County, NC,at locations upstream and downstream of AZP's permitted discharge
outfall in accordance with the NPDES requirements and the approved Plan..
TRC Environmental Corporation /American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary 1
\\GREENVILLE-FP1\WPGVL\PJT21479013\0000\R4 79 013 0000-001_FINAL.DOCX October 2022

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Section 2
NPDES Permit Requirements
The facility's modified NPDES Permit NC0089109 was signed on June 9, 2020, and effective on
July 1, 2020. The Permit expires on July 31, 2023.
NPDES Permit NC0089109, Part I, A. (4) stipulates fish tissue monitoring as follows:
A. (4.) FISH TISSUE MONITORING
[G. S. 143-215. 1(b)]
The facility shall conduct fish tissue monitoring once during the permit cycle and submit the
results with the NPDES permit renewal application. The objective of this monitoring is to
evaluate potential uptake of pollutants by fish tissue near the facility's discharge. The
parameters analyzed in fish tissue shall be arsenic, cadmium, and zinc. The monitoring shall be
conducted in accordance with the sampling plan approved by the Division. The plan should be
submitted to the Division within 180 days from the effective date of the permit modification.
TRC Environmental Corporation I American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary 3
\\GREENVILLE-FPI\WPGVL\PJT2\4790131o00DiR4790130000-001_FINAL.DOCX October 2022

Section 3
Project Overview
The primary objective of the fish tissue collection effort was to fulfill the NPDES permit fish tissue
monitoringcondition
ition requirement.
t. The q permit requires collection of fish tissue samples from two
locations (upstream and downstream of the AZP discharge point in the Broad River) for analysis of
arsenic, cadmium and zinc.
The upstream fish tissue sampling station is within North Carolina Stream Index Reach 9-(25.5)which is
classified bythe State to as WS IV. Class WS-IV waters are those used as sources of water supply
ppy for
drinking, culinary or food processing purposes where a WS-I, II, or III classification is not feasible. The
downstream fish tissue sampling station is within North Carolina Stream Index Reach 9-(36.5), which is
classified by the State as "C". Class C waters are those protected for uses such as aquatic life
propagation, survival and maintenance of biological integrity (including fishing and fish), wildlife,
secondary contact recreation, and agriculture.
The Broad River is a rocky,flashy, and swift waterbody capable of rapid changes in water flow and
depth. As such, site-specific sampling considerations were discussed in detail with the sampling team.
Prior to implementation of the tissue sampling program, EA developed a detailed Standard Operating
Procedures (SOP; April 2022) which integrated the NCDEQ approved Plan with site-specific
considerations and additional details of the sampling and analysis program implementation. TRC and
AZP reviewed the SOP for completeness and consistency with permit requirements prior to study
implementation. The SOP provided additional details on sample locations, sampling schedule, collection
methods, target species, sample processing and handling procedures and custody details. Attachment B
includes EA's Standard Operating Procedures(SOP)Standard Operating Procedures for NPDES Permit
(#NC0089109)Required Fish Tissue Collection(April 2022). EA obtained a Scientific Fish Collection License
(Permit Number 22-SFC00267)from the North Carolina Wildlife Resources Commission (NCWRC)that
specified the designated species, numbers of specimens, collection methods, and sampling locations.
g
A site reconnaissance was performed on March 22, 2022, to evaluate access points along the Broad
River study area. Both upstream and downs
tream access points were evaluated and identified during
the reconnaissance. AZP obtained landown
er permission for the
he reconnaissance access to evaluate
upstream and downstream access locations.
A sampling schedule was developed based on multiple site considerations including river stage. United
States Geological Survey(USGS) stream gaging Station 02151500,Broad River near Boiling Springs,
North Carolina, was utilized to monitor river stage and discharge conditions. AZP provided turbidity
readings to gauge water clarity during the sampling window. Sampling was conducted during May 2022
to target river levels and turbidity observations that would be optimal for sampling conditions.
TRC Environmental Corporation /American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary 4
\\GREENVILLE-FPI\WPGVL\PJT2\479013\0000\R4 7901 300 00-001_FINAL.DOL7C �- �^

Section 4
Summary of Fish Tissue Collection Efforts
Fish tissue sample collection was conducted from May 16 to May 22, 2022. Fish tissue samples were
collected from two locations on the Broad River, upstream and downstream of the AZP facility
(Figure 2). The upstream location extended from the Jack McKinney Road Bridge to approximately one
mile downstream of the bridge. The downstream location began near the Highway 221 Bridge and
extended approximately one mile downstream from the Highway 221 Bridge.
The project area is in a mixed forested, industrial, agricultural, and commercial property use area.
lnstream cover in the sampling locations on the Broad River was a combination of logs and woody
debris, rocky shoals, overhanging vegetation, and undercut banks. Two primary access points were
identified and utilized with access permissions in place. The primary collection method utilized was in
stream boat electrofishing. Gill nets were also deployed during the sampling effort. Attachment C
includes a photo log from the sampling event (presented in Appendix D of Attachment C).
The Plan identified three target species representing the following three separate troph
ic levels:
largemouth bass (Micropterus salmoides),top predator, redbreast sunfish (Lepomis auritus), mid-trophic
insectivore, and notchlip redhorse (Moxostoma hic omnivore. The minimum target
collapsum), mi p
p
number of individual fish was six of each species and the maximum was 10 individuals of each species,
from each sampling location. The Plan provided for substituting secondary species if target species were
not encountered in appropriate numbers. Potential secondary target species identified in the Plan were
bluegill, brassy jumprock, flat bullhead, smallmouth bass, white sucker, catfish, or carp. Edible-sized
individuals, based on the North Carolina Inland Fishing, Hunting &Trapping Regulations Digest 2021-2022,
or the 2019 NCDWR fish tissue monitoring data were targeted. Ten individual fish from each of the three
targeted species were collected at both the upstream and downstream locations. Each individual fish met
the minimum length requirements. Two duplicate samples were collected from both the upstream and
downstream sample locations. Duplicate samples were collected from different target species.
Attachment C provides a detailed accounting and information regarding fish processing, sample
shipping, and quality control procedures. Attachment C also includes the chain of custody forms,
laboratory analytical reports and field datasheets. TRC and EA performed quality control checks on the
field and analytical data deliverables and a detailed review of the data reports and data summary tables.
Fish tissue samples were shipped to Pace Analytical Services, Green Bay, Wisconsin,for analysis. Two
fish tissue samples were duplicated for laboratory analysis at each location,for a maximum of 64
samples submitted to the laboratory for analysis. The laboratory was responsible for processing fish
fillets, including scaling and filleting. All bass, suckers, and sunfish were processed as skin-on fillets. The
right-side fillet was analyzed in each instance and provided sufficient tissue quantity (2 grams) required
for analysis.
TRC Environmental Corporation I American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary 5
October 2022

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Section 5
Summary of Analytical Results
A summary of the fish tissue analytical results by location is presented in the following narrative and
tables. A summary of the analytical results for the May 2022 sampling event for upstream and downstream
locations are presented on Tables 1 and 2, respectively. A comparison to pertinent screening values is
presented below.Attachment C includes a summary of the field sampling effort and analytical results,as
described in Broad River Fish Tissue Collection and Analysis for NPDES Permit No. NC0089109(EA 2022).
5.1 Upstream
• Arsenic was detected in one upstream notchlip redhorse sample (BR-US-NLR-07) at a concentration
of 0.031 (J) mg/kg. The detected concentration was assigned a "J" or estimated qualifier by the
analytical laboratory.
• Arsenic was not detected in upstream any largemouth bass or redbreast sunfish tissue samples.
• Cadmium was not detected in any fish tissue samples collected from the upstream location.
• Zinc was detected in fish tissue samples collected from the upstream locations at concentrations
ranging from:
4.5 mg/kg to 10.4 mg/kg in largemouth bass
— 4.6 mg/kg to 6.5 mg/kg in notch lip red horse
— 4.7 mg/kg to 12.9 mg/kg in redbreast sunfish
5.2 Downstream
• Arsenic was not detected in any fish tissue samples collected from the downstream location.
• Cadmium was not detected in any largemouth bass fish tissue samples collected from the
downstream locations.
• Cadmium was detected in six of the 10 notchlip redhorse fish tissue samples collected from the
downstream locations at concentrations ranging from 0.11 (J) mg/kg to 0.032 (J) mg/kg. The six
detected concentrations were assigned a "J" or estimated qualifier by the analytical laboratory.
• Cadmium was detected in two of the 10 redbreast sunfish tissue samples collected from the
downstream locations at concentrations ranging from 0.012(J) mg/kg to 0.021 (J) mg/kg. The two
detected concentrations were assigned a "J" or estimated qualifier by the analytical laboratory.
TRC Environmental Corporation I American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary 7
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• Zinc was detected in fish tissue samples collected from the downstream locations at concentrations
ranging from:
— 4.0 (J) mg/kg to 8.9 mg/kg in largemouth bass
— 5.2 mg/kg to 8.1 mg/kg in notchlip redhorse
— 5.1 mg/kg to 11.7 mg/kg in redbreast sunfish
TRC Environmental Corporation /American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary 8
\\GREENVILLE-FPI\WPGVL\PJT21479013\000O\R4 79 01 300 00-001_FINAL.DOCX October 2022

Table 1
Summary of Analytical Results for Fish Tissue Samples(Upstream)—May 2022
American Zinc Products
NPDES Broad River
BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-
Sample Location: 01 02 03 04 05 06 07 08 09 10
BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-BR-US-LMB-
01-18MAY22-02-18MAY22-03-18MAY22-04-18MAY22.05-18MAY22-06-19MAY22.07-19MAY22.08-19MAY22.09-19MAY22.10-19MAY22-
Sample Name: NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES
Lab Sample ID:40245388011 40245388012 40245388013 40245388014 40245388015 40245402011 40245402012 40245402013 40245402014 40245402015
Sample Date: 5/18/2022 5/18/2022 5/18/2022 5/18/2022 5/18/2022 5/19/2022 5/19/2022 5/19/2022 5/19/2022 5/19/2022
Analysis Analyte Unit
Metals,total
Arsenic mg/kg 0.088 U 0.092 U 0.091 U 0.093 U 0.088 U 0.096 U 0.098 U 0.099 U 0.097 U 0.094 U
Cadmium mg/kg 0.088 U 0.092 U 0.091 U 0.093 U 0.088 U 0.096 U 0.098 U 0.099 U 0.097 U 0.094 U
Zinc mg/kg 5.4 6.7 4.8. 4.5 5.9 5.9 6.7 6.1 5.3 10.4
Moisture
!Percent Moisture % 79.7 80.1 80.0 79.8 79.8 78.6 80.2 80.0 79.0 79.3
Notes:
mg/kg-milligrams per kilogram.
.1-Estimated value.
U-Analyze was not detected at specified gnantitation limit.
Values in bold indicate the analyte was detected.
BR Broad River
DS Downstream
US Upstream
LMB Largemouth bass
NLR Notchlip redhorse
RBS Redbrease sunfish

Table 1
Summary of Analytical Results for Fish Tissue Samples(Upstream)-May 2022
American Zinc Products
NPDES Broad River
BR-US-NLR-BR-US-NLR-BR-US-NLR-BR-US-NLR-BR-US-NLR-BR-US-NLR-BR-US-NLR-BR-US-NLR- BR-US-NLR-
Sample Location: 01 02 03 04 05 06 07 08 BR-US-NLR-09 10
BR-US-NLR- BR-US-NLR- BR-US-NLR- BR-US-NLR- BR-US-NLR- BR-US-NLR- BR-US-NLR- BR-US-NLR- BR-US-NLR- BR-US-NLR- BR-US-NLR-
01-16MAY22.02-16MAY22 03-16MAY22-04-16MAY22-05-16MAY22.06-16MAY22-07-16MAY22.08-16MAY22.09-16MAY22.09-16MAY22.10-16MAY22-
Sample Name: NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES-DUP NPDES
Lab Sample ID:40245402006 40245402007 40245402008 40245402009 40245402010 40245388006 40245388007 40245388008 40245388009 40245388016 40245388010
Sample Date: 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022
Analysis Analyte Unit Field Dup
Metals,total
Arsenic mg/kg 0.10 U 0.095 U 0.092 U 0.092 U 0.094 U 0.10 U 0.031 J 0.099 U 0.093 U 0.092 U 0.090 U
Cadmium mg/kg 0.10 U 0.095 U 0.092 U 0.092 U 0.094 U 0.10 U 0.094 U 0.099 U 0.093 U 0.092 U 0.090 U
Zinc mg/kg 6.3 6.0 5.9 6.4 6.5 6.0 4.6 5.4 5.8 5.7 5.7
Moisture
Percent Moisture % 80.1 79.6 79.4 79.9 79.7 80.3 793 79.4 79.2 79.3 79.7
Notes:
mg/kg-milligrams per kilogram.
J-Estimated value.
U-Analyte was not detected at specified quantitation limit.
Values in bold indicate the analyte was detected.
BR Broad River
DS Downstream
US Upstream
LMB Largemouth bass
NLR Notchlip redhorse
RBS Redbrease sunfish

Table 1
Summary of Analytical Results for Fish Tissue Samples(Upstream)—May 2022
American Zinc Products
NPDES Broad River
BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS-
Sample Location. 01 02 03 04 05 06 07 08 09 BR-US-RBS-10
BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS- BR-US-RBS-
01-16MAY22.02-16MAY22.03-16MAY22-04-16MAY22-05-16MAY22.06-16MAY22-07-I6MAY22-08-17MAY22-09-17MAY22.10-17MAY22.10-17MAY22
Sample Name: NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES-DUP
Lab Sample ID:40245388001 40245388002 40245388003 40245388004 40245388005 40245402001 40245402002 40245402003 40245402004 40245402005 40245402016
Sample Date: 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/16/2022 5/17/2022 5/17/2022 5/17/2022 5/17/2022
Analysis Analyze Unit Field Dup
Metals,total
Arsenic mg/kg 0.093 U 0.094 U 0.092 U 0.087 U 0.099 U 0.10 U 0.096 U 0.098 U 0.094 U 0.092 U 0.096 U
Cadmium mg/kg 0.093 U 0.094 U 0.092 U 0.087 U 0.099 U 0.10 U 0.096 U 0.098 U 0.094 U 0.092 U 0.096 U
Zinc mg/kg 5.5 11.1 10.8 12.9 12.3 10.3 7.4 10.3 11.2 4.7 7.0,
Moisture
'Percent Moisture % 80.3 81.0 80.5 78.8 79.8 79.9 79.7 80.9 79.9 78.5 79.6
Notes:
mg/kg-milligrams per kilogram.
J-Estimated value.
U-Analyte was not detected at specified gnantitation limit.
Values in bold indicate the analyte was detected.
BR Broad River
DS Downstream
US Upstream
LMB Largemouth bass
NLR Notchlip redhorse
RBS Redbrease sunfish

Table 2
Summary of Analytical Results for Fish Tissue Samples(Downstream)--May 2022
American Zinc Products
NPDES Broad River
BR DS-LMB-BR-DS-LMB-BR-DS-LMB- BR-DS-LMB.BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-
Sample Location: 01 02 03 BR-DS-LMB-04 05 06 07 08 09 10
BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-BR-DS-LMB-
01-20MAY22.02-20MAY22-03-20MAY22.04-20MAY22-04-20MAY22.05-20MAY22-06-21MAY22-07-21MAY22-08-21MAY22-09-21MAY22-10-21MAY22-
Sample Name: NPDES NPDES NPDES NPDES NPDES-DUP NPDES NPDES NPDES NPDES NPDES NPDES
Lab Sample ID: 40245367011 40245367012 40245367013 40245367014 40245367016 40245367015 40245368011 40245368012 40245368013 40245368014 40245368015
Sample Date: 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/21/2022 5/21/2022 5/21/2022 5/21/2022
Analysis Analyte Unit Field Dup
Metals,total
Arsenic mg/kg 0.096 U 0.10 U 0.096 U 0.098 U 0.098 U 0.10 U 0.096 U 0.096 U 0.096 U 0.097 U 0.095 U
Cadmium mg/kg 0.096 U 0.10 U 0.096 U 0.098 U 0.098 U 0.10 U 0.096 U 0.096 U 0.096 U 0.097 U 0.095 U
Zinc mg/kg 5.4 7.2 5.3 4.1 J 4 J 5.1 7.0 6.2 6.6 4.9 8.9
Moisture
'Percent Moisture % 79.5 79.6 78.7 79.6_ 79.8 79.5 79.7 78.5 78.9 79.5 80.0
Notes:
mg/kg-milligrams per kilogram.
J-Estimated value.
U-Analyze was not detected at specified quantitation limit.
Values in bold indicate the analyze was detected.
BR Broad River
DS Downstream
US Upstream
LMB Largemouth bass
NLR Notchlip redhorse
RBS Redbrease sunfish

Table 2
Summary of Analytical Results for Fish Tissue Samples(Downstream)—May 2022
American Zinc Products
NPDES Broad River
BR-DS-NLR-BR-DS-NLR-BR-DS-NLR-BR-DS-NLR- BR-DS-NLR-BR-DS-NLR-BR-DS-NLR-BR-DS-NLR-BR-DS-NLR-
Sample Location: 01 02 03 04 BR-DS-NLR-05 06 07 08 09 10
BR-DS-NLR- BR-DS-NLR- BR-DS-NLR- BR-DS-NLR- BR-DS-NLR- BR-DS-NLR- BR-DS-NLR- BR-DS-NLR- BR-DS-NLR- BR-DS-NLR- BR-DS-NLR-
01-20MAY22.02-20MAY22.03-20MAY22.04-20MAY22-05-20MAY22-05-20MAY22-06-20MAY22-07-20MAY22-08-20MAY22.09-20MAY22-10-20MAY22-
Sample Name: NPDES NPDES NPDES NPDES NPDES NPDES-DUP NPDES NPDES NPDES NPDES NPDES
Lab Sample ID: 40245368006 40245368007 40245368008 40245368009 40245368010 40245368016 40245367006 40245367007 40245367008 40245367009 40245367010
Sample Date: 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022
Analysis Analyte Unit Field Dup
Metals,total
Arsenic mg/kg 0.099 U 0.096 U 0.093 U 0.093 U 0.095 U 0.098 U 0.099 U 0.097 U 0.099 U 0.098 U 0.099 U
Cadmium mg/kg 0.099 U 0.011 J 0.093 U 0.093 U 0.02 J 0.018 J 0.023 J 0.097 U 0.099 U 0.032 J 0.012 J
Zinc mg/kg 6.5 8.1 7.0 5.8 5.9 6.3 7.7 5.2 5.7 5.7 6.3
Moisture
'Percent Moisture % 79.7 78.1 79.7 78.4 79.5 79.2 79.6 80.3 79.3 80.0 78.6
Notes:
mg/kg-milligrams per kilogram.
J-Estimated value.
U-Analyte was not detected at specified quantitation limit.
Values in bold indicate the analyte was detected.
BR Broad River
DS Downstream
US Upstream
LMB Largemouth bass
NLR Notchlip redhorse
RBS Redbrease sunfish

Table 2
Summary of Analytical Results for Fish Tissue Samples(Downstream)--May 2022
American Zinc Products
NPDES Broad River
BR-DS-RBS- BR-DS-RBS- BR DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS-
Sample Location: 01 02 03 04 05 06 07 08 09 10
BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS- BR-DS-RBS-
01-20MAY22-02-20MAY22-03-20MAY22-04-20MAY22.05-20MAY22-06-20MAY22-07-20MAY22-08-20MAY22-09-20MAY22-10-20MAY22-
Sample Name: NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES NPDES
Lab Sample ID: 40245368001 40245368002 40245368003 40245368004 40245368005 40245367001 40245367002 40245367003 40245367004 40245367005
Sample Date: 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022 5/20/2022
Analysis Analyte Unit
Metals,total
Arsenic mg/kg 0.096 U 0.098 U 0.094 U 0.097 U 0.10 U 0.098 U 0.092 U 0.098 U 0.094 U 0.099 U
Cadmium mg/kg 0.096 U 0.098 U 0.094 U 0.097 U 0.10 U 0.021 J 0.092 U 0.098 U 0.012 J 0.099 U
Zinc mg/kg 6.8 7.4 10.4 7.7' 11.7 5.1 8.9 6.7 11.1 7.7
Moisture
Percent Moisture % 79.8 79.3 80.8 80.9 79.9 79.8 80.0 81.0 79.5 80.8
Notes:
mg/kg-milligrams per kilogram.
J-Estimated value.
U-Analyte was not detected at specified quantitation limit.
Values in bold indicate the analyte was detected.
BR Broad River
DS Downstream
US Upstream
LMB Largemouth bass
NLR Notchlip redhorse
RBS Redbrease sunfish

Section 6
Conclusions
Consistent with requirements outlined in the in NCDEQ approved Plan,fish tissue data were compared
to fish consumption screening levels set by the North Carolina Department of Health and Human
Services (NCDHHS).
NCDHHS developed the following fish tissue screening levels in 2018 using USEPA published regional
screening levels (RSLs) for fish tissue:
■ Arsenic:
— 0.141 mg/kg; noncarcinogenic basis
— 0.00031 mg/kg; carcinogenic basis
■ Cadmium: 0.471 mg/kg; noncarcinogenic basis
■ Zinc: 141 mg/kg; noncarcinogenic basis
Detected concentrations of arsenic, cadmium, and zinc in fish tissue samples collected during the
sampling event were less than the NCDHHS noncarcinogenic fish tissue screening values. A single
detected concentration of arsenic in one upstream notchlip redhorse sample (BR-US-NLR-07) at a
concentration of 0.031 (J) mg/kg is greater than the 0.00031 mg/kg NCDHHS carcinogenic target risk
value for arsenic. The current NCDHHS screening levels are conservatively based on a subsistence
fisherman exposure scenario.
The AZP fish tissue sampling program meets the requirements of the permit and compares favorably to
the NCDHHS screening levels.
TRC Environmental Corporation /American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary 15
\\GREENVILLE-FP1�WPGVL\PJT2\479013V0000\R4 79 01 3 0 000-001_FINAL.DOCX October 2022

Appendix A
AZR Revised Fish Sampling Plan 2020
TRC Environmental Corporation l American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary
\\GREENV/LLE-FP1\WPGVL\PJT2\479013\0000\R4790130000-001_FINAL.DOCX October 2022

TIMOTHY R BASILONE
A h Vice President- Environmental Affairs
ZR
AM E R(CAN
3000 GSIi Drive T 724-7 73-fit'?i www:azr_com
Z I hl C R E C'YC Li t Suite 201 F 412-788-4528 tbasilone@ezr,co'n
Delivering_=Sustainatlle Moon Township,PA 15108
April 16,2020
Division of Water Resources
WQ Permitting Section-NPDES
1617 Mail Service Center
Raleigh, NC 27699-1617
(Electronic Version Only(pdf and CD))
Division of Water Resources
Water Sciences Section
1621 Mail Service Center
Raleigh, NC 27699-1621
(Electronic Version (pdf and CD.)and Hard Copy)
Re: Revised Fish Tissue Monitoring Plan
NPDES Permit NC0089109
American Zinc Products
Condition Part I,A.(4.)
In accordance with NPDES Permit NC0089109 issued to American Zinc Products(AZP) in Rutherford County,
NC, enclosed is a Revised Fish Tissue Monitoring Plan(Revised Plan)developed for the collection,
preparation and chemical analysis of fish samples collected from the Broad River upstream and downstream
of AZP's permitted discharge outfall. The Revised Plan was edited to address comments provided to AZP by
DWR in a letter dated December 20, 2019, and according to permit condition Part I,A. (4). A responsiveness
summary is included to facilitate the Department's review of the Revised Plan.
The Revised Plan identifies certified labs that may be used for the analytical evaluation of samples that are
collected. A list of potential contractors for field work,including the collection,of fish and sample
preservation is also provided. This information does not representa commitment by AZP to use any of the
listed contractors or laboratories. AZP will select appropriate and qualified service providers to perform
monitoring activities in accordance with the approved monitoring plan.
Following agency approval of the monitoring plan,AZP will follow the revised plan to perform monitoring
within the current permit cycle. Results from monitoring activities will be included with the Company's
application for renewal of the NPDES Permit that is submitted to the Department.
Please advise me if you have any questions. Thank you for your attention to this matter.
Sincerely,
Timothy R. Basilone
End.

Responsiveness Summary AZR Fish Tissue Revised Monitoring Plan and DWR Review Comments(12/20/2019)
• Note addition of CZR Inc. Environmental Consultants Wilmington NC to contractor list.
• Duplicate samples of two duplicates per site for a total of four duplicates
1. Comment: As stated in the permit,fish tissue monitoring of arsenic(As),cadmium(Cd),and zinc (Zn)must be
performed once during the 5-year AZR NPDES permit cycle. For clarity please include these terms in the beginning of
the AZR fish tissue monitoring plan, as well as in the final report.
Response: Page one of the AZR revised Fish Sampling Plan incorporates the exact requirements of the NPDES Fish
Tissue Monitoring requirement and is reproduced in the plan and labeled as Permit Item A. (4.).
2. Comment: Please omit the last two paragraphs on page 2 through page 4(including Figure 1 and Table 1).The referenced
2019. NCDWR fish tissue monitoring activities were conducted via internal agency request,and not specifically intended
to serve as a model for NPDES fish tissue contaminant monitoring of the Broad River. However,it would be reasonableto
list those species collected by DWR in 2019,and to specify which of those species are being targeted for the required
AZR fish tissue monitoring.
Response:The requested deletions have been made as requested. Target species have been identified based on the
DWR suggestions and the 2019 collections.
3. Comment:The plan should outline AZR's proposal to compare arsenic(As),cadmium(Cd),and zinc(Zn) fish fillet
concentrations from two separate locations in the vicinity of the AZR waste water discharge(upstream control, and
downstream). Site boundaries should be separated by a reasonable distance(— I mile)to characterize the potential impact
of AZR's waste water discharge on As,Cd,and Zn concentrations in fish. All of the current NPDES fish tissue monitoring
plans in the state of North Carolina share this paradigm of upstream-downstream comparisons for the purpose of
determining a facility's potential impact on fish contaminant levels.
Response:The AZR revised Fish Sampling Plan incorporates two monitoring locations,one upstream and one
downstream of the AZR facility.
4. Comment: The boundaries of the proposed downstream fish collection reach are reasonable and therefore will be
accepted as is.
Response:No changes necessary related to this comment.
5. Comment: We suggest placement of the upstream sample reach(control)to be above the Jack McKinney Road bridge
(approximately 3 river miles above the AZR waste water discharge),to create considerable distance between the two
reaches and provide similar habitat types and species assemblages for contaminant comparisons.
Response: The AZR revised Fish Sampling Plan incorporates the addition of a Broad River sampling reach from the Jack
McKinney Road Bridge to one mile downstream.
6. Comment:The plan should outline an attempt to collect 10 individuals of 3 targeted species from both sample reaches
(total of 30 fish from each sample reach),with a minimum of 6 individuals per species meeting the permit requirement
(total of 18 fish from each sample reach).
Response: The revised Fish Sampling Plan now targets a goal of 3 species composed of 10 individual fish at each location
with a minimum objective goal of 18 fish from each location.
7. Comment:Based on the NCDWR's 2019 fish collections, the most likely target species in this section of the Broad River
include Largemouth Bass(top predator),Redbreast Sunfish (mid-trophic insectivore),and Notchlip Redhorse(mid-
trophic omnivore). Other suitable species of bass,sunfish,suckers,catfish, or carp should also be retained during
collection efforts.These fish samples may be submitted for analysis if target species are absent or low in numbers,or as
supplemental observations.
Response:The AZR revised Fish Sampling Plan has incorporated the suggested primary target species and the secondary
target species as identified in the DWR comments.
8. Comment: In the final monitoring report,please provide data comparisons to fish consumption screening levels set by the
North Carolina Department of Health and Human Services(NCDHHS)and the Environmental Protection Agency.
Response: AZR is aware that EPA and NCDHHS fish tissue screening levels may be established based on different
assumptions at different times and for different purposes. AZR will reference established standards and criteria and other
such information available at the time the monitoring report is submitted. AZR will submit a final fish monitoring report
with the NPDES permit renewal application as required in our NPDES permit Item A.(4.).

Revised Fish Tissue Sampling Plan
American. Zinc Recycling, LLC NPDES Permit Condition
Permit Item A. (4.)
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Revised March, 2020
1JPage
Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Introduction
This Sampling.Plan is designed to assist with the planning and responses necessary for the
successful compliance of the Fish Tissue Monitoring Condition included in the American Zinc
Recycling (AZR), LLC Forest City,Rutherford County NPDES Permit NC0089109. The Permit
as modified is scheduled with an effective date of June 1, 2019. This Study Plan was revised.
based on NCDWR Comments dated December 20,2019. The NPDES Fish Tissue Monitoring
requirement is included as Permit Item A. (4.) as follows (taken directly from the permit):
A. (4.) FISH TISSUE MONITORING
fG.S. 143-215:.1(b)]
The facility shall conduct fish tissue monitoring once during the permit cycle and submit the
results with the NPDES permit renewal application. The objective of this monitoring is to
evaluate potential uptake of pollutants by fish tissue near the facility's discharge. The
parameters analyzed in fish tissue shall be arsenic, cadmium, and zinc. The monitoring shall
be conducted in accordance with the sampling plan approved by the Division. The plan should
be submitted to the Division within 180 days from the effective date of the permit modification.
Upon approval, the plan becomes an enforceable part of the permit.
Copies of all the study plans, study results, and any other applicable materials should be
submitted.to:
1) Electronic Version Only (pdf and. CD) 2) Electronic Version (pdf and CD) and Hard Copy
Division of Water Resources Division of Water Resources
WQ Permitting Section - NPDES Water Sciences Section
1617 Mail Service Center 1621 Mail Service Center
Raleigh, NC 27699-1 6 1 7 Raleigh, NC 27699-1621
Objectives
All fish tissue sampling performed by American Zinc Recycling(AZR) will be conducted based
on an approved sampling plan (this plan) according to the NPDES permit condition. Any
exceptions to this approved Sampling Plan either due to unforeseen logistical challenges,
difficulty in obtaining target species, safety concerns or other issues will be specifically detailed
in writing and communicated to the NCDWR either during or after field sample collections are
performed.
The purpose of this Sampling Plan is to document sample collection and analytical procedures to
be followed by AZR contractors for the collection and processing of fish samples for analysis of
Arsenic, Cadmium, and Zinc as maybe found in the edible portion(fillet) of target species in the
vicinity of the AZR waste water discharge. After obtaining the appropriate fish samples, fillet
portions will be processed and delivered to a North Carolina certified laboratory for total arsenic,
total cadmium, and total zinc. Results from this sampling and laboratory analysiswill be
reported to the NCDWR with the next AZR NPDES permit renewal application as specified in
the current NPDES permit under:A. (4.)FISH TISSUE MONITORING.
It is the goal of this Sampling Plan to obtain ten individual fish for each of three different target
species at two different locations. One location will be geographically upstream of the AZR
facility and another location will be located geographically downstream of the facility. All fish
submitted for chemical analysis will be representative of edible sizes. This goal, if attainable,
2 ' Page
Fish Tissue Sampling Plan American Zinc Recycling NPDES:NC0089109

will represent a total of 60 individual fish fillet samples for total arsenic, total cadmium, and total
zinc. Sample duplicates will also be submitted for laboratory analysis on four samples.
Sampling Target Species
The resident fish species of the Broad River near the American Zinc Recycling(AZR) facility
are expected to include a number of different fish species based on North Carolina Division of
Water Resources (NCDWR) fish sampling conducted on March 13, 2019. NCDWR Water
Sciences Staff collected fish samples from the Broad River both upstream and downstream of the
AZR facility's discharge. The following eight species were collected for metals analysis by
NCDWR in March of 2019:
Bluegill Sunfish Notchlip Redhorse (Sucker)
Brassy Jumprock(Sucker) Redbreast Sunfish
Flat Bullhead Smallmouth Bass
Largemouth Bass White Sucker
Based on the results of NCDWR fish collection sampling efforts in March 2019, this AZR
Sampling Plan represents a lofty goal. At a minimum, this AZR Sampling Plan will strive for
representation at each location with at least three edible species and a minimum of at least six
individuals from each species selected from the target species list. Thus, a minimum total of 18
fish samples will be selected for laboratory analysis from each location. Because ten individual
representatives of each species may not be attainable at each location, the sampling effort will be
well documented by the selected AZR contractor.
Based on NCDWR's 2019 fish collections and recommendations, the three species chosen as
primary targets for collection in this study include: Largemouth Bass, Redbreast Sunfish, and
Notchlip Redhorse. Each of these three species represent different trophic levels—top predator,
mid-trophic insectivore, and mid trophic omnivore, respectively. If these three primary target
species are absent from each location or a minimum of six individuals from each species are not
attainable then secondary target species may be substituted. Secondary target species may
include: Bluegill Sunfish,Brassy Jumprock, Flat Bullhead, Smallmouth Bass, White Sucker,
catfish, carp or other species.
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Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Broad River Sampling Reach Locations
The Broad River in the vicinity of the AZR facility can be a challenge for many fish collection
approaches including gill nets,hook and line, electrofishing, and other practices. Fish samples
will be obtained from two locations on the Broad River. The Broad River is a rocky, flashy, and
swift waterbody capable of rapid changes in water depth.
The first sampling reach location on the Broad River will start at the Jack McKinney Road
Bridge(approximately three river miles above the AZR facility). The downstream extent of this
sampling reach will be located no further than one mile downstream of the Jack McKinney Road
Bridge.
The second fish sampling reach will obtain fish from the Broad River below the AZP discharge.
The second river sampling reach will start below the AZP discharge in the vicinity of the
Highway 221 bridge over the Broad River(GPS location approximately Latitude 35.20585
Longitude -81.83773). The downstream extent of the sampling reach will be located
approximately one mile downstream of the Highway 221 bridge over the Broad River(GPS
location approximately Latitude 35.205356 Longitude -81.821633).
In any case,depending on the availability of fish, the extent of each actual sampling reach will
be measured and reported using reliable GPS positioning equipment. The agent or contractor
selected for fish sample collections will provide copies of any figures, maps, and photographs
needed to document the location of the sampling reach. Photographs documenting sampling
collection activities will also be provided.
Sampling Technique Methods
It is anticipated that the AZR fish collection contractor will employ boat mounted powered
electrofishing as the primacy means of fish collection. Depending on the selection of a suitable
fish collection contractor, collections may also be accomplished using back pack electrofishing
techniques,hook and line, trot lines,traps, or gilinets. In any case, the collection contractor will
implement measures necessary to ensure that samples are collected and handled properly with
minimal contamination and that each sampling reach is GPS verified. Field sampling efforts will
continue at each location until either the primary or secondary target fish samples have been
collected with a sufficient number of individuals. A minimum of three different species with six
individuals will be collected from each location. Thus, fish collections are expected to result in a
minimum of 36 laboratory samples for individual fish analysis (plus 4 duplicates) for arsenic,
cadmium, and zinc. Regardless of collection method, the successful contractor will have
knowledge,skills, and experience with all sampling techniques used to obtain fish samples. All
personnel involved with electrofishing or other methods employed will be familiar with
operational and safety procedures. At least two fish tissue samples will be duplicated for
laboratory analysis at each location regardless of the total number of individual fish collected at
each location.
If field sampling approaches for fish collections are not successful in obtaining sufficient
individuals(18 per site) for laboratory analysis NCDWR will be consulted to determine
appropriate modifications.
4 1 P sg e
Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Field Data Sheet#1 and Field Data Sheet#2 will document Fish Tissue Collection Results on
the day(s)of Field sampling. One set of Data Sheets (2) will be completed for each location for
p
each day sampling is conducted.
Field Data Sheet#1
Fish Tissue Collections: Broad River downstream American Zinc Products Discharge.
Collection Date:
Location:
Study Reach Start From: Latitude: Longitude:
Study Reach Finish at: Latitude: Longitude:
Nearest Landmark at Start of Reach: Highway 221 bridge over the Broad River Rutherford Co.
Duration of Daily Collection Activities: Hours: Minutes:
Collection Staff: (list name and affiliation: example John Doe, Agency Blue Inc.
Describe Collection.Methods: (ex. Electrofishing Boat, Back Pack electrofishing, hook and line,
trot lines, traps, or gillnets).
Describe:
Comment and Describe Access to River : ( example boat ramp, bank, bridge etc.)
Each day of sampling personnel must fill out the following table ((Field Data Sheet#2)
completing information for all individual fish. Any deviation from this Sampling Plan must be
noted and described on daily records.
Exceptions to Sampling Plan if any:
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Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Field Data Sheet#2
Fish# Sample Location Species Total Length Weight Comments
ID in cm in grams
1 Date of collection:
2
3 Lat/Long Site Coordinates
4
5 The upstream extent was:
6 Latitude:
7 Longitude:
8 The Downstream extent was:
9 Latitude:
10 Longitude:
11 Reach Length in miles(include decimals)
12
13 Fish Collection Goal per location
14 3 Target Species
15 Ten fish per Species:30 fish total
16
17 Primary Target Species Include
18
19 largemouth bass
20 redbreast sunfish
21 notchlip redhorse sucker
22
23
24 Secondary Target Species Include
25 bluegill sunfish
26 brassy jumprock
27 white sucker
28 flat bullhead
29 catfish
30 carp
31 Dup#1 of Fish Sample# others
32 Dup#2 of Fish Sample#
Additional Comments:
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Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Analytical Requirements—
Fish Tissue Samples will be analyzed by a North Carolina Laboratory certified by the Division
of Water Resources. All fish tissue samples will be analyzed for total arsenic, cadmium, and
zinc. Laboratory analytical capabilities will be evaluated and compared to the DWR PQL
reporting limits for arsenic, cadmium, and zinc prior to contractor selection. At least two fish
tissue samples will be duplicated for laboratory analysis at each location regardless of the total
number of individual fish collected at each location.
Sample Handling and Delivery/Shipment
Fish tissue samples collected for analyses must be processed and delivered/shipped to the
selected certified laboratory in order to prevent decomposition or contamination. In all activities
the selected contractor will avoid potential sources of arsenic, cadmium, and zinc contamination
—i.e. no use of galvanized buckets,no cigarette smoking, powderless nitrile gloves will be worn
in all fish handling activities. Fish will be removed from plastic live wells, holding tanks, or
buckets, and rinsed with ambient water to remove foreign matter, and placed on a clean or new
protective surface (i.e. aluminum foil) for sorting,weighing, length measurements, and
wrapping. All samples will be processed individually. No fish will be composited into
composite samples.
• An individual whole fish wet weight will be determined for each fish to the nearest gram
and recorded on Field Data. Sheet#2. All individual samples will be weighed on
scales/balances that are properly calibrated and of adequate accuracy and precision to
weigh samples to the nearest gram. Scales and or balances will be checked for calibration
at the beginning of each weighing session.
• A total length will be determined for each fish to the nearest centimeter using a length
board such as the Wildco® Model 118 and recorded on Field Data Sheet#2). Individual
fish will be identified to species under the supervision of an experienced staff familiar
with North Carolina fish. Fish will be identified using current, identification manuals and
other appropriate taxonomic literature (i.e.: Menhinick, E. F. 1991).
• Skins on fish selected for analysis will be examined for breaks or lacerations from
sampling gear as a possible source of contamination. Fish samples will be identified by
species and sorted by species before any packaging or processing for delivery/shipment
to the certified laboratory.
• Fish selected for metals �
analysis will be weighed and measured for length. Fish will be
individually wrapped and labeled with sample number, species name, weight, and length
in appropriate arsenic, cadmium, and zinc free wrap (i.e. new aluminum foil) and placed
by species in polyethylene bags. After removing as much air as possible, the bags will be
closed and tagged with the date, time, station name, species, and collector(s).
• All fish (in bags)will be placed on wet ice and chilled to 4 degrees C for transport to
either the certified laboratory or other suitable tissue processing location for preparation
of fillet samples within 48 hours.
• All fish will be processed as fillet samples. No fish samples for whole body metals
analysis will be sent to the certified laboratory for whole body metals analysis.
• All bass and sunfish species will be processed as fish fillet samples with skin-on intact.
• All Suckers, Catfish, and Bullheads, and Carp will be processed as fillet samples with
skin-off(no skin included).
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Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Fish Tissue Sample Processing Procedures
• Individual fish selected for filleting will be unwrapped and inspected carefully to ensure that
they have not been compromised in any way(i.e., not properly preserved during shipment).
Any specimen deemed unsuitable for further processing and analysis should be discarded and
identified on the sample processing record.
• Equipment used in processing fish samples for metals analysis will be free from arsenic,
cadmium, and zinc contamination. As such, glass and plastic use will be prioritized. Only
when necessary(i.e. knives) stainless steel will be used. Prior to preparing fish samples, all
hard surfaces used in the processing will be washed with a detergent and rinsed with verified
metal free water(treated by reverse osmosis—R.O.). Any necessary utensils and containers
will be thoroughly cleaned and rinsed with tap water, soaked in 50 percent HNO3 (at least
reagent grade)for 12 to 24 hours, and then rinsed with metal-free water.
• All processing will be performed on surfaces covered with heavy duty aluminum foil.
Aluminum foil will be rinsed with R.O. water between fish or new foil will be used. Filleting
will be performed using talc free disposable gloves. Gloves will be rinsed between samples to
prevent cross contamination. Fillets will be resected using high grade stainless steel knives.
Knives are rinsed with R.O. water between fish species from the same station.
• Fillets will be removed from the lateral area of the fish behind the head and pectoral fin and
will include the belly flap. Extreme care will be taken not to cut into the gut cavity as it may
contaminate the fillet tissue.
• Filleting will be done on cutting boards covered with heavy duty aluminum foil that is
changed after each filleting. Fillet tissues will be removed from whole fish with clean,high
quality, corrosion-resistant stainless steel or with titanium blade knives and polypropylene
handles.
• Skin-on fillets will be processed by removing scales from the intact fish. Fish will be scaled
prior to filleting using an automatic rotary scaler or hand scaler. Fish will then be rinsed with
R.O. water to remove slime and foreign matter. Any scaling instruments will also be rinsed
between fish to prevent contamination. The scale free fish fillet will be finely minced using
the same knives to prepare individual fillet homogenates to ensure equal distribution of
contaminants throughout the sample. These individual fillet tissue homogenates will be
stored in heavy duty aluminum foil and appropriately labeled for delivery to the certified
laboratory for chemical analysis. Where possible the final individual homogenized sample
should be composed of approximately 100 g of tissue to ensure an adequate amount of
material for analysis. Since samples will be composed of individual fish fillets it may not be
possible to achieve 100g of sample in every case.
• Fish fillet for skin-off analysis will be separated from the skin using knives. Fish will be
skinned prior to filleting for all catfish and bullheads. Sucker and Carp fillets will be
separated from the fish body and subsequently separated from the skin using knives. The skin
free fish fillet will be finely minced using the same knives to prepare individual fillet
homogenates to ensure equal distribution of contaminants throughout the sample. These
individual fillet tissue homogenates will be stored in heavy duty aluminum foil and
appropriately labeled for delivery to the certified laboratory for chemical analysis. Where
possible the final individual homogenized sample should be composed of approximately 100
g of tissue to ensure an adequate amount of material for analysis.
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Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Commercial Certified laboratories in North Carolina, South Carolina and Tennessee
Cert B J Lab Name Lab Contact Lab Addresel Lab City State] Zip Phone E-mail Address
1 Beacham Labs-Division of Environmental Chemists Ray Porter 6602 Windmill Way Wilmington NC 28405- 910-392-0223 [e-mail]
10 Environment 1 Inc, Mark Oliveira P.O.Box 7085 Greenville NC 27835- 252.756.6208 [e-mail]
11 Mlcrobac Laboratories Inc. James Williams 2592 Hope Mills Road Fayetteville NC 28306- 910-864-1920 [e-mail]
12 Pare Analytical Services LLC-Huntersville NC Cheryl Johnson 9800 Kincey Avenue,Suite 100 Huntersviile NC 28078- 704-875-9092 Cheryl.Johnson@pacelahs_com
20 PAR Laboratories Inc. Russell Everett Box 411483 Charlotte NC 28273- 704-588-8333 [e-mail]
22 Vann Laboratories James W.Vann P.O.Box 668 Wallace NC 28466- 910-285-3966 [e-mail]
34 Research&Analytical Laboratories Sidney L Champion P.O.Box 473 Kernersvllle NC 27285- 336-996-2841 [e-mail]
37 TBL Environmental Laboratory Inc. Pamela S.Hester P.O.Box 589 Lumberton NC 28359- 910-738-6190 [e-mail]
40 Pace Analytical Services LLC- Asheville NC Barry Johnson 2225 Riverside Drive Asheville NC 28804- 828-254-7176 [e-mail]
S0 Water Tech Labs Inc. LaFayette A.Gragg P,O.Box 1056 Granite Falls NC 28630- 828-396-4444 [e-mail]
57 Environmental Inc. AnthonyTirona P.O.Box954 Cullowhee NC 28723- 828-586-5588 [e-mail]
67 Pace Analytical Services LLC-Raleigh NC Barry Johnson 4915 Waters Edge Drive Suite 125 Raleigh NC 27606- 919-834-4984 [e-mail]
94 Environmental Chemists Inc.(Envirochem) Ray Porter 6602 Windmill Way Wilmington NC 28405- 910-392-0223 [e-mail]
165 Merltech Inc. David Merritt P.O.Box 27 Reidsville NC 27323- 336-342-4748 [e-mail]
177 Water&Sewer Authority of Cabarrus County Cayce Atkinson 6400 Breezy Lane Concord NC 28025- 704-788-4164 [e-mail]
192 Charlotte Water-Environmental Laboratory Services Rhonda Hutson 4222 Westmont Drive Charlotte NC 28217- 704-336-3690 [e-mail]
210 City of Gastonia-Crowders Creek Laboratory Annette McMurray P.O.Box 1748 Gastonia NC 28054- 704-854-6658 [e-mail]
235 Cherokee WWTP Laboratory Michael Bolt P.O.Box 547 Cherokee NC 28719- 828-359.6772 [e-mail]
245 Perdue Incorporated Tina B.Rawls P.O.Box 460 Lewiston Woodville NC 27849- 252-348-4400 [e-mail]
275 Blue Ridge Labs David Wessinger P.O.Box 2940 Lenoir NC 28645- 828-728-0149 [e-mail]
352 Earth Environmental Services Mark Bentley 75 Bison Lane Murphy NC 28906- 828-837-9543 [e-mail]
402 Prism Laboratories Inc, Paul Fitzgerald P.O.Box 240543 Charlotte NC 28224- 704-529-6364 [e-mail]
440 Statesville Analytical Holdings LLC Dena Myers P.O.Box 228 Statesville NC 28687- 704.872-4697 [e-mail]
481 SGS North America Inc.-Wilmington Jeannie Milholland 5500 Business Drive Wilmington NC 28405- 910-350-1903 [e-mail]
482 James&James Environmental Management Inc. Juanita James P.O.Box 519 Mountain Home NC 28758- 828-697-0063 [e-mail]
544 Water Quality Labs Inc_ Paul Isenhour P.O_Box 1167 Banner Elk NC 28604- 828-898-6277 [e-mail]
559 K&W Laboratories Gosia Kraska 1121 Hwy.24/27 W Midland NC 28107- 704-888-1211 [e-mail]
572 Agronomic Division Laboratory•NCDA Colleen Hudak-Wise 1040 Mail Service Center Raleigh NC 27699- 919-733-2655 [e-mail]
591 Environmental Conservation Laboratories inc. Dale Mori 102 Woodwinds Industrial Ct.Ste.A Cary NC 27511- 919-467-3090 [e-mail]
600 Environmental Testing Solutions Inc. Kelley E.Keenan P.O.Box 7565 Asheville NC 28802- 828-350-9364 [e-mail]
602 Statesville Analytical Holdings,LLC Dena Myers 4350 Sea Pines Drive Southport NC 28461- 910-617-1353 [e-mail]
604 Element One Inc. Ken Smith 6319-0 Carolina Beach Rd Wilmington NC 28412- 910-793-0128 [e-mail]
628 Environmental Chemists Inc./Outer Banks Div. Ray Porter P.O Box 2228 Manteo NC 27954- 252-473-5702 [e-mail]
633 Pace Analytical Services LLC-Eden NC Barry Johnson 205 East Meadow Road-Suite A Eden NC 27288- 828-254-7176 [e-mail]
638 Aquatic Ecology Lab-LJNCW Center for Marine Science Matthew McIver 5600 Marvin Moss Lane Wilmington NC 28409- 910-962-2357 [e-mail]
654 Cameron Testing Services Inc. Chris Cameron 219 S.Steele Street Sanford NC 27330- 919-208-4240 [e-mail]
677 First Analytical Laboratories NC,LLC Matt Loftin 4620-B Industry Lane Durham NC 27713- 919-942-8607 [e-mail]
687 RTI International Andrea McWilliams 3040 E-Cornwallis Road RTP NC 27709- 919-485-5520 [e-mail]
27 Rogers&Callcott Engineers Inc. Melisa Ramey P.O.Box 5655 Greenville SC 29606- 864-232-1556 [e-mail]
233 GEL Laboratories LLC Nancy Matters P,O.Box 30712 Charleston SC 29417- 843-556-8171 nancy.mattern@geLcom
329 Shealy Environmental Services Inc. Stephanie Atkins 106 Vantage Paint Dr. West Columbia SC 29172- 803-227-3167 [e-mail]
686 ETT Environmental Inc. Robert W.Kelley P,O.Box 16414 Greenville SC 29606- 864-877-6942 [e-mail]
64 TestAmerica Knoxville Kevin McGee 5815 Middlebrook Pike Knoxville TN 37921- 865-291-3000 kevin.mcgee@testamericainc,com
375 Pace Analytical Shari Pfalmer 12065 Lebanon Road Mt.Juliet TN 37122- 615-773-9755 [e-mail]
. 387 TestAmerica Nashville Glenn Baun 2960 Foster Creighton Drive Nashville TN 37204- 615-301-5739 [e-mail]
415 Waypoint Analytical LLC Richard Medina 2790 Whitten Road Memphis TN 38133- 901-213-2447 rmedina8iwaypointanalytical.com
9 1 Page
Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Examples of Some Potential Electrotishing Contractors
CZR Inc. Environmental Consultants
http://czr-inc.com/index.php?go=homesnain
4709 College Acres Drive
Suite 2
Wilmington, NC 28403-1725
[phone]
Foster.Lake & Pond Management
htt.ps://fosterlalce.coin/fisheries-ingmt/
9020 White Oak Road
P.O. Box 1294
Garner,.NC 27529
Raleigh,NC [phone]
Charlotte, NC [phone]
Aquatic Environmental Services, INC.
littp://lakework.com/
2050 Howell Bridge Road
Ball Ground, GA 30107
'United States
Phone: [phone]
Platinum.Ponds and Lake Management
https:l/www.platinuinl akemanagetnent.corn/solutions/fisheries/e lectrolishiiig
Greenville,SC Charlotte, NC
1361 W. Hampton Blvd, Suite F 3611 Mt Holly-Huntersville Rd, Ste. 204
Greer, SC 29650 Charlotte,NC 28216
864-381-7663 704-816-0526
Solitude Lake Management
https://www_soIitudelakemanagenlent.com/
Charlotte:.980.248.2979
Raleigh: 984.444.2548
10IPag.e
Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Taxonomic References for Fish Identification
Boschung, H. T. and R. L., Mayden. 2004.
Fishes of Alabama. Smithsonian Books, Birmingham,AL.
Marcy, B. C., D. E. Fletcher, F. D. Martin, M. H. Pallor, M. J. M. Reichert. 2005.
Fishes of the Middle Savannah River Basin with Emphasis on the Savannah River
Site. University of Georgia Press. Athens, GA.
Menhinick, E. F. 1991. The Freshwater Fishes of North Carolina. North Carolina
Wildlife Resources Commission, Raleigh, N.C.
Murphy, B. R. and D. W. Willis. 1996.
Fisheries Techniques. American Fisheries Society. Bethesda, MD.
q tY
Jenkins, R. E. and N. M. Burkhead. 1993.
Freshwater Fishes of Virginia. American Fisheries. Society, Bethesda, MD.
Page, L. M. and B. M. Burr. 1991. A Field Guide to Freshwater Fishes. Houghton
Mifflin Co., Boston, MA.
11I Page
Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

sTATt
ROY COOPER - !'
Governor ~ r
MICHAEL S.REGAN
Secretary
LINDA CULPEPPER -'"'°'.0.4..
Director NORTH CAROLINA
Environmental Quality
April 18,2019
Mr.Robert Williamson, Plant Manager
American Zinc Products,LLC
484 Hicks Grove Road
Mooresboro,North Carolina 28114
Subject: Final NPDES Permit
Permit.NC0089109
American Zinc.Products,LLC
Rutherford County
Grade II PCWPCS
Dear Mr. Williamson:
Division personnel have reviewed and approved your application for a renewal of the subject permit..
Accordingly, we are forwarding the attached NPDES permit. This permit is issued pursuant to the
requirements of North Carolina General Statute 143-215.1 and the Memorandum of Agreement
between North Carolina and the U.S. Environmental Protection Agency dated October 15,-2007 (or
as subsequently amended).
No major changes were made to the draft permit sent to you on January 29,2019.
The final permit maintains the following significant changes identified in the letter sent on
January 29,2019:
• The flow limit was increased to 0.98 MGD
• The requirement for fish tissue monitoring was added to the permit to address a comment
from the Regional Office.
• The requirement for pollutant scan was added to the permit to address a comment.from the
Regional Office.
• The limits for Total Cadmium were recalculated (reduced).based on the new flow estimate
and the recent update to the North Carolina water quality standards.A cadmium limit
compliance schedule was added to the permit.
• The limits for Total Chromium,Total Lead,and Total Fluoride were removed from the
permit based on the results of the Reasonable Potential Analysis.
• Quarterly monitoring for Hexavalent Chromium was added to the permit based on the
review of the effluent data.
E
!�cxfi�CarrAT4tkrertwInnr'tamoimenc:t2imui, tt1v.,vnnarlkelttfterlurtrs

Permit NC0089 109
STATE OF NORTH CAROLINA
DEPARTMENT OF ENVIRONMENTAL QUALITY
DIVISION OF WATER RESOURCES
PERMIT
TO DISCHARGE WASTEWATER UNDER THE
NATIONAL POLLUTANT DISCHARGE ELIMINATION SYSTEM
In compliance with the provision of North Carolina General Statute 143-215.1,
other lawful standards and regulations promulgated and adopted by the North Carolina
Environmental Management Commission, and the Federal Water Pollution Control Act, as
amended,
American Zinc Products, LLC
is hereby authorized to discharge wastewater from a facility located at
American Zinc Products, LLC
Forest City
Rutherford County
to receiving waters designated as the Broad River in the Broad River Basin in accordance with
effluent limitations, monitoring requirements, and other applicable conditions set forth in
Parts I, II, III and IV hereof.
This permit modification shall become effective June 1, 2019.
This permit and authorization to discharge shall expire at midnight on July 31, 2023.
Signed this day April 18, 2019.
hard copy signed by Julie Grzyb
Linda Culpepper, Director
Division of Water Resources
By Authority of the Environmental Management Commission
Page 1 of 9

Permit NC0089 109
SUPPLEMENT TO PERMIT COVER SHEET
All previous NPDES Permits issued to this facility, whether for operation or discharge are hereby
revoked. As of this permit issuance, any previously issued permit bearing this number is no longer
effective. Therefore, the exclusive authority to operate and discharge from this facility arises under the
permit conditions, requirements, terms, and provisions included herein.
American Zinc Products, LLC is hereby authorized to:
1. Operate the process effluent discharge system including the following
components:
Automatic sampler
Instrumented flow measurement, and
Diffuser
The facility is located near Forest City, Rutherford County; and
2. Discharge effluent from this location as specified on the attached map into the
Broad River which is classified WS-IV waters in the Broad. River Basin.
Page 2 of 9

Permit NC0089 109
Part I
A.(1.) EFFLUENT LIMITATIONS AND MONITORING REQUIREMENTS
[15A NCAC 02B .0400 et seq., 02B .0500 et seq.]
During the period beginning on the effective date of the permit and lasting until expiration, the Permittee
is authorized to discharge from outfall(s) serial number 001. Such discharges shall be limited and
monitoreds by the Permittee as specified below:
EFFLUENT LIMITS MONITORING REQUREMENTS
CHARACTERISTICS
Monthly Daily Measureme Sample Sample
Average Maximum nt Type Location'
Frequency
Flow (MGD) 0.98 Continuous Recording I or E
Total Suspended Solids, 2/Month Composite E
mg/L
NH3-N, mg/L Quarterly Composite E
Total Aluminum, µg/L Quarterly Composite E
Total Antimony, µg/L Quarterly Composite E
Total Arsenic, µg/L Quarterly Composite E
Total Cadmium 90.4 µg/L6 454.4 µg/LJ 2/Month Composite E
Chlorides, mg/L Quarterly Composite E
Chromium (VI), µg/L Quarterly Composite E
Total Cobalt, µg/L Quarterly Composite E
Total Copper, µg/L Quarterly Composite E
Total Fluoride, mg/L Quarterly Composite E
Total Iron, mg/L Quarterly Composite E
Total Lead, µg/L 2/Month Composite E
Total Nickel, µg/L Monthly Composite E
Total Tin, µg/L Quarterly Composite E
Total Zinc, µg/L 2/Month Composite E
pH2 6.0 s pH s 9.0 Daily Grab E
Chronic Toxicity3 Quarterly Composite E
Turbidity4 Monthly Grab E, U, D
NOTES:
1. Sample Locations: I - Influent, E - Effluent, U - upstream (50 ft. upstream of the
discharge), D- downstream (50 ft. downstream of the discharge).
2. The pH shall not be less than 6.0 standard units or greater than 9.0 standard units.
3. Chronic Toxicity (Ceriodaphnia) P/F @ 0.9%; Jan., April, July, and October; See
condition A. (2.) of the Supplement to Effluent Limitations and Monitoring Section of
this permit.
4. The discharge from this facility shall not cause turbidity in the receiving stream to exceed 50
NTU. If the instream turbidity exceeds 50 NTU due to natural background conditions, the
discharge cannot cause turbidity to increase in the receiving stream. Therefore, if the effluent
measurement exceeds 50 NTU, the Permittee shall sample upstream and downstream
turbidity in the receiving waterbody, within 24 hours, to demonstrate the existing turbidity
level in the receiving waterbody was not increased. All data shall be reported on the DMRs.
(See 15A NCAC 2B .0211 (21)).
NTU - Nephelometric Turbidity Unit.
Page 3 of 9

Permit NCO 089109
5. The permittee shall submit Discharge Monitoring Reports electronically using NC DWR's
eDMR application system. See Special Condition.A. (3.).
6. The limit becomes effective 90 months from the effective date of the permit. Please see A.
(6.) for Compliance Schedule.
THERE SHALL BE NO DISCHARGE OF FLOATING SOLIDS OR FOAM VISIBLE IN OTHER THAN
TRACE AMOUNTS.
A. (2.) CHRONIC TOXICITY PASS/FAIL PERMIT LIMIT (QUARTERLY)
[15A NCAC 02B .0200 et seq.]
The effluent discharge shall at no time exhibit observable inhibition of reproduction or significant
mortality to Ceriodaphnia dubia at an effluent concentration of 0.9%.
The permit holder shall perform at a minimum, quarterlrq monitoring using test procedures
outlined in the "North Carolina Ceriodaphnia Chronic Effluent Bioassay Procedure," Revised
December 2010, or subsequent versions or "North Carolina Phase II Chronic Whole Effluent
Toxicity Test Procedure" (Revised- December 2010) or subsequent versions. The tests will be
performed during the months of January, April, July and October. These months signify the
first month of each three-month toxicity testing quarter assigned to the facility. Effluent
sampling for this testing must be obtained during representative effluent discharge and shall be
performed at the NPDES permitted final effluent discharge below all treatment processes.
If the test procedure performed as the first test of any single quarter results in a failure or
ChV below the permit limit, then multiple-concentration testing shall be performed at a
minimum, in each of the two following months as described in "North.Carolina Phase II
Chronic Whole Effluent Toxicity Test Procedure" (Revised-December 2010) or subsequent
versions.
All toxicity testing results required as part of this permit condition will be entered on the Effluent
Discharge Monitoring Form (MR-1) for the months in which tests were performed, using the
parameter code TGP3B for the pass/fail results and THP3B for the Chronic Value. Additionally,
DWR Form AT-3 (original) is to be sent to the following address:
Attention: North Carolina Division of Water Resources
Water Sciences Section/Aquatic Toxicology Branch
1621 Mail Service Center
Raleigh, NC 27699-1621
Completed Aquatic Toxicity Test Forms shall be filed with the Water Sciences Section no later
than 30 days after the end of the reporting period for which the report is made.
Test data shall be complete, accurate, include all supporting chemical/physical measurements
and all concentration/response data, and be certified by laboratory supervisor and ORC or
approved designate signature. Total residual chlorine of the effluent toxicity sample must be
measured and reported if chlorine is employed for disinfection of the waste stream.
Should there be no discharge of flow from the facility during a month in which toxicity monitoring
is required, the permittee will complete the information located at the top of the aquatic toxicity
(AT) test form indicating the facility name, permit number, pipe number, county, and the
month/year of the report with the notation of"No Flow" in the comment area of the form. The
report shall be submitted to the Water Sciences Section at the address cited above.
Should the permittee fail to monitor during a month in which toxicity monitoring is required,
monitoring will be required during the following month. Assessment of toxicity compliance is
Page 4 of 9

Permit NCO 089109
based on the toxicity testing quarter, which is the three month time interval that begins on the
first day of the month in which toxicity testing is required by this permit and continues until the
final day of the third month.
Should any test data from this monitoring requirement or tests performed by the North Carolina
Division of Water Resources indicate potential impacts to the receiving stream, this permit may be
re-opened and modified to include alternate monitoring requirements or limits.
NOTE: Failure to achieve test conditions as specified in the cited document, such as minimum
control organism survival, minimum control organism reproduction, and appropriate
environmental controls, shall constitute an invalid test and will require immediate follow-up
testing to be completed no later than the last day of the month following the month of the initial
monitoring.
A. (3.)ELECTRONIC REPORTING OF DISCHARGE MONITORING REPORTS
[G.S. 143-215.1(b)]
Federal regulations require electronic submittal of all discharge monitoring reports (DMRs) and
program reports. The final NPDES Electronic Reporting Rule was adopted and became effective on
December 21, 2015.
NOTE: This special condition supplements or supersedes the following sections within Part II of
this permit (Standard Conditions for NPDES Permits):
• Section B. (11.) Signatory Requirements
• Section D. (2.) Reporting
a Section D. (6.) Records Retention
• Section E. (5.) Monitoring Reports
1. Reporting Requirements [Supersedes Section D. (2.) and Section E. (5.) (all
The permittee shall report discharge monitoring data electronically using the NC DWR's
Electronic Discharge Monitoring Report (eDMR) internet application.
Monitoring results obtained during the previous month(s) shall be summarized for each
month and submitted electronically using eDMR. The eDMR system allows permitted facilities
to enter monitoring data and submit DMRs electronically using the internet. Until such time
that the state's eDMR application is compliant with EPA's Cross-Media Electronic Reporting
Regulation (CROMERR), permittees will be required to submit all discharge monitoring data to
the state electronically using eDMR and will be required to complete the eDMR submission by
printing, signing, and submitting one signed original and a copy of the computer printed
eDMR to the following address:
NC DEQ / Division of Water Resources / Water. Quality Permitting Section
ATTENTION: Central Files
1617 Mail Service Center
Raleigh, North Carolina 27699-1617
If a permittee is unable to use the eDMR system due to a demonstrated hardship or due to the
facility being physically located in an area where less than 10 percent of the households have
broadband access, then a temporary waiver from the NPDES electronic reporting requirements
may be granted and discharge monitoring data may be submitted on paper DMR forms (MR 1,
1.1, 2, 3) or alternative forms approved by the Director. Duplicate signed copies shall be
Page 5 of 9

Permit:NC0089109
submitted to the mailing address above. See "How to Request a Waiver from Electronic
Reporting' section below.
Regardless of the submission method, the first DMR is due on the last day of the month
following the issuance of the permit or in the case of a new facility, on the last day of the
month following the commencement of discharge.
Starting on December 21, 2020, the permittee must electronically report the following
compliance monitoring data and reports, when applicable:
• Sewer Overflow/Bypass Event Reports;
• Pretreatment.Program Annual Reports; and.
• Clean.Water Act(CWA) Section 316(b) Annual Reports.
The permittee may seek an electronic reporting waiver from the Division (see "How to Request
a Waiver from Electronic Reporting' section below).
2. Electronic Submissions
In accordance with 40 CFR 122.41(1)(9), the permittee must identify the initial recipient at the
time of each electronic submission. The permittee should use the EPA's website resources to
identify the initial recipient for the electronic submission.
Initial recipient of electronic NPDES information from NPDES-regulated facilities means the
entity (EPA or the state authorized by EPA to implement the NPDES program) that is the
designated entity for receiving electronic NPDES data (see 40 CFR 127.2(b)J..
EPA plans to establish a website that will also link to the appropriate electronic reporting tool
for each type of electronic submission and for each state. Instructions:on,how to access and
use the.appropriate electronic reporting tool will be available as well. Information on EPA's
NPDES Electronic Reporting Rule is found at:
https:/1'www.federalregis ter.gov/documents/2015/10/22/2015-24954/national-pollutant-
discharge-elimination-system-npdes-electronic-reporting-rule
Electronic submissions must start by the dates listed in the "Reporting Requirements" section
above.
3. How to Request a Waiver from Electronic Reporting
The permittee may seek a temporary electronic reporting waiver from the Division. To obtain
an electronic reporting waiver, a permittee must first submit an electronic reporting waiver
request to the Division. Requests for temporary electronic reporting waivers must be
submitted in writing to the Division for written approval at least sixty (60) days prior to the
date the facility would be required under this permit to begin submitting monitoring data and
reports. The duration of a temporary waiver shall not exceed 5 years and shall thereupon
expire. At such time, monitoring data and reports shall be submitted electronically to the
Division unless the permittee re-applies for and is granted a new temporary electronic
reporting waiver by the Division. Approved electronic reporting waivers are not transferrable.
Only permittees with an approved reporting waiver request may submit monitoring data and
reports on paper to the Division for the period that the approved reporting waiver request is;
effective.
Information On.eDMR and the application for a temporary electronic reporting waiver are
found on the following web page:
http:J/deq.nc_govf about/divisions/water-resources/edmr
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Permit NC0089 109
4. Signatory Requirements [Supplements Section B. (11.) (b) and Supersedes Section B.
(11.) (d)]
All eDMRs submitted to the permit issuing authority shall be signed by a person described in
Part II, Section B. (11.)(a) or by a duly authorized representative of that person as described in
Part II, Section B. (11.)(b). A person, and not a position, must be delegated signatory
authority for eDMR reporting purposes.
For eDMR submissions, the person signing and submitting the DMR must obtain an eDMR
user account and login credentials to access the eDMR system. For more information on
North Carolina's eDMR system, registering for eDMR and obtaining an eDMR user account,
please visit the following web page:
http:/jden.nc.govj about]divisions/water-resources/edmr
Certification. Any person submitting an electronic DMR using the state's eDMR system shall
make the following certification. [40 CFR 122.22). NO OTHER STATEMENTS OF
CERTIFICATION WILL BE ACCEPTED:
"I certify, under penalty of law, that this document and all attachments were prepared under my
direction or supervision in accordance with a system designed to assure that qualified personnel
properly gather and evaluate the information submitted. Based on my inquiry of the person or
persons who manage the system, or those persons directly responsible for gathering the
information, the information submitted is, to the best of my knowledge and belief, true, accurate,
and complete. I am aware that there are significant penalties for submitting false information,
including the possibility of fines and imprisonment for knowing violations."
5. Records Retention [Supplements Section D. (6.)j
The permittee shall retain records of all Discharge Monitoring Reports, including eDMR
submissions. These records or copies shall be maintained for a period of at least 3 years from
the date of the report. This period may be extended by request of the Director at any time [40
CFR 122.411.
A. (4.) FISH TISSUE MONITORING
.S. 143-215.1 b
The facility shall conduct fish tissue monitoring once during the permit cycle and submit the results
with the NPDES permit renewal application. The objective of this monitoring is to evaluate potential
uptake of pollutants by fish tissue near the facility's discharge. The parameters analyzed in fish
tissue shall be arsenic, cadmium, and zinc. The monitoring shall be conducted in accordance with
the sampling plan approved by the Division. The plan should be submitted to the Division within
180 days from the effective date of the permit modification. Upon approval, the plan becomes an
enforceable part of the permit.
Copies of all the study plans, study results, and any other applicable materials should be
submitted to:
1) Electronic Version Only (pdf and CD)
Division of Water Resources
WQ Permitting Section - NPDES
1617 Mail Service Center
Raleigh, NC 27699-1617
2) Electronic Version (pdf and CD) and Hard Copy
Division of Water Resources
Water Sciences Section
1621 Mail Service Center
Raleigh, NC 27699-1621
Page 7 of 9

Perrnit NC0089109
A. (5.) PRIORITY POLLUTANT ANALYSIS
[G.S. 143-215.1(h)]
TheePerrnittee shall perform:one Effluent Pollutant Scan for all parameters listed below. The analytical
methods shall be in accordance with 40 CFR Part 136 and shall be sufficiently sensitive to determine
whether parameters are present in concentrations greater than applicable standards and criteria.
Unless otherwise indicated, metals shall be analyzed as "total recoverable_"
Ammonia(as N) Trans-1,2-dichloroethylene Bis (2-chloroethyl) ether
Chlorine (total residual, TRC) 1.,1-dichloroethylene Bis (2-chloroisopropyl) ether
Dissolved oxygen 1,2-dichloropropane Bis:(2-ethylhexyl)phthalate
Nitrate/Nitrite 1,3-dichloropropylene 4-bromophenyl phenyl ether
Kjeldahl nitrogen Ethylbenzene Butyl benzyl phthalate
Oil and grease Methyl bromide 2-chloronaphthalene
Phosphorus Methyl chloride 4-chlorophenyl phenyl ether
Total dissolved solids Methylene chloride Chrysene
Hardness 1,1,2,2-tetrachioroethane Din-butyl phthalate
Antimony Tetrachloroethyiene Di-n-octyl phthalate
Arsenic Toluene Dibenzo(a,h)anthracene
Beryllium 1,1,1-trichloroethane 1,2-dichlorobenzene
Cadmium 1,1,2-trichloroethane 1,3-dichlorobenzene
Chromium Trichloroethylene 1 4-dichlorobenzene
Copper Vinyl chloride 3,3-dichlorobenzidine
Lead Acid-extractable compounds: Diethyl.phthalate
Mercury (EPA Method 1631E) P-chloro-m-cresol Dimethyl phthalate
Nickel 2-chlorophenol 2,4-dinitrotoluene
Selenium 2,4-dichlorophenol 2,6-dinitrotoluene
Silver 2,4-dimethylphenol 1,2-diphenylhydrazine
Thallium 4,6-dinitro-o-cresol Fluoranthene-
Zinc 24-dinitrophenol Fluorene.
Cyanide 2-nitrophenol Hexachlorobenzene
Total phenolic compounds 4-nitrophenol Hexachlorobtitadiene
Volatile organic compounds: Pentachlorophenol Hexachlorocyclo-pentadicne
Acrolein Phenol Hexachloroethane
Acrylonitrile 2,4,6-trichlorophenol Indeno(1;2,3-cd)pyrene
Benzene Base-neutral compounds: lsophorone.
Bromoforrn Acenaphthene Naphthalene
Carbon tetrachloride Acenaphthylene Nitrobenzene
Chlorobenzene Anthracene N-nitrosodi-n-propylemine
Chlorodi.bromomethane l3enzidine N-rxitrosodimethylamine
Chloroethane Benzo(a)anthracene N-nitrosodiphennylamine
2-chloroethylvinyl ether Benzo(a)pyrene Phenanthrene
Chloroform 3,4 benzofluoranththe Pyrene
Dichlorobromomethane Benzo(ghi)perylene 1,2,4-trichlorobenzene
1,1-dichloroethane Benzo(k)fluoranthene
1,2-dichloroethane Bis (2-chloroethoxy)
methane
Reporting. The effluent pollutant scan shall be performed once during the permit cycle and test
results shall be submitted to.the Division within 270 days of the sampling.
Page 8 of 9

Permit NC0089109
A. (6.) CADMIUM COMPLIANCE SCHEDULE
[G.S. 143-215.1(b)]
Activity Description Deadline
1. Commence production of Zinc at Mooresboro Facility. June 1, 2019
2. Ramp-up production to 75%. December 1,2019
3. Stabilize plant operation and commence evaluation of permit June 1, 2020
compliance.
4. Complete evaluation period. June 1, 2021
5. Prepare a Preliminary Engineering Report (PER) of process December 1, 2021
alternatives and/or pollution prevention/waste minimization (parallel with activity 4)
alternatives designed to achieve compliance. This report would
include the results of the compliance evaluation. Submit to DWR
for review and comment.
6. Agency review and addressing comments February 1, 2022
7. Bench scale test work of process alternatives (start in parallel April 1, 2020
with Activity 6).
8. Evaluate business case and funding requirements for April 1, 2022
technically suitable alternative(s). (parallel with activity 7)
9. Complete pilot test work for selected technology option(s) and August 1, 2022
final technology selection. Develop a summary of the results of
this evaluation. Submit summary to DWR for review.
10. Agency review and addressing comments October 1, 2022
11. Detailed engineering and design of selected option. Submit to February 1, 2023
DWR for comment.
12. Agency review and addressing comments April 1, 2023
13. Prepare capital project application and secure funding for June 1, 2023
selected option, obtain building permits and all needed (much of this work will be done in
approvals for implementation. parallel with activities 11,12)
14. Project implementation, including design completion, June 1, 2024
procurement and construction.
15. Commission and ramp-up. June 1, 2025
16. Stabilize operation and evaluate performance. December 1, 2025
17. Make necessary final modifications to optimize and obtain full August 1, 2026
operational status.
18. Achieve full compliance. December 1, 2026
Page 9 of 9

The Division is unable to grant your request for changing the Fish Tissue Monitoring Special
Condition., the Division used the standard language that applies to all the facilities required to monitor
fish tissue.
If any parts, measurement frequencies or sampling requirements contained in this permit are
unacceptable to you,you have the right to an adjudicatory hearing upon written request within thirty
(30) days following receipt of this letter. This request must be in the form of a written petition,
conforming to Chapter 150B of the North Carolina General Statutes, and filed with the Office of
Administrative Hearings (6714 Mail Service Center, Raleigh, North. Carolina 27699-6714). Unless
such demand is made, this decision shall be final and binding.
Please note that this permit is not transferable except after notice to the Division. The Division may
require modification or revocation and reissuance of the permit. This permit does not affect the legal
requirements to obtain other permits which may be required by the Division of Water Resources or
any other Federal, State, or Local governmental regulations.
If you have any questions concerning this permit, please contact Sergei Chernikov at [phone]
or via email at [e-mail].
Sincerely,
Linda Culpepper,Director.
Division of Water Resources,NCDEQ
Hardcopy: NPDES Files
Central Files
E-copy: DWR/Asheville Regional Office/Water Quality
DWR/Aquatic Toxicology Branch
Page 2 of 2

Appendix B
Broad River SOP - EA
TRC Environmental Corporation I American Zinc Products,LLC
Broad River NPDES Fish Tissue Study Summary
\\GREENVILLE-FP1\WPGVLAPJT2\479013‘0000\R4790130000-001_FINAL.DOCX October 2022

Standard Operating Procedures for NPDES Permit
(#NC0089109) Required Fish Tissue Collection
Broad River, Rutherford County, North Carolina
Prepared for
TRC Companies, Inc.
50 International Drive, Suite 150
Greenville, SC, 29615
Prepared by
EA Engineering, Science, and Technology, Inc., PBC
225 Schilling Circle, Suite 400
Hunt Valley, Maryland 21031
410-584-7000
May 2022
Version: FINAL
EA Project No. 16244.01
Broad River,Rutherford County,North Carolina SOP-NPDES Fish Tissue Collection

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Broad River,Rutherford County,North Carolina SOP-NPDES Fish Tissue Collection

Standard Operating Procedures for NPDES Permit
(#NC0089109) Required Fish Tissue Collection
Broad River, Rutherford County, North Carolina
Prepared for
TRC Companies, Inc.
50 International Drive, Suite 150
Greenville, SC, 29615
Prepared by
EA Engineering, Science, and Technology, Inc., PBC
225 Schilling Circle, Suite 400
Hunt Valley, Maryland 21031
410-584-7000
-/4ce
12 May 2022
Martha McCauley Date
Project Manager
7 �mNp�Qe 12 May 2022
T. Vondruska Date
Senior Technical Reviewer
May 2022
Version: FINAL
EA Project No. 16244.01
Broad River,Rutherford County,North Carolina SOP-NPDES Fish Tissue Collection

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CONTENTS
Page
LIST OF TABLES iii
LIST OF FIGURES iv
LIST OF APPENDICES v
LIST OF ACRONYMS AND ABBREVIATIONS vii
1. INTRODUCTION 1
1.1 NPDES Permit Requirements 1
1.2 Objective 1
2. METHODS AND MATERIALS 3
2.1 Sampling Locations 3
2.2 Sampling Schedule 4
2.3 Collection Methods 6
2.4 Target Fish Species 6
2.5 Field Sample Processing 7
2.5.1 Label Format 7
2.5.2 Chain-of-Custody 8
2.5.3 Sample Shipment and Delivery 8
3. LABORATORY PROCESSING AND ANALYSIS 9
4. QUALITY CONTROL 11
4.1 Equipment Calibration 11
4.1.1 Measuring Boards 11
4.1.2 Measuring Scales 11
4.2 Field Work 11
4.3 Field and Laboratory Data 12
5. HEALTH AND SAFETY 13
5.1 Boating and Electrofishing 1
5.2 Weather Hazards 13
5.3 Heat Stress 13
5.3.1 Heat Rash(Prickly Heat) 14
5.3.2 Heat Cramps 14
5.3.3 Heat Exhaustion 14
5.3.4 Heat Stroke 14
5.3.5 Preventative Measures 15
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5.4 Biological Hazards—Insect Bites/Stings 15
5.5 Biological Hazards—Snakes 16
5.6 Biological Hazards—Fish 16
5.7 Poison Ivy and Related Plants 16
5.8 Allergic Reactions 17
5.9 Emergency Response Plan 18
5.10 Coronavirus Disease 2019 (COVID-19) 18
6. COMMUNICATION AND CONTACT INFORMATION 19
7. REFERENCES 21
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LIST OF TABLES
Table 1. Monthly Mean River Discharge and Stage of the Broad River 4
Table 2. Proposed Fish Tissue Sampling Schedule 5
Table 3. Minimum Lengths for Target Fish Species 6
Table 4. Site, Species, and Contract Codes for External Labels 8
Table 5. Hydration Targets based on Air Temperature and Time Periods between Breaks 15
Table 6. Work/Rest Schedule based on Air Temperature 15
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LIST OF FIGURES
Figure 1. Upstream Sampling Location 3
Figure 2. Downstream Sampling Location 4
Figure 3. Daily Mean River Discharge of the Broad River, 1 March-30 June 2021 5
Broad River,Rutherford County,North Carolina SOP-NPDES Fish Tissue Collection

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LIST OF APPENDICES
Appendix A. NCWRC Scientific Fish Collection License
Appendix B. Field Data Sheet Templates
Appendix C. Internal Label Template
Appendix D. Chain-of-Custody Template—Pace Analytical Services
Appendix E. Laboratory Reporting Limits—Pace Analytical Services
Appendix F. SOPs and QC Manual—Pace Analytical Services
Appendix G. Equipment Checklist
Appendix H. EA SOPs
Appendix I. NCWRC Watercraft and Trailer Registrations
Appendix J. Health and Safety Documents
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LIST OF ACRONYMS AND ABBREVIATIONS
°F Degrees Fahrenheit
As Arsenic
AZP American Zinc Products
Cd Cadmium
cfs Cubic feet per second
COVID-19 Coronavirus Disease 2019
DC Direct Current
EA EA Engineering, Science, and Technology, Inc., PBC
EDD Electronic Data Deliverable
FDA U.S. Food and Drug Administration
g Gram(s)
GPS Global Positioning System
hr. Hour(s)
NBS National Bureau of Standards
NC North Carolina
NCDWR North Carolina Division of Water Resources
NCWRC North Carolina Wildlife Resources Commission
NPDES National Pollutant Discharge Elimination System
oz. Ounce(s)
Pace Pace Analytical Services
PPE Personal Protective Equipment
PQL Practical Quantitation Limit
QA/QC Quality Assurance/Quality Control
SOP Standard operating procedures
STR Senior Technical Reviewer
TRC TRC Companies, Inc.
USGS U.S. Geological Survey
Zn Zinc
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1. INTRODUCTION
The American Zinc Products (AZP),LLC was required to develop a sampling plan to maintain
compliance with the requirements issued in National Pollutant Discharge Elimination System
(NPDES)permit#NC0089109. The plan was submitted to the North Carolina Division of Water
Resources (NCDWR) Water Quality Permitting Section and Water Sciences Section for review
and comment. Comments were addressed in December 2019 and a final version of the sampling
plan was submitted in April 2020. The primary component of the sampling plan required a fish
collection for evaluation of target metal concentrations present within the fish tissue. EA
Engineering, Science, and Technology, Inc.,PBC (EA) will be performing fish tissue collection
and facilitation services to meet the tissue collection and analysis requirements.
1.1 NPDES PERMIT REQUIREMENTS
In accordance with NPDES permit#NC0089109, the following Fish Tissue Monitoring
Condition requirement was stipulated therein:
A. (4)FISH TISSUE MONITORING
[G. S. 143-215. 1(b)j
The facility shall conduct fish tissue monitoring once during the permit cycle and submit the
results with the NPDES permit renewal application. The objective of this monitoring is to
evaluate potential uptake of pollutants by fish tissue near the facility's discharge. The
parameters analyzed in fish tissue shall be arsenic, cadmium, and zinc. The monitoring shall
be conducted in accordance with the sampling plan approved by the Division. The plan should
be submitted to the Division within 180 days from the effective date of the permit modification.
AZP provided an updated revised fish tissue monitoring plan to the NCDWR NPDES Water
Quality Permitting Section in April 2020 (AZP 2020). EA has reviewed the AZP Sampling Plan
and integrated it into this SOP.
1.2 OBJECTIVE
The primary objective is to fulfill the NPDES #NC0089109 Fish Tissue Monitoring Condition
requirement, which consists of collecting fish tissue samples upstream and downstream of the
AZP discharge in the Broad River to be analyzed for arsenic (As), cadmium(Cd), and zinc (Zn).
Broad River,Rutherford County,North Carolina SOP-NPDES Fish Tissue Collection

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2. METHODS AND MATERIALS
The sampling locations, sampling schedule, collection methods, target species, sample
processing procedures, and shipping details are described below. Sampling will be performed at
two locations near the AZP facility within Broad River during Spring of 2022 with a target of
mid-May. Three species of edible-size fish representing three different trophic levels will be
targeted for tissue collection. The primary sampling gear will be boat electrofishing, which may
be augmented by hook-and-line, gill nets, hoop nets, and trap nets.
2.1 SAMPLING LOCATIONS
Fish samples will be obtained from two locations on the Broad River, one upstream(Figure 1)
and the other downstream of the AZP facility(Figure 2). The upstream location will extend from
the Jack McKinney Road Bridge to approximately one mile downstream of the bridge (Figure 1):
jUpstream Start`
\too1
111
4Upstream End
Figure 1. Upstream Sampling Location
Based on AZP's reconnaissance and the site visit on 22 March, the primary access area to the
upstream sampling location will be via Jones Farms (0 Montgomery Rd. Ext.,Mooresboro,NC
28114) for which AZP has obtained permission for access and use. This area is depicted in the
photographs below:
•1'
.:? tom .."$q,,,iC 1 h ! l ✓.
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Based on AZP (2020),the downstream sampling location will start in the vicinity of the
Highway 221 Bridge (Global Positioning System [GPS] waypoint Latitude 35.20585 and
Longitude -81.83773), and end approximately one mile downstream of the Highway 221 Bridge
(GPS waypoint Latitude 35.205356 and Longitude -81.821633) (Figure 2):
t � rrr �
Sampling Play Downstream Slant
\j r�-�. f�-� pMg Plan Diwnslream End
Figure 2. Downstream Sampling Location
The primary access area to the downstream sampling area will be via Ameri-con Materials (505
Hines Rd., Mooresboro,NC 28114) for which AZP has obtained permission for access and use.
This area is depicted in the photographs below:
�a ' • l .� { W •
5 •$ins-K3 4
1144.
i $ •
� art' $ ' '' r�'i. 'N� Tit
2.2 SAMPLING SCHEDULE
Based on monthly mean river stage and flow data(USGS 02151500 Broad River near Boiling
Springs,NC; Table 1) and river discharge data from 2021 (Figure 3), it was determined that
sampling would be conducted no earlier than approximately mid-May to minimize river levels
that would be unsafe and/or too turbid for sampling. The proposed sampling scheduled is
provided in Table 2.
Table 1. Monthly Mean River Discharge and Stage of the Broad River
Monthly Mean River Discharge (cfs) Monthly Mean River Stage (ft)
Years Mar Apr May Jun Years Mar Apr May Jun
1925-2021 2,020 1,890 1,560 1,290 1925-2021 2.85 2.82 2.65 2.33
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USGS
USGS 02151500 BROAD RIVER NEAR BOILING SPRINGS,NC
30080
. 28888
,
18888
\\)\1
4e.
11
fil#111 , (1)
-5 g141-1
688
Mar 13 Mar 27 Apr 18 Rpr 24 May 88 May 22 Jun 05 Jun 19
2021 2021 2021 2021 2021 2021 2821 2821
—Discharge —Period of approved data
Figure 3. Daily Mean River Discharge of the Broad River, 1 March-30 June 2021
Table 2. Proposed Fish Tissue Sampling Schedule
Date Activity(a) Personnel
5/14-5/15 Travel to Broad River site EA/TRC
5/16 8:00 AM Kickoff Tailgate Meeting at AZP EA/TRC/AZP
5/16-5/17 Upstream Site Sampling, Overnight Gear EA
5/18 -5/19 Downstream Site Sampling, Overnight Gear EA
5/19 Sample Processing and Evaluation EA
5/20 AM Status Tailgate Meeting at Upstream Launch Site EA/TRC/AZP
5/20-5/21 Upstream Site Sampling, Overnight Gear EA
5/22- 5/23 Downstream Site Sampling, Overnight Gear EA
5/23 Sample Processing and Evaluation EA
5/24 AM Closeout Meeting at AZP EA/TRC/AZP
5/24 Sample Shipping EA
5/24-5/25 Demobilization and Site Departure(') EA/TRC
EA=EA Engineering, Science,and Technology,Inc.,PBC;TRC=TRC Companies,Inc.;AZP=American Zinc
Products
(a)Daily email updates will be provided to TRC and AZP regarding numbers of target species and any issues
encountered.
(b)This could be delayed by inclement weather or additional days of sampling if requested by AZP.
EA will track river stage and discharge conditions via the Broad River USGS gaging station
prior to sampling, as well as predicted conditions via the Advanced Hydrologic Prediction
Service. In addition, EA will also contact Mr. Charles Howell (AZP Environmental Manager)to
gauge water clarity via turbidity readings. Turbid conditions can mask boating hazards (e.g.,rock
outcrops, deadfalls, shallow riffle/run areas), and make electrofishing inefficient in terms of the
ability to observe stunned fish.
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2.3 COLLECTION METHODS
EA's primary collection method will consist of DC-pulsed electrofishing equipment that will
either be boat-mounted(16-ft jon boat with 9.9 hp outboard) or wadeable. However, gill nets,
trap nets, hoop nets, and limb/trot lines may also be deployed overnight at each location. The
sampling effort is estimated to encompass eight days, which will consist of four days of
electrofishing and potentially two overnight sets of gill nets, trap nets, hoop nets, and/or limb/trot
lines at each location. EA has obtained a Scientific Fish Collection License from the North
Carolina Wildlife Resources Commission(NCWRC) that specifies the designated species,
numbers of specimens, collection methods, and sampling locations (Appendix A). EA personnel
assigned to this project have the knowledge, skills, and experience with all sampling techniques
proposed to obtain the fish samples. In addition, all personnel involved with electrofishing or
other methods employed are familiar with operational and safety procedures.
2.4 TARGET FISH SPECIES
The three target species are Largemouth Bass, Redbreast Sunfish, and Notchlip Redhorse. They
each represent different trophic levels—top predator, mid-trophic insectivore, and mid-trophic
omnivore, respectively. If these three primary target species are absent from each location or a
minimum of six appropriately-sized individuals from each species are not attainable, then
secondary target species will be substituted: Bluegill, Brassy Jumprock, Flat Bullhead,
Smallmouth Bass, White Sucker, catfish, carp, or other species. Edible-sized individuals,based
on the North Carolina Inland Fishing, Hunting& Trapping Regulations Digest 2021-2022, or
the 2019 NCDWR fish tissue monitoring data (NCDWR 2019), will be retained for each game
fish species; however, minimum lengths for nongame species will be those reported by the
NCDWR(2019) fish tissue monitoring data:
Table 3.Minimum Lengths for Target Fish Species
Species Minimum Length Inches Minimum Length Inches
(Regulations Digest) (2019 NCDWR)
Largemouth Bass 14 (allows 2 fish<14 [356 mm]) 8.5 (215 mm)
Redbreast Sunfish none 5.0 (128 mm)
Notchlip Redhorse none 10.8 (275 mm)
Bluegill none 5.4 (138 mm)
Brassy Jumprock none 12.7 (323 mm)
Flat Bullhead none 6.7 (171 mm)
Smallmouth Bass 14 (allows 2 fish<14 [356 mm]) 8.5 (216 mm)
White Sucker none 11.7 (1 fish; 297 mm)
Golden Redhorse none 14.3 (364 mm)
The goal is to obtain six to 10 individual fish for each of the three different target species at the
two sampling locations. Therefore, 18 to 30 individuals will be selected for laboratory analysis
from each location. If field sampling is not successful in obtaining sufficient individuals (18 per
location), the NCDWR will be consulted by TRC Companies, Inc. (TRC)/AZP personnel to
determine appropriate modifications. Because sufficient individuals of each species may not be
attainable at each location, the sampling effort will be well documented by EA. To that end,
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Field Data Sheet# 1 and Field Data Sheet# 2 (Appendix B) from the Sampling Plan will be
used to document the fish tissue collection results. One set of data sheets (2 pages)will be
completed for each location for each day sampling is conducted. In addition, the extent of each
actual sampling reach will be measured and reported using GPS positioning equipment. EA will
provide a map and photographs to document the sampling activities within both locations.
2.5 FIELD SAMPLE PROCESSING
Fish tissue samples collected for analyses will be processed and delivered/shipped to Pace
Analytical Services (Pace) in a manner to prevent decomposition or contamination. During all
activities, EA will avoid potential sources of arsenic, cadmium, and zinc contamination (e.g., no
use of galvanized buckets,no cigarette smoking, powderless nitrile gloves will be worn during
all fish handling activities). Fish will be removed from plastic live wells,holding tanks, or
buckets, rinsed with ambient water to remove foreign matter, and placed on a clean or new
protective surface (i.e.,plastic wrap) for sorting, weighing, length measurements, and wrapping.
All samples will be processed individually as noted below:
• An individual whole fish wet weight will be determined for each fish to the nearest gram
and recorded on Field Data Sheet#2 (Appendix B). All individual samples will be
weighed on scales/balances that are properly calibrated and of adequate accuracy and
precision to weigh samples to the nearest gram.
• Total length will be determined for each fish to the nearest millimeter using a calibrated
measuring board and recorded on Field Data Sheet#2 (Appendix B). Individual fish will
be identified to species by experienced staff using current identification manuals and other
appropriate taxonomic literature (e.g., Boschung and Mayden 2004; Jenkins and Burkhead
1993; Marcy et al 2005; Menhinick 1991; Page and Burr 2011).
• Fish with lesions or lacerations will not be kept for analysis.
• Each fish will be placed in a clean plastic bag that will be externally labeled with the
sample number, species name, weight, and length (Appendix C). The self-adhesive label
will be additionally secured to the bag by clear packing tape. The labeled bag will be
placed in a second clean plastic bag to protect the label. The sample information will then
be documented on a chain-of-custody Form (Appendix D).
2.5.1 Label Format
External labels will include a sample identification code that will be unique to each specimen:
SITE—SPP-##-DDMMMYY-CONT: where, SITE =Location Code, SPP= Species Code, ##
=chronological specimen number for this species, DDMMMYY=day,month, and year, and
CONT =Contract Code (NPDES).
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For example, the sample identification code for the third Bluegill for the NPDES contract at the
upstream sampling location of Broad River on 15 May 2022, will be: BR-US—BGL-03-
15MAY22-NPDES.
Table 4. Site, Species, and Contract Codes for External Labels
Location Species Species
Site Code Species Code Species Code
Broad River-Upstream BR-US Bluegill BGL Notchlip Redhorse NLR
Broad River-Downstream BR-DS Redbreast Sunfish RBS Brassy Jumprock BSJ
Contract Contract Smallmouth Bass SMB White Sucker WHT
Code
NPDES NPDES Largemouth Bass LMB Golden Redhorse GDR
Flat Bullhead FLB
2.5.2 Chain-of-Custody
EA will complete a chain-of-custody provided by Pace (Appendix D)that will be included with
the fis
h tissue samples when sent to the analytical laboratory. The chain-of-custody will include
the unique sample number, date, and time of collection, and the name and signature of the field
collector. The analytical laboratory will counter-sign and provide copies to EA with the
analytical report.
2.5.3 Sample Shipment and Delivery
Whole fish samples will be double-bagged and frozen in an on-site chest freezer during the
sampling effort. Upon sample effort completion, fish will be placed on wet ice and chilled to
4°C in insulated and water-tight coolers. Coolers will be lined with trash bags to contain ice
melt and cushioned with absorbent pads and bubble wrap as needed. Packed coolers will be
sealed with packaging tape to ensure proper closure of cooler lid and cooler plug (if present).
A completed chain-of-custody(Appendix D) will be placed in a Ziploc®bag and taped to the
lid of the cooler. Coolers will be shipped for next day delivery to Pace via FedEx or UPS.
2.6 DELIVERABLES
EA will provide TRC the field datasheets, GPS waypoints, maps,photographs, additional field
notes (those not included on the field datasheets), and the analytical report from the laboratory.
EA will also develop summary tables describing number and type of species collected at each
sampling location and designation of fish that were sent to the laboratory for analysis. All
information will be reviewed by appropriate personnel prior to submittal.
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3. LABORATORY PROCESSING AND ANALYSIS
Fish tissue samples will be analyzed by Pace, which maintains accreditation in North Carolina. It
should be noted that based on a review of applicable fields of accreditation, NCDWR does not
certify for tissue analysis. All fish tissue samples will be analyzed for total arsenic, cadmium,
and zinc. Laboratory analytical capabilities have been evaluated and compared to the NCDWR
Practical Quantitation Limit(PQL)reporting limits for arsenic, cadmium, and zinc (Appendix
E). Two fish tissue samples will be duplicated for laboratory analysis at each location regardless
of the total number of individual fish collected at each location. Therefore, a maximum of 64
samples will be analyzed by the laboratory. The laboratory will be responsible for filleting. Their
Laboratory Standard Operating Procedures (SOPs) for relevant analytical methods and the
Laboratory Quality Manual have been included in Appendix F. All bass and sunfish species will
be processed as skin-on fillets. Pursuant to our discussion on 13 December 2021, all suckers and
carp will also be processed as skin-on fillets. In contrast, all catfish and bullheads will be
processed as skin-off(no skin included) fillets. Also based on that discussion, only the right fillet
will be analyzed for all samples with the left fillet saved for potential future analysis. However,
for those instances where the right fillet does not provide sufficient mass for analysis, then both
fillets will be combined and analyzed. The minimum mass per sample for Pace is 2g.
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4. QUALITY CONTROL
This SOP manual provides EA's staff with guidance regarding sampling methodologies, the
equipment required, and specifications regarding acceptable calibration intervals and procedures
for various field gear (e.g., scales/balances), communication, quality control and assurance
measures, as well as health and safety information. It also establishes various other protocols to
be followed through this project.
In accordance with EA's Corporate Quality Management Plan (the master document for all
disciplines at EA), we use SOPs to efficiently promote quality through consistency. This SOP is
a project-specific document that integrates the methodologies and guidance with detailed
specifications. It ensures that the AZP NPDES Permit objectives will be met and that the
integrity of EA will be maintained. It also allows each staff member to understand his or her
duties and responsibilities, as well as providing a means for minimizing disruptions associated
with staff turnover.
4.1 EQUIPMENT CALIBRATION
4.1.1 Measuring Boards
Measuring boards and rulers used to determine lengths of fish are calibrated once after purchase,
manufacture, or repair. The measuring board is calibrated with a ruler or tape that is certified by
the manufacturer to be traceable to the National Bureau of Standards (NBS). Ten randomly
selected points between 20 and 600 mm are visually checked against the standard ruler. Only
those measuring boards that are within the stated accuracy of the standard ruler(±1.5 mm) are
used. Measuring boards that are outside the accuracy of the standard ruler are discarded. The
results of the calibration are entered on a Calibration Record Form.
4.1.2 Measuring Scales
Spring scales are calibrated semi-annually by weighing 3-5 weights that are within the
appropriate weight range. All weights are class T or better, and are certified by the manufacturer
to be traceable to the NBS. The readings are compared to the known weight and the results are
recorded on a Calibration Record Form. Scales having less than 10 percent error are retained in
service whereas those that exceed 10 percent error are adjusted and recalibrated, or removed
from service and destroyed.
4.2 FIELD WORK
Each field crew member will be expected to have read and have on hand at all times a copy of
the SOP. A master field equipment checklist has been prepared so that the field crew has all the
appropriate equipment needed for sampling (Appendix G). All specifications detailed
previously will be carefully followed. Additional care will be taken to sample at the locations
specifically needed to meet NPDES requirements; GPS coordinates are provided in AZP (2020)
and Section 2.1 (see Figure 2) of the SOP. Two experienced(10 years or more) EA biologists
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will conduct the field collections, which will ensure strict adherence to the SOP,proper
identification of fish captured,and sound judgment regarding collection procedures and during
potentially hazardous conditions. The sampling crew will be required to have our current
NCWRC Scientific Fish Collection License on hand when in the field (Appendix A).
4.3 FIELD AND LABORATORY DATA
EA will compare all (i.e., 100%) hand-entered field data against the hard copy field or
laboratory data sheets. These comparisons will be kept as part of the project file, documented on
a data processing log sheet, and be made available to the client at their request. In addition, the
comparisons will be done by an experienced fisheries biologist; data will not be checked by a
non-biologist. EA routinely provides this type of QC for all its projects.
EA will review and perform quality control checks on the analytical data provided by Pace. After
the data are received, EA will perform a data assessment screening on the laboratory's analytical
data packages and electronic data deliverables (EDDs). Data will be reviewed for completeness
by comparing them to the chain-of custody. Review of data usability will be accomplished by
comparing the contents of the analytical data packages and quality assurance/quality control
(QA/QC) results to the requirements contained in the Quality Assurance Project Plan or Work
Plan, the respective methods, and the laboratory SOPs. EA will resolve any discrepancies with
the laboratory and will inform AZP of any issues or delays.
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5. HEALTH AND SAFETY
Due to limited boating access of the study area, the use of electrofishing equipment, and
maneuvering across forested and developed regions, personnel may potentially be exposed to a
variety of hazards. Since crew safety is of the utmost importance,no personnel will be required
or instructed to work in surroundings or under conditions that are unsafe or dangerous to his or
her health and each individual employee will be responsible for complying with applicable safety
requirements, wearing prescribed safety equipment, and preventing avoidable accidents.
5.1 BOATING AND ELECTROFISHING
EA's Corporate Vessel and Operations Manual and Small Boat Operations SOP (Appendix H)
provides the basic policies and procedures regarding safety and health during the performance of
work involving boating and watercraft activities, which are to be followed during this study.
Prior to sampling, the EA field crew will notify on-site AZP and TRC staff of EA's planned
sampling route for the day. At a minimum, all boats will be equipped with required Coast Guard
safety equipment(e.g., approved personal floatation devices, fire extinguisher, signal flares,
horn, etc.) and a first aid kit. EA staff on board the boat will also have cell phones available to
contact on-site AZP and TRC staff or emergency services in the event of an emergency. A GPS
will be on board to provide emergency personnel with GPS location information if needed.
EA's Electrofishing Field Manual (Appendix H)provides details on basic concepts and safety
issues involving electrofishing systems, including safe equipment operations and appropriate
personal protective equipment (PPE) during active sampling.
Watercraft and Trailer Registrations are provided in Appendix I.
5.2 WEATHER HAZARDS
Weather conditions will be taken into consideration during each sampling effort. Heavy rains,
electrical storms, high winds, and extreme temperatures, for example, may create extremely
dangerous situations for employees. Inclement weather may also impair equipment performance.
Whenever unfavorable conditions arise, the Crew Leader will evaluate both the safety hazards
and ability of the employees to effectively perform given tasks under such conditions. Work on
the sampling vessel will be suspended during thunderstorms, tornadoes, hurricanes, or other
severe weather events. Weather conditions will be monitored via broadcast from marine radio
channel to identify the approach of severe weather situations.
5.3 HEAT STRESS
Prolonged exposure to heat can result in heat rash (prickly heat),heat cramps, heat exhaustion, or
heat stroke. Heat stroke is life threatening and requires immediate professional medical attention.
An overview of these heat-induced illnesses and proper preventative actions are described below.
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5.3.1 Heat Rash (Prickly Heat)
Heat rash, which is commonly observed in tropical climates, is a painful temporary condition
caused by clogged sweat pores, typically from sleeping in hot, humid quarters. Heat rash appears
as tiny red bumps on the skin and can impair sweating, resulting in diminished heat tolerance.
Heat rash can usually be cured by providing cool sleeping quarters;body powder may also help
absorb moisture.
5.3.2 Heat Cramps
Heat cramps are characterized by painful intermittent spasms of the voluntary muscles following
hard physical work in a hot environment. Heat cramps usually occur after heavy sweating and
often begin towards the end of the workday. The cramps are caused by a loss of electrolytes,
principally salt. This results in fluids leaving the blood and collecting in muscle tissue, resulting
in painful spasms. Treatment consists of increased ingestion of commercially available
electrolytic"sports" drinks (because of individual sensitivity, it is best to dilute by doubling the
amount of water required by package directions or add water to the liquid form).
5.3.3 Heat Exhaustion
This condition is characterized by profuse sweating, weakness, low blood pressure, rapid pulse,
dizziness, and frequently nausea and/or headache. The skin is cool and clammy and appears pale.
The body core temperature is normal or depressed. Victim may faint and/or vomit. This is the
most common work-related heat illness, and usually occurs after an extended period of work—
look for signs of onset after lunch—an employee may suddenly need to sit down, feel faint,
weak,or nauseated.
First aid consists of placing the victim in a cool area, loosening clothing,placing in a head-low
(shock prevention)position, and providing rest and plenty of fluids. Any worker who is a victim
of heat exhaustion may not be exposed to a hot working environment for an absolute minimum
of 24 hours, and if fainting has occurred, the victim should not return to any work until
authorized by a physician.
5.3.4 Heat Stroke
This is the most serious heat disorder, is life threatening, and is a true medical emergency. It
results when the body's heat dissipating system is overwhelmed and shuts down
(thermoregulatory failure). Heat stroke results in a continual rise in the victim's deep core body
temperature, which is fatal if not checked. The symptoms are hot, dry, flushed skin, elevated
body core temperature, convulsions, delirium, unconsciousness, and possibly death.
First aid consists of immediately moving victim to a cool area; cool the body rapidly by
immersion in cool (not cold) water or sponging the body with cool water; treat for shock and
obtain immediate medical assistance. Treatment response time is critical when assisting a victim
of heat stroke! Do not give coffee, tea, or alcoholic beverages.
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5.3.5 Preventative Measures
Unfortunately, there are no known PPE to prevent heat-related illnesses. However,some
preventative measures to avoid heat stress include:
• Frequent resting in cool or shaded areas,
• Consumption of large quantities of potable water or diluted electrolyte beverages,
following the suggested hydration target in Table 5:
Table 5.Hydration Targets based on Air Temperature and Time Periods between Breaks
Temperature Work Level Maximum Minutes Worked Hydration Target
Between Hydration Breaks
<80°F Normal -- 8-12 oz./hr.
80-85°F Normal -- 8-16 oz./hr.
86-90°F Normal 50 12-20 oz./hr.
91-95°F Normal 45 16-24 oz./hr.
>96°F Normal 40 24-32 oz./hr.
• Following a work/rest regiment from Table 6:
Table 6. Work/Rest Schedule based on Air Temperature
Ambient Temperature Work(hours) Rest(minutes)
70°F 3 15
75°F 2'/2 15
80°F 2 15
85°F 1'/2 15
90°F 1 15
Other factors, such as a worker's acclimatization, level of physical fitness, and age, may increase
or decrease his/her susceptibility to heat stress. Before assigning a task to an individual worker,
these factors will be taken into account to ensure that the task will not endanger the worker's
health.
If a heat-related illness is suspected or observed, the affected person must be moved to a cool or
shaded area and given plenty of liquids to consume. If symptoms of a heat stroke are observed,
the victim will be cooled immediately and treated as a medical emergency. Liquids will be
readily available to ensure that workers stay hydrated.
5.4 BIOLOGICAL HAZARDS—INSECT BITES/STINGS
Protective outer clothing such as gloves,hard hats, and coveralls can reduce the potential for
insect bites and stings. Insect bite symptoms may include redness, rash, swelling, chills, fever,
diarrhea, and vomiting. Any worker who has been bitten or stung and shows symptoms of a
severe reaction should seek medical assistance immediately. Workers who know of their
allergies to insects should advise their supervisor prior to field activities and should carry an
antidote kit, if necessary.
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When working in areas near heavy vegetation (possibly the riverbank) and to prevent contact
with disease-carrying ticks, workers should wear long-sleeved shirts, long pants, and boots that
extend above the ankle with socks pulled over pant cuffs or with pants legs taped to boots.
Insect repellant is also an effective means of tick control. Workers should check clothing, skin,
and hair for the presence of ticks periodically and thoroughly at the end of each workday. If a
tick attaches to the body, it should be removed by gently tugging with tweezers where the mouth
enters the skin. The tick should not be killed prior to removal.
5.5 BIOLOGICAL HAZARDS —SNAKES
There are six species of venomous snakes present in North Carolina and care must be taken to
avoid encounters and potential bites. Staff will be aware of physical appearances of venomous
snakes but will take care to avoid all snakes. When walking through wooded areas, check the
location of your next step prior to moving forward to ensure it is clear of snakes. Wear closed-
toed shoes and long pants to reduce the likelihood of a snake bite if a venomous snake is
disturbed.
5.6 BIOLOGICAL HAZARDS—FISH
Care must be taken and the proper PPE used when handling certain fish species to avoid getting
cut, spined, or bitten. Proper handling of fish will be performed by experienced EA staff to
reduce the likelihood if injury. Any worker that gets injured from a fish should seek medical
attention immediately.
5.7 POISON IVY AND RELATED PLANTS
Poison ivy,poison oak, and poison sumac have poisonous sap (urushiol) in their roots, stems,
leaves, and fruits. The urushiol may be deposited on the skin by direct contact with the plant or
by contact with contaminated objects, such as clothing, shoes, tools, and animals. Preventative
measures include: wear long-sleeved shirts and long pants tucked into boots; wear cloth or
leather gloves; apply barrier creams (e.g., Ivy Block) to exposed skin; and be able to identify
poison ivy, oak, and sumac plants. If you are exposed, according to the U.S. Food and Drug
Administration (FDA), you should quickly (within 10 minutes): 1) cleanse exposed areas with
rubbing alcohol; 2) wash the exposed areas with water only (no soap yet, since soap can move
the urushiol, which is the oil from the poison ivy that triggers the rash, around your body and
actually make the reaction worse); 3) take a shower with soap and warm water; and 4)put gloves
on and wipe everything you had with you, including shoes, tools, and your clothes, with rubbing
alcohol and water.
Unfortunately, if you wait more than 10 minutes, the urushiol will likely stay on your skin and
trigger the poison ivy rash. You may not be able to stop it on your skin, but you might still scrub
your nails and wipe off your shoes, etc., so that you do not spread the urushiol to new areas.
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5.8 ALLERGIC REACTIONS
When in the field, personnel may be exposed to allergens that can cause mild to severe allergic
reactions. The following guidelines will explain how to help a person having an allergic reaction.
For a mild to moderate reaction:
• Calm and reassure the person having the reaction, as anxiety can worsen symptoms.
• Try to identify the allergen and have the person avoid further contact with it. If the
allergic reaction is from a bee sting, scrape the stinger off the skin with something firm
(such as a fingernail or plastic credit card). Do not use tweezers; squeezing the stinger
will release more venom.
• If the person develops an itchy rash, apply calamine lotion and cool compresses.
Avoid medicated lotions.
• Watch the person for signs of increasing distress.
• Get medical help. For a mild reaction, a physician may recommend over-the-
counter medications (such as antihistamines).
For a severe allergic reaction:
• Check the person's airway, breathing, and circulation(the ABCs of Basic Life
Support). A warning sign for dangerous throat swelling is a very hoarse, whispered
voice or coarse sounds when the person is breathing air in. If the victim is having
difficulty breathing,is very weak, or is losing consciousness, call for emergency
medical assistance.
• Calm and reassure the person.
• If the person has emergency allergy medication on hand, help the person take or
inject the medication. Avoid oral medication if the person is having difficulty
breathing.
• Take steps to prevent shock. Have the person lie flat, elevate the person's feet about
12- inches, and cover him or her with a coat or blanket. DO NOT place the person
in this position if a head,neck,back, or leg injury is suspected or if it causes
discomfort.
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5.9 EMERGENCY RESPONSE PLAN
In the event of an emergency, the information available at the time must be properly evaluated
and the appropriate steps taken to implement the emergency response plan. The Crew Leader or
senior onsite supervisor will assume command of the situation and call 911 from the nearest
telephone or cell phone, notify authorities of your location(the docking point at which you will
meet them), evacuate personnel as needed, and take other steps needed to gain control of the
emergency.
Appropriate first aid will be given and emergency contacts will be made. Emergency situations
will be handled by offsite support personnel; however, initial response and first aid will be
available from qualified onsite personnel. Once the situation is under control, the Crew Leader
or designee will immediately call EA's Corporate Safety and Health Officer(Rob Marcase at
410-329-5192)and must complete an Accident/Loss Report(Appendix J).
The nearest hospital to the project site is Spartanburg Regional Hospital, located at 101 East
Wood Street in Spartanburg,South Carolina(864-560-6000).Driving directions from the study
area are provided in Appendix J.
5.10 CORONAVIRUS DISEASE 2019 (COVID-19)
All EA staff will be fully vaccinated against COVID-19 prior to arrival on-site. EA staff
will adhere to current state and/or local PPE and social distancing requirements, as
necessary. Appropriate PPE, including face masks and hand sanitizer, will be available to
EA staff as needed.
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6. COMMUNICATION AND CONTACT INFORMATION
LOCAL EMERGENCY TELEPHONE NUMBERS
Rutherford Co. Sherriff 911 or(828) 287-6247
Chesnee Police Department(Chesnee, SC) 911 or(864)461-2225
Cliffside Area Fire Department (Cliffside,NC) 911 or(828) 657-5671
Spartanburg Regional Hospital (Spartanburg, SC) [phone]
Poison Control Center [phone] or(800) 222-1222
District 8 Department of Natural Resources Personnel
Christopher Wood-Fisheries Biologist Office (0): [phone]/Cell (C): (828)
475-9643
David Goodfred-Assistant Fisheries Biologist 0: [phone]/C: [phone]
Dan Vogel - Area Sgt. (Law Enforcement) [phone]
Jesse Weicker-Master Officer(Law Enforcement) [phone]
PROJECT-RELATED TELEPHONE NUMBERS
EA Engineering, Science, and Technology, Inc., [phone]
PBC (HV)
Joe Vondruska, STR(EA) 0: [phone]/C: [phone]
Rob Marcase, Health and Safety (EA) 0: [phone]/C: [phone]
Michele Bailey, Human Resources (EA) 0: [phone]/C: [phone]
Jeff Boltz,WNR Director(EA) 0: [phone]/C: [phone]
Martha McCauley, Scientist, Project Manager(EA) [phone]
Patrick Hilbert, Scientist, Field Lead (EA) [phone]
Larry Bushing, Scientist(EA) [phone]
Heather Smith (TRC Companies) [phone]
Rob Hanley(TRC Companies) [phone]
Richard Mayer (TRC Companies—Health and [phone]
Safety Coordinator)
Benjamin Medlin (TRC Companies—on-site [phone]
Support)
Charles Howell (AZP) 0: [phone]/C: [phone]
Aidan Morse(AZP) [phone]
_AZP Emergency Number [phone]
Jamie Spears-Inman Sod [phone]
Mason-EnMeccio-Assistant Inman Sod [phone]
Pace Analytical Services [phone]
Federal Express 1-800-463-3339 (1-800-GO-FEDEX)
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7. REFERENCES
Boschung, H. T. and R. L. Mayden. 2004. Fishes of Alabama. Smithsonian Books, Biuliiingham,
AL.
Jenkins, R. E. and N. M. Burkhead. 1993. Freshwater Fishes of Virginia. American Fisheries
Society, Bethesda, MD.
Marcy, B. C.,D. E. Fletcher, F. D. Martin,M. H. Paller, M. J. M. Reichert. 2005. Fishes of the
Middle Savannah River Basin with Emphasis on the Savannah River Site. University of
Georgia Press, Athens, GA.
Menhinick, E. F. 1991. The Freshwater Fishes of North Carolina. North Carolina Wildlife
Resources Commission, Raleigh,N.C.
North Carolina Division of Water Resources (NCDWR). 2019.NCDWR Broad River March
201913 Fish Tissue Metals.
Page, L. M. and B. M. Burr. 2011. Peterson Field Guide to Freshwater Fishes of North America
North of Mexico. Second Edition. Houghton Mifflin Harcourt Publishing Company,New
York,NY.
Broad River,Rutherford County,North Carolina SOP-NPDES Fish Tissue Collection

Version:FINAL
Page 22
EA Engineering,Science,and Technology,Inc.,PBC May 2022
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Broad River,Rutherford County,North Carolina SOP-NPDES Fish Tissue Collection

Appendix A
NCWRC Scientific Fish Collection License

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AUTHORITY
NORIW Scientific Fish Collecting License
CAROL AA STATUTES
' 113-281,113-262,&113-272.4
"1.1"'"% North Carolina Wildlife Resources Commission
RULES
Division of Inland Fisheries 15A NCAC 10C.0214
Phone:[phone] MSC 1721
Fax:[phone] Raleigh, NC 27699-1721
Page 1 of 1
PERMITTEE/LICENSEE PERMIT NUMBER
22-SFC00267
MARTHA MARIE MCCAULEY
EA ENGINEERING SCIENCE&TECHNOLOGY,INC EFFECTIVE EXPIRES
225 SCHILLING CIR STE 400 02/21/2022 12/31/2022
HUNT VALLEY,MD 21031
SPECIES/ORGANISMS: Print Date: 03/04/2022
Catostomus commersonii; Cyprinus carpio; Lepomis auritus; Lepomis macrochirus; Micropterus dulomieu; Micropterus
salmoides; Moxostoma collapsum; Moxostoma erythrurum; Moxostoma sp. cf.lachneri; lctaluridae
RIVER BASINS/COUNTIES:
BROAD-Rutherford
SAMPLING METHOD:
Electrofishing, Backpack; Electrofishing, Boat; Net, Dip; Net, Fyke; Net, Gill; Net, Trap; Net, Other; Seines; Other;
Hook and Line
ASSISTANTS:
LARRY BUSHING, PATRICK.HILBERT, JUSTIN DORIAN, MICHAEL DURBANO, KIERSTEN MILLER,WILL BROBERG
CONDITIONS AND AUTHORIZATIONS:
The above licensee is authorized to collect the species/organisms by the sampling methods as listed below without
restriction to season, size, or creel limits unless otherwise specified under Special Conditions. These species/organisms
may be collected in the River Basins/Counties listed below. Sampling in Collection-Sensitive Waters is not authorized
under this license unless specified under Special Conditions or allowed through a Commission-issued Endangered Species
Permit. For a current list of Collection-Sensitive Waters,see www.ncwildlife.org/Licensing/fishcollection.aspx. The take or
possession of federally or state listed endangered,threatened, or special concern species is not authorized under this
license except in conjunction with a valid Endangered Species Permit. The licensee is required to comply with all
requirements and laws specified by the U.S. Fish and Wildlife Service and National Marine Fisheries Service as they
pertain to federally-listed species. Fora current list of federally or state listed endangered,threatened, or special concern
species, see.www.ncwildlife.org/Learning/Species.
SPECIAL CONDITIONS:
Collection of macroinvertebrates: Mussels, crayfish, or aquatic snails are regulated by the NC Wildlife Resources
Commission,.and they may not be collected unless specifically listed above under species/organisms. Otherwise,this
license does not restrict the collection of other benthic macroinvertebrates.
This license was issued based on the requirements of the North Carolina Wildlife Resources Commission. It is the duty of
the licensee/permittee to ensure that they are in compliance with all additional applicable local, state, and federal laws.
This permit/license is non-transferable and expires at midnight on the above specified expiration date.
ISSUED BY: TITLE:
Chief
22-SFC00267

Appendix B
Field Data Sheet Templates

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Field Data Sheet#1 and Field. Data Sheet#2 will document Fish Tissue Collection Results on
the day(s) of Field sampling. One set of Data Sheets (2) will be completed for each location for
each day sampling is conducted.
Field Data Sheet#1
Fish Tissue Collections: Broad River downstream American Zinc Products Discharge.
Collection Date:
Location:
Study Reach Start From: Latitude: Longitude:
Study Reach Finish at: Latitude: Longitude:
Nearest Landmark at Start of Reach: Highway 221 bridge over the Broad River Rutherford Co.
Duration of Daily Collection Activities: Hours: Minutes:
Collection Staff: (list name and affiliation: example John Doe, Agency Blue Inc.
Describe Collection Methods: (ex. Electrofishing Boat, Back Pack electrofishing, hook and line,
trot lines,traps,or gillnets).
Describe:
Comment and Describe Access to River : ( example boat ramp,bank, bridge etc.)
Each day of sampling personnel must fill out the following table ((Field Data Sheet#2)
completing infoiuiation for all individual fish. Any deviation from this Sampling Plan must be
noted and described on daily records.
Exceptions to Sampling Plan if any:
5 Page
Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Field Data Sheet#2
Fish# Sample Location Species Total Length Weight Comments
ID in cm in grams
1 Date of collection:
2
3 Lat/Long Site Coordinates
4
5 The upstream extent was:
6 Latitude:
7 Longitude:
8 The Downstream extent was:
9 Latitude:
10 Longitude:
11 Reach Length in miles(include decimals)
12
13 Fish Collection Goal per location
14 3 Target Species
15 Ten fish per Species:30 fish total
16
17 Primary Target Species Include
18
19 largemouth bass
20 redbreast sunfish
21 notchlip redhorse sucker
22
23
24 Secondary Target Species Include
25 bluegill sunfish
26 brassy jumprock
27 white sucker
28 flat bullhead
29 catfish
30 carp
31 Dup#1 of Fish Sample# others
32 Dup#2 of Fish Sample#
Additional Comments:
Wage
Fish Tissue Sampling Plan American Zinc Recycling NPDES NC0089109

Appendix C
Internal Label Template

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EA Englneadng, Project: 16244.01 E n�elnaadng' Project: 16244.01
Science,and
Technology,Inc.,PBC Broad River, NC, Tissue Collection Technology,Inc..PBC Broad River, NC, Tissue Collection
Sample Number: BR- - - - MAY22- Sample Number: BR- - - - MAY22-
Contract: NPDES Confidential Date: Contract: NPDES Confidential Date:
Site: Upstream Downstream Time: Site: Upstream Downstream Time:
Species Length (mm) Weight (g) Species Length (mm) Weight(g)
EAEAEngeinzng, Project: 16244.01 c/�Sci e,anang, Project: 16244.01
Science,and �.i
Technology,Inc.,PBC Broad River, NC, Tissue Collection Technology,Inc.,PBC Broad River, NC, Tissue Collection
Sample Number: BR- - - - MAY22- Sample Number: BR- - - - MAY22-
Contract: NPDES Confidential Date: Contract: NPDES Confidential Date:
Site: Upstream Downstream Time: Site: Upstream Downstream Time:
Species Length (mm) Weight (g) Species Length (mm) Weight(g)
EAEAEngineedng, Project: 16244.01 SA ncehandng' Project: 16244.01
Science,antl
Technology,Inc„PBC Broad River, NC, Tissue Collection Technology,Inc.,PBC Broad River, NC, Tissue Collection
Sample Number: BR- - - - MAY22- Sample Number: BR- - - - MAY22-
Contract: NPDES Confidential Date: Contract: NPDES Confidential Date:
Site: Upstream Downstream Time: Site: Upstream Downstream Time:
Species Length (mm) Weight (g) Species Length (mm) Weight (g)
Science eedng. Project: 16244.01 Sc Englnand g' Project: 16244.01
Science,and
Technology,Inc„PBC Broad River, NC, Tissue Collection Teehnology,Ine.,PBC Broad River, NC, Tissue Collection
Sample Number: BR- - - - MAY22- Sample Number: BR- - - - MAY22-
Contract: NPDES Confidential Date: Contract: NPDES Confidential Date:
Site: Upstream Downstream Time: Site: Upstream Downstream Time:
Species Length (mm) Weight (g) Species Length (mm) Weight(g)
EAEAEngceM,eedng, Project: 16244.01 E enclneendnI Project: 16244.01
Scien
Technology,Inc.,PBC Broad River, NC, Tissue Collection Technology,Inc.,PBC Broad River, NC, Tissue Collection
Sample Number: BR- - - - MAY22- Sample Number: BR- - - - MAY22-
Contract: NPDES Confidential Date: Contract: NPDES Confidential Date:
Site: Upstream Downstream Time: Site: Upstream Downstream Time:
Species Length (mm) Weight (g) Species Length (mm) Weight (g)

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Appendix D
Chain-of-Custody Template
Pace Analytical Services

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CHAIN-OF-CUSTODY/Analytical Request Document
aCe A.,ar lC l' The Chain-of-Custody is a LEGAL DOCUMENT.All relevant fields must be completed accurately.
vrl:^.v.p lece.rabs.com
action A Section B Section C
Page: of
.quired Client Information: Required Project Information: Invoice Information:
rmpany: Report To: Attention:
(dress: Copy To: Company Name: REGULATORY AGENCY
Address: E NPDES [ GROUND WATER 1— DRINKING WATER
nail To: Purchase Order No.: Pace Quote — UST (— RCRA )— OTHER
Reference:
one: Fax: Project Name: Pace Project Site Location
'�d'Isua �/f �f°(v �
Manager:
:quested Due Date/TAT: Project Number: Pace Profile#: STATE:
N
Requested Analysis Filtered(YIN) /;''l4;;Z i q/ vy /�jj
Section D Valid Matrix Codes 1 E. z
Required Client Information MATRIX CODE COLLECTED Preservatives } y .. „, /i
DRINKING WATER ow 0
y U
WATER WT g 0 f-
WASTE WATER ww _ m COMPOSITE COMPOSITE 0 Z
PRODUCT p Q START END/GRAB
SOIL/SOLID SL K d }
OIL OL N T O ,
SAMPLE ID WIPE WP y C0 Q W y
AIR AR W Z I� O
(A-Z,0-9/,-) OTHER OT 0 00 D- N to U
Sample IDs MUST BE UNIQUE TISSUE Ts U Lu Z Z O To
X J O J U OpI CON mto a# Y a D- u_ co _c
C 5
w 2 a DATE TIME DATE TIME a TE D 2 I I ZZ Z 20 ... IY Pace Project No./Lab I.D.
1
2
3
4
5
6
7
8
9
10
11
12
ADDITIONAL COMMENTS RELINQUISHED BY/AFFILIATION DATE TIME ACCEPTED BY/AFFILIATION DATE TIME SAMPLE CONDITIONS
SAMPLER NAME AND SIGNATURE O ` d U
o r s
0
2 ?z v o,
PRINT Name of SAMPLER: a } u,v y d}
.S N > e).� 0.—
SIGNATURE of SAMPLER: DATE Signed i `2 O d m
(MMIDDIYY): co co
'Important Note:By signing this form you are accepting Pace's NET 30 day payment terms and agreeing to late charges of 1.5%per month for any Invoices not paid within 30 days. FALL-Q-020fev.06,12-Oct-2007

Appendix E
Laboratory Reporting Limits
Pace Analytical Services

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Pace Analytical Services,LLC Detection Limits and Reporting Limits
1241 Bellevue St.,Suite 9 I Green Bay,WI 54302 Analytical I Digestion Method:SW846 6020E 130505 Mod.
(Main Line)920-469-2436 Matrix Tissue
wvna_pacelabs.com
LCS/LCSD 131 MS/MSD(3)
Analyte CAS Number MDL 1;21(mg/kg) PO,L II?)(mg/kg) Lower Upper RPD Lower Upper RPD
Aluminum(Al) 7429-90-5 5.7439 25.00 80 120 20 75 125 20
Antimony(Sb) 7440-36-0 0.021 0.10 80 120 20 75 125 20
Arsenic(As) 7440-38-2 0.0302 0.10 80 120 20 75 125 20
Beryllium(Be) 7440-41-7 0.0331 0.11 80 120 20 75 125 20
Cadmium(Cd) 7440-43-9 0.01095 0.10 80 120 20 75 125 20
Chromium(Cr) 7440-47-3 0.0885 0.29 80 120 20 75 125 20
Copper(Cu) 7440-50-8 0.2844618 0.95 80 120 20 75 125 20
Iron(Fe) 7439-89-6 5.086 25.00 80 120 20 75 125 20
Lead(Pb) 7439-92-1 0.03 0.10 80 120 20 75 125 20
Nickel(Ni) 7440-02-0 0.0569 0.14 80 120 20 75 125 20
Phosphorus(P) 7723-14-0 338.952 1129.84 80 120 20 75 125 20
Selenium(Se) 7782-49-2 0.0507 0.17 80 120 20 75 125 20
Silver(Ag) 7440-22-4 0.011162578 0.05 80 120 20 75 125 20
Thallium(1) 7440-28-0 0.013 0.10 80 120 20 75 125 20
Zinc (Zn) 7440-66-6 1.398 4.66 80 120 20 75 125 20
1)Samples may be diluted due to the presence of high levels of target and non-target analytes,or other matrix interferences.
2)Laboratory MDLs and PQLs are subject to change.
3)Method Derived Control Limit

Pace Analytical Services,LLC Detection Limits and Reporting Limits
1241 Bellevue St,Suite 9 1 Green Bay,WI 54302 Analytical I Digestion Method:EPA 245.6
(Main Line)920-469-2436 Matrix:Tissue
www.pacelabs.com
LCS/LCSDl31 MS/M5Di31
Analyte CAS Number MDL(mg/kg)1423 PQL(Total mg/kg)(mil Lower Upper RPD Lower Upper RPD
Mercury 7439-97-6 0.00564 0.0188 85. 115 10 70 130 10
1)Samples may be diluted due to the presence of high levels of target and non-target analytes,or other matrix interferences.
2)Laboratory MDLs and PQLs are subject to change.
3)Method Derived Control Limit

Appendix F
SOPs and QC Manual
Pace Analytical Services

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ace Analytical
ENVIRONMENTAL SCIENCES
Document Information
Document Number: ENV-MAN-GBAY-0001 Revision: 03
Document Title: Quality Manual
Department(s):
Quality
Date Information
Effective Date: 20 Sep 2021
Notes
Document Notes:
All Dates and Times are listed in: Central Time Zone

Signature Manifest
Document Number: ENV-MAN-GBAY-0001 Revision: 03
Title: Quality Manual
All dates and times are in Central Time Zone.
ENV-MAN-GBAY-0001-Rev.03 Quality Manual
QM Approval
Name/Signature Title Date Meaning/Reason
Anthony Haag III (991579) Manager-Quality 13 Sep 2021, 01:59:31 PM Approved
Management Approval
Name/Signature Title Date Meaning/Reason
Brian Basten(007101) Manager 13 Sep 2021, 12:47:55 PM Approved
Chad Rusch(007163) General Manager 2 13 Sep 2021, 01:40:44 PM Approved
Christopher Haase(007121) Manager 13 Sep 2021, 03:20:31 PM Approved
Brian King(991565) Manager 16 Sep 2021, 03:43:40 PM Approved
Karl Anderson(004767) Regional Vice President-Oper 17 Sep 2021,09:50:35 AM Approved
Ryan Smith (008764) Systems Administrator 2 20 Sep 2021, 10:03:43 AM Approved
Elizabeth Turner(007857) Manager-Quality Program 20 Sep 2021, 10:33:09 AM Approved
Scott Turner(007177) Manager 20 Sep 2021,01:23:30 PM Approved

aceAnaIjicaI©
LABORATORY QUALITY MANUAL
Pace Analytical Services,LLC
COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
TITLE PAGE
LABORATORY QUALITY MANUAL
Prepared for:
Pace Analytical Services,LLC
1241 Bellevue Street,Suite 9
Green Bay,WI 54302
Phone: [phone]
Pace Analytical Services,LLC
870 East Higgins Road, Suite 143
Schaumburg,IL 60173
Phone: [phone]
Pace Analytical Services,LLC
6409 Odana Road,Suite 3-E
Madison,WI 53719
Phone: [phone]
Page 1 of 100

aeAna/ icaI
LABORATORY QUALITY MANUAL
Pace Analytical Services,LLC
COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
Quality Manual Approval Signatories
Approval of this quality manual by managerial personnel is recorded on the Signature Manifest located before
the Title Page of this manual.
The individuals listed below represent the management team that was in place on the effective date of this
version of the manual for the following location:
Pace Analytical Services,LLC
1241 Bellevue Street,Suite 9
Green Bay,WI 54302
Phone: [phone]
Each of the following individuals is a signatory for the quality manual for the location listed above. The
application of their signature to the manual signifies their commitment to communicate,implement,and uphold
the requirements, policies and procedures specified in this manual and their commitment to continuously
improve the effectiveness of the quality management system based on customer feedback and internal
assessment.
Name1 Title Address2 Phone2
Elizabeth Turner Corporate Quality Program Manager 400 W Bethany Drive,Suite 190 469-675-7071
Allen,TX 75013
Karl Anderson Regional Vice-President-Operations 7726 Moeller Rd 317-228-3119
Indianapolis,IN 46268
Chad Rusch General Manager II 920-321-9438
Anthony Haag Quality Manager 920-321-9426
Jill Duranceau Safety Officer 920-321-9441
Ryan Smith Systems Administrator 920-321-9449
Brian Basten Manager-Client Services 920-321-9411
Brian King Manager-Inorganics3 920-321-9420
Christopher Haase Manager-Semi-Volatiles3 920-321-9453
Scott Turner Manager-Volatiles3 920-321-9425
1 Members of the local management team are subject to change during the lifeeycle of this document version.
2lnclude if dferent from the physical address and phone number of the facility.
3This individual serves as an Acting Technical Manager for TNI for one or more fields of accreditation.
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LABORATORY QUALITY MANUAL
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COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
TABLE OF CONTENTS
1.0 PURPOSE AND SCOPE 7
1.1 PURPOSE 7
1.2 SCOPE AND APPLICATION 7
1.2.1 QUALITY MANUAL TEMPLATE 8
1.2.2 LABORATORY QUALITY MANUAL 8
1.2.3 REFERENCES TO SUPPORTING DOCUMENTS 9
2.0 REFERENCES 9
3.0 TERMS AND DEFINITIONS 10
4.0 MANAGEMENT REQUIREMENTS 10
4.1 ORGANIZATION 10
4.1.1 LEGAL IDENTITY 10
4.1.2 COMPLIANCE RESPONSIBILITY 11
4.1.3 SCOPE OF THE QUALITY MANAGEMENT SYSTEM 11
4.1.4 ORGANIZATION HISTORY AND INFORMATION 11
4.1.5 MANAGEMENT REQUIREMENTS 12
4.2 QUALITY MANAGEMENT SYSTEM 18
4.2.1 QUALITY MANAGEMENT SYSTEM OBJECTIVES 18
4.2.2 QUALITY POLICY STATEMENT 20
4.2.3 MANAGEMENT COMMITMENT: QUALITY MANAGEMENT SYSTEM 22
4.2.4 MANAGEMENT COMMITMENT:CUSTOMER SERVICE 22
4.2.5 SUPPORTING PROCEDURES 23
4.2.6 ROLES AND RESPONSIBILITIES 24
4.2.7 CHANGE MANAGEMENT 24
4.3 DOCUMENT CONTROL 24
4.3.1 GENERAL 24
4.3.2 DOCUMENT APPROVAL AND ISSUE 25
4.3.3 DOCUMENT REVIEW AND CHANGE 25
4.4 ANALYTICAL SERVICE REQUEST,TENDER,AND CONTRACT REVIEW 25
4.5 SUBCONTRACTING AND IN-NETWORK WORK TRANSFER 26
4.6 PURCHASING SERVICES AND SUPPLIES 27
4.7 CUSTOMER SERVICE 27
4.7.1 COMMITMENT TO MEET CUSTOMER EXPECTATIONS 27
4.7.2 CUSTOMER FEEDBACK 28
4.8 COMPLAINTS 28
4.9 NONCONFORMING WORK 29
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COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
4.9.1 DEFINITION OF NONCONFORMING WORK 29
4.10 CONTINUOUS IMPROVEMENT 30
4.11 CORRECTIVE ACTION 31
4.11.1 CAUSE ANALYSIS 32
4.11.2 EFFECTIVENESS REVIEW 32
4.11.3 ADDITIONAL AUDITS 32
4.12 PREVENTIVE ACTION 32
4.12.1 CHANGE MANAGEMENT 33
4.13 CONTROL OF RECORDS 33
4.13.1 GENERAL REQUIREMENTS 33
4.13.2 TECHNICAL RECORDS 35
4.14 AUDITS 36
4.14.1 INTERNAL AUDIT 36
4.15 MANAGEMENT REVIEW 37
4.16 DATA INTEGRITY 38
5.0 TECHNICAL REQUIREMENTS 38
5.1 GENERAL 38
5.2 PERSONNEL 38
5.2.1 PERSONNEL QUALIFICATIONS 38
5.2.2 TRAINING (REQUIRED) 40
5.2.3 PERSONNEL SUPERVISION 44
5.2.4 JOB DESCRIPTIONS 44
5.2.5 AUTHORIZATION OF TECHNICAL PERSONNEL 44
5.3 ACCOMMODATIONS AND FACILITIES 45
5.3.1 FACILITIES 45
5.3.2 ENVIRONMENTAL CONDITIONS 45
5.3.3 SEPARATION OF INCOMPATIBLE ACTIVITIES 45
5.3.4 LABORATORY SECURITY 45
5.3.5 GOOD HOUSEKEEPING 46
5.4 TEST METHODS 46
5.4.1 GENERAL REQUIREMENTS 46
5.4.2 METHOD SELECTION 46
5.4.3 LABORATORY DEVELOPED METHODS 46
5.4.4 NON-STANDARD METHODS 47
5.4.5 METHOD VALIDATION 47
5.4.6 MEASUREMENT UNCERTAINTY 50
5.4.7 CONTROL OF DATA 50
5.5 EQUIPMENT 52
5.5.1 AVAILABILITY OF EQUIPMENT 52
5.5.2 CALIBRATION 52
5.5.3 EQUIPMENT USE AND OPERATION 52
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COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
5.5.4 EQUIPMENT IDENTIFICATION 53
5.5.5 EQUIPMENT LISTS AND RECORDS 53
5.5.6 OUT OF SERVICE PROTOCOL 54
5.5.7 CALIBRATION STATUS 54
5.5.8 RETURNED EQUIPMENT CHECKS 54
5.5.9 INTERMEDIATE EQUIPMENT CHECKS 54
5.5.10 SAFEGUARDING EQUIPMENT INTEGRITY 54
5.6 MEASUREMENT TRACEABILITY 55
5.6.1 GENERAL 55
5.6.2 EQUIPMENT CORRECTION FACTORS 55
5.6.3 SPECIFIC REQUIREMENTS 55
5.6.4 REFERENCE STANDARDS AND REFERENCE MATERIALS 55
5.7 SAMPLING 58
5.7.1 SAMPLING PLANS AND SOPS 58
5.7.2 CUSTOMER REQUESTED DEVIATIONS 58
5.7.3 RECORDKEEPING 58
5.8 SAMPLE MANAGEMENT&HANDLING 58
5.8.1 PROCEDURES 58
5.8.2 UNIQUE IDENTIFICATION 60
5.8.3 SAMPLE RECEIPT CHECKS AND SAMPLE ACCEPTANCE POLICY 60
5.8.4 SAMPLE CONTROL AND TRACKING 62
5.8.5 SAMPLE STORAGE,HANDLING,AND DISPOSAL 62
5.9 ASSURING THE QUALITY OF TEST RESULTS 63
5.9.1 QUALITY CONTROL(QC) PROCEDURES 63
5.9.2 QC CORRECTIVE ACTION 67
5.9.3 DATA REVIEW 67
5.9.4 CALIBRATION CERTIFICATES 68
5.9.5 OPINIONS AND INTERPRETATIONS 69
5.9.6 SUBCONTRACTOR REPORTS 69
5.9.7 ELECTRONIC TRANSMISSION OF RESULTS 69
5.9.8 FORMAT OF TEST REPORTS 69
5.9.9 AMENDMENTS TO TEST REPORTS 69
5.10 REPORTING 70
5.10.1 GENERAL REQUIREMENTS 70
5.10.2 TEST REPORTS: REQUIRED ITEMS 70
5.10.3 TEST REPORTS:SUPPLEMENTAL ITEMS 71
6.0 REVISION HISTORY 72
7.0 APPENDICES 73
7.1 APPENDIX A:CERTIFICATION/ACCREDITATION LISTING 73
7.1.1 PAS-GREEN BAY 73
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7.2 APPENDIX B:CAPABILITY LISTING 74
7.2.1 PAS-GREEN BAY 74
7.3 APPENDIX C:GLOSSARY 77
7.4 APPENDIX D:ORGANIZATION CHART(S) 92
7.4.1 CORPORATE ORGANIZATIO
N CHART 92
7.4.2 QUALITY SYSTEMS MANAGEMENT 93
7.4.3 PACE—GREEN BAY—ORGANIZATION CHART 94
7.5 APPENDIX E: EQUIPMENT LISTING 95
7.5.1 PAS-GREEN BAY 95
8.0 ADDENDUM: PROGRAM REQUIREMENTS 98
8.1 DOD/DOE 98
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M Y
'ace Analytical
LABORATORY QUALITY MANUAL
Pace Analytical Services,LLC
COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
1.0 PURPOSE AND SCOPE
1.1 Purpose
This quality manual (manual) outlines the quality management system (QMS) and management
structure of the laboratories and service centers affiliated with the environmental sciences (ENV)
division of Pace Analytical Services, LLC (PAS). A laboratory is defined by ENV as any facility,
however named, that provides testing, sampling, or field measurement services. When the term
`laboratory" is used in this manual, the term refers to all locations listed on the Tide Page of this
manual and in Section 4.1.3 unless otherwise specified.
The ENV quality management system is also referred to as the quality program throughout this
document. In this context, the phrase "quality management system" and "quality program" are
synonymous and may be referred to by the acronym QMS.
The quality management system is the collection of policies and processes established by ENV
management to consistently meet customer requirements and expectations, and to achieve the goals
of providing PAS customers with high quality, cost-effective,analytical measurements and services.
The quality management system is also intended to establish conformance1 and compliance with the
current versions of the following international and national quality system standards:
■ ISO/IEC 17025: General requirements for the competence of testing and calibration laboratories
• NELAC/TNI Standard Volume 1:Management and Technical Requirements for Laboratories Performing
Environmental Analysis
'The statement of conformity to these Standards pertains only to testing and sampling activities carried out by the laboratory
at its physical address,in temporary or mobile facilities,in-network,or by laboratory personnel at a customer's facility.
In addition to the international and national standards,the quality management system is designed to
achieve regulatory compliance with the various federal and state programs for which the laboratory
provides compliance testing and/or holds certification or accreditation. When federal or state
requirements do not apply to all ENV locations, the requirements for compliance to those
specifications are provided in addendum to this manual or in other documents that supplement the
manual. Customer-specific project and program requirements are not included in the manual in order
to maintain client confidentiality.
• A list of accreditation and certifications held by each laboratory associated with this manual is
provided in Appendix A.
• A list of analytical testing capabilities offered by each laboratory associated with this manual is
provided in Appendix B.
1.2 Scope and Application
This manual applies to each of the PAS locations listed on the Tide Page.
The manual was prepared from the quality manual template (template) created by ENV corporate
quality personnel. The template outlines the minimum requirements ENV management considers
necessary for every ENV location,regardless of scope of services or number of personnel,to establish
in order to maintain a quality management system that achieves the objectives of the Quality Policy
(See 4.2.2). In this regard, the template is the mechanism used by the corporate officers (a.k.a. 'top
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LABORATORY QUALITY MANUAL
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COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
management') to communicate their expectations and commitment for the quality program to ENV
personnel.
Each location also has the responsibility to comply with federal and state regulatory and program
requirements for which it provides analytical services and holds certification or accreditation. When
those requirements are more stringent than the template, the requirements for compliance are
provided in addendum to this manual or in other documents that supplement the manual. This
document structure maintains consistency in the presentation of the quality management system
across the network while providing the location a mechanism to describe and achieve compliance
requirements on a program basis.
1.2.1 Quality Manual Template
The quality manual template is developed by the Corporate Quality Director with contribution
and input from corporate quality personnel and the corporate officers. Approval of the
template by the corporate officers (aka "top management") confirms their commitment to
develop and maintain a quality management system appropriate for the analytical services
offered by the organization and to communicate their expectations of the quality program to
all personnel.
The template and instructions for use of the template are released by corporate quality
personnel to the quality assurance manager responsible for each location (Local QM). The
local QM uses the template to prepare the laboratory's manual by following the instructions
provided. Since the template provides the minimum requirements by which ENV locations
must abide,the laboratory may not alter the font, structure or content of the template except
where specified by instruction to do so. As previously stated,program specific requirements
are provided in addendum or in documents that supplement this manual.
The template is reviewed by corporate quality personnel annually and updated if needed. More
frequent review and revision may be necessary to manage change, to maintain conformance
and compliance to relevant standards,or to meet customer expectations.
See standard operating procedure (SOP) ENV-SOP-CORQ-00015 Document Management and
Control(most recent revision or replacement) for more information.
1.2.2 Laboratory Quality Manual
The manual is approved and released to personnel under the authority of local management
whose signatures are identified on the Manual Signatory Page of this manual. The manual is
reviewed annually, and location specific information is updated, if needed. More frequent
review and revision may be necessary when there are significant changes to the organizational
structure, capabilities,and resources of the laboratory. Review and revision of the manual is
managed by the local QM. If review indicates changes to the main body of the manual are
necessary to maintain conformance and compliance to relevant standards,or to meet customer
expectations, the local QM will notify corporate quality personnel to initiate review and/or
revision of the template.
See SOP ENV-SOP-CORQ-00015 Document Management and Control(most recent revision or
replacement) for more information.
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1.2.3 References to Supporting Documents
The template and the manual include references to other laboratory documents that support
the quality management system such as policies and standard operating procedures (SOPs).
These references include the document's document control number and may include the
document title.
This information is subject to change. For example, an SOP may be converted to a policy or
the document's title may change. For these types of administrative changes,the manual and
template are updated to reflect the editorial change during the manual's next scheduled
review/revision cycle or the next time a new version of the manual is released,whichever is
sooner.
The local QM maintains a current list of controlled documents used at each location that
support the quality management system. This list, known as the "Master List", lists each
document used by document control number, title, version, effective date, and reference to
any document(s) that the current version supersedes.When there is a difference between the
manual and the Master List, the document information in the Master List takes precedence.
The current Master List is readily available to personnel for their use and cross-reference.
Parties external to the laboratory should contact the laboratory for the most current version.
2.0 REFERENCES
References used to prepare this manual include:
•
• "Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act."
Federal Register,40 CFR Part 136,most current version.
• "Test Methods for Evaluating Solid Wastes: Physical/Chemical Methods." SW-846.
• "Methods for Chemical Analysis of Water and Wastes",EPA 600-4-79-020, 1979 Revised 1983,U.S.
EPA.
• U.S.EPA Contract Laboratory Program Statement of Work for Organic Analysis,current version.
• U.S.EPA Contract Laboratory Program Statement of Work for Inorganic Analysis,current version.
• "Standard Methods for the Examination of Water and Wastewater." Current Edition APHA-AWWA-
WPCF.
• "Annual Book of ASTM Standards",Section 4: Construction,Volume 04.04: Soil and Rock;Building
Stones,American Society of Testing and Materials.
• "Annual Book of ASTM Standards", Section 11: Water and Environmental Technology, American
Society of Testing and Materials.
• "NIOSH Manual of Analytical Methods",U.S.Department of Health and Human Services,National
Institute for Occupational Safety and Health,most current version.
• "Methods for the Determination of Organic Compounds in Finished Drinking Water and Raw Source
Water",U.S. EPA,Environmental Monitoring and Support Laboratory—Cincinnati (Sep 1986).
• Quality Assurance of Chemical Measurements,Taylor,John K.;Lewis Publishers,Inc. 1987.
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• Methods for Non-conventional Pesticides Chemicals Analysis of Industrial and Municipal Wastewater,
Test Methods,EPA-440/1-83/079C.
• Environmental Measurements Laboratory(EML)Procedures Manual,HASL-300,US DoE,February
1992.
■ Requirements for Quality Control of Analytical Data,HAZWRAP,DoE/HWP-65/R1,July 1990.
• Quality Assurance Manual for Industrial Hygiene Chemistry,AIHA,most current version.
• National Environmental Laboratory Accreditation Conference (NELAC) Standard- most current
version.
■ ISO/IEC 17025,General requirements for the competence of testing and calibration laboratories,2nd
Edition 2005-05-15;3rd Edition 2017-11
The following are implemented by normative reference to ISO/IEC 17025:
o ISO/IEC Guide 99,International vocabulary of metrology—Basic and general concepts and associated terms
o ISO/IEC 17000,Conformity assessment— Vocabulary and general principles
• Department of Defense Quality Systems Manual(QSM),most current version.
• TNI (The NELAC Institute) Standard,2009 and 2016 versions.
■ UCMR Laboratory Approval Requirements and Information Document,most current version.
• US EPA Drinking Water Manual,most current version.
3.0 TERMS AND DEFINITIONS
Refer to Appendix C for terms, acronyms, and definitions used in this manual and in other documents
used by the laboratory to support the quality management system.
4.0 MANAGEMENT REQUIREMENTS
4.1 Organization
4.1.1 Legal Identity
Pace Analytical Services,LLC is authorized under the State of Minnesota to do business as a
limited liability company.
4.1.1.1 Change of Ownership
If there is a change of ownership,if a location goes out of business, or if the entire
organization ceases to exist, Pace Analytical Services, LLC ensures that regulatory
authorities are notified of the change within the time-frame required by each state
agency for which the location is certified or accredited.
Requirements for records and other business information are addressed in the
ownership transfer agreement or in accordance with appropriate regulatory
requirements,whichever takes precedence.
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4.1.2 Compliance Responsibility
Laboratory management has the responsibility and authority to establish and implement
procedures and to maintain sufficient resources necessary to assure its activities are carried out
in such a way to meet the compliance requirements of the quality management system.
4.1.3 Scope of the Quality Management System
The quality management system applies to work carried out at each location covered by this
manual including permanent facilities, at sites away from its permanent facilities, or in
associated temporary or mobile facilities.
The permanent and mobile facilities to which this manual applies are listed on the Title Page
of this manual.
4.1.4 Organization History and Information
Founded in 1978, Pace Analytical Services, LLC (PAS) is a privately held scientific services
firm operating one of the largest full-service contract laboratory and service center networks
in the United States. The company's network offers inorganic, organic and radiochemistry
testing capabilities; specializing in the analysis of trace level contamination in air, drinking
water,groundwater,wastewater, soil,biota,and waste.
With over 90 laboratories and services centers in the contiguous US and in Puerto Rico, the
network provides project support for thousands of industry, consulting, engineering and
government professionals.
PAS delivers the highest standard of testing and scientific services in the market.We offer the
most advanced solutions in the industry, backed by truly transparent data, a highly trained
team,and the service and support that comes from four decades of experience.
4.1.4.1 Organization Structure
Each location maintains a local management structure under the oversight and
guidance of corporate personnel. Local management is responsible for making day-
to-day decisions regarding the operations of the facility, implementing the quality
management system, upholding the requirements of the quality program, and for
supervision of personnel.
Local management is provided by the Regional Vice-President-Operations (RVPO),
Corporate Quality Program Manager (QPM), General Manager (GM), Quality
Manager (QM),and department specific management and supervisory personnel.
The GM reports to a Vice-President of Operations (RVPO), who is responsible for
the management of multiple laboratories and service centers across the division. The
RVPO reports directly to the Chief Operating Officer(COO).
The QM reports to a Quality Program Manager (QPM), who is responsible for
managing quality personnel for multiple locations across the division. The QPM
reports directly to the Corporate Quality Director (CQD). The QM also maintains
an indirect reporting relationship to the GM of each location that the QM manages.
Technical oversight for each location is provided by corporate personnel, RVPO,
QPM,GM,QM,and department-specific management.
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Refer to the organization charts provided in Appendix D to view the management
structure,reporting relationships,and the interrelationships between positions.
4.1.5 Management Requirements
4.1.5.1 Personnel
The laboratory is staffed with administrative and technical personnel who perform
and verify work under the supervision of managerial personnel.
■ Technical personnel include analysts and technicians that generate or contribute
to the generation of analytical data and managerial personnel that oversee day to
day supervision of laboratory operations. Including the reporting of analytical
data and results, monitoring QA/QC performance, and monitoring the validity
of analysis to maintain data integrity and reliability.
■ Administrative personnel support the day-to-day activities of the laboratory.
■ IT personnel maintain the information technology systems and software used at
the laboratory.
■ Client services personnel include project managers and support staff that manage
projects.
■ Managerial personnel make day-to-day and long-term decisions regarding the
operations of the facility,supervise personnel,implement the quality management
system and uphold the requirements of the quality program.
All personnel regardless of responsibilities are expected to carry out their duties in
accordance with the policies and processes outlined in this manual and in accordance
with standard operating procedures (SOPs) and other quality system documents. The
laboratory's policies and procedures are designed for impartiality and integrity.When
these procedures are fully implemented,personnel remain free from undue pressure
and other influences that adversely impact the quality of their work or data.
4.1.5.1.1 Key Personnel
Key personnel include the management positions that have the
authority and responsibility to plan,direct,and control,activities of
the division (corporate) or the laboratory.
The following tables list key personnel positions by PAS job title and
the position's primary deputy:
Key Personnel: Corporate
Key Personnel Primary Deputy
Chief Executive Officer Chief Operating Officer
Chief Operating Officer Chief Executive Officer
Chief Compliance Officer Quality Director
Corporate Quality Director Chief Compliance Officer
Health and Safety Director Chief Compliance Officer
IT Director LIMS Administrator,however named.
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Key Personnel:Laboratory
Key Personnel Primary Deputy
Regional Vice President- Chief Operating Officer or as designated.
Operations
Quality Program Manager A different QPM or Corporate Quality
Director
General Manager Regional Vice President of Operations
Quality Manager Quality Program Manager
Manager—Client Services General Manager or as designated.
Local IT Corporate IT Director or as designated.
Department Manager General Manager
Technical Directors/Managers Another qualified employee
Acting Technical Manager TNI
Operations Managers General Manager
1 Position may not be staffed at each location.
Some state certification programs require the agency to be notified
when there has been a change in key personnel. Program-specific
requirements and timeframes for notification by agency,are tracked
and upheld by the local QM,when these requirements apply.
4.1.5.2 Roles and Responsibilities
The qualifications, duties, and responsibilities for each position are detailed in job
descriptions maintained by PAS's corporate Human Resource's Department(HR).
The following summaries briefly identify the responsibility of key personnel positions
in relation to the ENV quality management system.
Chief Executive Officer (CEO): The CEO has overall responsibility for
performance of the organization and endorses the quality program. Working with
corporate and laboratory management, the CEO provides the leadership and
resources necessary for ENV locations to achieve the goals and objectives of the
quality management system and quality policy statement.
Chief Operating Officer (COO): The COO oversees all aspects of operations
management including, strategic planning, budget, capital expenditure, and
management of senior management personnel for ENV In this capacity, the COO
provides leadership and resources necessary to help top management at each ENV
location achieve the goals and objectives of the quality management system and
quality policy statement.
Chief Compliance Officer (CCO): The CCO oversees the quality assurance and
environmental health and safety programs (EHS) for each business unit. The CCO
is responsible for planning and policy development for these groups to ensure
regulatory compliance and to manage risk. The position provides leadership and
guidance necessary for all PAS locations to achieve the goals and objectives of the
quality and EHS programs.
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The CCO also serves as the Ethics Officer (ECO). The ECO develops the Ethics
and Data Integrity Policy and Training Program and provides oversight for reporting
and investigation of ethical misconduct to maintain employee confidentiality during
the process. The ECO provides guidance and instruction for follow-up actions
necessary to remedy the situation and deter future recurrence.
Corporate Director of Quality (CQD): The Corporate Director of Quality is
responsible for developing and maintaining the ENV quality program under guidance
and assistance from the CEO, COO, and CCO. This position develops corporate
quality policy and procedure and analyzes metric data and other performance
indicators to assess and communicate the effectiveness of the quality program to top
tYP g
management. The position provides leadership and guidance for implementation of
the quality program across all ENV locations.
Corporate Quality Program Manager (QPM): The Quality Program Manager is
responsible for managing the implementation of the ENV qua
lity program for one or
more locations in the network. Working with the CQD and local laboratory
management to which they are assigned,the QPM provides leadership,guidance and
resources, including allocation of personnel, necessary to achieve the goals of ENV
quality program.
Corporate Director of Information Technology: The Corporate Director of IT
oversees the systems and processes of information technology used to support the
quality program. These systems include Laboratory Information Management
Systems (LIMS);data acquisition,reduction,and reporting software;virus-protection,
communication tools,and ensuring the integrity and security of electronic data.
Regional Vice-President of Operations): The RVPO has full glresponsibility for
administrative and operations management and p g performance of a group of ENV
� P
laboratories and service centers. Working with the COO and local laboratory
management, the RVPO provides leadership, guidance and resources, including
allocation of personnel,necessary to achieve the goals of ENV quality program.
General Manager (GM): The GM is responsible for the overall performance and
administrative and operations management of an ENV location and associated service
center(s). This position is responsible to provide leadership and resources,including
allocation and supervision of personnel,necessary for the location to implement and
achieve the goals of the PAS quality program. In this capacity, the position assures
laboratory personnel are trained on and understand the structure and components of
the quality program defined in this manual as well as the policies and procedures in
place to implement the quality management system.
The GM of NELAC/TNI Accredited laboratories is also responsible for the
designation of technical personnel to serve as acting technical managers for TNI for
the fields of accreditation held by the laboratory (See Section 4.1.5.2.1) and for
notifying the accreditation body (AB) of any extended absence or reassignment of
these designations.
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Quality Manager (QM): The QM oversees and monitors implementation of the
quality management system for each ENV location assigned and communicates
deviations to laboratory management. The QM is independent of the operation
activities for which they provide oversight and has the authority to carry out the roles
and responsibilities of their position without outside influence.
Additionally,in accordance with the TNI Standard,the QM:
• serves as the focal point for QA/QC and oversees review of QC data for trend
analysis;
• evaluates data objectively and perform assessments without outside influence;
• has documented training and experience in QA/QC procedures and the
laboratory's quality system;
• has a general knowledge of the analytical methods offered by the laboratory;
• coordinates and conducts internal systems and technical audits;
• notifies laboratory management of deficiencies in the quality system;
• monitors corrective actions;
• provides support to technical personnel and may serve as the primary deputy for
the acting TNI Technical Manager(s).
Manager-Client Services (CSM): This position is responsible for training and
management of client facing staff that serve as the liaison between PAS and the
customer to ensure that projects are successfully managed to meet the expectations
and needs of PAS customers. This position is also responsible for sharing positive
and negative customer feedback with laboratory management so that this information
may be used to improve the quality program.
Local IT Manager, however named: Local IT managers are responsible for
maintaining the IT systems used to support the quality program. These systems
include Laboratory Information Management Systems (LIMS); data acquisition,
reduction, and reporting software; virus-protection, communication tools, and
ensuring the integrity and security of electronic data.
Department Manager (DM): The DM is responsible for administrative and
operations management and implementation of the quality management system in the
work area he/she oversees. These responsibilities include but are not limited to:
training and supervision of personnel, monitoring work activity to maintain
compliance with this manual,SOPs,policies and other instructional documents that
support the quality management system; method development, validation and the
establishment and implementation of SOPs to assure regulatory compliance and
suitability for intended purpose; monitoring QA/QC performance, proper handling
and reporting of nonconforming work, purchasing of supplies and equipment
adequate for use, maintaining instrumentation and equipment in proper working
order and calibration, and general maintenance of administrative and technical
processes and procedures established by the laboratory.
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Operations Manager(OM): The OM is responsible for management of production
and/or other duties assigned by the GM.
4.1.5.2.1 Acting Technical Manager(TNI Accreditation):
For ENV locations that are NELAC/TNI accredited:
The TNI Standard specifies requirements for the qualification and
duties of technical personnel with managerial responsibility. These
requirements are associated in the Standard to the designation
`technical manager(s), however named'. These responsibilities may
be assigned to multiple individuals and are not associated with any
specific job tide.
The TNI requirements for personnel that provide technical
oversight correlate with ENV job descriptions for Department
Manager or Supervisor. However,the duties may be assigned to any
PAS employee that meets the TNI specified qualifications.
Personnel assigned this designation retain their assigned job title.
The job title may be appended with "acting as technical manager forTNI"
and the technology or field of accreditation for which the employee
is approved,if necessary.
When TNI Accreditation Bodies (AB) refer to these employees as
`technical manager' or `technical director' on the official certificate
or the scope of accreditation, this reference is referring to their
approval to carry out duties of the `technical manager, however
named'as specified in the TNI Standard.
In accordance with the TNI Standard, the acting Technical
Manager(s) for TNI are responsible for monitoring the performance
of QC/QA in the work areas they oversee.
If the absence of any employee that is approved as acting technical
manager for TNI exceeds 15 calendar days, the duties and
responsibilities specified in the TNI Standard are temporarily
reassigned to another employee that meets the qualifications for the
technology or field of accreditation. If the employee's absence
exceeds 35 calendar days, the QM will formally notify the TNI
primary AB of the absence and the details of reassignment of duties
in writing.
Refer to the applicable TNI Standard for requirements for technical
oversight and required qualifications of the acting Technical
Manager(s) for each discipline (chemical, limited inorganic
chemistry,and microbiology).
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4.1.5.3 Conflict of Interest
A conflict of interest is a situation where a person has competing interests.
Laboratory management looks for potential conflict of interest and undue pressures
that might arise in work activities and then includes countermeasures in policies and
procedures to mitigate or eliminate the conflict.
See policy COR-POL-0004 Ethics Policy for more information.
4.1.5.4 Confidentiality
Laboratory management is committed to preserving the confidentiality of PAS
customers and confidentiality of business information.
Procedures used by the laboratory to maintain confidentiality include:
■ A Confidentiality Agreement which all employees are required to sign at the time
of employment and abide by the conditions of throughout employment;
• Record retention and disposal procedures that assure confidentiality is
maintained;
• Physical access controls and encryption of electronic data;and
• Protocol for handling Confidential Business Information(CBI).
Client information obtained or created during work activities is considered
confidential and is protected from intentional release to any person or entity other
than the client or the client's authorized representative,except when the laboratory is
required by law to release confidential information to another party, such as a
regulatory agency or for litigation purposes. In which case,the laboratory will notify
the client of the release of information and the information provided.
The terms of client confidentiality are included in ENV Standard Terms and
Conditions (T&C). With the acceptance of ENV Terms and Conditions and/or the
implicit contract for analytical services that occurs when the client sends samples to
the laboratory for testing, the client authorizes PAS to release confidential
information when required.
See policy COR-POL-0004 Ethics Policy for more information.
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4.1.5.5 Communication
Communication is defined as the imparting or exchanging of news and information.
Effective (good) communication occurs when the person(s) you are exchanging
information with actively gets the point and understands it.
4.1.5.5.1 Workplace Communication
Good communication in the workplace is necessary to assure work
is done correctly, efficiently, and in accordance with client
expectations.
Instructions for how to carry out work activities are communicated
to personnel via written policy, standard operating procedures,and
standard work instructions.
Information about laboratory performance (positive and negative)
and ideas for improvement are communicated using various
communication channels such as face to face meetings, video
conferencing, conference calls, email, memoranda, written reports,
and posters.
4.1.5.5.2 External Communication
Communication with external parties such as customers, vendors,
business partners,and regulatory agencies takes place every day.
Laboratory management ensure personnel learn to communicate in
professional and respectful ways in order to build strong
relationships and learn to communicate effectively to avoid
misunderstanding.
4.2 Quality Management System
4.2.1 Quality Management System Objectives
The objectives of the laboratory's quality management system are to provide clients with
consistent, exemplary professional service, and objective work product that is of known and
documented quality that meets their requirements for data usability and regulatory compliance.
Objective work product is analytical services, data, test results, and information that is not
influenced by personal feeling or opinions. The quality of being objective is also known as
`impartiality'.
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4.2.1.1 Impartiality
The laboratory achieves and maintains impartiality by implementing and adhering to
the policies and processes of the quality management system, which are based on
industry accepted standards and methodologies.
The laboratory's procedures for handling nonconforming work (See 4.9), corrective
and preventive actions (See 4.11, 4.12) and management review (See 4.15) are the
primary mechanisms used to identify risk to impartiality and to prompt actions
necessary to eliminate or reduce the threat when risk to impartiality is suspected or
confirmed.
4.2.1.2 Risk and Opportunity Assessment
Risks are variables that make achieving the goals and objectives of the quality
management system uncertain. An opportunity is something that has potential
positive consequences for the laboratory.
Laboratory personnel manage risks and opportunities on a daily basis by carrying out
the processes that make up the quality management system. Some of the ways in
which the quality management system is designed to identify,minimize,or eliminate
risk on a daily basis include but are not limited to:
• Capability and capacity reviews of each analytical service request to assure the
laboratory can meet the customer's requirements;
• Maintenance of accreditation and certification for test methods in multiple states
and programs to cover a broad range of jurisdiction for regulatory compliance;
• SOPs and other controlled instructional documents are provided to personnel to
eliminate variability in process. These documents include actions to counter risk
factors inherent in the process and are reviewed on a regular basis for on-going
suitability and relevancy;
• Participation in proficiency testing programs and auditing activities to verify on-
going competency and comparability in performance;
• Provision of on-the-job training and established protocol for quality control(QC)
corrective action for nonconforming events;
• An established program for ethics,and data integrity;
• Tiered data review process;
• Culture of continuous improvement;
• Monitoring activities to assess daily and long-term performance;and
• Annual critical review of the effectiveness of the quality management system.
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ENV also promotes a continuous improvement culture based on the principles of
lean manufacturing. These principles include 3P(Process,Productivity,Performance)
and Kaizen. 3P is a platform used by Pace to share best practices and standardization
across the network to achieve operational excellence. Kaizen is a team-based process
used to implement tools and philosophies of lean to reduce waste and achieve flow
with the purpose of improving both external and internal customer satisfaction.
ENV's lean programs and activities help to mitigate risk because they generate a
collective understanding of vulnerabilities and utilize group-effort to develop and
implement solutions at all levels.
Risk and opportunities may also be formally identified using specific risk and
opportunity assessment methods such as SWOT Analysis (Strength, Weakness,
Opportunity,Threats) and 3-Stage Impact/Probability Grids.
4.2.1.3 Communication of the Quality Management System
This manual is the primary mechanism used by laboratory management to
communicate the quality management system to laboratory personnel.
To assure personnel understand and implement the quality program outlined in the
manual:
• All laboratory personnel are required to sign a Read and Acknowledgement
Statement to confirm the employee has: 1) been informed of the manual by
laboratory management, 2) has access to the manual, 3) has read the manual 4)
understands the content of the manual, and 5) agrees to abide by the
requirements,policies and procedures therein.
• Personnel are informed that the manual provides the "what" of the quality
management system. The"how to"implementation of the quality management
system is provided in policy, SOPs, standard work instructions, and other
controlled instructional documents.
4.2.2 Quality Policy Statement
The quality policy of the laboratory is to provide customers with data of known and
documented quality fit for their intended purpose. The laboratory achieves this policy
by implementing the quality management system defined in this manual,by following
industry accepted protocol for analytical testing and quality assurance and quality
control (QA/QC) activities, by conformance with published and industry accepted
testing methodologies, and by compliance with international and national standards
for the competency and/or accreditation of testing laboratories.
Intrinsic to this policy statement is each of the following principles:
• The laboratory will provide customers with reliable, consistent,and professional
service. This is accomplished by making sure the laboratory has the resources
necessary to maintain capability and capacity;that staff are trained and competent
to perform the tasks they are assigned; that client-facing staff are trained and
prepared to find solutions to problems and to assist customers with their needs
for analytical services. Customer feedback,both positive and negative,is shared
with personnel and used to identify opportunities for improvement.
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■ The laboratory maintains a quality program that complies with applicable state,
federal,and industry standards for analytical testing and competency.
ISO/IEC 17025 and the TNI (The NELAC Institute) Standard is used by ENV
to establish the minimum requirements of the ENV quality program.
ISO/IEC 17025 is a competency standard that outlines the general requirements
for the management system for calibration and testing laboratories. It is the
primary quality system standard from which other quality system standards,such
as the TNI Standard,are based.The TNI Standards are consensus standards that
provides management and technical requirements for laboratories performing
environmental analysis.
• Laboratory management provides training to personnel so that all personnel are
familiar with the quality management system outlined in this manual and that they
understand that implementation of the quality management system is achieved by
adherence to the organization's policies and procedures.
• Laboratory management continuously evaluates and improves the effectiveness
of the quality management system by responding to customer feedback,and other
measures of performance, such as but not limited to: the results of
internal/external audits, proficiency testing, metrics, trend reports, and annual
and periodic management reviews.
4.2.2.1 Ethics Policy/Data Integrity Program
PAS has established a comprehensive ethics and data integrity program that is
communicated to all PAS employees in order that they understand what is expected
of them. The program is designed to promote a mindset of ethical behavior and
professional conduct that is applied to all work activities.
The key elements of the PAS Ethics /Data Integrity Program include:
■ Ethics Policy(COR-POL-0004);
■ Ethics Officer;
• Standardized data integrity training course taken by all new employees on hire
and a yearly refresher data integrity training course for all existing employees;
• Policy Acknowledgement Statements that all PAS personnel, including contract
and temporary, are required to sign at the time of employment and again during
annual refresher training to document the employee's commitment and
obligation to abide by the company's standards for ethics, data integrity and
confidentiality;
• SOPs that provide instructions for how to carry out a test method or process to
assure tasks are done correctly and consistently by each employee;
• On the Job Training;
• Data integrity monitoring activities which include,but are not limited to,primary,
secondary and completeness data reviews, internal technical and system audits,
data audits,data surveillance,and proficiency testing;and
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■ Confidential reporting process for alleged ethics and data integrity issues.
All laboratory managers are expected to provide a work environment where personnel
feel safe and can report unethical or improper behavior in complete confidence
without fear of retaliation.Retaliation against any employee that reports a concern is
not tolerated.
PAS has engaged Lighthouse Services,Inc. to provide personnel with an anonymous
reporting process available to them 24 hours a day/7 days per week. The alert line
may be used by any employee to report possible violations of the company's ethics
and data integrity program. When using the reporting process, the employee does
need to specify the location of concern and when reporting by email,also include the
company name.Messages are collected,documented,reviewed,and will be followed
up on by the Ethics Compliance Officer to resolve the matter. Investigations
concerning data integrity are kept confidential.
Lighthouse Compliance Alert Lines:
English Speaking US&Canada [phone]
Spanish Speaking North America [phone]
Internet www/li hthouse-services.com/ acelabs
g P
Email [e-mail]
4.2.3 Management Commitment: Quality Management System
Evidence of management's commitment for the development, maintenance, and on-going
improvement of the quality management system is provided by the application of their
signature of approval to this manual. Their signature confirms they understand their
responsibility to implement the quality management system outlined in this manual, to
communicate the quality program to personnel, and to uphold requirements of the program
during work activities.
4.2.4 Management Commitment: Customer Service
Management communicates the importance of meeting customer and regulatory requirements
to personnel by training personnel on the quality management system outlined in this manual,
implementing the quality management system outlined in this manual, and upholding these
requirements for all work activities.
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4.2.5 Supporting Procedures
Documents that support this manual and quality management system are referenced
throughout this manual. The structure of the document management system is outlined in
SOP ENV-SOP-CORQ-0015 Document Management and Control (most recent revision or
replacement) and summarized in the following subsections.
4.2.5.1 Quality Management System Document Structure
Documents associated with the quality management system are classified into
document types that identify the purpose of the document and establish how the
document is managed and/or controlled.
Document types are ranked to establish which documents takes precedence when
there is an actual or perceived conflict between documents and to establish the
hierarchal relationships between documents. The ranking system also provides
information to document writers and reviewers to assure downline documents are in
agreement with documents of higher rank. Project specific documents are not ranked
because client specific requirements are not incorporated into general use documents
in order to maintain client confidentiality.
Examples:ENV QMS Documents: Internal
Document Type Purpose
Quality Manual Outlines the laboratory's quality management system and structure and how
it works for a system including policy,goals,objectives and detailed
explanation of the system and the requirements for implementation of
system. Includes roles and responsibilities,relationships,procedures,
systems and other information necessary to meet the objectives of the
system described.
Policy Provide requirements and rules for a PAS process and is used to set course
of actions and to guide and influence decisions. Policy describes the"what",
not the"how".
Standard Operating Provide written and consistent set of instructions or steps for execution of a
Procedure routine process,method,or set of tasks performed by PAS. Includes both
fundamental and operational elements for implementation of the systems
described in PAS manual(s). Assures that activities are performed properly
in accordance with applicable requirements. Designed to ensure
consistency,protect EHS of employees and environment,prevent failure in
the process and ensure compliance with company and regulatory
requirements. SOPs describes the"how"based on policy.
Standard Work Provide step by step visual and/or written instruction to carry out a specific
Instruction task to improve competency,minimize variability,reduce work injury and
strain,or to boost efficiency and quality of work(performance). SWI are
associated with an SOP unless the task described is unrelated to generation
of or contribution to environmental data or analytical results.
Template Pre-formatted document that serves as a starting point for a new document.
Guide Provide assistance to carry out a task.
Form Used for a variety of purposes such as to provide a standardized format to
record observations,to provide information to supplement an SOP.
Guidance Non-binding advice used to explain internal policies,procedures,or
practices.
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Example:ENV QMS Documents:External
Certificate Lists
parameters,
methods,and matrices for which the laboratory y is
certified/accredited to perform within the jurisdiction of the issuing
regulatory agency or accreditation body.
Reference Provide information,protocol,instructions,and/or requirements. Issued by
Document the specifier.Examples include quality system standards such as ISO/IEC,
TNI,DoD and published referenced methods such as Standard Methods,
ASTM,SW846,EPA,and federal and state regulatory bodies.
Project Document Provides requirements necessary to meet individual client expectations for
intended use of data. Examples include project quality assurance plans
(QAPP),client-program technical specifications,contracts,and other
agreements.
Document Hierarchy
Rank Document
1 Reference Documents
2 Corporate Manual
3 Corporate Policy
4 Corporate SOP
5 Corporate SWI,Templates,Guides,Forms,Guidance
6 Laboratory Manual
7 Laboratory SOP
8 Laboratory SWI,Templates,Guide,Forms,Guidance
NA Project Documents
4.2.6 Roles and Responsibilities
The roles and responsibilities for technical management and the quality manager is provided
in section 4.1.5.2.
4.2.7 Chang
e Management
ement g
When significant changes to the ENV quality management system are planned,these changes
are managed by corporate quality personnel to assure that the integrity of the quality
management system is maintained.
4.3 Document Control
4.3.1 General
The laboratory's procedures for document control are provided in SOP ENV-SOP-CORQ-
0015 Document Management and Control(most recent revision or replacement).
The laboratory uses electronic document management software (eDMS) to carry out the
document control procedures of the SOP. eDMS automates the process for unique document
identification, version control, approval, access, and archival. The eDMS software used by
ENV restricts access to archived documents except to authorized users to prevent the use of
obsolete documents.
The local QM maintains a master list of controlled documents used at the laboratory. The
master list includes the document control number,document title,and current revision status
and is made available to personnel for their reference.
See SOP ENV-SOP-CORQ-0015 Document Management and Control(most recent revision or
replacement) for more information.
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4.3.2 Document Approval and Issue
Documents that support the quality management system are reviewed by qualified personnel
and approved by laboratory management prior to release for general use.
Only the approved versions of documents are available to personnel for use unless use of a
draft document is authorized by management.
See SOP ENV-SOP-CORQ-0015 Document Management and Control(most recent revision or
replacement) for more information.
4.3.3 Document Review and Change
Unless a more frequent review is required by regulatory,certification or accreditation program
the laboratory formally reviews documents at least every two years to ensure the document
remains current,appropriate,and relevant.
Documents are also informally reviewed every time the document is used. Personnel are
expected to refer to and follow instructions in controlled documents when they carry out their
work activities. Consequently,any concerns or problems with the document should be caught
and brought to the attention of laboratory management on an on-going basis.
Documents are revised whenever necessary to ensure the document remains usable and
correct. Older document versions and documents no longer needed are made obsolete and
archived for historical purposes.
ENV does not allow hand-edits to documents. If an interim change is needed pending re-
issue of the document, the interim change is communicated to those that use the document
using a formal communication channel, such as SOP Change in Progress form, email, or
memorandum.
The document review, revision, and archival process is managed by quality personnel at the
location from which the document was released using the procedures established in SOP
ENV-SOP-CORQ-0015 Document Management and Control (most recent revision or
replacement).
4.4 Analytical Service Request,Tender, and Contract Review
The laboratory's management and/or client service personnel perform thorough reviews of requests
and contracts for analytical services to verify the laboratory has the capability,capacity,and resources
necessary to successfully meet the customer's needs. These review procedures are described in
laboratory SOP ENV-SOP-GBAY-0006,Sample Management and Review of Analytical Requests.
The proceduresSOP(s)in this SOP s) are established to ensure that:
■ The laboratory understands the purpose of data collection in order to ensure the test methods
requested are appropriate for the intended use of the data and capable of meeting the client's data
quality objectives;
• The laboratory and any subcontractor has the capability, capacity, and resources to meet the
project requirements and expectations within the requested time frame for delivery of work
product;
■ Any concerns that arise from review are discussed and resolved with the client;and
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• The results of review and any correspondence with the client related to this process and/or any
changes made to the contract are recorded and retained for historical purposes.
Capability review confirms that the in-network laboratories and any potential subcontractors hold
required certification/accreditation for the test method,matrix,and analyte and verifies the laboratory
can achieve the client's target compound list and data quality objectives (DQOs) for analytical
sensitivity and reporting limits, QA/QC protocol, and hardcopy test report and electronic data
deliverable (EDD) formats.
Capacity review verifies that the in-network laboratories and any potential subcontractors are able to
handle the sample load and deliver work production within the delivery timeframe requested.
Resource review verifies that the laboratory and any potential subcontractors have adequate qualified
personnel with the skills and competency to perform the test methods and services requested and
sufficient and proper equipment and instrumentation needed to perform the services requested.
4.5 Subcontracting and In-Network Work Transfer
The terms `subcontract' and "subcontracting" refers to work sent to a business external to Pace
Analytical Services,LLC (PAS) and the term`subcontractor'refers to these external businesses,which
are also called vendors.
Work transferred within the ENV network is referred to as interregional work orders (IRWO) and
network laboratories are referred to as IRWO,IR,or a network laboratory.
The network of ENV laboratories offers comprehensive analytical capability and capacity to ensure
PAS can meet a diverse range of client needs for any type of project. If the laboratory receives a
request for analytical services and it cannot fulfill the project specifications, the laboratory's client
services team will work with the client to place the work within the ENV network. When it is not
possible to place the work within network, the laboratory will, with documented client approval,
subcontract the work to a subcontractor that has the capabilities to meet the project specifications
and can meet the same commitment agreed on between the laboratory and the client. Some client
programs require client consent even for in-network work transfer, and when this applies, the client
services team obtains consent as required. The laboratory retains the record of client notification and
their consent in the project record for historical purposes.
Whenever work is transferred to a subcontractor or an in-network laboratory, the laboratory
responsible for management of the project verifies each of these qualifications:
■ The subcontractor or in network laboratory has the proper accreditation/certifications required
for the project and these are current;and
■ The use of the subcontractor or in network laboratory is approved by the client and/or regulatory
agency,when approval is required. Record of approval is retained in the project record.
All subcontractor laboratories must maintain a quality management system like ENV and that
complies with ISO/IEC 17025 and the TNI Standard(s).
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ENV also evaluates and pre-qualifies subcontractors as part of the company's vendor qualification
program. The complete list of approved vendors is maintained by the corporate procurement
department and is made available to all ENV locations. Pre-qualification of a subcontractor does not
negate the requirement for the placing laboratory to verify the capability, capacity, and resources of
any selected subcontractor on a project-specific basis to confirm the subcontractor can meet the
client's needs.
For both subcontracting and in-network work transfer, the project specifications are always
communicated to the subcontractor or the in-network laboratory by the project manager so that the
laboratory performing the work is aware of and understands these requirements.
The procedures for subcontracting are outlined in laboratory SOP ENV-SOP-GBAY-0005,
Subcontracting Samples.
�
4.6 Purchasing Services and Supplies
Vendors thatprovide services and supplies to the laboratoryare pre qualified to verifythe vendor's
pP p q
capability to meet the needs of PAS. These needs include but are not limited to competitive pricing,
capacity to fill purchase orders, quality of product, customer service, and business reputation and
stability. The records of vendor evaluation and the list of approved vendors is maintained by the
corporate procurement department.
The procedures for vendor qualification are specified in the corporate process for vendor
qualification,however named.
The laboratory may purchase goods and services from any supplier on the approved vendor list.
The specifications (type,class,grade,tolerance,purity,etc.) of supplies,equipment,reagents,standard
reference materials and other consumables used in the testing process are specified in SOPs. The
SOP specifications are based on the governing requirements of the approved reference methods and
any additional program driven regulatory specification, such as drinking water compliance. All
requisitions for materials and consumables are approved by the department supervisor to confirm the
purchase conforms with specified requirements. After approval the requisition is handled by the
laboratory's designated purchasing agent. On receipt, the product is inspected and verified before
use,when applicable.
The laboratory's procedure for the purchase of services and supplies is specified in laboratory SOP
ENV-SOP-GBAY-0145,Laboratory Supply Procedures.
4.7 Customer Service
Project details and management is handled by the laboratory's customer service team. Each customer
is assigned a Project Manager (PM) that is responsible for review of contract requirements and
handling laboratory to customer communication about the project status.
4.7.1 Commitment to Meet Customer Expectations
The laboratory cooperates and works closely with our customers to ensure their needs are met
and to establish their confidence in the laboratory's capability to meet their needs for analytical
services and expectations for service.
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The PM is the customer's primary point of contact for each analytical service request. The
PM gathers information from the customer to ensure the details of their request are
understood.After samples are received,the PM monitors the progress of the project and alerts
the customer of any delays or excursions that may adversely impact data usability. Laboratory
supervisors are expected to keep the PM informed of project status and any delays or major
issues,so that the PM can keep the client informed.
The laboratory encourages customers to visit the laboratory to learn more about the
laboratory's capabilities,observe performance and to meet laboratory personnel.
ENV customers expect confidentiality. Laboratory personnel will not divulge or release
information to a third party without proper authorization unless the information is required
for litigation purposes. See Section 4.1.5.4 of this manual and policy COR-POL-0004 Ethics
Policy for more information on the laboratory's policy for client confidentiality.
4.7.2 Customer Feedback
The laboratory actively seeks positive and negative feedback from customers through surveys
and direct communication. Information from the client about their experience working with
the laboratory and their satisfaction with workproduct is used to enhance processes and
practices and to improve decision making. Customer feedback is communicated to laboratory
management and corporate personnel in management reports and analyzed yearly during
management review (See 4.15) to identify risk and opportunity. Corrective, preventive, or
continuous improvement actions are taken based on nature of and/or feedback trends.
Also see sections 4.9,4.10,4.11,4.12,4.14,and 4.15 for more information about how customer
feedback is managed by the laboratory and used to enhance the quality management system.
4.8 Complaints
Complaints provide opportunities to improve processes and build stronger working relationships with
our clients.
The laboratory's complaint resolutionprocess includes three steps. First, handle and resolve the
r3' P P
complaint to mutual satisfaction. Second,perform corrective action to prevent recurrence (See 4.11).
Third,record and track the complaint and use these records for risk and opportunity assessment and
preventive action (See 4.12).
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4.9 Nonconforming Work
4.9.1 Definition of Nonconforming Work
Nonconforming work is work that does not conform to customer requirements, standard
specifications,laboratory policies and procedures,or that does not meet acceptance criteria.
The discovery of non-conforming work comes from various sources which include, but are
not limited to:
• results of quality control samples and instrument calibrations;
• quality checks on consumables and materials;
• general observations of laboratory personnel;
• data review;
• proficiency testing;
• internal and external audits;
• complaints and feedback;
• management review and reports;and
• regulatory and certification and accreditation actions.
The way in which the laboratory handles nonconforming work depends on the significance
and impact(risk) of the issue. Some issues may simply require correction,others may require
investigation, corrective action(See 4.11) and/or data recall(See 4.16). When the laboratory
releases data and test results associated with nonconforming QC and acceptance criteria, test
results are qualified, or non-conformances are noted in the final analytical report to apprise
the data user of the situation. (See 5.10)
Nonconforming work also includes unauthorized departure from laboratory policies,
procedures and test methods. Authorized departures are explained in the following
subsections. Situations that do not conform to these conditions are considered unauthorized
departure(s).
4.9.1.1 Authorized Departure from SOP
An authorized departure from a test method SOP is one that has been reviewed and
approved by the Department Manager,designated Acting Technical Manager for TNI
for the discipline the SOP pertains to (Chemistry, Inorganic Chemistry,
Microbiology), Quality Manager, or the General Manager. Management review is
conducted to confirm the departure does not conflict with regulatory compliance
requirements for which the data will be used or does not adversely affect data integrity.
The departure may originate from client request or may be necessary to overcome a
problem.
An authorized departure from administrative or process-oriented SOP is typically
necessary to correct an error in the SOP. These departure requests are reviewed and
pre-approved by the QA Manager.
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Documentation of SOP departures and approval decisions are retained by the
laboratory as evidence that the departure was authorized.When necessary,approved
departures from test method SOPs are noted in the final test report to advise the data
user of any ramification to data quality.
4.9.1.2 Authorized Departure from Test Methods (Method Modifications)
When test results are associated to a published reference test method,the laboratory's
test method SOP must be consistent with the test method. If the test method is
mandated for use by a specific regulatory program such as drinking water or
wastewater or a certification or accreditation program, such as TNI/NELAC, the
SOP must also comply with or include these requirements. If the procedures in the
SOP are modified from the test method,these modifications must be clearly identified
in the SOP. The conditions under which the laboratory may establish an SOP that
is modified from these reference documents, and what is considered a modification
are specified in ENV-SOP-CORQ-0011 Method Validation and Instrument Verification
(most recent revision or replacement).
Modifications that do not meet the requirements of this SOP (ENV-SOP-CORQ-
0011) are unauthorized. Client requests to deviate from the test method are handled
as client requests to depart from the test method SOP since it is the SOP that the
laboratory follows when performing work.
4.9.1.3 Stop Work Authority
Stop Work Authority provides laboratory personnel with the responsibility and
obligation to stop work when there is a perceived unsafe condition or behavior that
may result in an unwanted event.
All laboratory and corporate personnel have the authority to stop work when needed
to preserve data integrity or safety of workers.
Once a stop work order has been initiated and the reason for doing so is confirmed
valid;laboratory management is responsible for immediate correction and corrective
action (see section 4.11) before resumption of work.
Laboratory management refers to the positions listed as key personnel in section
4.1.5.1.1 of this manual.
For stop work orders related to safety,the decision to resume to work after correction
or corrective action may be made by the Chief Compliance Officer,the EHS Director,
and the General Manager or the designees for these positions.
For stop work orders related to data integrity, the decision to resume to work after
correction or corrective action may be made by the Chief Compliance Officer, the
Corporate Quality Director, the Corporate Program Manager, the local Quality
Manager or the designees for these positions.
4.10 Continuous Improvement
The laboratory's quality management system is designed to achieve continuous improvement through
the implementation of the quality policy and objectives outlined in this manual. Information about
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the laboratory's activities and performance is gained from many sources such as customer feedback,
audits, QC, trend analysis, business analytics, management reports, proficiency testing, and
management systems review. This information is subsequently used during the laboratory's corrective
action (see section 4.11) and preventive action(see section 4.12) processes and during annual review
of the management system (see section 4.15) to establish goals and objectives for improvement.
ENV also promotes a continuous improvement culture based on the principles of lean manufacturing.
These principles include 3P (Process,Productivity,Performance) and Kaizen. 3P is a platform used
by Pace to share best practices and standardization across the network to achieve operational
excellence. Kaizen is a team-based process used to implement tools and philosophies of lean to
reduce waste and achieve flow with the purpose of improving both external and internal customer
satisfaction.
4.11 Corrective Action
Corrective action is a process used to eliminate the cause of a detected nonconformity. It is not the
same as a correction. A correction is an action taken to fix an immediate problem. The goal of the
corrective action process is to find the underlying cause(s) of the problem and to put in place fixes to
prevent the problem from happening again. The corrective action process, referred to as CAPA by
ENV, is one of the most effective tools used by the laboratory to prevent nonconforming work,
identify risk and opportunity,and improve service to our customers.
The laboratory has two general processes for corrective action:
The process used for actions taken in response to day to day quality control (QC) and acceptance
criteria exceptions (nonconformance) that occur during the day to day testing process are called
corrections.These events do not usually include formal methods for cause analysis;instead the reason
for the failure is investigated through troubleshooting or other measures. Required actions for
correction of routine nonconformance is specified in laboratory SOPs. When corrective action is not
taken, cannot be taken,or is not successful,test results associated with the nonconforming work are
qualified in the final test report.Documentation of the nonconformance and corrective action taken
is documented in the analytical record.
A 7-stage corrective action process is used when there is a problem or departure from the quality
management system,technical activities,or when the extent of a single problem has significant impact
on data, regulatory compliance or customer needs. These problems are identified through various
activities such as but not limited to: quality control trends,internal and external audits,management
review, customer feedback,and general observation.
The laboratory's 7 Stage CAPA Process includes:
1) Identification and Containment
2) Evaluation
3) Investigation
4) Cause Analysis
5) Action Plan
6) Implementation
7) Follow Up and Effectiveness Review
The 7 stage CAPA process may be initiated by any employee. Once the process is initiated it is
overseen and coordinated by laboratory management. The CAPA process is documented using a
software-based workflow process called Qualtrax. The Qualtrax CAPA record includes tracking
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information,dates,individuals involved,those responsible for action plan implementation and follow-
up,and timelines and due dates.
ENV's procedures for corrective action, are specified in corporate SOP ENV-SOP-CORQ-0018,
Procedure for Corrective and Preventive Action (most recent revision or replacement). Additional
explanation about certain aspects of the laboratory's corrective action process are outlined in the next
three subsections.
4.11.1 Cause Analysis
Cause analysis is the process of investigation used by the laboratory to identify the underlying
cause(s) of the problem. Once causal factors are identified,ways to mitigate the causal factors
are reviewed and corrective action(s) most likely to eliminate the problem are selected.
The laboratory uses different methods to conduct this analysis.The most common approach
is 5-Why,but fishbone diagrams,or even brainstorming may be appropriate depending on the
situation. The method used is documented in the CAPA record.
4.11.2 Effectiveness Review
Monitoring corrective actions for effectiveness is an activity shared by laboratory supervisors
and quality assurance personnel. Effectiveness means the actions taken were sustainable and
appropriate. Sustainable means the change is still in place. Appropriate means the action(s)
taken prevented recurrence of the problem since the time corrective action was taken.
The timeframe in which effectiveness review takes place depends on the event and is recorded
in the CAPA record with anyaddition
a on actions that need to be taken.
Corrective action trends are also monitored by laboratory management and used to identify
opportunities for preventive action or to gain lessons learned when actions taken were not
adequate to solve the problem. See Section 4.12 (Preventive Action) and 4.15 (Management
Review) for more information.
4.11.3 Additional Audits
When non-conformities or other problems cast doubt on compliance with the laboratory's
policies,procedures,or compliance to regulatory requirements;the quality manager schedules
a special audit of the area of activity in accordance with Section 4.14.1 as soon as possible.
These special audits are used to determine the scope of the problem and to provide
information for the CAPA process. Additional full-scale audits are done when a serious issue
or risk to the laboratory's business is identified.
4.12 Preventive Action
Preventive action is an action taken to eliminate the cause of a potential nonconformity and to achieve
improvement.Preventive action is a forward-thinkingprocess designed to prevent problems opposed
to reacting to them (corrective action).
Some examples of preventative action include,but are not limited to:
! Scheduled instrument maintenance (Preventative maintenance)
! Addition of Staff and Equipment
! Professional Development Activities
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! Implementation of New Technology
The laboratory looks for opportunities for preventive action from a variety of sources including but
not limited to: employee idea's,customer feedback,business partners input, trend analysis,business
analytics,management reviews,proficiency testing results,lean management events, and risk-benefit
analysis.
Laboratory management evaluates the success of preventive actions taken in any given year during
annual management review. See Section 4.15 for more information.
4.12.1 Change Management
Preventive actions may sometimes result in significant changes to processes and procedures
used by the laboratory.Laboratory management evaluates the risks and benefits of change and
includes in its implementation of change process, actions to minimize or eliminate any risk.
The types of changes for which risk are considered and managed include: infrastructure
change, change in analytical service offerings, certification or accreditation status,
instrumentation,LIMS changes,and changes in key personnel.
4.13 Control of Records
A record is a piece of evidence about the past, especially an account of an act or occurrence kept in
writing or some other permanent form. Laboratory records document laboratory activities and
provide evidence of conformity to the requirements established in the quality management system.
These records may be hardcopy or electronic on any form of media.
4.13.1 General Requirements
4.13.1.1 Procedure
The requirements for control of records is specified in corporate policy ENV-POL-
CORQ-0013 Record Management. The procedure used to implement the policy is
described in laboratory SOP ENV-SOP-CORQ-0015 Document Management and Control
(most recent revision or replacement) and ENV-SOP-GBAY-0119 Data and Records
Archival(most recent revision or replacement).
The policy is established to assure quality and technical records are identified,retained,
indexed,and filed to allow for retrieval during the entire retention time frame.During
storage,records are kept secure and protected from deterioration. At the end of the
retention time, the records are disposed of properly in order to maintain client
confidentiality and to protect the interests of the company.
In general, laboratory records fall into three categories: quality, technical, and
administrative.
Examples of each are provided in the following table:
Record Type Includes Records of:
Quality Document Types listed in SOP ENV-SOP-CORQ-0015 (most
recent revision or replacement)
Audits:Internal and External
Certificates and Scopes of Accreditation
Corrective&Preventive Action
Management Review
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Data Investigations
Method Validation
Instrument Verification
Training Records
Technical Raw Data
Logbooks
Certificates of Traceability
Analytical Record
Test Reports&Project Information
Technical Training Records&Demonstration of Capability
Administrative Personnel Records
Finance/Business
4.13.1.2 Record Legibility and Storage
Records are designed to be legible and to clearly identify the information recorded.
Manual entries are made in indelible ink;automated entries are in a typeface and of
sufficient resolution to be read. The records identify laboratory personnel that
performed the activity or entered the information. Records are archived and stored
in a way that they are retrievable. Access to archived records is controlled and
managed.
For records stored electronically, the capability to restore or retrieve the electronic
record is maintained for the entire retention period. Hardcopy records are filed and
stored in a suitable environment to protect from damage, deterioration, or loss.
Hardcopy records may be scanned to PDF for retention. Scanned records must be
checked against the hardcopyto verifythe scan is complete and legible.
Administrative records are kept for a minimum of 5 years and technical and quality
records are kept for 10 years unless otherwise specified by the client or regulatory
program.
The date from which retention time is calculated depends on the record. In general,
the retention time of technical records of original observation and measurement is
calculated from the date the record is created. If the technical record is kept in a
chronological logbook, the date of retention may be calculated from the date the
logbook is archived.The retention time of test reports and project records,which are
considered technical records, is calculated from the date the test report was issued.
The retention time of quality records is usually calculated from the date the record is
archived.
Refer to the record management policy and the laboratory SOP for more information.
4.13.1.3 Security
The laboratory is a secure facility and access to records is restricted to laboratory
personnel.
4.13.1.4 Electronic Records
The data systems used to store electronic records is backed up in accordance with
laboratory SOP ENV-SOP-GBAY-0162 Electronic Records Backup (most recent
revision or replacement). Access to archived records stored electronically is
maintained by personnel responsible for management of the electronic system.
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4.13.1.5 Electronic Signature Policy
Work done by ENV locations include activities that require the application of a
signature. Some of this work product is in electronic format and signatures are
applied electronically.
The Electronic Signatures in Global and National Commerce Act (E-Sign Act)
clarifies that electronic signatures are legally valid and enforceable under United States
law.
ENV's policy for use and application of electronic signatures is specified in corporate
policy ENV-POL-CORQ-0014 Electronic Signature Policy.
All employees of ENV, including temporary and contract personnel, must sign an
Electronic Signature Agreement to acknowledge that they understand and accept that
work activities performed by them may be authenticated with application of an
electronic signature and that electronic signature has the same validity as a
handwritten signature. Their signed agreement also confirms the individual has read
and understands the policy and agrees to abide by the requirements for use of
electronic signature stated in the policy.
4.13.2 Technical Records
In addition to the requirements specified in subsections 4.13.1.1 through 4.13.1.5, the
requirements in the following subsections also apply to technical records.
4.13.2.1 Description
Technical records are the accumulation of data and information generated from the
analytical process. These records may include forms, worksheets, workbooks,
checklists, notes, raw data, calibration records, final test reports, and project record.
The accumulated record essentially needs to provide adequate detail to historically
reconstruct the process and identify the personnel that performed the tasks associated
with a test result.
4.13.2.2 Real Time Recordkeeping
Personnel are instructed and expected to always record observations, data, and
calculations at the time they are made. Laboratory managers are responsible to assure
that data entries,whether made electronically or on hardcopy, are identifiable to the
task.
4.13.2.3 Error Correction
Errors in records must never be erased, deleted or made illegible. Use of correction
fluid, such as white-out is prohibited. In hardcopy records,the error is corrected by
a single strike through the original entry and the new entry recorded alongside or
footnoted to allow for readability. Corrections are initialed and dated by the person
making the correction. If the correction is not self-explanatory, a reason for the
correction is recorded.
For electronic records, equivalent measures of error correction or traceability of
changes made is kept. For example,audit trails provide records of change.
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Maintenance of proper practices for error correction is monitored through the tiered
data review process described in Section 5.9.3. Laboratory records are reviewed
throughout the data review process. Individuals performing these reviews flag errors
that are not properly corrected and bring these to the attention of the department
manager or supervisor of the work area in which the record was generated so that the
problem may be addressed and corrected with the individual(s) that did not make the
correction properly.
4.14 Audits
The laboratory performs internal systems and technical audits to assess implementation of the QMS
and compliance to this manual and to procedures,such as policy,SOP and SWI. Since the processes
in this manual are based on the relevant quality system standards and regulatory and
accreditation/certification program requirements the laboratory provides services for, the internal
audits also assess on-going compliance to these programs.
The laboratory is also audited by external parties such as regulatory agencies, customers,consultants
and non-government assessment bodies (NGAB).
Information from internal and external audits is used by laboratory management to address
compliance concerns and opportunities where improvement will increase the reliability of data.
Deficiencies,observations and recommendations from audits are managed by the local QM using the
laboratory's formal CAPA process. See Section 4.11 for more information.
4.14.1 Internal Audit
The laboratory's internal audit program is managed by the local QM in accordance with an
audit plan established at the beginning of each calendar year. The schedule is prepared to
assure that all areas of the laboratory are reviewed over the course of the year. Conformance
to the schedule is reported to both laboratory management and corporate quality personnel in
a monthly QA report prepared by the quality manager.
Although the local QM creates the audit schedule, it is the shared responsibility of local
management to assure the schedule is maintained. Laboratory supervisors cooperate with the
quality personnel to provide the auditors with complete access to the work area, personnel,
and records needed.
Internal audits are performed by personnel approved by the quality manager. In general,
personnel may not audit their own activities unless it can be demonstrated that an effective
and objective audit will be carried out. The auditor must be trained, qualified, and familiar
enough with the objectives,principles,and procedures of laboratory operations to be able to
perform a thorough and effective evaluation.
The laboratory's internal audit program ensures daily practice is consistent with laboratory's
SOPs and to verify SOPs are compliant with policy and procedures. Test reports are audited
to verify the final product is consistent with customer/project requirements, the work was
carried out in accordance with policy and SOPs, the SOP complies with the cited reference
method,test results are accurate,and of known and documented quality and properly qualified,
when necessary.
Special audits are performed ad hoc to follow up on a specific issue such as a client complaint,
negative feedback,concerns of data integrity or ethics,or a problem identified through other
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audits. Special audits may be scheduled or unscheduled. Unscheduled internal audits are
conducted whenever doubts are cast on the laboratory's compliance with regulatory
requirements or its own policies and procedures. These unscheduled internal audits may be
conducted at any time and may be performed without an announcement to laboratory
personnel.
When observations and findings from any audit(internal or external) cast doubt on the validity
of the laboratory's testing results,the laboratory takes immediate action to initiate investigate
the problem and take corrective action. (Also see 4.11 and 4.16)
The laboratory's internal audit program and auditing procedures are further described in
laboratory SOP ENV-SOP-GBAY-0108 Internal and External Audits(most current revision or
replacement.
4.14.1.1 Corporate Compliance Audit
ENV locations are also periodically audited by corporate quality personnel to assess
the location's compliance to ENV's quality management program and to evaluate the
effectiveness of implementation of the policies and procedures that make up the
quality management system. The purpose of the compliance audit is to identify risks
and opportunities and to assist laboratory management achieve the goals and
objectives of the company's quality program.
4.15 Management Review
The management team formally reviews the management system of each location under their purview
on an annual basis to assess for on-going suitability and effectiveness and to establish goals,objectives,
and action plans for the upcoming year.
The process and procedures used to conduct this review are outlined in corporate SOP ENV-SOP-
CORQ-0005 Management Review(most recent revision or replacement).
At a minimum,the following topics are reviewed and discussed:
• The on-going suitability of policies and procedures including EHS and waste management;
• Reports from managerial and supervisory personnel including topics discussed at regular
management meetings held throughout the year;
• The outcome of recent internal audits;
■ Corrective and preventive actions;
• Assessments by external bodies;
• The results of interlaboratory comparisons or proficiency tests;
• Changes in the volume and type of the work;
■ Customer and personnel feedback,including complaints;
• Effectiveness of improvements /preventive actions made since last review;
• Internal and external issues of relevance and risk identification;
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• A review of the status of actions from prior management reviews;and
• Other relevant factors,such as quality control activities,resources,and staff training.
The discussion and results of this review are documented in a formal report prepared by laboratory
management. This report includes a determination of the effectiveness of the management system
and its processes; goals and objectives for improvements in the coming year with timelines and
responsibilities,and any other need for change.
Goals and action items from annual management systems review are shared with local employees and
with corporate management to highlight focus areas for improvement in addition to areas in which
the laboratory has excelled.
4.16 Data Integrity
ENV's procedures for the investigation and response to events that may affect data integrity are
described in the corporate SOPs for data inquiries and data recall and corrective and preventive action,
however named.
Customers whose data are affected by these events are notified in a timely manner,usually within 30
days after the impact of the problem is understood. Some accreditation programs also require
notification to the accreditation body (AB) within a certain timeframe from date of discovery when
the underlying cause of the issue impacts accreditation. The laboratory follows any program or project
specific client notification requirements for notification,when applicable.
5.0 TECHNICAL REQUIREMENTS
5.1 General
Many factors contribute to the correctness and reliability of the technical work performed by the
laboratory.These factors fall under these general categories:
• Human Performance
• Facility and Environmental Conditions
• Test Method Performance and Validation
• Measurement Traceability ty
• Handling of Samples
The impact of each of these factors varies based on the type of work performed. To minimize
negative effects from each of these factors,the laboratory accounts for the contribution from each of
these categories when developing test method and process (administrative) SOPs, evaluating
personnel qualifications and competence,and in the selection of equipment and supplies used.
5.2 Personnel
5.2.1 Personnel Qualifications
The laboratory's program for personnel management is structured to ensure personnel are
selected, qualified,and competent to perform the roles and responsibilities of their position
based on education,experience,and training.
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Qualifications, duties, responsibilities, and authorities of each position are specified in job
descriptions maintained by corporate HR(See Section 5.2.4).These job descriptions provide
the general basis for the selection of personnel for hire and are used by the laboratory to
communicate to personnel the duties,responsibilities,and authorities of their position.
The term "personnel" refers to individuals employed by the laboratory directly as full-time,
part-time, or temporary, and individuals employed by the laboratory by contract, such as
through an employment agency.The term"personnel"is used interchangeably with the term
"employee"throughout this manual. For purposes of this manual,these terms are equivalent.
The personnel management program is structured to establish and maintain records for each
of the following:
• Selection of personnel;
• Training of personnel;
• Supervision of personnel;
• Authorization of personnel;and
• Monitoring Competence of personnel.
5.2.1.1 Competence
Competence is the ability to apply a skill or series of skills to complete a task or series
of tasks correctly within defined expectations.
Competence for technical personnel authorized by ENV to provide opinion and
interpretation of data to customers also includes the demonstrated ability to:
• Apply knowledge, experience, and skills needed to safely and properly use
equipment,instrumentation,and materials required to carry out testing and other
work activities in accordance with manufacturer specifications and laboratory
SOPs;
• Understand and apply knowledge of general regulatory requirements necessary to
achieve regulatory compliance in work product;and
• Understand the significance of departures and deviations from procedure that
may occur during the analytical testing process and the capability and initiative to
troubleshoot and correct the problem, document the situation and decision-
making process,and to properly qualify the data and analytical results.
The laboratory's requirements for the competence of personnel (education,
qualification, work experience, technical skills, and responsibilities) are specified in
job descriptions created by management and kept by human resources (HR).The job
description provides the basis for the selection of personnel for each position.
An employee is considered competent when he/she has completed required training.
The policies and standard operating procedures (SOPs) for the following topics are
established by management as minimum required training for all personnel:
■ Ethics and Data Integrity
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• Quality Manual
• Safety Manual
• Quality Management System
• Technical Process and Procedure relevant to their job tasks
• Successful Demonstration of Capability(DOC)—Analytical Personnel Only
Personnel are initially authorized competent to independently carry out their assigned
duties when required training is complete and documented.
Records of required training and qualification provide the record of competence for
the individual. Qualification records may include but are not limited to diploma,
transcripts,and curriculum vitae (CV).
The on-going competence of each employee is monitored by laboratory management
through on-the-job performance. Analytical employees are also required to
successfully complete another demonstration of capability for each test method
performed on an annual basis.
5.2.2 Training (Required)
ENV's training requirements are outlined in policies COR-POL-0023 Mandatory Training Policy,
COR-POL-0004 Ethics Policy,and laboratory SOP ENV-SOP-GBAY-0094 Employee Orientation
and Training.
5.2.2.1 Required Training
The laboratory's training program includes these elements:
• Scheduling of Required Training
• Execution of Required Training
• Documentation and Tracking of Required Training
• Evaluation of Training Effectiveness
Required training is delivered using various methods that incorporate techniques that
appeal to the main learning styles:visual,aural,linguistic,and kinesthetic.Techniques
include,on-the-job,instructor-led,self-study,eLearning,and blended.
The employee's direct supervisor is responsible for oversight of completion of the
employee's required training and for providing adequate time to the employee to
complete training assignments. Both the supervisor and employee are responsible to
make sure the employee's training status and training records for required training are
current and complete.
The status of completion of required training is monitored by the local QM, who
provides the status to the GM at least monthly or more frequently, if necessary, to
ensure required training for personnel is complete and up to date.
The following subsections describe the elements of ENV's required training program.
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5.2.2.1.1 New Hire Training
New hire training requirements apply to new personnel and to
existing employees starting in a new position or different work area.
Required new hire training includes each of the following:
• Ethics and Data Integrity(See 5.2.2.1.3)
• Quality Manual/ Quality Management System (See 5.2.2.1.4)
• Safety Manual and any training requirements specified in the
manual.
• Policies&SOPs relevant to their job tasks
• Technical personnel that test samples must also successfully
complete an initial demonstration of capability (IDOL) for the
test methods performed before independently testing customer
samples. (See 5.2.2.1.5). Independent testing means handling of
client samples without direct supervision of the work activity by
the supervisor or a qualified trainer.
All required training must be current and complete before the
employee is authorized to work independently. Until then, the
employee's direct supervisor is responsible for review and
acceptance of the employee's work product.
5.2.2.1.2 On-Going Training
Personnel receive on-going training in each of the following topics:
• Ethics and Data Integrity(See 5.2.2.1.3)
• Quality Manual/ Quality Management System (See 5.2.2.1.4)
• Safety Training
• Changes to Policies&SOPs
• Technical employees that carry out testing must also successfully
complete on-going demonstration of capability(CDOC) for all
test methods performed on an annual basis. (See 5.2.2.1.5)
Personnel are expected to maintain their DOCs current and
complete and to complete training assignments in a timely manner.
5.2.2.1.3 Ethics and Data Integrity Training
Data integrity training is provided to all new personnel and refresher
data integrity training is provided to all employees on an annual basis.
Personnel are required to acknowledge they understand that any
infractions of the laboratory data integrity procedures will result in a
detailed investigation that could lead to very serious consequences
including immediate termination, debarment, or civil/criminal
prosecution.
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Completion of data integrity training is documented by employee
signature to provide evidence that the employee has participated in
training on this topic and understand their obligations related to data
integrity.
The following topics and activities are covered:
• Policy for honesty and full disclosure in all analytical reporting;
• Prohibited Practices;
• How and when to report data integrity issues;
• Record keeping. The training emphasizes the importance of
proper written documentation on the part of the analyst with
respect to those cases where analytical data may be useful, but
are in one sense or another partially nonconforming;
1 • Training Program, including discussion regarding all data
integrity procedures;
• Data integrity training documentation;
• In-depth procedures for data monitoring;and
• Specific examples of breaches of ethical behavior such as
improper data manipulations, adjustments of instrument time
clocks, and inappropriate changes in concentrations of
standards.
All PAS personnel, including contract and temporary, are required
to sign an"Attestation of Ethics and Confidentiality"at the time of
employment and during annual refresher training. This document
clearly identifies inappropriate and questionable behavior.
Violations of this document result in serious consequences,
including prosecution and termination,if necessary.
Also see SOP-ENV-COR-POL-0004 Ethics Policy (most recent
revision or replacement) for more information.
.2.2.1.4 Management System Document Training
The Quality Manual and ENV manuals, policies, and SOPs are the
documents used by regulatory bodies and PAS customers to verify
the laboratory's capability, competency, and compliance with their
requirements and expectations.
In addition to on-the-job training, employees must have a signed
Read and Acknowledgement Statement (R&A) on record for the
laboratory quality manual, and the policies and SOPs relating to
his/her job responsibilities. This statement, whether signed by the
employee electronically or by wet signature, confirms that the
employee has received, read, and understands the content of the
document, that the employee agrees to follow the document when
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carrying out their work tasks; and the employee understands that
unauthorized change to procedures in an SOP is not allowed except
in accordance with the SOP departure policy(See 4. 9.1).
See SOP ENV-CORQ-0016 Standard Operating Procedures and Standard
Work Instructions (most recent revision or replacement) for more
information.
5.22.1.5 Demonstration of Capability(DOC)
Demonstration of capability is based on the employee's capability to
achieve acceptable precision and accuracy for each analyte reported
by the laboratory for the test method using the laboratory's test
method SOP.
Technical employees must complete an initial demonstration of
capability (IDOC) prior to independent work on client samples
analyzed by the test methods they perform.After successful IDOC,
the employee must demonstrate continued proficiency(CDOC) for
the test method on an annual basis. If more than a year has passed
since the employee last performed the method;then capability must
be re-established with an IDOC.
Records of IDOC and CDOC are kept in the employee's training
file.
5.2.2.2 Effectiveness of Training
The results of the performance measures used to identify training needs are the same
measures used by the laboratory to measure effectiveness of the training program.
Improvement in key performance measures suggest the training program is successful
(See 5.2.2.1).
Effectiveness of individual employee training is measured by their demonstrated
ability to comprehend the training material and apply knowledge and skills gained to
their job task. Measurements include but are not limited to:
• Testing of the employee's knowledge of the quality management system,policies,
and technical and administrative procedures through various mechanisms, such
as quizzes,observation,and interviews.
• Demonstrated ability to convey information correctly and factuallyin written and
verbal communication to internal and external parties.
• Demonstrated ability to carry out tasks in accordance with SOPs and other work
instructions.
• Demonstrated ability to make sound decisions based on guidance and
information available.
• Demonstrated initiative to seek help or guidance when the employee is unsure of
how to proceed.
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5.2.2.3 Supplemental Learning
Supplemental learning objectives are established for newly hired personnel to aid in
their development of administrative and technical skills.These learning objectives and
materials, referred to as Learning Plans (LP), are created and maintained by ENV's
3P program and managed by the employee's direct supervisor.
In addition to LPs, PAS maintains a wide variety of supplemental learning courses
that are made available to all PAS employees for professional development. These
learning materials,maintained by PAS's corporate training personnel,are accessed via
the company's employee portal, PaceConnect. The learning may be self-initiated
based on an employee's interest or may be assigned to the employee at the discretion
of management as professional development as part of an employee's annual
goals. Supplemental learning courses and learning plan activities are not prerequisites
for competency (Section 5.2.1.1) and are not part of the required QMS training
specified in Section 5.2.2.1.
5.2.3 Personnel Supervision
Every employee is assigned a direct supervisor,however named,who is responsible for their
supervision. Supervision is the set of activities carried out by the supervisor to oversee the
progress and productivity of the employees that report to them.
General supervisory responsibilities may include but are not limited to:
■ Hiring Employees
■ Training Employees
■ Performance Management
■ Development, oversight,and execution of personnel training plans
■ Monitoring personnel work product to assure the work is carried out in accordance with
this quality manual, policies, SOPs, and other documents that support the quality
management system.
5.2.4 Job Descriptions
Job Descriptions that define the required education,qualifications, experience,skills,roles and
responsibilities, and reporting relationships for each PAS position are established by top
management and kept by corporate HR. PAS laboratories use these job descriptions as the
source of positions and job titles for the laboratory. The job descriptions apply to employees
who are directly employed by PAS,part-time,temporary,technical and administrative and by
those that are under contract with PAS through other means.
The job descriptions include the education,expertise,and experience required for the position
and the responsibilities and duties,including any supervisory or managerial duties assigned to
the position.
5.2.5 Authorization of Technical Personnel
Laboratory management authorizes technical personnel to perform the technical aspects of
their position after it has been verified that the employee meets the qualifications for the
position,has successfully completed required training(Section 5.2.2.1),and the employee has
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completed initial demonstrated capability (Section 5.2.2.1.5). After initial authorization,
technical personnel are expected to maintain a current and complete training record,
demonstrate on-going capability at least annually for each test method performed,and produce
reliable results through accurate analysis of certified reference materials, proficiency testing
samples,and/or routine quality control samples in order to remain authorized to continue to
perform their duties.
Records to support authorization including, education, experience, training, and other
evaluations are kept by the laboratory.
5.3 Accommodations and Facilities
5.3.1 Facilities
The laboratory is designed to support the correct performance of procedures and to not
adversely affect measurement integrity or safety. Access to the laboratory is controlled by
various measures,such as card access,locked doors,main entry. Visitors to the laboratory are
required to sign-in and to be escorted by laboratory personnel during their visit. A visitor is
any person that is not an employee of the laboratory.
5.3.2 Environmental Conditions
The laboratory is equipped with energy sources,lighting,heating,and ventilation necessary to
facilitate proper performance of calibrations and tests. The laboratory ensures that
housekeeping, electromagnetic interference, humidity, line voltage, temperature, sound and
vibration levels are appropriately controlled to ensure the integrity of specific measurement
results and to prevent adverse effects on accuracy or increases in the uncertainty of each
measurement.
Environmental conditions are monitored,controlled,and recorded as required by the relevant
specifications,methods,and procedures.Laboratory operations are stopped if it is discovered
that the laboratory's environmental conditions jeopardize the analytical results.
5.3.3 Separation of Incompatible Activities
The layout and infrastructure of each work area including air handling systems,power supplies,
and gas supplies of each laboratory work area is specifically designed for the type of analytical
activity performed. Effective separation between incompatible work activities is maintained.
For example, sample storage,preparation,and chemical handling for volatile organic analysis
(VOA) is kept separate from semi-volatile organic (SVOA).
The laboratory separates samples known or suspected to contain high concentration of
analytes from other samples to avoid the possibility for cross-contamination. If contamination
is found, the source of contamination is investigated and resolved in accordance with
laboratory SOPs.
5.3.4 Laboratory Security
Security is maintained by controlled access to the building and by surveillance of work areas
by authorized personnel. Access is controlled to each area depending on the required
personnel,the sensitivity of the operations performed,and possible safety concerns.The main
entrance is kept unlocked during normal business hours for visitors and is continuously
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monitored by laboratory staff. All visitors must sign a visitor's log,and a staff member must
accompany them during the duration of their stay.
5.3.5 Good Housekeeping
The laboratory ensures good housekeeping practices in work areas to maintain a standard of
cleanliness necessary for analytical integrity and personnel health and safety. Minimally,these
measures include regular cleaning of the work area. Where necessary, areas are periodically
monitored to detect and resolve specific contamination and/or possible safety issues.
5.4 Test Methods
5.4.1 General Requirements
The laboratory uses test methods and procedures that are appropriate for the scope of
analytical services the laboratory offers.
Instructions on the use and operation of equipment and sample handling, preparation, and
analysis of samples are provided in SOPs. The instructions in SOPs may be supplemented
with other documents including but not limited to,standard work instructions (SWI),manuals,
guides,project documents and reference documents.
These documents are managed using the procedures described in SOP ENV-SOP-CORQ-
0015 Document Management and Control(most recent revision or replacement) and SOP ENV-
SOP-CORQ-0016 Standard Operating Procedures and Standard 'Work Instructions (most recent
revision or replacement).
5.4.2 Method Selection
The test methods and protocols used by the laboratory are selected to meet the needs of the
customer, are appropriate for the item tested and intended use of the data, and to conform
with regulatory requirements when regulatory requirements apply.
In general,the test methods offered are industry accepted methods published by international,
regional, or national standards. The laboratory bases its procedure on the latest approved
edition of a method unless it is not appropriate or possible to do so, or unless regulatory
requirements specify otherwise.
The laboratory confirms that it can perform the test method and achieve desired outcome
before analyzing samples (see section 5.4.5). If there is a change in the published analytical
method,then the confirmation is repeated.
When a customer does not specify the test method(s) to be used,the laboratory may suggest
test methods that are appropriate for the intended use of the data and the type of samples to
be tested. The laboratory will also inform customers when test methods requested are
considered inappropriate for their purpose and/or out of date. This discourse takes place
during review of analytical service requests (See Section 4.4).
5.4.3 Laboratory Developed Methods
A laboratory developed method is a method developed from scratch (no published source
method), a procedure that modifies the chemistry from the source method, or a procedure
that exceeds the scope and application of the source method.
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Laboratory developed methods must be validated prior to use (see section 5.4.5) and the
procedure documented in a test method SOP.
The requirements for non-standard methods(Section 5.4.4)also apply to laboratory developed
methods. 1
5.4.4 Non-standard Methods
A non-standard method is a method that is not published or approved for use by conventional
industry standards for the intended purpose of the data. Non-standard methods must be
validated prior to use (see section 5.4.5) and the procedure developed and documented in a
test method SOP.
At a minimum,the following information must be included in the procedure:
• Title/Identification of Method;
• Scope and Application;
• Description of the type of item to be analyzed;
• Parameters or quantities and ranges to be determined;
• Apparatus and equipment,including technical performance requirements;
• Reference standards and reference materials required;
• Environmental conditions required and any stabilization period needed;and
• Description of the procedure,including:
o Affixing identification marks, handling, transporting, storing and preparing of
items;
o Checks to be made before the work is started;
o Verifying equipment function and,where required, calibrating and/or adjusting
the equipment before each use;
o Method of recording the observations and results;
o Any safety measures to be observed;
o Criteria and/or requirements for approval/rejection;
o Data to be recorded and method of analysis and presentation;and
o Uncertainty or procedure for estimating uncertainty.
Use of a non-standard method for testing must be agreed upon with the customer. The
agreement, which is retained by the laboratory in the project record, must include the
specifications of the client's requirements, the purpose of testing,and their authorization for
use of the non-standard method.
5.4.5 Method Validation
5.4.5.1 Validation Description
Validation is the process of conformation and the provision of objective evidence
that the stated requirements for a specific method/procedure are fulfilled.
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The laboratory's requirements and procedures for method validation are outlined in
SOP ENV-SOP-CORQ-0011 Method Validation and Instrument Verification(most recent
revision or replacement).
5.4.5.2 Validation Summary
All test methods offered by the laboratory are validated before use to confirm the
procedure works and the data and results achieved meet the goals for the method and
repeated when there are major changes to the laboratory procedure.
Results of validation are retained are kept in accordance with method validation SOP
and the corporate policy ENV-CORQ-POL-0013 Record Management (most recent
revision or replacement).
5.4.5.3 Validation of Customer Need
The validation process includes review of accuracy, precision, sensitivity, selectivity,
linearity, repeatability, reproducibility, robustness, and cross-sensitivity of the
procedure against general customer needs to ensure the laboratory's procedure will
meet those needs.
The following subsections highlight some of these concepts:
5.4.5.3.1 Accuracy
Accuracy is the degree to which the result of a measurement,
calculation, or specification conforms to the correct value or a
standard. When the result recovers within a range from the known
value (control limit); the result generated using the laboratory's test
method SOP is considered accurate.
5.4.5.3.2 Precision
Precision refers to the closeness of two or more measurements to
each other. It is generally measured by calculating the relative
percent difference (RPD) or relative standard deviation(RSD) from
results of separate analysis of the same sample. Precision provides
information about repeatability, reproducibility, and robustness of
the laboratory's procedure.
5.4.5.3.3 Limits of Detection(LOD) (Chemistry)
The LOD is the minimum result which can be reliably discriminated
• from a blank with a predetermined confidence level. The LOD
establishes the limit of method sensitivity and is also known as the
detection limit(DL) or the method detection limit(MDL).
Values below the LOD cannot be reliably measured and are not
reported by the laboratory unless otherwise specified by regulatory
program or test method.
The LOD is established during method validation and after major
changes to the analytical system or procedure that affect sensitivity
are made.
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5.4.5.3.4 Limits of Quantitation (LOQ) and Reporting Limit (RL)
The LOQ is the minimum level, concentration, or quantity of a
target analyte that can be reported with a specified degree of
confidence. The LOQ is established at the same time as the LOD.
The LLOQ is the value of the lowest calibration standard included
in the calibration curve. The LLOQ establishes the lower limit of
quantitation.
The LOQ and LLOQ represent quantitative sensitivity of the test
method.
■ The LOQ must always be equal to or greater than the LLOQ
and the LLOQ must always be greater than the LOD.
• Any reported value (detect or non-detect) less than the LLOQ
is a qualitative value.
The RL is the value to which the presence of a target analyte is
reported as detected or not detected. The RL is project-defined
based on project data quality objectives (DQO). In the absence of
project specific requirements, the RL is usually set to the LOQ or
the LLOQ.
The laboratory's procedures for LOD/LOQ determination is
detailed in laboratory SOP ENV-SOP-GBAY-0106,Determination of
the LOD and LOQ.
The local SOP is based on guidance provided by corporate quality
and must comply with 40CFR 136 Appendix B and the TNI
Standard.
5.4.5.3.5 Linearity
Linearity is a mathematical concept applied to calibration models
that employ multiple points to establish a calibration range used for
quantitative analysis. Linearity is measured differently based on the
calibration model. In general, if linearity is demonstrated then the
slope of the response of standards are sufficiently close to one
another. The accuracy of the linear regression and non-linear curves
is verified by checking percent error or relative standard error(RSE),
which is the process of refitting calibration data back to the model
to determine if the results are accurate. For linear curves that use
average calibration or response factor, error is measured by relative
standard difference (RSD).
Linearity also establishes the range of quantitation for the test
method used which directly impacts the sensitivity of the test
method and uncertainty in measurement results. As previously
noted, the LLOQ establishes the lower limit of quantitation.
Similarly, the upper range of linearity establishes the upper limit of
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quantitation. In general,results outside of this range are considered
qualitative values. However, some inorganic methods allow for
extension of the linear range above the upper limit of quantitation
when accuracy at this value is verified.
Linearity can also be used to establish repeatability, reproducibility,
and robustness of the laboratory's test method. When linearity is
demonstrated using a specific calibration model during method
validation, then use of this same calibration model to achieve
linearity on a day to day basis confirms the laboratory's method is
repeatable,reproducible,and robust.
5.4.5.3.6 Demonstration of Capability(DOC)
The DOC performed during method validation confirms that the
procedure demonstrated acceptable precision and accuracy. The
procedure used for DOC for method validation is the same as
described in section 5.2.2.1.5 for demonstration of analyst capability.
5.4.6 Measurement Uncertainty
The laboratory provides an estimate of uncertainty in testing measurements when required or
on client request. In general, the uncertainty of the test method is reflected in the control
limits used to evaluate QC performance. (See 5.9.1.1.9). ISO/IEC supports this concept with
language that reads when a well-recognized test method specifies limits to the values of the
major source of uncertainty of measurement and specifies the form of presentation of
calculated results, the laboratory has satisfied the requirements on analytical uncertainty by
following the test method and reporting instructions.
When measurement uncertainty cannot be satisfied through control limits,the laboratory will
provide a reasonable estimation of uncertainty. A reasonable estimation is based on
knowledge of method performance and previous experience. When estimating the analytical
uncertainty, all uncertainty components which are of importance in the given situation are
taken into account.
5.4.7 Control of Data
The laboratory has policies and processes in place to assure that reported data is free from
calculation and transcription errors,that quality control is reviewed and evaluated before data
is reported,and to address manual calculation and integration.
5.4.7.1 Calculations,Data Transfer, Reduction and Review
Whenever possible, calculations, transfer of data, and data reduction are performed
using validated software programs (See 5.4.7.2).
If manual calculations are performed, the results of these calculations are verified
during the data review process outlined in section 5.9.3.
5.4.7.11 Manual Integration
The laboratory's policy and procedures for manual integration are
provided in corporate SOP ENV-SOP-CORQ-0006 Manual
Integration (most recent revision or replacement).
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This SOP includes the conditions under which manual integration is
allowed and the requirements for documentation.
Required documentation of manual integration includes:
■ complete audit trail to permit reconstruction of before and after
results;
■ identification of the analyst that performed the integration and
the reason the integration was performed;and
• identification of the individual(s) that reviewed the integration
and verified the integration was done and documented in
compliance with the SOP.
5.4.7.2 Use of Computers and Automated Acquisition
Whenever possible the laboratory uses software and automation for the acquisition,
processing,recording,reporting,storage, and/or retrieval of data.
Software applications developed by PAS are validated by corporate IT for adequacy
before release for general use. Commercial off the shelf software is considered
sufficiently validated when the laboratory follows the manufacturer or vendor's
manual for set-up and use. Records of validation are kept by the corporate
information technology (IT) group or by the local laboratory, whichever group
performed the validation.
The laboratory's process for the protection of data stored in electronic systems
include:
• Individual user names and passwords for Laboratory Information Management
Systems (LIMS) and auxiliary systems used to store or process data.
• Employee Training in Computer Security Awareness
• Validation of spreadsheets used for calculations to verify formulas and logic yield
correct results and protection of these cells to prevent unauthorized change.
• Operating system and file access safeguards
• Protection from Computer Viruses
• Regular system backup;and testing of retrieved data
The laboratory's process for software development and testing process includes:
• Verification the software application works as expected and is adequate for use
and fulfills compliance requirements,such as the need to record date/time of data
generation.
• Change control to assure requests for changes are reviewed and approved by
management before the change is made.
• Communication channels to assure all staff are aware of changes made.
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■ Version Control and maintenance of historical records.
These procedures are detailed in laboratory SOPs ENV-SOP-CORQ-0015 Document
Management and Control.
5.5 Equipment
5.5.1 Availability of Equipment
The laboratory is furnished with all equipment and instrumentation necessary to correctly
perform the tests offered in compliance with the specifications of the test method and to
achieve the accuracy and sensitivity required.
5.5.2 Calibration
Equipment and instrumentation are checked prior to use to verify it performs within tolerance
for its intended application.
Laboratory management is made aware of the status of equipment and instrumentation and
any needs for either on a daily basis. This information is obtained during laboratory
walkthroughs (LDM) that are conducted as part of the laboratory's lean program.
5.5.2.1 Support Equipment
The laboratory confirms support equipment is in proper working order and meets the
specifications for general laboratory use prior to placement in service with
intermediate checks thereafter. Equipment that does not meet specifications is
removed from service until repaired or replaced. Records of repair and maintenance
activities are maintained.
Procedures used to carry out and record these checks are outlined laboratory in SOP
ENV-SOP-GBAY-0115 Support Equipment.
5.5.2.2 Analytical Instruments
Analytical instruments are checked prior to placement in service in accordance with
SOP ENV-SOP-CORQ-0011 Method Validation and Instrument Verification(most recent
revision or replacement). After the initial service date,the calibration of instruments
and verification calibration is performed in accordance with local test method SOPs.
The calibration procedures in the test method SOPs comply with the requirements
for acceptable calibration practices outlined in corporate policy ENV-POL-CORQ-
0005 Acceptable Calibration Practices(most recent revision or replacement),the reference
methods,and any applicable regulatory or program requirements.
5.5.3 Equipment Use and Operation
Equipment is operated and maintained by laboratory personnel that are trained on the test
method SOP. Up-to-date instructions and procedures for the use and maintenance of
analytical equipment are included in SOPs and/or supplemental documents such as standard
work instructions (SWI) or instrument manuals which are made readily accessible in the work
area to all laboratory personnel.
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5.5.4 Equipment Identification
The laboratory uniquely identifies equipment by serial number or any other unique ID system,
when practical. The identifier is included in the equipment list maintained by the quality
department.
5.5.5 Equipment Lists and Records
5.5.5.1 Equipment List
The laboratory maintains a master list of equipment that includes information about
the equipment including a description, manufacturer, serial number, date placed in
service, condition when received,identity,and the current location in the laboratory.
The date of purchase is tracked by the procurement record. The equipment list(s) for
each location covered by this manual is provided in Appendix E.
5.5.5.2 Equipment Records
In addition to the equipment list,the laboratory maintains records of equipment that
include:
• Verification that equipment conforms with specifications.
• Calibration records including dates, results, acceptance criteria, and next
calibration dates.
• Maintenance plan and records
• Records of damage,malfunction,or repair
The laboratory follows an equipment maintenance program designed to optimize
performance and to prevent instrument failure which is described in laboratory SOP
ENV-SOP-GBAY-0098 Preventative, Routine, or Non-routine Maintenance (most recent
revision or replacement) or in individual test method SOPs.
The maintenance program includes routine maintenance activities which are
performed as recommended by the manufacturer at the frequency recommended and
non-routine maintenance, which is performed to resolve a specific problem such as
degradation of peak resolution, shift in calibration relationship,loss of sensitivity, or
repeat failure of instrument performance checks and quality control samples.
Maintenance is performed by laboratory personnel or by outside service providers.
All maintenance activities performed by laboratory personnel are recorded by the
individual(s) that performed the activity at the time the maintenance was performed
in an instrument maintenance log.
The maintenance record minimally includes the date of maintenance, the initials of
the person(s) performing maintenance, a description of the activity performed,why
(when the maintenance is non-routine), and the return to analytical control. When
maintenance is performed by an external vendor, the laboratory staples the service
record into hardcopy maintenance logs or scans the record for easy retrieval. The
laboratory provides unrestricted access to instrument maintenance logs in order to
promote good instrument maintenance and recordkeeping practices.
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If an instrument must be moved, the laboratory will use safe practices for handling
and transport to minimize damage and contamination.
5.5.6 Out of Service Protocol
Equipment that has been subjected to overloading, mishandling, gives suspect results, has
been shown to be defective,or is performing outside of specified limits is taken out of service
and either removed from the work area or labeled to prevent accidental use until it has been
repaired and verified to perform correctly.
When analytical equipment is taken out of service,the laboratory examines the potential effect
it may have had on previous analytical results to identify any non-conforming work. (See
section 4.9).
5.5.7 Calibration Status
The laboratory labels support equipment to indicate calibration status, whenever practicable
or otherwise maintains the calibration status in a visible location in the work area. These
procedures are described in laboratory SOP ENV-SOP-GBAY-0115 Support Equipment(most
recent revision or .re lacement
P )
The calibration status of analytical instruments is documented in the analytical record.Analysts
verify on-going acceptability of calibration status prior to use and with instrument
performance check standards. These procedures are described in test method SOPs.
5.5.8 Returned Equipment Checks
When equipment or an instrument is sent out of the laboratory for service, the laboratory
ensures that the function and calibration status of the equipment is checked and shown to be
satisfactory before the equipment is returned to service.These procedures are outlined in SOP
ENV-SOP-CORQ-0011 Method Validation and Instrument Verification (most recent revision or
replacement).
5.5.9 Intermediate Equipment Checks
The laboratory performs intermediate checks on equipment to verify the on-going calibration
status. For example, most test methods require some form of continuing calibration
verification check and these procedures are included in the test method SOP. Periodic checks
of support equipment are also performed;see laboratory SOP ENV-SOP-GBAY-0115 Support
Equipment(most recent revision or replacement) for more information.
5.5.10 Safeguarding Equipment Integrity
The laboratory safeguards equipment integrity using a variety of mechanisms that include but
are not limited to:
• Adherence to manufacturer's specification for instrument use so that settings do not
exceed manufacturer's recommendation or stress the performance of the equipment.
• Established maintenance programs.
• Transparent maintenance records and unrestricted access to maintenance logs.
• Validation and approval of software before use.
• Audits to confirm instrument settings are consistent with SOPs.
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■ On-the-job training for safe and proper use of laboratory equipment.
5.6 Measurement Traceability
5.6.1 General
Measurement traceability refers to a property of a measurement result whereby the result can
be related to a reference through an unbroken chain of calibration, each contributing to the
measurement uncertainty. Traceability requires an established calibration hierarchy of
equipment (instruments) used during testing including equipment used for subsidiary
measurements. The laboratory assures this equipment is calibrated prior to being put into
service and that the reference standard and materials used for calibration are traceable to the
international standard of units (SI) or national measurement standard.
When strict traceability to SI units cannot be made,the laboratory establishes traceability with
the use of reference standards and equipment obtained from competent suppliers that provide
calibration certificates and/or certificates of analysis (COA).
5.6.2 Equipment Correction Factors
When correction factors are used to adjust results the laboratory will assure that results in
computer software are also updated. For example,if the direct instrument or reading output
must be corrected based on preparation factor or concentration factors, laboratory
management will assure the corrected result is also updated in the software.
5.6.3 Specific Requirements
5.6.3.1 Requirements for Calibration Laboratories
The laboratory does not offer calibration services to customers.
5.6.3.2 Requirements for Testing Laboratories
The laboratory has procedures in place to verify equipment is calibrated prior to being
put into service (See 5.5.2) and ensures the reference standard and materials used for
calibration are traceable to the international standard of units (SI) or national
measurement standard. When strict traceability to SI units cannot be made, the
laboratory establishes traceability with the use of reference standards and equipment
obtained from competent suppliers that provide calibration certificates and/or
certificates of analysis (COA).
5.6.4 Reference Standards and Reference Materials
5.6.4.1 Reference Standards
The laboratory uses reference standards of measurement to verify adequacy of
working weights and thermometers. The working weight is the weight(s) used for
daily balance calibration checks and the working thermometers are used for
temperature measurements on a daily basis.
Intermediate checks of the working reference measurement standards are performed
to verify adequacy between calibration from an external calibration laboratory. The
measurements from working weights and thermometers are compared to
measurements taken by the reference standard which is traceable to SI or a national
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standard. The reference weights and thermometers are used solely for verification
purposes unless the laboratory can prove that daily use does not adversely affect
performance of the reference standard.
The laboratory performs intermediate checks of the working weights at least annually.
Working thermometers (glass and digital) are checked against the reference
thermometer prior to placement in service to establish a correction factor and then
rechecked annually(glass) or quarterly(digital) thereafter.
The calibration of liquid in glass reference thermometers is verified every 5 years and
the calibration of digital reference thermometers is verified annually by an ISO/IEC
17025 accredited calibration laboratory or service provider that provides traceability
to a national standard.
The calibration of the reference weight(s) is verified every 5 years by an ISO/IEC
17025 accredited calibration laboratory.
If criteria for the intermediate checks or recertification is not acceptable, the impact
on previously reported results is evaluated using the process for evaluation of
nonconforming work(See 4.9).
See laboratory SOP ENV-SOP-GBAY-0115 SupportEquipment(most recent revision
or replacement)for more information about this process.
5.6.4.2 Reference Materials
The laboratory purchases chemical reference materials (also known as stock
standards) from vendors that are accredited to ISO 17034 or Guide 34. Purchased
reference materials must be received with a Certificate of Analysis (COA) where
available. If a reference material cannot be purchased with a COA,it must be verified
by analysis and comparison to a certified reference material and/or there must be a
demonstration of capability for characterization. COA are reviewed for adequacy and
retained by the laboratory for future reference.
All prepared standards, reference materials, and reagents are verified to meet the
requirements of the test method through routine analyses of quality control samples.
The laboratory procedure for traceability and use of these materials is provided in
laboratory SOP ENV-SOP-GBAY-0145 Laboratory Supply Procedures (most recent
revision or replacement.
This SOP includes each of the following requirements:
• Procedures for documentation of receipt and tracking. The record of entry
includes name of the material,the lot number,receipt date,and expiration date.
• Storage conditions and requirements. Reference materials must be stored
separately from samples, extracts,and digestates.
• Requirements to assure that preparations of intermediate or working solutions
are recorded and assigned a unique identification number for tracking. Records
of preparation include the lot number of the stock standard(s) used,the type and
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lot number of the solvent, the formulation, date, expiration date, and the
preparer's initials. The lot number of the working standards is recorded in the
analytical record to provide traceability to the standard preparation record. The
preparation record provides traceability to the COA,which is traceable to SI or
the national measurement standard.
■ A requirement that the expiration dates of prepared standards may not exceed
the expiration date of the parent standard. Standards, reference materials, and
reagents are not used after their expiration dates unless it is not possible to
procure a new standard and the reliability of the expired material is verified and
documented by the laboratory using a procedure approved by corporate quality
personnel. Otherwise, the expired material is promptly removed from the work
area or clearly labeled as acceptable for qualitative/troubleshooting purposes
only.
■ The second source materials used for verification of instrument calibration are
obtained from a different manufacturer or may be a different lot from the same
manufacturer.
• Procedures to check reference materials for degradation and replacement of
material if degradation or evaporation is suspected.
• Procedures for labeling. At a minimum the container must identify the material,
the ID of the material and the expiration date. Original containers should also
be labeled with date opened.
5.6.4.3 Intermediate Checks
Checks to confirm the calibration status of standards and materials are described in
laboratory SOPs. These checks include use of second source standards and reference
materials reserved only for the purpose of calibration checks.
5.6.4.4 Transport and Storage
The laboratory handles and transports reference standards and materials in a manner
that protects the integrity of the materials.Reference standard and material integrity
is protected by separation from incompatible materials and/or minimizing exposure
to degrading environments or materials. Standards and reference materials are stored
separately from samples, extracts, and digestates. All standards are stored according
to the manufacturer's recommended conditions. Temperatures colder than the
manufacturer's recommendation are acceptable if it does not compromise the
integrity of the material (e.g.remains in liquid state and does not freeze solid).In the
event a standard is made from more than a single source with different storage
conditions, the standard will be stored according to the conditions specified in the
analytical method.
See the applicable analytical SOPs for specific reference material storage and transport
protocols.
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5.7 Sampling
Sampling refers to the field collection of samples and to subsamples taken by the laboratory for
analysis from the field collected sample.
Subsampling procedures are included in each test method SOP or a stand-alone SOP to assure the
aliquot used for testing is representative of the field collected sample.
The requirements in the following subsections apply when field sampling is performed by the
laboratory.
5.7.1 Sampling Plans and SOPs
When the laboratory performs field collection of samples, sampling is carried out in
accordance with a written sample plan prepared by the customer or by the laboratory and by
relevant sampling SOPs. These documents are made readily accessible at the sampling
location. Sampling plans and SOPs are,whenever reasonable,based on appropriate governing
methods and address the factors to be controlled to ensure the validity of the analytical results.
5.7.2 Customer Requested Deviations
When the customer requires deviations, additions, or exclusions from the documented
laboratory sampling plan and/or procedure,the laboratory records the client's change request
in detail with the sampling record, communicates the change to sampling personnel, and
includes this information in the final test report.
5.7.3 Recordkeeping
The laboratory assures the sampling record includes the sampling procedure used, any
deviations from the procedure,the date and time of sampling,the identification of the sampler,
environmental conditions (if relevant),and the sampling location.
5.8 Sample Management &Handling
5.8.1 Procedures
The laboratory's procedures for sample management and handling are outlined in laboratory
SOP ENV-SOP-GBAY-0006,Sample Management and Review of Analytical Requests.
The procedures in these SOPs are established to maintain the safe handling and integrity of
samples from transport, storage,to disposal and during all processing steps to maintain client
confidentiality,and to protect the interests of PAS and its customers.
5.8.1.1 Chain of Custody
All samples received by the laboratory must be accompanied with a Chain of Custody
(COC) record. The COC provides information about the samples collected and
submitted for testing and documents the possession of samples from time of
collection to receipt by the laboratory.
The COC record must minimally include the following information:
• Client name,address,phone number;
• Project Reference;
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■ Client Sample Identification(Client ID);
• Date,Time,and Location of Sampling;
■ Sampler's Name or Initials;
• Matrix;
• Type of container,and total number collected for each sample;
• Preservatives;
• Analyses Requested;
• Mode of collection;
• Any special instructions;and
• The date and time and signature of each sample transfer from time of collection
to receipt in the laboratory. When the COC is transported inside the cooler,
independent couriers do not sign the COC, the shipping manifests and/or air
bills are the records of possession during transport. The shipping manifest must
be retained as part of the COC record and included in the test report when
required (See Section 5.10.3).
A complete and legible COC is required. If the laboratory observes that the COC is
incomplete or illegible,the client is contacted for resolution. The COC must be filled
out in indelible ink. Personnel correct errors by drawing a single line through the
initial entry so the entry is not obscured, entering the correct information, and
initialing,and dating the change.
5.8.1.2 Legal Chain of Custody
Legal chain of custody is a chain of custody protocol used for evidentiary or legal
purposes. The protocol is followed by the laboratory when requested by customer or
where mandated by a regulatory program.
Legal chain of custody(COC) protocol establishes an intact,continuous record of the
physical possession*, storage, and disposal of "samples" which includes sample
aliquots,and sample extracts/digestates/distillates.
Legal COC records account for all time periods associated with the samples and
identifies all individuals who physically handled individual samples.Legal COC begins
at the point established by legal authority, which is usually at the time the sample
containers are provided by the laboratory for sample collection or when sample
collection begins.
*A sample is in someone's custody if:
• It is in one's physical possession;
• It is in one's view after being in one's physical possession;
• It has been in one's physical possession and then locked or sealed so that no one
can tamper with it;and/or
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■ It is kept in a secure area,restricted to authorized personnel only.
Refer to laboratory SOP ENV-SOP-GBAY-0006, Sample Management and Review of
Analytical Requests for more information.
5.8.2 Unique Identification
Each sample is assigned a unique identification number by the laboratory (Lab ID) after the
sample has been checked and accepted by the laboratory in accordance with the laboratory's
sample acceptance policy (See 5.8.3). The Lab ID is affixed to the sample container using a
durable label.
The unique identification of samples also applies to subsamples,and prepared samples,such
as extracts,digestates, etc.
The lab ID is linked to the field ID (client ID) in the laboratory's record. Both IDs are linked
to the testing activities performed on the sample and the documentation records of the test.
Also see 5.8.4.
5.8.3 Sample Receipt Checks and Sample Acceptance Policy
The laboratory checks the condition and integrity of samples on receipt and compares the
labels on the sample containers to the COC record. Any problem or discrepancy is recorded.
If the problem impacts the suitability of the sample for analysis or if the documentation is
incomplete,the client is notified for resolution.Decisions and instructions from the client are
maintained in the project record.
5.8.3.1 Sample Receipt Checks
The following checks are performed:
■ Verification that the COC is complete and legible.
• Verification that each sample's container label includes the client sample ID,the
date and time of collection and the preservative in indelible ink.
■ The container type and preservative are appropriate for each test requested.
• Adequate volume is received for each test requested.
• Visual inspection for damage or evidence of tampering.
• Visual inspection for presence of headspace in VOA vials. (VOA = volatile
organic analysis).
• Thermal Preservation:Generally,for chemical testing methods for which thermal
preservation is required,temperature on receipt is acceptable if the measurement
is above freezing but <6°C. The requirements for thermal preservation vary
based on test method or by regulatory program. For example, for microbiology,
temperature on receipt is acceptable if the measurement is <10°C. Refer to the
laboratory's SOP for sample receipt for specific requirements. For samples that
are hand-delivered to the laboratory immediately after sample collection, there
must be evidence that the chilling process began immediately after sample
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collection and prior to delivery of the samples to the laboratory or service center,
such as arrival of the samples on ice.
• Chemical Preservation
■ Holding Time: Sample receiving personnel are trained to recognize tests where
the holding time is 48 hours or less and to expedite the log-in of these samples.
Except for tests with immediate holding times (15 minutes from time of
collection or less), when samples are received out of hold, the laboratory will
notify the client and request instruction.If the decision is made to proceed with
analysis,the final test report will include notation of this instruction.
5.8.3.2 Sample Acceptance Policy
The laboratory maintains a sample acceptance policy in accordance with regulatory
guidelines to clearly establish the circumstances in which sample receipt is accepted
or rejected.
When receipt does not meet criteria for any one of these conditions, the laboratory
must document the noncompliance, contact the customer, and either reject the
samples or fully document any decisions to proceed with testing.In accordance with
regulatory specifications, test results associated with receipt conditions that do not
meet criteria are qualified in the final test report.
All samples received must meet each of the following criteria:
• Be listed on a complete and legible COC;
• Be received in properly labeled sample containers;
• Be received in appropriate containers that identify preservative;
• The COC must include the date and time of collection for each sample;
• The COC must include the test method requested for each sample;
• Be in appropriate sample containers with clear documentation of the
preservatives used;
• Be received within holding time.Any samples received beyond the holding time
will not be processed without prior customer approval;
• Have sufficient sample volume to proceed with the analytical testing. If
insufficient sample volume is received,analysis will not proceed without customer
approval;and
• Be received within appropriate temperature ranges unless program requirements
or customer contractual obligations mandate otherwise.The cooler temperature
is recorded directly on the COC.
Samples that are delivered to the laboratory immediately after collection are
considered acceptable if there is evidence that the chilling process has been
started. For example, by the arrival of the samples on ice. If samples arrive that
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are not compliant with these temperature requirements, the customer will be
notified. The analysis will NOT proceed unless otherwise directed by the
customer. If less than 72 hours remain in the hold time for the analysis, the
analysis may be started while the customer is contacted to avoid missing the hold
time. Data associated with any deviations from the above sample acceptance
policy requirements will be appropriately qualified.
5.8.4 Sample Control and Tracking
The samples are controlled and tracked using the Laboratory Information Management
System (LIMS). The LIMS stores information about the samples and project. The process of
enteringinformation into the LIMS is called log-in and these procedures are described in
g
laboratory SOP ENV-SOP-GBAY-0006, Sample Management and Review of Analytical Requests.
After log-in, a label is generated and affixed to each sample container. Information on this
label, such as the lab ID,links the sample container to the information in LIMS.
At a minimum,the following information is entered during log-in:
• Client Name and Contact Information;
• The laboratory ID linked to the client ID;
• Date and time of sample collection;
• Date and time of sample receipt;
• Matrix;and
• Tests Requested.
5.8.5 Sample Storage,Handling, and Disposal
The laboratory procedures for sample storage,handling and disposal are detailed in laboratory
SOPs ENV-SOP-GBAY-0006, Sample Management and Review of Analytical Requests and ENV-
SOP-GBAY-0126, Waste Handling and Management(most current revision(s) or replacement(s).
5.8.5.1 Sample Storage
The samples are stored according to method and regulatory requirements as per test
method SOPs. Samples are stored away from all standards, reagents, or other
potential sources of contamination and stored in a manner that prevents cross
contamination.Volatile samples are stored separately from other samples.All sample
fractions, extracts,leachates,and other sample preparation products are stored in the
same manner as actual samples or as specified by the analytical method.
Refrigerated storage areas are maintained at 5_6°C (but not frozen) and freezer storage
areas are maintained at <-10°C, unless otherwise required per method or program.
The temperature of each storage area is checked and documented at least once for
each day of use.If the temperature falls outside the acceptable limits, then corrective
actions are taken and appropriately documented.
The laboratory is operated under controlled access protocols to ensure sample and
data integrity.Visitors must register at the front desk and be properly escorted while
on-site. Samples are taken to the appropriate storage location immediately after
sample receipt and log-in procedures are completed. All sample storage areas have
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limited access. Samples are removed from storage areas by designated personnel and
returned to the storage areas as soon as possible after the required sample quantity
has been taken.
5.8.5.2 Sample Retention and Disposal
The procedures used by the laboratory for sample retention and disposal are detailed
in laboratory SOP ENV-SOP-GBAY-0126, Waste Handling and Management.
In general,unused sample volume and prepared samples such as extracts,digestates,
distillates and leachates (samples) are retained by the laboratory for the timeframe
necessary to protect the interests of the laboratory and the customer.
Samples may be stored at ambient temperature when all analyses are complete, the
hold time is expired, the report has been delivered, and/or when allowed by the
customer or program. Samples requiring storage beyond the minimum sample
retention time due to special requests or contractual obligations may be stored at
ambient temperature unless the laboratory has a capacity and their presence does not
compromise the integrity of other samples.
After this period expires, non-hazardous samples are properly disposed of as non-
hazardous waste. The preferred method for disposition of hazardous samples is to
return the excess sample to the customer.
5.9 Assuring the Quality of Test Results
5.9.1 Quality Control(QC) Procedures
The laboratory monitors the validity and reliability of test results using quality control (QC)
samples that are prepared and analyzed concurrently with field samples in the same manner as
field samples. QC results are always associated to and reported with the field samples they
were prepared and analyzed with from the same preparation or analytical batch. See the
glossary for definition of preparation and analytical batch.
The results of QC performed during the testing process are used by the laboratory to assure
the results of analysis are consistent, comparable,accurate, and/or precise within a specified
limit. When the results are not within acceptance criteria or expectations for method
performance, correction and corrective action(s) are taken. These actions may include
retesting or reporting of data with qualification to alert the end user of the situation.
Other QC measures performed include the use of certified reference materials (see 5.6.4),
participation in interlaboratory proficiency testing(see 5.9.1.2),verification that formulae used
for reduction of data and calculation of results is accurate (see 5.9.3),on-going monitoring of
environmental conditions that could impact test results (see 5.3.2), and evaluation and
verification of method selectivity and sensitivity(see 5.4.5).
QC results are also used by the laboratory to monitor performance statistical trends over time
and to establish acceptance criteria when no method or regulatory criteria exist.(See 5.9.1.1.9)).
5.9.1.1 Essential QC
Although the general principles of QC for the testing process apply to all testing,the
QC protocol used for each test depends on the type of test performed.
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QC protocol used by the laboratory to monitor the validity of the test are specified in
test method SOPs. The SOP includes QC type, frequency, acceptance criteria,
corrective actions,and procedures for reporting of nonconforming work.
These requirements in the SOP conform to the reference method and any applicable
regulations or certification and accreditation program requirement for which results
of the test are used. When a project requires more stringent QC protocol than
specified in the SOP,project specification is followed. When the project requires less
stringent QC protocol, the project specification may be followed as an authorized
departure from the SOP when the project specifications meet the requirements in the
mandated method and any regulatory compliance requirements for which the data
will be used.
The following are examples of essential QC for Chemistry:
5.9.1.1.1 Second Source Standard (ICV/QCS)
The second source standard is a standard obtained from a different
vendor than the vendor of the standards used for calibration or it
may be from a different lot from the same vendor when there are
limited vendors that offer the material. It is a positive control used
to verify the accuracy of a new calibration relative to the purity of
the standards used for calibration. This check is referred to in test
method and quality system standards as the initial calibration
verification (ICV) or quality control sample (QCS). The second
source standard is analyzed immediately after the calibration and
before analysis of any samples. When the ICV is not within
acceptance criteria,a problem with the purity or preparation of the
standards may be indicated.
5.9.1.1.2 Continuing Calibration Verification(CCV)
CCV results are used to determine if the analytical response has
significantly changed since initial calibration. If the response of the
CCV is within criteria, the calibration is considered valid. If not,
there is a problem that requires further investigation. Actions taken
are technology and method specific.
5.9.1.1.3 Method Blank(MB) / Other Blanks
A method blank is a negative control used to assess for
contamination during the prep/analysis process. The MB consists
of a clean matrix, similar to the associated samples that is known to
be free of analytes of interest. The MB, unless otherwise specified
by the test method, is processed with and carried through all
preparation and analytical steps as the associated samples.
In general, contamination is suspected when the target analyte is
detected in the MB above the reporting limit. Some programs may
require evaluation of the MB to 1/2 the reporting limit or the
detection limit. When contamination is evident, the source is
investigated, and corrections are taken to reduce or eliminate it.
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Analytical results associated with MB that does not meet criteria are
qualified in the final test report.
Other types of blanks that serve as negative controls in the process
may include:
■ Trip Blanks (VOA)
■ Storage Blanks
■ Equipment Blanks
■ Field Blanks
• Calibration Blanks
• Cleanup Blanks
• Instrument Blanks
5. .1.1. Laboratory Control Sample (LCS)
The LCS is positive control used to measure the accuracy of process
in a blank matrix. The LCS is spiked by the laboratory with a known
amount of analyte. The spike is a standard solution that is pre-made
or prepared from a certified reference standard.Like the MB,unless
otherwise specified in the test method, the LCS is processed with
and carried through all preparation and analytical steps as the
associated samples.
When the percent recovery(%R) of the LCS is within the established
control limit, sufficient accuracy has been achieved. If not, the
source of the problem is investigated and corrected, and the
procedure may be repeated. Analytical results associated with LCS
that does not meet criteria are qualified in the final test report.
5. .1.1. Matrix Spike (MS) and Matrix Spike Duplicate (MSD)
Matrix spikes measure the effect the sample matrix has on precision
and accuracy of the determinative test method. The MS and MSD
are replicates of a client sample that is spiked with known amount of
target analyte. •
Due to the heterogeneity of matrices even of the same general matrix
type, matrix spike results mostly provide information on the effect
of the matrix to the client whose sample was used and on samples
of the same matrix from the same sampling site. Therefore, MS
should be client-specific when the impact of matrix on accuracy and
precision is a project data quality objective. When there is not a
client-specified MS for any sample in the batch, the laboratory
randomly selects a sample from the batch; the sample selected at
random is called a"batch"matrix spike.
The MS/MSD results for percent recovery and relative percent
difference are checked against control limits. Because the
performance of matrix spikes is matrix-dependent, the result of
matrix spikes is not used to determine the acceptability of the test.
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5.9.1.1.6 Sample Duplicate (SD)
A sample duplicate is a second replicate of sample that is prepared
and analyzed in the laboratory along another replicate. The SD is
used to measure precision.
The relative percent difference between replicates are evaluated
against the method or laboratory derived criteria for relative percent
difference (RPD), when this criterion is applicable. If RPD is not
met,associated test results are reported with qualification.
5.9.1.1.7 Surrogates
Surrogates are compounds that mimic the chemistry of target
analytes but are not expected to occur naturally in real world
samples. Surrogates are added to each sample and matrix QC
samples (MS, MSD, SD) at known concentration to measure the
impact of the matrix on the accuracy of method performance.
Surrogates are also added to the positive and negative control
samples (MB, LCS) to evaluate performance in a clean matrix, and
included in the calibration standards and calibration check standards.
The percent recovery of surrogates is evaluated against method-
specified limits or statistically derived in-house limits. Project-
specific limits and/or program-specific limits are used when
required. Results with surrogate recovery out of limits in samples
are reported with qualification. Samples with surrogate failures can
also be re-extracted and/or re-analyzed to confirm that the out-of-
control value was caused by the matrix of the sample and not by
some other systematic error.
5.9.1.1.8 Internal Standards
Internal Standards are compounds not expected to occur naturally
in field samples. They are added to every standard and sample at a
known concentration prior to analysis for the purpose of adjusting
the response factor used in quantifying target analytes. The
laboratory follows specific guidelines for the treatment of internal
standard recoveries and further information can be found in the
applicable laboratory SOP.
5.9.1.1.9 QC Acceptance Criteria and Control Limits
The QC acceptance criteria are specified in test method SOPs. The
criteria in the SOP are based on the requirements in the published
test method or regulatory program. When there are no established
acceptance criteria, the laboratory develops acceptance criteria in
accordance with recognized industry standards.
Some methods and programs require the laboratory to establish
control limits for LCS, MS/MSD, and surrogate evaluation using
historical data. Laboratory developed limits are referred to as "in-
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house" control limits. In-house control limits represent ± 3
Standard Deviations (99% confidence level) from the average
recovery of at least 20 data points generated using the same
preparation and analytical procedure in a similar matrix.
See laboratory SOP ENV-SOP-GBAY-0116, Control Charting and
Trend Analysis for more information about the procedures used to
establish in-house control limits.
5.9.1.2 Proficiency Testing(PT)
The laboratory participates in interlaboratory proficiency testing (PT) studies to
measure performance of the test method and to identify or solve analytical problems.
PT samples measure laboratory performance through the analysis of unknown
samples provided by an external source.
The PT samples are obtained from accredited proficiency testing providers (PTP) and
handled as field samples which means they are included in the laboratory's normal
analytical processes and do not receive extraordinary attention due to their nature.
The laboratory does not share PT samples with other laboratories, does not
communicate with other laboratories regarding current PT sample results during the
duration of the study, and does not attempt to obtain the assigned value of any PT
sample from the PT provider.
The laboratory investigates and implements corrective action whenever PT results are
scored unacceptable by the PT provider.
The frequency of PT participation is based on the certification and accreditation
requirements held by the laboratory.
5.9.2 QC Corrective Action
When the results of QC are not within acceptance criteria or expectations for method
performance, correction and corrective action(s) are taken per the specifications in the test
method SOP. These actions may include retesting or reporting of data with qualification to
alert the end user of the situation.
5.9.3 Data Review
The laboratory uses a tiered system for data review. The tiered process provides sequential
checks to verify data transfer is complete; manual calculations, if performed, are correct,
manual integrations are appropriate and documented, calibration and QC requirements are
met,appropriate corrective action was taken when required,test results are properly qualified,
process and test method SOPs were followed,project specific requirements were met,when
applicable,and the test report is complete.
The sequential process includes three tiers referred to as primary review, secondary review,
and administrative/completeness review.
Detailed procedures for the data review process are described in laboratory SOP ENV-SOP-
GBAY-0120,Data Review and Final ReportProcess. The general expectations for the tiered review
process are described in the following sections:
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5.9.3.1 Primary Review
Primary review is performed by the individual that performed the task. All laboratory
personnel are responsible for review of their work product to assure it is complete,
accurate,documented,and consistent with policy and SOPs.
Checks performed during primary review include but are not limited to:
■ Verification that data transfer and acquisition is complete
• Manual calculations,if performed,are documented and accurate
• Manual integrations,if performed,are documented and comply with SOP ENV-
SOP-CORQ-006 Manual Integration(most recent revision or replacement)
■ Calibration and QC criteria were met, and/or proper correction and corrective
actions were taken, and data and test results associated with QC and criteria
exceptions are properly qualified
• Work is consistent with SOPs and any other relevant instructional document such
as SWI,program requirements,or project QAPP.
5.9.3.2 Secondary Review
Secondary review is performed by a qualified peer or supervisor. Secondary review is
essentially a repeat of the checks performed during primary review by another person.
In addition to the checks of primary review, secondary review includes
chromatography review to check the accuracy of quantitative analyte identification.
5.9.3.3 Completeness Review
Completeness review is an administrative review performed prior to release of the test
report to the customer. Completeness review verifies that the final test report is
complete and meets project specification. This review also assures that information
necessary for the client's interpretation of results are explained in the case narrative
or footnoted in the test report.
5.9.3.4 Data Audits
In addition to the 3-tier data review process, test reports may be audited by local
quality personnel to verify compliance with SOPs and to check for data integrity,
technical accuracy,and regulatory compliance. These audits are not usually done prior
to issuance of the test report to the customer. The reports chosen for the data audits
are selected at random.
If any problems with the data or test results are found during the data audit,the impact
of the nonconforming work is evaluated using the process described in Section 4.9.
Also see Section 4.14 for internal audits.
5.9.4 Calibration Certificates
The laboratory does not perform calibration activities for its customers and calibration
certificates are not offered or issued.
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5.9.5 Opinions and Interpretations
The laboratory provides objective data and information to its customers of sufficient detail
for their interpretation and decision making. Objective data and information are based solely
on fact and does not attempt to explain the meaning(interpret) or offer a view or judgement
(opinion). Sometimes the customer may request the laboratory provide opinion or
interpretation to assist them with their decisions about the data.
When opinions and interpretations are included in the test report, the laboratory will
document the basis upon which the opinions and interpretations have been made and clearly
identify this content as opinion or interpretation in the test report.
Examples of opinion and interpretation include but are not limited to:
■ The laboratory's viewpoint on how a nonconformance impacts the quality of the data or
usability of results.
■ The laboratory's judgment of fulfillment of contractual requirements.
• Recommendations for how the customer should use the test results and information.
• Suggestions or guidance to the customer for improvement.
When opinions or interpretations are verbally discussed with the customer, the content of
these conversations is summarized by the laboratory and kept in the project record.
5.9.6 Subcontractor Reports
When analytical work has been subcontracted to an organization external to PAS, the test
report from the subcontractor is included in its entirety as an amendment to the final test
report.
Test results performed by multiple locations within the PAS network may be merged into a
single test report. The test report issued clearly identifies the location and address of each
network location that performed testing,and which tests they performed. (See 5.10.2)
5.9.7 Electronic Transmission of Results
When test results and/or reports are submitted to the customer through electronic
transmission, the procedures established in this manual for confidentiality and protection of
data apply.
5.9.8 Format of Test Reports
The test formats offered by the laboratory are designed to accommodate each type of analytical
test method carried out by the laboratory and to minimize the possibility of misunderstanding
or misuse of analytical results. The format of electronic data deliverables (EDD) follow the
specifications for the EDD.
5.9.9 Amendments to Test Reports
Test reports that are revised or amended by the laboratory after date of release of the original
final test report to the customer are issued as a new test report that is clearly identified as an
amendment or revision and that includes a reference to the originally issued final test report.
The customer is the organization doing business with PAS external to PAS.
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Changes made to test results and data before the final test report is issued to the customer are
not amendments or revisions, these are corrections to errors found during the laboratory's
data verification and review process.
The laboratory's procedure for report amendments and revision are outlined in laboratory
SOP ENV-SOP-GBAY-0120,Data Review and Final Report Process.
5.10 Reporting
5.10.1 General Requirements
The laboratory reports results of testing in a way that assures the results are clear, and
unambiguous.All data and results are reviewed prior to reporting to assure the results reported
are accurate and complete.
Test results are summarized in test reports that include all information necessary for the
customer's interpretation of the test results. Additional information necessary to clarify the
data or disclose nonconformance, exceptions,or deviations that occurred during the analytical
process are also reported to the customer in the test report.
The specifications for test reports and EDD are established between the laboratory and the
customer at the time the request
est for analytical services is initiated. The rep
ort y specifications
include the test report format, protocol for the reporting limit (RL), conventions for the
reporting of results less than the limit of quantitation (LOQ), and specification for the use of
project or program specific data qualifiers. Information about review of analytical service
requests is provided in Section 4.4.
5.10.2 Test Reports: Required Items
Test Reports are prepared by the laboratory at the end of the testing process. The format of
the report depends on the level of reporting requested by the customer. The laboratory offers
a variety of standardized test report formats and can provide custom test report formats,when
necessary.
The level of detail required in the test report depends on the customer's needs for data
verification, validation, and usability assessments that occur after the laboratory releases the
test report to the customer. The test report formats offered by the laboratory provide gradient
levels of detail to meet the unique needs of each customer. The laboratory project manager
helps the customer select the test report format that best meets their needs. When a specific
report format or protocol is required for a regulatory or program compliance,the laboratory
project manager must ensure the test report selected meets those requirements.
Every test report issued by the laboratory includes each of the following items:
a) Title
b) Name and phone number of a point of contact from the laboratory issuing the report.
c) Name and address of the laboratory where testing was performed. When testing is done
at multiple locations within network (IRWO), the report must clearly identify which
network laboratory performed each test and must include the physical address of each
laboratory.
d) Unique identification of the test report and an identifier on each page of the report to link
each page to the test report and clear identification of the end of the report.
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e) The name and address of the customer
f) Identification of test methods used
g) Cross reference between client sample identification number (Sample ID) and the
laboratory's identification number for the sample (Lab ID) to provide unambiguous
identification of samples.
h) The date of receipt of samples, condition of samples on receipt,and identification of any
instance where receipt of the samples did not meet sample acceptance criteria.
i) Date and times of sample collection,receipt,preparation,and analysis.
j) Test results and units of measurement, and qualification of results associated with QC
criteria exceptions,and identification of reported results outside of the calibration range.
k) All chains of custody (COC) including records of internal transfer between locations
within the PAS network.
1) Name, title, signature of the person(s) authorizing release of the test report and date of
release.
m) A statement that the results in the test report relate only to the items tested.
n) Statement that the test report may not be reproduced except in full without written
approval from the laboratory.
5.10.3 Test Reports: Supplemental Items
5.10.3.1 Supplemental Requirements
The following items are included in the test report when required or relevant:
a) Shipping manifests / bill of ladings as applicable when common couriers are
utilized for shipment of samples,
b) Explanation of departure from test method SOPs including,what the departure
was and why it was necessary.
c) Statistical methods used. (Required for Whole Effluent Toxicity)
d) For solid samples, specification that results are reported on a dry weight or wet
weight basis.
e) Signed Affidavit,when required by client or regulatory agency.
f) A statement of compliance/non-compliance with requirements or specifications
(client, program, or standard) that includes identification of test results that did
not meet acceptance criteria.
g) When requested by the client, statement of estimated measurement uncertainty.
In general, for environmental testing, estimated uncertainty of measurement is
extrapolated from LCS control limits. Control limits incorporate the expected
variation of the data derived from the laboratory's procedure.When the control
limits are specified by the test method or regulatory program, the control limits
represent the expected variation of the test method and/or matrices for which
the test method was designed.
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h) Opinions and Interpretations
i) If a claim of accreditation/certification is included in the test report,identification
of any test methods or analytes for which accreditation/certification is not held
by the laboratory if the accrediting body offers accreditation/certification for the
test method/analyte. The fields of accreditation/certification vary between
agencies and it cannot be presumed that because accreditation/certification is not
held that it is offered or required.
j) Certification Information,including certificate number and issuing body.
5.10.3.2 Test Reports: Sampling Information
The following items are included in the test report when samples are collected by the
laboratory or when this information is necessary for the interpretation of test results:
a) Date of Sampling.
•
b) Unambiguous identification of material samples.
c) Location of sampling including diagrams, sketches,or photographs.
d) Reference to the sampling plan and procedures used.
e) Details of environmental conditions at time of sample that may impact test
results.
f) Any standard or other specification for the sampling method or procedure, and
deviations,additions to or exclusions from the specification concerned.
6.0 REVISION HISTORY
This Version:
Section Description of Change
Manual Approval Updated the list of required signatories and job titles to match current employees.
Signatory Page
7.1.1 Added A2LA certification
7.2.1 Updated to current method versions.
7.4.2 Inserted updated flowchart
7.4.3 Inserted updated flowchart
8.1 All"DOE"replaced with"DoE"
This document supersedes the following documents:
Document Number Title Version
ENV-MAN-CORQ-0001 Quality Manual 00
ENV-MAN-GBAY-0001 Quality Manual 00
ENV-MAN-GBAY-0001 Quality Manual 01
ENV-MAN-GBAY-0001 Quality Manual 02
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7.0 APPENDICES
7.1 Appendix A: Certification /Accreditation Listing
The certifications / accreditation lists provided in this manual represent those that were held by the
named location on the effective date of this manual. This information is subject to change without
notice and must not be considered valid proof of certification or accreditation status. Current
certificates are maintained by the local QM and a copy of the certificate is posted to ENV eDMS
Portal for access by all ENV employees. External parties should contact the laboratory for the most
current information.
7.1.1 PAS-Green Bay
Authority ID Authority ID
Florida Department of E87948 Virginia Department of 5537
Health,Bureau of General Services
Laboratories
Georgia,Environmental E87948 Wisconsin Department of 405132750
Protection Division Natural Resources
Illinois EPA 200050 Wisconsin Department of 105-444
Agriculture,Trade and
Consumer Protection
Kentucky Environmental 82 Wisconsin Department of 009-1093-01
and Public Protection Health Services,Bureau of
Cabinet Environmental and
Occupational Health,
Radioactive Materials
License
Louisiana Department of 04168 USDA Soil Permit P330-21-00008
Environmental Quality Regulated by 7 CFR330
Minnesota Department of 055-999-334 USDA Compliance WI-Soil-2020-01
Health Agreement _
New York Department of 12064 US Fish and Wildlife 51774A
Health Service Import/Export
License
North Dakota Department R-150 US DOT Hazardous 061719550153BD
of Health Chemistry Materials Certificate of
Division Registration
South Carolina Department 83006001 Commercial Emergency 0166B-1241
of Health and Alarm Permit(Brown
Environmental Control County Ordinance)
Texas Commission on T104704529-14-1 A2LA 6154.01
Environmental Quality
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7.2 Appendix B: Capability Listing
The capabilities listed in this Appendix were held by the location referenced on the effective date of
this manual. This information is subject to change without notice. External parties should contact
the laboratory for the most current information.
Table Legend:
! Air=Air
! DW=Drinking Water
! NPW=Non-Potable Water
! SCM= Solid and Chemical Materials
! Waste = Non-Aqueous Phase Liquid (NAPL),Oil
! Tissue=Biota and Tissue
7.2.1 PAS-Green Bay
Parameter Method Matrices
DW NPW SCM Waste Tissue
Lipids ENV-SOP-GBAY-0131 x1
Homogenization ENV-SOP-GBAY-0129 xl
Dry Weight ASTM D2974-87 x x x
ASTM Leach ASTM D3987-85 x
Flashpoint EPA 1010A x x
Specific Conductance EPA 120.1 x
TCLP Leach EPA 1311 x x x
SPLP Leach EPA 1312 x x x
Solids,Total(TS) SM 2540 B x
Solids,Total Dissolved
(TDS) SM 2540 C x
Solids,Total Suspended
(TSS) SM 2540 D x
Solids,Total Volatile
Suspended(TVSS) SM 2540 E x
Solids,Total Volatile
(TVS) EPA 160.4 x x
Solids,Volatile Suspended
(TVSS) EPA 160.4 x
Solids,Total Percent SM 2540 G x
AVS/SElv11 EPA 1629 x
Turbidity EPA 180.1 x
Turbidity SM 2130 B x
Ion Chromatography EPA 300.0 x x x
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Parameter Method Matrices
DW NPW SCM Waste Tissue
Ion Chromatography EPA 9056A x
Acidity,Total EPA 305.1 x
Acidity,Total SM 2310 B x x
Alkalinity,Total EPA 310.2 x
Alkalinity,Total SM 2320 B x
Cyanide,Total EPA 335.4 x
Cyanide,Total EPA 9012B x x
Ammonia,Total EPA 350.1 x x
Total Kjeldahl Nitrogen EPA 351.2 x x
Nitrogen,NO2/NO3 EPA 353.2 x x
Phosphorous,Total EPA 365.4 x x
Chemical Oxygen
Demand EPA 410.4 x
pH EPA 9040C x x
pH SM 4500-H+-B x
pH EPA 9045D x
Carbon,Total Organic SM 5310C x
Carbon,Total Organic
(Quad/Mod) EPA 9060A x x
Carbon,Total Organic Lloyd Kahn x
Carbon,Total Organic Walkley-Black x
Paint Filter Liquid Test EPA 9095A x
Iron,Ferrous HACH 8146 x
Iron,Ferric Calculation EPA6010/6020-HACH 8146 x
Apparent Color SM 2120 B x
Specific Gravity SM 2710 F x
Chromium,Hexavalent SM 3500-Cr B x
Oxygen,Dissolved SM 4500-0 G x
Sulfide SM 4500-S F x
Biochemical Oxygen
Demand/Carbonaceous
Biological Oxygen SM 5210 B x x
Heterotrophic Plate
Count SM 9215B xt xi
Coliform,Fecal SM 9222D xl x'
Coliform,Total SM 9223 xi
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Parameter Method Matrices
DW NPW SCM Waste Tissue
Mercury,Low Level EPA 1631E x x x
Mercury,Total EPA 7470A x
Mercury,Total EPA 7471B x x
Mercury,Total EPA 245.1 x
Mercury,Total EPA 245.6 x
Mercury,Totals EPA 7473 x
ICP-Metals SW846 6010D/EPA 200.7 x x
ICPMS-Metals SW846 6020B/EPA 200.8 x x x
TPH-Diesel SW846 8015C/D x x x
Diesel Range Organics WI Modified DRO x x x
Organochlorine
Pesticide/
Toxaphene/Chlorinated
Camphenes/Technical SW846 8081A/8081B/EPA
Chlordane 608/608.3 x x x
Polychlorinated Biphenyls SW846 8082/8082A/EPA
(PCB) 608/608.3 x x x
Polyaromatic SW846 8270E—SIM/EPA
Hydrocarbons(PAH) 625.1 SIM x x x
Semi-Volatile Organics SW846 8270E/EPA 625.1 x x
TPH-Gasoline SW846 8015C x x
Gasoline Range Organics WI Modified GRO x x
Methane,Ethene,Ethane SW846 8015C Mod xi
PVOC SW846 8021B/EPA 602 x x
SW846 8260B/8260D/EPA
Volatile Organics 624.1 x x
1=Laboratory does not hold TNI Accreditation for this test method.
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7.3 Appendix C: Glossary
This glossary provides common terms and definitions used in the laboratory. It is not intended to
be a complete list of all terms and definitions used.The definitions have been compiled mostly
from the TNI Standard and DoD QSM. Although this information has been reproduced with care,
errors cannot be entirely excluded. Definitions for the same term also vary between sources. When
the meaning of a term used in a laboratory document is different from this glossary or when the
glossary does not include the term, the term and definition is included or defined in context in the
laboratory document.
Term Definition
3P Program PAS-The continuous improvement program used by PAS that focuses on Process,Productivity,and
Performance.
Acceptance Criteria TNI-Specified limits placed on characteristics of an item,process,or service defined in requirement
documents.
Accreditation TNI-The process by which an agency or organization evaluates and recognizes a laboratory as meeting
certain predetermined qualifications or standards,thereby accrediting the laboratory.
DoD-Refers to accreditation in accordance with the DoD ELAP.
Accreditation Body(AB) TNI-The organization having responsibility and accountability for environmental laboratory
accreditation and which grants accreditation under this program.
DoD-Entities recognized in accordance with the DoD-ELAP that are required to operate in accordance
with ISO/IEC 17011,Conformity assessment:General requirements for accreditation bodies accrediting conformity
assessment bodies. The AB must be a signatory,in good standing,to the International Laboratory
Accreditation Cooperation(ILAC)mutual recognition arrangement(MRA)that verifies,by evaluation
and peer assessment,that its signatory members are in full compliance with ISO/IEC 17011 and that its
accredited laboratories comply with ISO/IEC 17025. —
Accuracy TNI-The degree of agreement between an observed value and an accepted reference value.Accuracy
includes a combination of random error(precision)and systematic error(bias)components that are due
to sampling and analytical operations;a data quality indicator.
Activity,Absolute TNI-Rate of nuclear decay occurring in a body of material,equal to the number of nuclear
disintegrations per unit time.NOTE:Activity(absolute)may be expressed in becquerels(Bq),curies(C),
or disintegrations per minute(dpm),and multiples or submultiples of these units.
Activity,Areic TNI-Quotient of the activity of a body of material and its associated area.
Activity,Massic TNI-Quotient of the activity of a body of material and its mass;also called specific activity.
Activity,Volumic TNI-Quotient of the activity of a body of material and its volume;also called activity concentration.
NOTE:In this module[TNI Volume 1,Module 6],unless otherwise stated,references to activity shall
include absolute activity,areic activity,massic activity,and volumic activity.
Activity Reference Date TNI-The date(and time,as appropriate to the half-life of the radionuclide)to which a reported activity
result is calculated.NOTE:The sample collection date is most frequently used as the Activity Reference
Date for environmental measurements,but different programs may specify other points in time for
correction of results for decay and ingrowth.
Aliquot DoD-A discrete,measured,representative portion of a sample taken for analysis.
American Society for An international standards organization that develops and publishes voluntary consensus standards for a
Testing and Materials wide range of materials,products,systems and services.
(ASTM)
Analysis DoD-A combination of sample preparation and instrument determination.
Analysis Code(Acode) All the set parameters of a test,such as Analytes,Method,Detection Limits and Price.
Analysis Sequence A compilation of all samples,standards and quality control samples run during a specific amount of time
on a particular instrument in the order they are analyzed.
Analyst TNI-The designated individual who performs the"hands-on"analytical methods and associated
techniques and who is the one responsible for applying required laboratory practices and other pertinent
quality controls to meet the required level of quality.
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Analyte TNI-A substance,organism,physical parameter,property,or chemical constituent(s)for which an
environmental sample is being analyzed.
DoD-The specific chemicals or components for which a sample is analyzed;it may be a group of
chemicals that belong to the same chemical family and are analyzed together.
Analytical Method DoD-A formal process that identifies and quantifies the chemical components of interest(target
analytes)in a sample.
Analytical Uncertainty TNI-A subset of Measurement Uncertainty that includes all laboratory activities performed as part of the
analysis.
Aliquot DoD-A discrete,measured,representative portion of a sample taken for analysis.
Annual(or Annually) Defined by PAS as every 12 months±30 days.
Assessment TNI-The evaluation process used to measure or establish the performance,effectiveness,and
conformance of an organization and/or its system to defined criteria(to the standards and requirements
of laboratory accreditation).
DoD-An all-inclusive term used to denote any of the following.audit,performance evaluation,peer
review,inspection,or surveillance conducted on-site.
Atomic Absorption Instrument used to measure concentration in metals samples.
Spectrometer
Atomization A process in which a sample is converted to free atoms.
Audit TNI-A systematic and independent examination of facilities,equipment,personnel,training,procedures,
record-keeping,data validation,data management,and reporting aspects of a system to determine
whether QA/QC and technical activities are being conducted as planned and whether these activities will
effectively achieve quality objectives.
Batch TNI-Environmental samples that are prepared and/or analyzed together with the same process and
personnel,using the same lot(s)of reagents.A preparation batch is composed of one to 20
environmental samples of the same quality systems matrix,meeting the above-mentioned criteria and
with a maximum time between the start of processing of the first and last sample in the batch to be 24
hours or the time-frame specified by the regulatory program.An analytical batch is composed of
prepared environmental samples(extracts,digestates or concentrates)which are analyzed together as a
group.An analytical batch can include prepared samples originating from various quality system matrices
and can exceed 20 samples.
Batch,Radiation TNT-An RMB is composed of 1 to 20 environmental samples that are counted directly without
Measurements(RMB) preliminary physical or chemical processing that affects the outcome of the test(e.g.,non-destructive
gamma spectrometry,alpha/beta counting of air filters,or swipes on gas proportional detectors).The
samples in an RMB share similar physical and chemical parameter,and analytical configurations(e.g.,
analytes,geometry,calibration,and background corrections).The maximum time between the start of
processing of the first and last in an RMB is 14 calendar days.
Bias TNT-The systematic or persistent distortion of a measurement process,which causes errors in one
direction(i.e.,the expected sample measurement is different from the sample's true value).
Blank TNI and DoD-A sample that has not been exposed to the analyzed sample stream in order to monitor
contamination during sampling,transport,storage or analysis.The blank is subjected to the usual
analytical and measurement process to establish a zero baseline or background value and is sometimes
used to adjust or correct routine analytical results(See Method Blank).
DoD-Blank samples are negative control samples,which typically include field blank samples(e.g.,trip
blank,equipment(rinsate)blank,and temperature blank)and laboratory blank samples(e.g.,method
blank,reagent blank,instrument blank,calibration blank,and storage blank).
Blind Sample A sub-sample for analysis with a composition known to the submitter.The analyst/laboratory may know
the identity of the sample but not its composition.It is used to test the analyst's or laboratory's
proficiency in the execution of the measurement process.
BNA(Base Neutral Acid A list of semi-volatile compounds typically analyzed by mass spectrometry methods.Named for the way
compounds) they can be extracted out of environmental samples in an acidic,basic or neutral environment.
BOD(Biochemical Chemical procedure for determining how fast biological organisms use up oxygen in a body of water.
Oxygen Demand)
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Calibration TNI-A set of operations that establish,under specified conditions,the relationship between values of
quantities indicated by a measuring instrument or measuring system,or values represented by a material
measure or a reference material,and the corresponding values realized by standards.1)In calibration of
support equipment,the values realized by standards are established through the use of reference
standards that are traceable to the International System of Units(SI);2)In calibration according to test
methods,the values realized by standards are typically established through the use of Reference Materials
that are either purchased by the laboratory with a certificate of analysis or purity,or prepared by the
laboratory using support equipment that has been calibrated or verified to meet specifications.
Calibration Curve TNI-The mathematical relationship between the known values,such as concentrations,of a series of
calibration standards and their instrument response. _
Calibration Method A defined technical procedure for performing a calibration. _
Calibration Range DoD-The range of values(concentrations)between the lowest and highest calibration standards of a
multi-level calibration curve.For metals analysis with a single-point calibration,the low-level calibration
check standard and the high standard establish the linear calibration range,which lies within the linear
dynamic range.
Calibration Standard TNI-A substance or reference material used for calibration.
Certified Reference TNI-Reference material accompanied by a certificate,having a value,measurement uncertainty,and
Material(CRM) stated metrological traceability chain to a national metrology institute.
Chain of Custody An unbroken trail of accountability that verifies the physical security of samples,data,and records. —
Chain of Custody Form TNI-Record that documents the possession of the samples from the time of collection to receipt in the
(COC) laboratory.This record generally indudes:the number and type of containers;the mode of collection,the
collector,time of collection;preservation;and requested analyses.
Chemical Oxygen A test commonly used to indirectly measure the amount of organic compounds in water.
Demand(COD)
Client(referred to by Any individual or organization for whom items or services are furnished or work performed in response
ISO as Customer) to defined requirements and expectations.
Code of Federal A codification of the general and permanent rules published in the Federal Register by agencies of the
Regulations(CFR) federal government.
Comparability An assessment of the confidence with which one data set can be compared to another.Comparable data
are produced through the use of standardized procedures and techniques.
Completeness The percent of valid data obtained from a measurement system compared to the amount of valid data
expected under normal conditions.The equation for completeness is:
%Completeness=(Valid Data Points/Expected Data Points)*100
Confirmation TNI-Verification of the identity of a component through the use of an approach with a different
scientific principle from the original method.These may include,but are not limited to:second-column
confirmation;alternate wavelength;derivatization;mass spectral interpretation;alternative detectors;or
additional deanup procedures.
DoD-Includes verification of the identity and quantity of the analyte being measured by another means
(e.g.,by another determinative method,technology,or column). Additional cleanup procedures alone are
11 not considered confirmation techniques. _
Conformance An affirmative indication or judgment that a product or service has met the requirements of the relevant
specifications,contract,or regulation;also the state of meeting the requirements.
Congener A member of a class of related chemical compounds(e.g.,PCBs,PCDDs).
11 Consensus Standard DoD-A standard established by a group representing a cross-section of a particular industry or trade,or a
part thereof.
Continuing Calibration A blank sample used to monitor the cleanliness of an analytical system at a frequency determined by the
Blank(CCB) analytical method.
Continuing Calibration Compounds listed in mass spectrometry methods that are used to evaluate an instrument calibration from
Check Compounds the standpoint of the integrity of the system.High variability would suggest leaks or active sites on the
(CCC) instrument column.
Continuing Calibration DoD-The verification of the initial calibration. Required prior to sample analysis and at periodic
Verification intervals.Continuing calibration verification applies to both external and internal standard calibration
techniques,as well as to linear and non-linear calibration models.
Continuing Calibration Also referred to as a Calibration Verification Standard(CVS)in some methods,it is a standard used to
Verification(CCV) verify the initial calibration of compounds in an analytical method.CCVs are analyzed at a frequency
Standard determined by the analytical method.
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Continuous Emission A flue gas analyzer designed for fixed use in checking for environmental pollutants.
Monitor(CEM)
Continuous The delineation of tasks for a given laboratory department or committee to achieve the goals of that
Improvement Plan(CIP) department.
Contract Laboratory A national network of EPA personnel,commercial labs,and support contractors whose fundamental
Program(CLP) mission is to provide data of known and documented quality.
Contract Required Detection limit that is required for EPA Contract Laboratory Program(CLP)contracts.
Detection Limit(CRDL)
Contract Required Quantitation limit(reporting limit)that is required for EPA Contract Laboratory Program(CLP)
Quantitation Limit contracts.
(CRQL)
Control Chart A graphic representation of a series of test results,together with limits within which results are expected
when the system is in a state of statistical control(see definition for Control Limit)
Control Limit A range within which specified measurement results must fall to verify that the analytical system is in
control.Control limit exceedances may require corrective action or require investigation and flagging of
non-conforming data.
Correction DoD-Action taken to eliminate a detected non-conformity.
Corrective Action DoD-The action taken to eliminate the causes of an existing non-conformity,defect,or other
undesirable situation in order to prevent recurrence. A root cause analysis may not be necessary in all
cases.
Corrective and The primary management tools for bringing improvements to the quality system,to the management
Preventative Action of the quality system's collective processes,and to the products or services delivered which are an
(CAPA) output of established systems and processes.
Critical Value TNI-Value to which a measurement result is compared to make a detection decision(also known as
critical level or decision level).NOTE:The Critical Value is designed to give a specified low probability a
of false detection in an analyte-free sample,which implies that a result that exceeds the Critical Value,
gives high confidence(1—a)that the radionuclide is actually present in the material analyzed.For
radiometric methods,a is often set at 0.05.
Customer DoD-Any individual or organization for which products or services are furnished or work performed in
response to defined requirements and expectations.
Data Integrity TNI-The condition that exists when data are sound,correct,and complete,and accurately reflect
activities and requirements.
Data Quality Objective Systematic strategic planning tool based on the scientific method that identifies and defines the type,
(DQO) quality,and quantity of data needed to satisfy a specified use or end user.
Data Reduction TNI-The process of transforming the number of data items by arithmetic or statistical calculation,
standard curves,and concentration factors,and collating them into a more usable form.
Definitive Data DoD-Analytical data of known quantity and quality. The levels of data quality on precision and bias
meet the requirements for the decision to be made. Data that is suitable for final decision-making.
Demonstration of TNI-A procedure to establish the ability of the analyst to generate analytical results of acceptable
Capability(DOC) accuracy and precision.
DoD-A procedure to establish the ability of the analyst to generate analytical results by a specific method
that meet measurement quality objectives(e.g.,for precision and bias).
Department of Defense An executive branch department of the federal government of the United States charged with
(DoD) coordinating and supervising all agencies and functions of the government concerned directly with
national security.
Detection Limit(DL) DoD-The smallest analyte concentration that can be demonstrated to be different than zero or a blank
concentration with 99%confidence.At the DL,the false positive rate(Type 1 error)is 1%. A DL may
be used as the lowest concentration for reliably reporting a detection of a specific analyte in a specific
matrix with a specific method with 99%confidence.
Detection Limit(DL)for TNI-Laboratories that analyze drinking-water samples for SDWA compliance monitoring P P must use
Safe Drinking Water Act methods that provide sufficient detection capability to meet the detection limit requirements established
(SDWA)Compliance in 40 CFR 141.The SDWA DL for radioactivity is defined in 40 CFR Part 141.25.c as the radionuclide
concentration,which can be counted with a precision of plus or minus 100%at the 95%confidence level
(1.96a where a is the standard deviation of the net counting rate of the sample).
Deuterated Monitoring DoD-SIM specific surrogates as specified for GC/MS SIM analysis.
Compounds(DMCs)
Diesel Range Organics A range of compounds that denote all the characteristic compounds that make up diesel fuel(range can
(DRO) be state or program specific).
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Digestion DoD-A process in which a sample is treated(usually in conjunction with heat and acid)to convert the
target analytes in the sample to a more easily measured form.
Document Control The act of ensuring that documents(and revisions thereto)are proposed,reviewed for accuracy,
approved for release by authorized personnel,distributed properly and controlled to ensure use of the
correct version at the location where the prescribed activity is performed.
Documents DoD-Written components of the laboratory management system(e.g.,policies,procedures,and
instructions).
Dry Weight The weight after drying in an oven at a specified temperature.
Duplicate(also known as The analyses or measurements of the variable of interest performed identically on two subsamples of the
Replicate or Laboratory same sample.The results of duplicate analyses are used to evaluate analytical or measurement precision
Duplicate) but not the precision of sampling,preservation or storage internal to the laboratory.
Electron Capture Device used in GC methods to detect compounds that absorb electrons(e.g.,PCB compounds).
Detector(ECD)
Electronic Data A summary of environmental data(usually in spreadsheet form)which clients request for ease of data
Deliverable(EDD) review and comparison to historical results.
Eluent A solvent used to carry the components of a mixture through a stationary phase.
Elute To extract,specifically,to remove(absorbed material)from an absorbent by means of a solvent.
Elution A process in which solutes are washed through a stationary phase by movement of a mobile phase.
Environmental Data DoD-Any measurements or information that describe environmental processes,locations,or conditions;
ecological or health effects and consequences;or the performance of environmental technology.
Environmental The process of measuring or collecting environmental data.
Monitoring
Environmental An agency of the federal government of the United States which was created for the purpose of
Protection Agency protecting human health and the environment by writing and enforcing regulations based on laws passed
(EPA) by Congress.
Environmental Sample A representative sample of any material(aqueous,non-aqueous,or multimedia)collected from any source
for which determination of composition or contamination is requested or required.Environmental
samples can generally be classified as follows:
! Non Potable Water(Includes surface water,ground water,effluents, water treatment
chemicals,and TCLP leachates or other extracts)
! Drinking Water-Delivered(treated or untreated)water designated as potable water
! Water/Wastewater-Raw source waters for public drinking water supplies,ground waters,
municipal influents/effluents,and industrial influents/effluents
! Sludge-Municipal sludges and industrial sludges.
! Soil-Predominately inorganic matter ranging in classification from sands to clays.
i Waste-Aqueous and non-aqueous liquid wastes,chemical solids,and industrial liquid and
solid wastes
Equipment Blank A sample of analyte-free media used to rinse common sampling equipment to check effectiveness of
decontamination procedures.
Extracted Internal Isotopically labeled analogs of analytes of interest added to all standards,blanks and samples analyzed.
Standard Analyte Added to samples and batch QC samples prior to the first step of sample extraction and to standards and
instrument blanks prior to analysis.Used for isotope dilution methods.
Facility A distinct location within the company that has unique certifications,personnel and waste disposal
identifications.
False Negative DoD-A result that fails to identify(detect)an analyte or reporting an analyte to be present at or below a
level of interest when the analyte is actually above the level of interest
False Positive DoD-A result that erroneously identifies(detects)an analyte or reporting an analyte to be present above
a level of interest when the analyte is actually present at or below the level of interest.
Field Blank A blank sample prepared in the field by filling a clean container with reagent water and appropriate
preservative,if any,for the specific sampling activity being undertaken.
Field Measurement Determination of physical,biological,or radiological properties,or chemical constituents that are
measured on-site,close in time and sPAS to the matrices being sampled/measured,following accepted
test methods.This testing is performed in the field outside of a fixed-laboratory or outside of an enclosed
structure that meets the requirements of a mobile laboratory.
Field of Accreditation TNI-Those matrix,technology/method,and analyte combinations for which the accreditation body
offers accreditation.
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Field of Proficiency TNI-Matrix,technology/method,analyze combinations for which the composition,spike concentration
Testing(FoPT) ranges and acceptance criteria have been established by the 1'I'PEC.
Finding TNI-An assessment conclusion referenced to a laboratory accreditation standard and supported by
objective evidence that identifies a deviation from a laboratory accreditation standard requirement.
DoD-An assessment conclusion that identifies a condition having a significant effect on an item or
activity. An assessment finding may be positive,negative,or neutral and is normally accompanied by
specific examples of the observed condition. The finding must be linked to a specific requirement(e.g.,
this standard,ISO requirements,analytical methods,contract specifications,or laboratory management
systems requirements).
Flame Atomic Instrumentation used to measure the concentration of metals in an environmental sample based on the
Absorption Spectrometer fact that ground state metals absorb light at different wavelengths.Metals in a solution are converted to
(FAA) the atomic state by use of a flame.
Flame Ionization A type of gas detector used in GC analysis where samples are passed through a flame which ionizes the
Detector(FID) sample so that various ions can be measured.
Gas Chromatography Instrumentation which utilizes a mobile carrier gas to deliver an environmental sample across a stationary
(GC) phase with the intent to separate compounds out and measure their retention times.
Gas Chromatograph/ In conjunction with a GC,this instrumentation utilizes a mass spectrometer which measures fragments of
Mass Spectrometry compounds and determines their identity by their fragmentation patterns(mass spectra).
(GC/MS)
Gasoline Range Organics A range of compounds that denote all the characteristic compounds that make up gasoline(range can be
(GRO) state or program specific).
Graphite Furnace Instrumentation used to measure the concentration of metals in an environmental sample based on the
Atomic Absorption absorption of light at different wavelengths that are characteristic of different analytes.
Spectrometry(GFAA)
High Pressure Liquid Instrumentation used to separate,identify and quantitate compounds based on retention times which are
Chromatography dependent on interactions between a mobile phase and a stationary phase.
(HPLC)
Holding Time TNI-The maximum time that can elapse between two specified activities.
40 CFR Part 136-The maximum time that samples may be held prior to preparation and/or analysis as
defined by the method and still be considered valid or not compromised.
For sample prep purposes,hold times are calculated using the time of the start of the preparation
procedure.
DoD-The maximum time that may elapse from the time of sampling to the time of preparation or
analysis,or from preparation to analysis,as appropriate.
Homogeneity The degree to which a property or substance is uniformly distributed throughout a sample.
Homologue One in a series of organic compounds in which each successive member has one more chemical group in
its molecule than the next preceding member. For instance,methanol,ethanol,propanol,butanol,etc.,
form a homologous series.
Improper Actions DoD-Intentional or unintentional deviations from contract-specified or method-specified analytical
practices that have not been authorized by the customer(e.g.,DoD or DOE).
Incremental Sampling Soil preparation for large volume(1 kg or greater)samples.
Method(ISM)
In-Depth Data TNI-When used in the context of data integrity activities,a review and evaluation of documentation
Monitoring related to all aspects of the data generation process that includes items such as preparation,equipment,
software,calculations,and quality controls.Such monitoring shall determine if the laboratory uses
appropriate data handling,data use and data reduction activities to support the laboratory's data integrity
policies and procedures.
Inductively Coupled Analytical technique used for the detection of trace metals which uses plasma to produce excited atoms
Plasma Atomic Emission that emit radiation of characteristic wavelengths.
Spectrometry(ICP-AES)
Inductively Coupled An ICP that is used in conjunction with a mass spectrometer so that the instrument is not only capable of
Plasma-Mass detecting trace amounts of metals and non-metals but is also capable of monitoring isotopic speciation
Spectrometry(ICP/MS) for the ions of choice.
Infrared Spectrometer An instrument that uses infrared light to identify compounds of interest.
(IR)
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Initial Calibration(ICAL) The process of analyzing standards,prepared at specified concentrations,to define the quantitative
response relationship of the instrument to the analytes of interest.Initial calibration is performed
whenever the results of a calibration verification standard do not conform to the requirements of the
method in use or at a frequency specified in the method.
Initial Calibration Blank A blank sample used to monitor the cleanliness of an analytical system at a frequency determined by the
(ICB) analytical method. This blank is specifically run in conjunction with the Initial Calibration Verification
(ICV)where applicable.
Initial Calibration DoD-Verifies the initial calibration with a standard obtained or prepared from a source independent of
Verification(ICV) the source of the initial calibration standards to avoid potential bias of the initial calibration.
Injection Internal Isotopically labeled analogs of analytes of interest(or similar in physiochemical properties to the target
Standard Analyte analytes but with a distinct response)to be quantitated.Added to all blanks,standards,samples and batch
QC after extraction and prior to analysis.
Instrument Blank A clean sample(e.g.,distilled water)processed through the instrumental steps of the measurement
process;used to determine instrument contamination.
Instrument Detection Limits determined by analyzing a series of reagent blank analyses to obtain a calculated concentration.
Limits(IDLs) IDLs are determined by calculating the average of the standard deviations of three runs on three non-
consecutive days from the analysis of a reagent blank solution with seven consecutive measurements per
day.
Interference,spectral Occurs when particulate matter from the atomization scatters incident radiation from the source or when
the absorption or emission from an interfering species either overlaps or is so close to the analyte
wavelength that resolution becomes impossible.
Interference,chemical Results from the various chemical processes that occur during atomization and later the absorption
characteristics of the analyze.
Internal Standard TNI and DoD-A known amount of standard added to a test portion of a sample as a reference for
evaluating and controlling the precision and bias of the applied analytical method.
International An international standard-setting body composed of representatives from various national standards
Organization for organizations.
Standardization(ISO)
Intermediate Standard Reference solutions prepared by dilution of the stock solutions with an appropriate solvent.
Solution
International System of The coherent system of units adopted and recommended by the General Conference on Weights and
Units(S1) Measures. •
Ion Chromatography Instrumentation or process that allows the separation of ions and molecules based on the charge
(IC) properties of the molecules.
Isomer One of two or more compounds,radicals,or ions that contain the same number of atoms of the same
element but differ in structural arrangement and properties. For example,hexane(C6H14)could be n-
hexane,2-methylpentane,3-methylpentane,2,3-dimethylbutane,2,2-dimethylbutane.
Laboratory A body that calibrates and/or performs testing..
Laboratory Control TNI-(also known as laboratory fortified blank(LFB),spiked blank,or QC check sample):A sample
Sample(LCS) matrix,free from the analytes of interest,spiked with verified known amounts of analytes or a material
containing known and verified amounts of analytes and taken through all sample preparation and
analytical steps of the procedure unless otherwise noted in a reference method.It is generally used to
establish infra-laboratory or analyst-specific precision and bias or to evaluate the performance of all or a
portion of the measurement system.
Laboratory Duplicate Aliquots of a sample taken from the same container under laboratory conditions and processed and
analyzed independently.
Laboratory Information DoD-The entirety of an electronic data system(including hardware and software)that collects,analyzes,
Management System stores,and archives electronic records and documents.
(LIMS)
Learning Management A web-based database used by the laboratories to track and document training activities.The system is
System(LMS) administered by the corporate training department and each laboratory's learn centers are maintained by a
local administrator.
Legal Chain-of-Custody TNI-Procedures employed to record the possession of samples from the time of sampling through the
Protocols retention time specified by the client or program.These procedures are performed at the special request
of the client and include the use of a Chain-of-Custody(COC)Form that documents the collection,
transport,and receipt of compliance samples by the laboratory.In addition,these protocols document all
handling of the samples within the laboratory.
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Limit(s)of Detection TNI-The minimum result,which can be reliably discriminated from a blank with predetermined
(LOD) confidence level.
DoD-The smallest concentration of a substance that must be present in a sample in order to be detected
at the DL with 99%confidence.At the LOD,the false negative rate(Type II error)is 1%. A LOD may
be used as the lowest concentration for reliably reporting a non-detect of a specific analyte in a specific
matrix with a specific method at 99%confidence.
Lunit(s)of Quantitation TNI-The minimum levels,concentrations,or quantities of a target variable(e.g.,target analyte)that can
(LOQ) be reported with a specified degree of confidence.
DoD-The smallest concentration that produces a quantitative result with known and recorded precision
and bias.For DoD/DOE projects,the LOQ shall be set at or above the concentration of the lowest
initial calibration standard and within the calibration range.
Linear Dynamic Range DoD-Concentration range where the instrument provides a linear response.
Liquid chromatography/ Instrumentation that combines the physical separation techniques of liquid chromatography with the
tandem mass mass analysis capabilities of mass spectrometry.
spectrometry
(LC/MS/MS)
Lot TNI-A definite amount of material produced during a single manufacturing cycle,and intended to have
uniform character and quality.
Management Those individuals directly responsible and accountable for planning,implementing,and assessing work.
Management System System to establish policy and objectives and to achieve those objectives.
Manager(however The individual designated as being responsible for the overall operation,all personnel,and the physical
named) plant of the environmental laboratory.A supervisor may report to the manager.In some cases,the
supervisor and the manager may be the same individual.
Matrix TNI-The substrate of a test sample.
Matrix Duplicate TNI-A replicate matrix prepared in the laboratory and analyzed to obtain a measure of precision.
Matrix Spike(MS) TNI-A sample prepared,taken through all sample preparation and analytical steps of the procedure
(spiked sample or unless otherwise noted in a referenced method,by adding a known amount of target analyte to a specified
fortified sample) amount of sample for which an independent test result of target analyte concentration is available.Matrix
spikes are used,for example,to determine the effect of the matrix on a method's recovery efficiency.
Matrix Spike Duplicate TNI-A replicate matrix spike prepared in the laboratory and analyzed to obtain a measure of the
(MSD)(spiked sample or precision of the recovery for each analyte.
fortified sample
duplicate)
Measurement DoD-Criteria that may be general(such as completion of all tests)or specific(such as QC method
Performance Criteria acceptance limits)that are used by a project to judge whether a laboratory can perform a specified activity
(MPC) to the defined criteria.
Measurement Quality TNT-The analytical data requirements of the data quality objectives are project-or program-specific and
Objective(MQO) can be quantitative or qualitative.MQOs are measurement performance criteria or objectives of the
analytical process.Examples of quantitative MQOs include statements of required analyte detectability
and the uncertainty of the analytical protocol at a specified radionuclide activity,such as the action level.
Examples of qualitative MQOs include statements of the required specificity of the analytical protocol,
e.g.,the ability to analyze for the radionuclide of interest given the presence of interferences.
Measurement System TNI-A method,as implemented at a particular laboratory,and which includes the equipment used to
perform the test and the operator(s).
DoD-A test method,as implemented at a particular laboratory,and which includes the equipment used
to perform the sample preparation and test and the operator(s).
Measurement DoD-An estimate of the error in a measurement often stated as a range of values that contain the true
Uncertainty value within a certain confidence level. The uncertainty generally includes many components which may
be evaluated from experimental standard deviations based on repeated observations or by standard
deviations evaluated from assumed probability distributions based on experience or other information.
For DoD/DOE,a laboratory's Analytical Uncertainty(such as use of LCS control limits)can be reported
as the minimum uncertainty.
Method TNI-A body of procedures and techniques for performing an activity(e.g.,sampling,chemical analysis,
quantification),systematically presented in the order in which they are to be executed.
Method Blank TNI-A sample of a matrix similar to the batch of associated samples(when available)that is free from
the analytes of interest and is processed simultaneously with and under the same conditions as samples
through all steps of the analytical procedures,and in which no target analytes or interferences are present
at concentrations that impact the analytical results for sample analyses.
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Method Detection Limit TNI-One way to establish a Detection Limit;defined as the minimum concentration of a substance that
(MDL) can be measured and reported with 99%confidence that the analyte concentration is greater than zero
and is determined from analysis of a sample in a given matrix containing the analyte. _
Method of Standard A set of procedures adding one or more increments of a standard solution to sample aliquots of the same
Additions size in order to overcome inherent matrix effects.The procedures encompass the extrapolation back to
obtain the sample concentration.
Minimum Detectable TNI-Estimate of the smallest true activity that ensures a specified high confidence,1—(i,of detection
Activity(MDA) above the Critical Value,and a low probability R of false negatives below the Critical Value.For
radiometric methods,(i is often set at 0.05.NOTE 1:The MDS is a measure of the detection capability
of a measurement process and as such,it is an a priori concept.It may be used in the selection of
methods to meet specified MQOs.Laboratories may also calculate a"sample specific"MDA,which
indicates how well the measurement process is performing under varying real-world measurement
conditions,when sample-specific characteristics(e.g.,interferences)may affect the detection capability.
However,the MDA must never be used instead of the Critical Value as a detection threshold.NOTE 2:
For the purpose of this Standard,the terms MDA and minimum detectable concentration(MDC)are
equivalent.
Minimum Reporting the lowest concentration of standard used for calibration—Drinking Water Manual
limit(MRL)
MintMiner Commercial software program used to scan large amounts of chromatographic data to monitor for errors
or data integrity issues.
Mobile Laboratory TNI-A portable enclosed structure with necessary and appropriate accommodation and environmental
conditions for a laboratory,within which testing is performed by analysts. Examples include but are not
limited to trailers,vans,and skid-mounted structures configured to house testing equipment and
personnel.
National Environmental See definition of The NELAC Institute(TNI).
Laboratory Accreditation
Conference(NELAC)
National Institute of National institute charged with the provision of training,consultation and information in the area of
Occupational Safety and occupational safety and health.
Health(NTOSH)
National Institute of TNI-A federal agency of the US Department of Commerce's Technology Administration that is
Standards and designed as the United States national metrology institute(or NMI).
Technology(NISI)
National Pollutant A permit program that controls water pollution by regulating point sources that discharge pollutants into
Discharge Elimination U.S.waters.
System(NPDES)
Negative Control Measures taken to ensure that a test,its components,or the environment do not cause undesired effects,
or produce incorrect test results.
Nitrogen Phosphorus A detector used in GC analyses that urili7es thermal energy to ionize an analyte.With this detector,
Detector(NPD) nitrogen and phosphorus can be selectively detected with a higher sensitivity than carbon. _
Nonconformance An indication or judgment that a product or service has not met the requirement of the relevant
specifications,contract,or regulation;also the state of failing to meet the requirements. _
Not Detected(ND) The result reported for a compound when the detected amount of that compound is less than the
method reporting limit.
Operator Aid DoD-A technical posting(such as poster,operating manual,or notepad)that assists workers in
performing routine tasks. All operator aids must be controlled documents(i.e.,a part of the laboratory
management system).
Performance Based An analytical system wherein the data quality needs,mandates or limitations of a program or project are
Measurement System specified and serve as criteria for selecting appropriate test methods to meet those needs in a cost-
(PBMS) effective manner.
Physical Parameter TNI-A measurement of a physical characteristic or property of a sample as distinguished from the
concentrations of chemical and biological components.
Photo-ionization An ion detector which uses high-energy photons,typically in the ultraviolet range,to break molecules into
Detector(PID) positively charged ions.
Polychlorinated A class of organic compounds that were used as coolants and insulating fluids for transformers and
Biphenyls(PCB) capacitors.The production of these compounds was banned in the 1970's due to their high toxicity.
Positive Control Measures taken to ensure that a test and/or its components are working properly and producing correct
or expected results from positive test subjects.
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Post-Digestion Spike A sample prepared for metals analyses that has analytes spike added to determine if matrix effects may be
a factor in the results.
Power of Hydrogen(pH) The measure of acidity or alkalinity of a solution.
Practical Quantitation Another term for a method reporting limit The lowest reportable concentration of a compound based
Limit(PQL) on parameters set up in an analytical method and the laboratory's ability to reproduce those conditions.
Precision TNT-The degree to which a set of observations or measurements of the same property,obtained under
similar conditions,conform to themselves;a data quality indicator.Precision is usually expressed as
standard deviation,variance or range,in either absolute or relative terms.
Preservation 'INI and DoD-Any conditions under which a sample must be kept in order to maintain chemical,
physical,and/or biological integrity prior to analysis.
Primary Accreditation TNI-The accreditation body responsible for assessing a laboratory's total quality system,on-site
Body(Primary AB) assessment,and PT performance tracking for fields of accreditation.
Procedure TNI-A specified way to carry out an activity or process. Procedures can be documented or not.
Proficiency Testing(PT) TNI-A means to evaluate a laboratory's performance under controlled conditions relative to a given set
of criteria,through analysis of unknown samples provided by an external source.
Proficiency Testing TNI-The aggregate of providing rigorously controlled and standardized environmental samples to a
Program(PT Program) laboratory for analysis,reporting of results,statistical evaluation of the results and the collective
demographics and results summary of all participating laboratories.
Proficiency Testing TNI-A person or organization accredited by a TNI-approved Proficiency Testing Provider Accreditor to
Provider(PT Provider) operate a TNI-compliant PT Program.
Proficiency Testing TNI-An organization that is approved by TNI to accredit and monitor the performance of proficiency
Provider Accreditor testing providers.
(YTPA)
Proficiency Testing TNI-A statistically derived value that represents the lowest acceptable concentration for an analyte in a
Reporting Limit(PTRL) PT sample,if the analyte is spiked into the PT sample.The PTRLs are specified in the TNI FoPT tables.
Proficiency Testing TNI-A sample,the composition of which is unknown to the laboratory,and is provided to test whether
Sample(PT) the laboratory can produce analytical results within the specified acceptance criteria.
Proficiency Testing(PT) TNI-a)Scheduled PT Study:A single complete sequence of circulation and scoring of PT samples to all
Study participants in a PT program.The study must have the same pre-defined opening and closing dates for all
participants;b)Supplemental PT Study:A PT sample that may be from a lot previously released by a PT
Provider that meets the requirements for supplemental PT samples given in Volume 3 of this Standard
[TNT]but that does not have a pre-determined opening date and closing date.
Proficiency Testing Study TNI-a)Scheduled PT Study:The calendar date by which all participating laboratories must submit
Closing Date analytical results for a PT sample to a PT Provider;b)Supplemental PT Study:The calendar date a
laboratory submits the results for a PT sample to the PT Provider.
Proficiency Testing Study TNI-a)Scheduled PT Study:The calendar date that a PT sample is first made available to all participants
Opening Date of the study by a PT Provider;b)Supplemental PT Study:The calendar date the PT Provider ships the
sample to a laboratory.
Protocol TNI-A detailed written procedure for field and/or laboratory operation(e.g.,sampling,analysis)that
must be strictly followed.
Qualitative Analysis DoD-Analysis designed to identify the components of a substance or mixture.
Quality Assurance(QA) TNI-An integrated system of management activities involving planning,implementation,assessment,
reporting and quality improvement to ensure that a process,item,or service is of the type and quality
needed and expected by the client.
Quality Assurance A document stating the management policies,objectives,principles,organizational structure and
Manual(QAM) authority,responsibilities,accountability,and implementation of an agency,organization,or laboratory,to
ensure the quality of its product and the utility of its product to its users.
Quality Assurance A formal document describing the detailed quality control procedures by which the quality requirements
Project Plan(QAPP) defined for the data and decisions pertaining to a specific project are to be achieved.
Quality Control(QC) TNI-The overall system of technical activities that measures the attributes and performance of a process,
item,or service against defined standards to verify that they meet the stated requirements established by
the customer;operational techniques and activities that are used to fulfill requirements for quality;also the
system of activities and checks used to ensure that measurement systems are maintained within
prescribed limits,providing protection against"out of control"conditions and ensuring that the results
are of acceptable quality.
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Quality Control Sample TNT-A sample used to assess the performance of all or a portion of the measurement system.One of
(QCS) any number of samples,such as Certified Reference Materials,a quality system matrix fortified by spiking,
or actual samples fortified by spiking,intended to demonstrate that a measurement system or activity is in
control.
Quality Manual TNI-A document stating the management policies,objectives,principles,organizational structure and
authority,responsibilities,accountability,and implementation of an agency,organization,or laboratory,to
ensure the quality of its product and the utility of its product to its users.
Quality System TNI and DoD-A structured and documented management system describing the policies,objectives,
principles,organizational authority,responsibilities,accountability,and implementation plan of an
organization for ensuring quality in its work processes,products(items),and services.The quality system
provides the framework for planning,implementing,and assessing work performed by the organization
and for carrying out required quality assurance and quality control activities.
Quality System Matrix TNI and DoD-These matrix definitions shall be used for purposes of batch and quality control
requirements and may be different from a field of accreditation matrix:
Air and Emissions: Whole gas or vapor samples including those contained in flexible or rigid
wall containers and the extracted concentrated analytes of interest from a gas or vapor that are
collected with a sorbant tube,impinger solution,filter,or other device
Aqueous:Any aqueous sample excluded from the definition of Drinking Water or
Saline/Estuarine.Includes surface water,groundwater effluents,and TCLP or other
extracts.
Biological Tissue: Any sample of a biological origin such as fish tissue,shellfish or plant
material.Such samples shall be grouped according to origin.
Chemical Waste: A product or by-product of an industrial process that results in a matrix
not previously defined.
Drinking Water.Any aqueous sample that has been designated a potable or potentially
potable water source.
Non-aqueous liquid: Any organic liquid with<15%settleable solids
Saline/Estuarine: Any aqueous sample from an ocean or estuary,or other salt water source
such as the Great Salt Lake.
. Solids: Includes soils,sediments,sludges,and other matrices with>15%settleable solids.
Quantitation Range DoD-The range of values(concentrations)in a calibration curve between the LOQ and the highest
successively analyzed initial calibration standard used to relate instrument response to analyte
concentration.The quantitation range(adjusted for initial sample volume/weight,concentration/dilution
and final volume)lies within the calibration range.
Quantitative Analysis DoD-Anal is designed to determine the amounts or proportions of the components of a substance.
Random Error The EPA has established that there is a 5%probability that the results obtained for any one analyte will
exceed the control limits established for the test due to random error.As the number of compounds
measured increases in a given sample,the probability for statistical error also increases.
Raw Data TNI-The documentation generated during sampling and analysis. This documentation includes,but is
not limited to,field notes,electronic data,magnetic tapes,untabulated sample results,QC sample results,
print outs of chromatograms,instrument outputs,and handwritten records.
Reagent Blank(method A sample consisting of reagent(s),without the target analyte or sample matrix,introduced into the
reagent blank) analytical procedure at the appropriate point and carried through all subsequent steps to determine the
contribution of the reagents and of the involved analytical steps.
1 Reagent Grade Analytical reagent(AR)grade,ACS reagent grade,and reagent grade are synonymous terms for reagents
that conform to the current specifications of the Committee on Analytical Reagents of the American
Chemical Society.
Records DoD-The output of implementing and following management system documents(e.g.,test data in
electronic or hand-written forms,files,and logbooks).
Reference Material TNI-Material or substance one or more of whose property values are sufficiently homogenized and well
established to be used for the calibration of an apparatus,the assessment of a measurement method,or
for assigning values to materials.
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Reference Method TNI-A published method issued by an organization generally recognized as competent to do so.(When
the ISO language refers to a"standard method",that term is equivalent to"reference method').When a
laboratory is required to analyze by a specified method due to a regulatory requirement,the
analyte/method combination is recognized as a reference method.If there is no regulatory requirement
for the analyte/method combination,the analyte/method combination is recognized as a reference
method if it can be analyzed by another reference method of the same matrix and technology.
Reference Standard TNT-Standard used for the calibration of working measurement standards in a given organization or at a
given location.
Relative Percent A measure of precision defined as the difference between two measurements divided by the average
Difference(RPD) concentration of the two measurements.
Reporting Limit(RL) The level at which method,permit,regulatory and customer-specific objectives are met The reporting
limit may never be lower than the Limit of Detection(i.e.,statistically determined MDL).Reporting limits
are corrected for sample amounts,induding the dry weight of solids,unless otherwise specified.There
must be a sufficient buffer between the Reporting Limit and the MDL.
DoD-A customer-specified lowest concentration value that meets project requirements for quantitative
data with known precision and bias for a specific analyte in a specific matrix.
Reporting Limit A standard analyzed at the reporting limit for an analysis to verify the laboratory's ability to report to that
Verification Standard level.
(RLVS)
Representativeness A quality element related to the ability to collect a sample reflecting the characteristics of the part of the
environment to be assessed.Sample representativeness is dependent on the sampling techniques specified
in the project work plan.
Requirement Denotes a mandatory specification;often designated by the term"shall".
Retention Time The time between sample injection and the appearance of a solute peak at the detector.
Revocation TNI-The total or partial withdrawal of a laboratory's accreditation by an accreditation body.
Sample Portion of material collected for analysis,identified by a single,unique alphanumeric code.A sample may
consist of portions in multiple containers,if a single sample is submitted for multiple or repetitive
analysis.
Sample Condition Upon Form used by sample receiving personnel to document the condition of sample containers upon receipt
Receipt Form(SCURF) to the laboratory(used in conjunction with a COC).
Sample Delivery Group A unit within a single project that is used to identify a group of samples for delivery.An SDG is a group
(SDG) of 20 or fewer field samples within a project,received over a period of up to 14 calendar days.Data from
all samples in an SDG are reported concurrently.
Sample Receipt Form Letter sent to the client upon login to show the tests requested and pricing.
(SRF)
Sample Tracking Procedures employed to record the possession of the samples from the time of sampling until analysis,
reporting and archiving.These procedures include the use of a chain-of-custody form that documents the
collection,transport,and receipt of compliance samples to the laboratory.In addition,access to the
laboratory is limited and controlled to protect the integrity of the samples.
Sampling TNI-Activity related to obtaining a representative sample of the object of conformity assessment,
according to a procedure.
Selected Ion Monitoring A mode of analysis in mass spectrometry where the detector is set to scan over a very small mass range,
(SIM) typically one mass unit.The narrower the range,the more sensitive the detector.
DoD-Using GC/MS,characteristic ions specific to target compounds are detected and used to quantify
in applications where the normal full scan mass spectrometry results in excessive noise.
Selectivity TNI-The ability to analyze,distinguish,and determine a specific analyte or parameter from another
component that may be a potential interferent or that may behave similarly to the target analyte or
parameter within the measurement system.
Sensitivity TNI-The capability of a method or instrument to discriminate between measurement responses
representing different levels(e.g.,concentrations)of a variable of interest.
Serial Dilution The stepwise dilution of a substance in a solution.
Shall Denotes a requirement that is mandatory whenever the criterion for conformance with the specification
requires that there be no deviation.This does not prohibit the use of alternative approaches or methods
for implementing the specification as long as the requirement is fulfilled.
Should Denotes a guideline or recommendation whenever noncompliance with the specification is permissible.
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Signal-to-Noise Ratio DoD-A measure of signal strength relative to background noise. The average strength of the noise of
(S/N) most measurements is constant and independent of the magnitude of the signal. Thus,as the quantity
being measured(producing the signal)decreases in magnitude,S/N decreases and the effect of the noise
on the relative error of a measurement increases.
Source Water TNI-When sampled for drinking water compliance,untreated water from streams,rivers,lakes,or
underground aquifers,which is used to supply private and public drinking water supplies.
Spike A known mass of target analyte added to a blank sample or sub-sample;used to determine recovery
efficiency or for other quality control purposes.
Standard(Document) TNI-The document describing the elements of a laboratory accreditation that has been developed and
established within the consensus principles of standard setting and meets the approval requirements of
standard adoption organizations procedures and policies.
Standard(Chemical) Standard samples are comprised of a known amount of standard reference material in the matrix
undergoing analysis.A standard reference material is a certified reference material produced by US NIST
and characterized for absolute content,independent of analytical test method.
Standard Blank(or A calibration standard consisting of the same solvent/reagent matrix used to prepare the calibration
Reagent Blank) standards without the analytes.It is used to construct the calibration curve by establishing instrument
background.
Standard Method A test method issued by an organization generally recognized as competent to do so.
Standard Operating TNI-A written document that details the method for an operation,analysis,or action with thoroughly
Procedure(SOP) prescribed techniques and steps.SOPs are officially approved as the methods for performing certain
routine or repetitive tasks.
Standard Reference A certified reference material produced by the US NIST or other equivalent organization and
Material(SRM) characterized for absolute content,independent of analytical method.
Statement of A document that lists information about a company,typically the qualifications of that company to
Qualifications(SOQ) compete on a bid for services.
Stock Standard A concentrated reference solution containing one or more analytes prepared in the laboratory using
an assayed reference compound or purchased from a reputable commercial source.
Storage Blank DoD-A sample of analyte-free media prepared by the laboratory and retained in the sample storage area
of the laboratory. A storage blank is used to record contamination attributable to sample storage at the
laboratory.
Supervisor The individual(s)designated as being responsible for a particular area or category of scientific analysis.
This responsibility includes direct day-to-day supervision of technical employees,supply and instrument
adequacy and upkeep,quality assurance/quality control duties and ascertaining that technical employees
have the required balance of education,training and experience to perform the required analyses.
Surrogate DoD-A substance with properties that mimic the analyte of interest It is unlikely to be found in
environmental samples and is added to them for quality control purposes.
Suspension TNI-The temporary removal of a laboratory's accreditation for a defined period of time,which shall not
exceed 6 months or the period of accreditation,whichever is longer,in order to allow the laboratory time
to correct deficiencies or area of non-conformance with the Standard.
Systems Audit An on-site inspection or assessment of a laboratory's quality system.
Target Analytes DoD-Analytes or chemicals of primary concern identified by the customer on a project-specific basis.
Technical Director Individual(s)who has overall responsibility for the technical operation of the environmental testing
laboratory.
Technology TNI-A specific arrangement of analytical instruments,detection systems,and/or preparation techniques.
Test A technical operation that consists of the determination of one or more characteristics or performance of
a given product,material,equipment,organism,physical phenomenon,process or service according to a
specified procedure.The result of a test is normally recorded in a document sometimes called a test
report or a test certificate.
Test Method DoD-A definitive procedure that determines one or more characteristics of a given substance or
product.
Test Methods for EPA Waste's official compendium of analytical and sampling methods that have been evaluated and
Evaluating Solid Waste, approved for use in complying with RCRA regulations.
Physical/Chemical(SW-
846)
Test Source TNI-A radioactive source that is tested,such as a sample,calibration standard,or performance check
source.A Test Source may also be free of radioactivity,such as a Test Source counted to determine the
subtraction background,or a short-term background check.
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The NELAC Institute A non-profit organization whose mission is to foster the generation of environmental data of known and
(TNI) documented quality through an open,inclusive,and transparent process that is responsive to the needs of
the community.Previously known as NELAC(National Environmental Laboratory Accreditation
Conference).
Total Petroleum A term used to denote a large family of several hundred chemical compounds that originate from crude
Hydrocarbons(T'PH) oil.Compounds may include gasoline components,jet fuel,volatile organics,etc.
Toxicity Characteristic A solid sample extraction method for chemical analysis employed as an analytical method to simulate
Leaching Procedure leaching of compounds through a landfill.
cFCL1
Traceability TNI-The ability to trace the history,application,or location of an entity by means of recorded
identifications.In a calibration sense,traceability relates measuring equipment to national or international
standards,primary standards,basic physical conditions or properties,or reference materials.In a data
collection sense,it relates calculations and data generated throughout the project back to the requirements
for the quality of the project
Training Document A training resource that provides detailed instructions to execute a specific method or job function.
Trip Blank This blank sample is used to detect sample contamination from the container and preservative during
transport and storage of the sample.A cleaned sample container is filled with laboratory reagent water
and the blank is stored,shipped,and analyzed with its associated samples.
Tuning A check and/or adjustment of instrument performance for mass spectrometry as required by the
method.
Ultraviolet Instrument routinely used in quantitative determination of solutions of transition metal ions and highly
Spectrophotometer(UV) conjugated organic compounds.
Uncertainty,Counting TNI-The component of Measurement Uncertainty attributable to the random nature of radioactive
decay and radiation counting(often estimated as the square root of observed counts(MARLt1P).Older
references sometimes refer to this parameter as Error,Counting Error or Count Error(c.f.,Total
Uncertainty).
Uncertainty,Expanded TNI-The product of the Standard Uncertainty and a coverage factor,k,which is chosen to produce an
interval about the result that has a high probability of containing the value of the measurand(c.f.,
Standard Uncertainty).NOTE:Radiochemical results are generally reported in association with the Total
Uncertainty.Either if these estimates of uncertainty can be reported as the Standard Uncertainty(one-
sigma)or as an Expanded Uncertainty(k-sigma,where k >1).
Uncertainty, TNI-Parameter associated with the result of a measurement that characterizes the dispersion of the
Measurement values that could reasonably be attributed to the measurand.
Uncertainty,Standard TNI-An estimate of the Measurement Uncertainty expressed as a standard deviation(c.f.,Expanded
Uncertainty).
Uncertainty,Total TNI-An estimate of the Measurement Uncertainty that accounts for contributions from all significant
sources of uncertainty associated with the analytical preparation and measurement of a sample.Such
estimates are also commonly referred to as Combined Standard Uncertainty or Total Propagated
Uncertainty,and in some older references as the Total Propagated Error,among other similar items(c.f.,
Counting Uncertainty).
Unethical actions DoD-Deliberate falsification of analytical or quality control results where failed method or contractual
requirements are made to appear acceptable.
United States A department of the federal government that provides leadership on food,agriculture,natural resources,
Department of rural development,nutrition and related issues based on public policy,the best available science,and
Agriculture(USDA) effective management
United States Geological Program of the federal government that develops new methods and tools to supply timely,relevant,and
Survey(USGS) useful information about the Earth and its processes.
Unregulated EPA program to monitor unregulated contaminants in drinking water.
Contaminant Monitoring
Rule(UCMR)
Validation DoD-The confirmation by examination and provision of objective evidence that the particular
requirements for a specific intended use are fulfilled.
Verification TNI-Confirmation by examination and objective evidence that specified requirements have been met.In
connection with the management of measuring equipment,verification provides a means for checking
that the deviations between values indicated by a measuring instrument and corresponding known values
of a measured quantity are consistently smaller than the maximum allowable error defined in a standard,
regulation or specification peculiar to the management of the measuring equipment
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Voluntary Action A program of the Ohio EPA that gives individuals a way to investigate possible environmental
Program(VAP) contamination,clean it up if necessary and receive a promise from the State of Ohio that no more
cleanup is needed.
Whole Effluent Toxicity The aggregate toxic effect to aquatic organisms from all pollutants contained in a facility's wastewater
(WET) (effluent).
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7.4 Appendix D: Organization Chart(s)
7.4.1 Corporate Organization Chart
Disclaimer: The following organization chart shows the structure of the and the relationships and relative ranks of its parts and positions/jobs in place
on the date this version of this manual was published. This information is subject to change;contact the Quality Manager for the most current version.
eAnalyrk.a!
Corporate Organization Chart
Environmental Sciences Division President$CEO
Eric Roman
Chad Financial OFFicer Director HunMi Se VPI COO Chief Sales OlFrer Diet Information Cttlef Compliance
Rei4arte5 Officer Officer
MattheruWeiser Waite On M5eFU/er Gregory Whitman xyle KbRenowsti .. Judy MO an
Manager-Creeet and Manager-HR Director-Ora ty Rem rat VP Operations Overt or-M.rietng Direct°raF if {5.-ector-EHS
Correrrier Collectarri Operations
Stacy MCCIIntoC1. Clautlie Kixtiholm Ertanna Kottke 'cacti.Daigle KarlArderson Pamela gOmeredaai Diane Omer Adam Nate.
Director-Sapply Clain rianave-Finsaciel Director-Acraiisdon raiVP Operations VP-Sales Opera[lons Corporate lMerrut
F.tanager-Payroa Pe6+� AudYdr
Ma +ant Analysii in ratan
Nate Pact! loan PaF+r�eeihe:m Erik Larsen JeffChewy lea Graham Tammy Goodman Shaven Kew*,
rP'o Director-Ttainria and KFnecta*-P'oreiS rag VPOPeratlans
Corporate Development trespro nt VP-Sales
KathryrrLuarvv¢ Denise.Wadies Trevor Brenner
}aturc�F.�u NA
Ftergnral tR Managers Manager Product One Rr$'OsI mew-
caeratlpn5
MO tiro Sate Neat
GrreS Manager Gererai Manager
Jean-Plerre Fwuane,. David Kein pee icrr
General Manager Manager Operators
Aerob'tlle y iivob nlct;y
lachniml Director
AerolAlogy
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O
aceAnalytical
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COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
7.4.2 Quality Systems Management
Disclaimer: The following organization chart shows the structure of the and the relationships and relative ranks of its parts and positions/jobs in place
on the date this version of this manual was published. This information is subject to change;contact the Quality Manager for the most current version.
aceAnalytieal5 Chief Executive Officer
Eric Roman
f I I
Quality Systems Management --- President chief Compliance Officer -+
Environmental Sciences Division Greg Whitman Judith Morgan
I I
Quality Director Corporate Quality Director Corporate Internal Auditor Corporate Internal Auditor 1
Kirstin Daigle Shawn Kassner Calista Daigle
The QD has a
direct reporting Compliance Analyst
relationship to the Shari Pfalmer
President and I I I
indirect reporting Quality Program Manager Quality Program Manager Quality Program Manager Local Quality Managers
relationship to the Jonathan Waldorf Elizabeth Turner Stephanie Atkins
Chief Compliance Each QM has a direct
Officer. reporting relationship to
Jan Ward Ken Busch Anthony Haag--- Rebecca King Meghan Smith Kasey Raley a Quality Program
Manager and an indirect
OPEN reporting relationship to
M.Cavanaugh N.DeRubeis Erin Evans Kelly Nance Ross Simmons the General Manager of
(Indianapolis) each location for which
the QM is assigned.
Diana Losito Chris Fuller Maggie Elliot Pat Letterer J.Bendolph Tina
Buttermore
Katherine Michelle
Lisa Eads Allen LaGory Lauren Masterson Gabrielle Jones Eric Battista
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._(_ 1ace Analytical
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7.4.3 Pace—Green Bay—Organization Chart
Regional VP Operations
VP-Sates North Central Pace Analytical Services
Ron Kerr Kan finderion
Regional Director-Sales ' Green Bay, Vi
VP-SalesRicheni Hisson
John Gerken Sales Manager
Specially RSM Joshua Richards Genet al Manager
Mary Chnsl+e Heuser SSPM Account Executive Chad Pusch
Snane Clait.
Michael Dew Quality Director
Kirsten Daigle
Quality Program Manager
Administrative Support Fli:abeth Twee:
Human Resources Marge AIIM-Tnnkner Quality Manager
Nicole Oil-HR Director Tony Haag
Kim Moore-Enwrgnmenrai HR Direcicy Quality Assurance
Amanda Ouellette-HR Generalist Leigh Begelske
Jill Duranceau
•
Information Technology
Ryan Smith-Systems Admrn
Ryan Grubotski-PCILA)+Tech.
I t I ------���
Client Services Manager Volatile Lab Manager Semivolatlle Lab Manager Inorganic Lab Manager
Brian Beaten Scott TamerI Cnns Haase Brian King
I
Metals
Protect Management GC Donavan Setoff-Tech Spec ILeRdi •
m Saple Receiving Chris Hyskd Amanda Ddrnerer-Scientist2 GC1i15 - Amend-a Duclrovl-Scientist 2
Supervisor Atee Her Sieve Mleczkn Randy m Clon or-Sc an Tech gst a!Lead) Brad Hebert-Lab tech
Cindy Varga GCMS Jason hiurillo-Leo Tech 1
Sample Benson
Angela Lanc Kris Berns-Scientist r GC1LC Kan Schepprrien-scientist 1
Ann Le Greve-Lab Tech 2 Lon Stevens-Scientist 2
ilvdtHeather Benson-CS`T7 (?awn Haag-Scientist 2
Jeremiah Schietelbeln-Lab AssistantTiffany Walters-Scientist 1
Mai 1.e Car-C -CSTI Madison Service Center Matthew Stowe-Scientist 2 Bryan Meyemorer-Scientist 2 j
Sierra
far Her-•�STT Tan icsiterney Melisa Novoseleta-Scientist 1
orra Po-l-C T��rlWteme er Jill`Jan pee k-Scientist 1
y Shan Schweder-Scientist 2
Morgan Powell-CST, Lori ZemDel—$GBriust 2Wet Chem
Kendra Starr-LT1 iHaz Wale} 1Kes Barrette-Lab Assistant
Vials-Tech Anthony Wendel-CSTi I NicoleDonald Bratl Bradley-Lab Tech c.2Lean,
Susan Wybe"CST2 rolecl Coordinator Tyler Jenson-Scientist 2
P Organic Preo
a\IL B a Lab Assistant McKe n Cole Elliott Brabant-Lab Tech I • Ty Roerags-Scientist
Isaac Blakeslee-Lab Assistant 1dr.Kerna Amddi Desiree Cegeiski-Lab Tech 2 Brandy Mahoney-Scientst
Andy Dooangmale-Lab Tech 2 EntryMesita-Scientist I
Matt Koptenid-Lab Tech 1 Kirnoery 0 Brien-Lab Tech 3
Penny Lee-Lob Tech 1 Madeline Rohde-Lab Tech 1
Judy tiesMj-Lab Tech 2 Holly Trash-Scientist I
Caleb tbschke-Lab Tech I Heather Word-Scientist 1
Schaumberq Service Center Annette',Janke-Lab Tech 2
Grace Scoesen-Lab Assistant
J cvdan brieinhorst-Let Ass.stanl
Chicago IL Heidi Brcerman-Lab Assistant
Kathleen Hohmann
Matthew tkstelmann iTemp i
Last Reviewed Auguil 2021
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7.5 Appendix E: Equipment Listing
The equipment listed represents equipment were held by each location on the effective date of this
manual. This information is subject to change without notice. External parties should contact the
location for the most current information.
7.5.1 PAS-Green Bay
1 Equipment List: PAS-Green Bay
Description Manufacturer Model Serial Number Service Condition Location Internal Location of
Date ID Manual
Quick Trace Cetac M-7500 051104QTA 6/15/11 New Metals 40HG2 At Instrument
Mercury Dept
Analyzer P
Direct Milestone DMA-80 10070875 11/3/11 New Metals 40HG4 On-line
Mercury Dept
Analyzer P
ICPMS Thermo X Series 2 01301C 6/11/08 New Metals 40ICM2 On-line
Dept
ICPMS Thermo X Series 2 01780C 8/21/10 New Metals 40ICM3 On-line
Dept
ICP Thermo ICAP 6500 20073913 10/1/04 New Metals 40ICP2 On-line
Dept
Low Level Analytik Jena Mercur K170A0130 10/18/10 New LL Hg 40LHG4 On-line
Mercury
Low Level Cetac M-8000 111003QM8 8/17/12 New LL Hg 40LHG5 On-line
Mercury
GC/FID Hewlett 5890 Series II 3140A38457 10/1/04 Used SVOA 40GCS1 At instrument
Packard
GC/ECD Agilent 6890N US10538012 8/1/10 Used SVOA 40GCS7 At instrument
GC/ECD Hewlett- 6890 US00031701 10/1/04 Used SVOA 40GCS8 At instrument
Packard
GC/ECD Hewlett- 6890 US00021961 10/1/04 Used SVOA 40GCS9 At instrument
Packard
GC/ECD Agilent 6890 US00040655 10/1/04 Used SVOA 40GCSB At instrument
GC/ECD Hewlett- 6890 US00024921 10/1/04 Used SVOA 40GCSC At instrument
Packard _
GC/FID Agilent 7890 CN10912008 5/19/09 New SVOA 40GCSF At instrument
GC/ECD Agilent 7890B CN14043012 3/1/14 New SVOA 40GCSG At instrument
GC/ECD Hewlett- 6890 US10344089 3/1/14 New SVOA 40GCSH At instrument
Packard
GC/ECD Agilent 6890 US10443037 3/1/14 New SVOA 40GCSJ At instrument
GC/MS Hewlett- 6890 US81221570 2/1/00 New SVOA 40MSS2 At instrument
Packard
GC/MS Hewlett- 6890 US00024414 4/1/99 New SVOA 40MSS4 At instrument
Packard
GC/MS Hewlett- 5890 3310A49571 10/1/04 Used SVOA 40MSS6 At instrument
Packard
GC/MS Agilent 7890A CN10752040 8/5/10 New SVOA 40MSS7 At instrument
GC/MS Agilent 7890A CN10705029 9/4/13 New SVOA 40MSS8 At instrument
GC/MS Agilent 6890N US10540022 6/1/14 Used SVOA 40MSS9 At instrument
GC/MS Agilent 7890B 15483197 1/14/16 New SVOA 40MSSA At instrument
GC/MS Agilent 8890 US1949A020 1/14/20 New SVOA 40MSSB At instrument
GC/PID/ Hewlett- 5890 3310A48054 3/1/92 New VOA 40GCV1 At instrument
FID Packard
GC/PID/ Hewlett- 5890 3310A48054 3/1/92 New VOA 40GCV2 At instrument
FID Packard
GC/PID/ Hewlett- 5890 3140A39241 6/1/93 New VOA 40GCV3 At instrument
FID Packard
GC/PID/ Hewlett- 5890 3336A60500 12/1/95 New VOA 40GCV4 At instrument
FID Packard
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Description Manufacturer Model Serial Number Service Condition Location Internal Location of
Date ID Manual
GC/FID Hewlett- 5890 2843A20939 7/1/95 New VOA 40GCV8 At instrument
Packard
GC/MS Hewlett- 5890 3235A46437 5/14/93 New VOA 40MSV1 At instrument
Packard
GC/MS Hewlett- 6890 US00032794 10/18/0 New VOA 40MSV2 At instrument
Packard 4
GC/MS Agilent 6850 CN10719006 3/6/08 New VOA 40MSV3 At instrument
GC/MS Hewlett- 6890 US00040707 9/25/02 New VOA 40MSV7 At instrument
Packard
GC/MS Agilent 6850 CN1065-1003 7/9/07 New VOA 40MSV8 At instrument
GC/MS Hewlett- 7890 CN10031128 4/14/10 New VOA 40MSVA At instrument
Packard
GC/MS Hewlett- 7890A CN10811039 2/5/13 New VOA 40MSVB At instrument
Packard
GC/MS Hewlett- 7890B CN13283076 8/12/13 New VOA 40MSVC At instrument
Packard
GC/MS Hewlett- 7890B CN13283076 8/12/13 New VOA 40MSVD At instrument
Packard
GC/MS Hewlett- 7890B CN13133031 1/28/20 Used VOA 40MSVE At instrument
Packard
Oxygen YSI 5000 14F101753 8/20/14 New Wet 40WET2 At instrument
Meter Chem.
Turbidi- Hach 2100P 950400007487 10/1/04 Used Wet 40WET6 At instrument
meter Chem
Conductivit Mettler Toledo FiveEasy C129191955 9/1/21 New Wet 40WETK At instrument
y Meter Plus FP30 Chem
pH Meter Orion Star A211 X38338 7/25/17 New Wet 40WETF At instrument
Chem
EH Meter Accumet AB15 AB81200474 7/15/09 Used Wet 40WET9 At instrument
Chem
pH Meter Orion Star A211 X38362 7/25/17 New Wet 40WETG At instrument
Chem
pH Meter Orion Star A211 X5433 2/26/20 New Wet 40WETI At instrument
Chem
pH Meter Orion Star A211 C3026 3/2/20 New Wet 40WETJ At instrument
Chem
BOD Thermo/Orion 10060020 A0117 9/5/12 New Wet 40WETE At instrument
AutoEZ Chem
pH Meter Orion Star A211 X38338 7/25/17 New Wet 40WETF At instrument
Chem
pH Meter Orion Star A211 X38338 7/25/17 New Wet 40WETG At instrument
Chem
Flashpoint Tanaka Apm-8fc 33930 10/17/17 New Wet 40WETH At instrument
Chem
Direct Hach DR 2000 960300039446 10/1/04 Used Wet 4OWTA1 At instrument
Reading Chem
Spectro-
photometer
Apollo Tekmar/ Apollo 9000 99174002 10/1/04 Used Wet 4OWTA5 At instrument
Dohrmann Chem
Fusion Teledyne 14-9600-100 US08105007 10/1/04 Used Wet 4OWTA7 At instrument
Chem
Ion Thermo ICS-110 12051009 8/3/12 New Wet 4OWTAB At instrument
Chromato- Scientific Chem
graph
Quick Lachat 8500 Series 2 120600001428 8/13/12 New Wet 4OWTAC At instrument
Chem 8500 Chem
Series II
Ion Thermo ICS-1100 13040963 7/16/13 New Wet 4OWTAD At instrument
Chromato- Scientific Chem
graph
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Description Manufacturer Model Serial Number Service Condition Location Internal Location of
Date ID Manual
Quik Chem Lachat 8500 Series 2 140500001688 6/10/14 New Wet 4OWTAE At instrument
8500 Series Chem
II
Ion Thermo Aquion 160640270 8/19/16 New Wet 4OWTAF At instrument
Chromato- Scientific Chem
graph
Analytik Analytik Jena Multi EA N4-167/N 8/1/17 New Wet 4OWTAG At instrument
Jena 4000 Chem
Quik Chem Lachat 8500 Series 2 191000002249 12/6/19 New Wet 4OWTAH At instrument
8500 Series Chem
II
Omnis Metrohm 110010010 001000158371 12/9/19 New Wet 4OWTAI At instrument
Titrator Chem
TOC-VWP Shimadzu TOC-VWP H51725600347 12/16/19 New Wet 4OWTAJ At instrument
Chem
Ion Thermo ICS-1100 11121052 2/11/21 Used Wet 4OWTAK At instrument
Chromato- Scientific Chem
graph
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vr,:3
"ace Analytical
LABORATORY QUALITY MANUAL
Pace Analytical Services,LLC
COPYRIGHT©2021-2023 Pace Analytical Services,LLC.
8.0 ADDENDUM: PROGRAM REQUIREMENTS
Program specific information provided in this addendum supplements the main body of this manual.
Each subsection is stand-alone, meaning the requirements for the quality management system in each
subsection only apply to the program referenced. Additionally,only program requirements for the quality
management system that are more stringent than the content of the main body of the manual are included.
8.1 DoD/DoE
PAS-Green Bay maintains accreditation for DoD/DoE Environmental Laboratory Approval
Program(ELAP)
This addendum outlines additional policies and processes established by this laboratory to maintain
compliance with DoD/DOE program specific requirements as outlined in the DoD/DoE
Consolidated Quality Systems Manual (QSM) for Environmental Laboratories. The QSM
incorporates ISO/IEC 17025 and the TNI Standard and includes additional program-specific
requirements for laboratories that perform analytical testing services for DoD and DoE and which
must be followed for DoD / DoE projects.
Section 4.2.5: Supporting Documents
Technical SOPs used for DoD/DoE testing must also include instructions for equipment and
instrument maintenance, computer software/hardware,and troubleshooting.
The review frequency for technical SOPs used for DoD/DoE testing is annual, instead of every 2
years.
Section 4.4: Review of Analytical Service Requests
If the DoD/DoE customer requests a statement of conformity, the standard used for the decision
rule must be communicated to and agreed on with the customer and identified in the final test report.
Laboratory requests to deviate from the requirements specified in the DoD/DoE QSM must be
requested on a project-basis and include technical justifications for the deviation. These requests are
submitted to and approved by the DoD/DoE project chemist or contractor, however named, in
addition to the PAS client.
For DoD / DoE projects, will also seek clarification from the customer when the customer has
requested an incorrect, obsolete or improper method for the intended use of data; the laboratory
needs to depart from its test method SOP in order to meet project-specific data quality objectives;
information in project planning documents is missing or is unclear,
Section 4.5: Subcontracting
In addition to written client approval of any subcontractor for testing,the customer is notified of the
laboratory's intent to use a subcontractor for any management system element (such as data review,
data processing, project management or IT support) and consent for subcontracting is obtained
approved in writing by the DoD/DoE customer and record of consent kept in the project record.
Section 4.6: Purchasing and Supplies
The laboratory procedure for records of receipt of materials and supplies used in testing also include
a specification to record the date opened(DoE only).
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Section 4.9.3: Nonconforming Work
The laboratory's procedure for client notification includes the 15-business day DoD/DOE timeframe
for notification of the problem and the 30-business day timeframe for submission of the corrective
action plan or corrective actions taken.This procedure also includes the DoD/DoE requirement for
AB notification of discovery.
Section 4.13: Control of Records
Technical Records: The laboratory's procedure for logbooks includes measures to prevent the
removal of or addition of pages to the logbook(applies to both hardcopy and electronic). Hardcopy
logbooks are version controlled, pre-numbered and bound. Initials and entries and are signed or
initialed and dated by the person making the entry and the entry is made at the time the activity is
performed and in chronological order. Each page of the logbook must be closed by the last person
making the entry on the page. Closure is recorded by the initial and date of the person making the
last entry.
Section 5.4.5.3.3: Limit of Detection
For DoD/DoE the LOD is an estimate of the minimum amount of an analyte that can be reliably
detected by an analytical process. For clarification, the LOD is the analyte concentration necessary
to distinguish its presence from its absence. The LOD may be used as the lowest concentration for
reliably reporting a non-detect(ND). The LOD is specific to each suite of analyte,matrix,and method
including sample preparation.
After each DL determination,the laboratory establishes the LOD by spiking a quality system matrix
at a concentration of least 2X but no greater than 4X the DL (i.e. 2X DL <_ LOD Spike <_ 4X DL).
The spike concentration establishes the LOD and the concentration at which the LOD is verified.
The LOD is established during method validation and after major changes to the analytical system or
procedure that affects sensitivity of analysis or how the procedure is performed.
An LOD study is not required for any component for which spiking solutions or quality control
samples are not available. Additionally,an LOD study is not required if the laboratory does not report
data below the LOQ.
The LOD must be verified on a quarterly basis. Each preparation method listed on the scope of
accreditation must have quarterly LOD verifications; however, verification of all possible
combinations of preparation and clean-up techniques is not required. Where LOD verifications are
not performed on all combinations, the LOD verification is based on the worst-case combination
(preparation method with all applicable cleanup steps).
The laboratory's procedure for LOD determination and verification is detailed in laboratory SOP
ENV-SOP-GBAY-0106 Determination of the LOD and LQQ (most recent revision or replacement).
Section 5.4.5.3.4: Limit of Quantitation
For DoD/DoE, the LOQ is established for each analyte-matrix-method combination, including
surrogates. When an LOD is determined or verified by the laboratory,the LOQ must be above the
LOD [DL<LOD<LOQ].
At a minimum,the LOQ must be verified quarterly;however,verification of all possible combinations
of preparation and clean-up techniques is not required. Where LOQ verifications are not performed
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on all combinations,the LOQ verification on the worst-case combination (preparation method with
all applicable cleanup steps).
The laboratory's procedure for LOQ determination and verification is detailed in laboratory SOP
ENV-SOP-GBAY-0106 Determination of the LOD and LOQ (most recent revision or replacement).
Section 5.4.7: Control of Data
The laboratory will assure LIMS passwords are changed at least once per year.
An audit of the LIMS will be incorporated into the laboratory's annual internal audit schedule.
The laboratory will have procedures in place to notify DoD/DoE customers of changes to LIMS
software or hardware configurations that may impact the customer's integrity of electronic data
Section 5.9.1: Quality Control
For DoD/DoE,storage blanks are essential QC to monitor the storage of samples for volatile organic
analysis (VOA). The laboratory's SOP for storage of VOA samples must include a contamination
monitoring program based on the performance of storage blanks. (See QSM 5.3.3)
Section 5.8.5: Sample Disposal
For DoE projects, the record of disposal must also include how the sample was disposed and the
name of the person that performed the task.
Appendix E: Support Equipment Calibration
Mechanical Volumetric Pipette: In addition to the quarterly verification check, pipettes used for
DoD/DoE projects are checked daily before use using the same procedure and criteria specified for
the quarterly check.
Water Purification System: The performance of the water purification system is checked daily prior
to use in accordance with laboratory SOP ENV-SOP-GBAY-0127 Use and Maintenance of Water
Purification Systems(most recent revision or replacement).
Radiological Survey Equipment: The performance of the radiological survey equipment is checked
daily prior to use in accordance with laboratory SOP ENV-SOP-GBAY-0158 ECD Management(most
recent revision or replacement).
Additional: (DoE): Section 6.0 of the QSM outlines additional management system requirements
for the management of hazardous and radioactive materials management and health and safety
practices. The laboratory,if approved for DoE,will work with the PAS Health and Safety Director
to establish plans, policies and procedures that conform to these comprehensive specifications and
incorporate these documents into the quality management system.
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aceAr,alytical ®
ENVIRONMENTAL SCIENCES
Document Information
Document Number: ENV-SOP-GBAY-0010 Revision: 03
Document Title: Determination of Trace Metals in Waters and Wastes by Inductively Coupled
Plasma Mass Spectroscopy-6020/A/B 200.8
Department(s)
Metals
Date Information
Effective Date: 12 Apr 2021
Notes
Document Notes:
All Dates and Times are listed in: Central Time Zone

Signature Manifest
Document Number: ENV-SOP-GBAY-0010 Revision: 03
Title: Determination of Trace Metals in Waters and Wastes by Inductively Coupled Plasma Mass Spectroscopy
- 6020/A/B 200.8
All dates and times are in Central Time Zone.
ENV-SOP-GBAY-0010-Rev.03 6020E_200.8
QM Approval
Name/Signature Title Date Meaning/Reason
Elizabeth Turner(007857) Manager-Quality Program 09 Apr 2021,02:11:11 PM Approved
Management Approval
Name/Signature Title Date Meaning/Reason
Chad Rusch(007163) General Manager 2 07 Apr 2021,01:51:17 PM Approved

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
1.0 SCOPE AND APPLICATION
This standard operating procedure (SOP) describes the laboratory procedure for the determination of
sub-ppb (dig/L) concentrations of a large number of elements in biota, aqueous, and solid extracts or
digests by inductively coupled plasma-mass spectrometry (ICPMS). When dissolved constituents
are required, samples must be filtered and acid-preserved prior to analysis. Dissolved samples are
typically acid digested prior to analysis. Acid digestion prior to centrifuging and analysis is required
for aqueous and solid samples for which total (acid-leachable) elements are required.
1.1 Target Analyte List
Isotope Element Symbol CASRN
27 Aluminum Al 7429-90-5
121 Antimony Sb 7440-36-0
75 Arsenic As 7440-38-2
137 Barium Ba 7440-39-3
9 Beryllium Be 7440-41-7
10 Boron B 7440-42-8
111 Cadmium Cd 7440-43-9
43 Calcium Ca 7440-70-29
133 Cesium Cs 7440-46-2
52 Chromium Cr 7440-47-3
59 Cobalt Co 7440-48-4
63 Copper Cu 7440-50-8
54 Iron Fe 7439-89-6
7 Lithium Li 7439-93-2
208 Lead Pb 7439-92-1
25 Magnesium Mg 7439-95-4
55 Manganese Mn 7439-96-5
201 Mercury Hg 7439-97-6
95 Molybdenum Mo 7439-98-7
60 Nickel Ni 7440-02-0
105 Palladium Pd 7440-06-4
31 Phosphorous P 7723-14-0
195 Platinum Pt 7440-05-3
39 Potassium K 7440-09-7
78 Selenium Se 7782-49-2
28 Silicon Si 7440-21-3
-
107 Silver Ag 7440-22-4
23 Sodium Na 7440-23-5
88 Strontium Sr 7440-24-6
205 Thallium TI 7440-28-0
118 Tin Sn 7440-31-5
47 Titanium Ti 7440-32-6
182 Tungsten W 7440-33-7
238 Uranium U 7440-61-1
51 Vanadium V 7440-62-2
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
66 Zinc Zn 7440-66-6
90 Zirconium Zr 7440-67-7
1.2 Applicable Matrices
1.2.1 This SOP is applicable to aqueous (dissolved, total, waste) samples.
1.2.2 This SOP is applicable to ASTM, SPLP, and TCLP samples.
1.2.3 This SOP is applicable to solid/soil samples.
1.2.4 This SOP is applicable to Biota (biological) samples.
1.3 Personnel: Use of this method is restricted to analysts who are knowledgeable in the recognition
and in the correction of spectral, chemical, and physical interferences in ICPMS.
2.0 SUMMARY OF METHOD
2.1 Prior to analysis, samples which require total ("acid-leachable") values must be digested using
appropriate sample preparation methods. A number of methods are recommended in SW846
and EPAsamplepreparation/digestion
200.8 for the of various matrices for tr
ace metals
analysis by ICPMS. Applicable analytes are listed in the Target Analyte List.
2.2 Methods 6020B/200.8 describe the multi-elemental determination of analytes by ICPMS. The
method measures ions produced by a radio frequency inductively coupled argon plasma.
Analyte species originating in a liquid are nebulized and the resulting aerosol transported by
argon gas into the plasma torch. The ions produced are entrained in the plasma gas and
introduced, by means of an interface, into a mass spectrometer. The ions produced in the
plasma are sorted according to their mass-to-charge ratios and quantified with a channel
electron multiplier. Interferences must be assessed, and valid corrections applied, or the data
must be flagged to indicate problems. Interference correction must include compensation for
background ions contributed by the plasma gas, reagents, and constituents of the sample
matrix as well as isobaric elemental corrections.
3.0 INTERFERENCES
3.1 Isobaric Elemental Interferences — Isobaric elemental interferences result when isotopes of
different elements have the same nominal mass-to-charge ratio and cannot be resolved with
the instruments spectrometer. One way to solve this problem is to measure a different isotope
for which there is no interference. Alternatively, one can monitor another isotope of the
element and subtract an appropriate amount from the element being analyzed, using known
isotope ratio information. Corrections for most of the common elemental interferences are
programmed into the software.
3.2 Isobaric Polyatomic Interferences — Isobaric polyatomic interferences result when ions containing
more than one atom have the same nominal mass-to-charge ratio as an analyte of interest and
cannot be resolved by the instrument's spectrometer. An example includes CIO+ (mass 51),
which interferes with V, and must be corrected by measuring CIO+ at mass 53. When possible,
an interference free isotope should be chosen for measurement.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
A ,.f A 0

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
3.3 Physical interferences are associated with the sample nebulization and transport processes as
well as with ion-transmission efficiencies. Nebulization and transport processes can be
affected if a matrix component causes a change in surface tension or viscosity. Changes in
matrix composition can cause significant signal suppression or enhancement. Dissolved solids
can deposit on then nebuli
zer zer tip of a pneumatic nebulizer and on the interface skimmers
(reducing the orifice size and the instrument performance). Total solid levels below 0.2% (2,000
mg/L) have been currently recommended to minimize solid deposition. An internal standard
can be used to correct for physical interferences if it is carefully matched to the analyte so that
the two elements are similarly affected by matrix changes.
3.4 Memory interferences can occur when there are large concentration differences between
samples or standards which are analyzed sequentially. Sample deposition on the sampler and
skimmer cones, spray chamber design, and the type of nebulizer affects the extent of the
memory interferences which are observed. The rinse period between samples must be long
enough to eliminate significant memory interference.
3.5 It is important to note that matrix matching acid concentrations and compositions between
standards, blanks, and samples is required and cannot be ignored.
3.6 Chromic acid should never be used to clean any container used in ICPMS analysis.
3.7 Borosilicate glass in sample containers can lead to interference of Boron concentrations in
samples. This is also true of volumetric flasks, thus when dilution in the flask is complete the
standards must be removed as soon as possible from the dilution container and placed into a
clean plastic container.
4.0 DEFINITIONS
Refer to the Laboratory Quality Manual for a glossary of common lab terms and definitions.
5.0 HEALTH AND SAFETY
The toxicity or carcinogenicity of each chemical material used in the laboratory has not been fully
established. Each chemical should be regarded as a potential health hazard and exposure to these
compounds should be as low as reasonably achievable.
The laboratory maintains documentation of hazard assessments and OSHA regulations regarding
the safe handling of the chemicals specified in each method. Safety data sheets for all hazardous
chemicals are available to all personnel. Employees must abide by the health, safety and
environmental (HSE) policies and procedures specified in this SOP and in the Pace Chemical
Hygiene/Safety Manual.
Personal protective equipment (PPE) such as safety glasses, gloves, and a laboratory coat must be
worn in designated areas and while handling samples and chemical materials to protect against
physical contact with samples that contain potentially hazardous chemicals and exposure to
chemical materials used in the procedure.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Concentrated corrosives present additional hazards and are damaging to skin and mucus
membranes. Use these acids in a fume hood whenever possible with additional PPE designed for
handing these materials. If eye or skin contact occurs, flush with large volumes of water. When
working with acids, always add acid to water to prevent violent reactions. Any processes that emit
large volumes of solvents (evaporation/concentration processes) must be in a hood or apparatus that
prevents employee exposure.
Contact your supervisor or local HSE coordinator with questions or concerns regarding safety
protocol or safe handling procedures for this procedure.
6.0 SAMPLE COLLECTION, PRESERVATION, HOLDING TIME, AND STORAGE
Requirements for container type, preservation, and field quality control (QC) for the common list of
test methods offered by Pace are included in the laboratory's quality manual.
Samples should be collected in accordance with a sampling plan and procedures appropriate to
achieve the regulatory, scientific, and data quality objectives for the project.
The laboratory will provide containers for the collection of samples upon client request for analytical
services. Bottle kits are prepared in accordance with laboratory SOP ENV-SOP-GBAY-0007 Bottle
Preparation (most recent version or replacement).
6.1 All sample containers must be HDPE, glass, or Teflon. The containers are purchased pre-cleaned
and documented to be contaminant free. Where applicable, the bottle ware is demonstrated to
be fee of target analytes. When bottle ware not originating from the lab is used, the data may
be qualified with either one or both of the following data qualifiers:
6.1.1 Sample field preservation does not meet EPA or method recommendations for this
analysis.
6.1.2 Sample container did not meet EPA or method requirements.
6.2 Aqueous Samples
6.2.1 Dissolved samples must be filtered through a 0.45-pm pore diameter membrane filter at the
time of collection or as soon after as practically possible. The laboratory can perform the
filtration if the step was not performed in the field. The filtrate is then preserved to a pH<2
with nitric acid, acid not to exceed 2% of the container capacity.
6.2.2 Total samples are preserved to a pH<2 with nitric acid, acid not to exceed 2% of the
container capacity.
Note: Aqueous samples that react violently to the addition of acid maybe collected without
chemical preservation with proper variances approved by the regulatory authority. The
responsibility of requesting this variance lies with the sample collector.
Note: Samples may be preserved in the lab. The samples may not be processed until 24
hours after preservation with a pH test of <2, unless otherwise noted on the data. Samples
that do not attain a pH<2 or samples that are filtered in the lab must be flagged with P4.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
G2 ..f A')

eAnaIicaI®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
6.3 General Requirements
Matrix Routine Minimum
Container Sample Amount' Preservation Holding Time
Aqueous Thermal: None 6 months,excluding Hg.
(Total and 250mL plastic 50mL Chemical: HNO3(pH<2) 28 Days if Hg requested
Dissolved)
6 months to leach, 6
TCLP, months to digest (1 year
SPLP and 250mL plastic 50mL Thermal: None total),excluding Hg.
ASTM Chemical: HNO3(pH<2) 28 Days to leach, 28 Days
to digest (56 days total) if
Hg requested
Solid 4oz Glass 5g Thermal:56°Celsius 6 months,excluding Hg.
Chemical: None 28 Days if Hg requested
Thermal:56°Celsius during shipment 6 months after removal
Glass,Plastic, Lab Storage:<_-10°Celsius; from the freezer,excluding
(56°Celsius is acceptable based on
Biota or Aluminum 5g QAPjP and regulatory authority Hg.
Foil 28 Days after removal from
requirements for temporary storage)
Chemical:None the freezer if Hg requested
'Minimum amount needed for each discrete analysis.
Thermal preservation is checked and recorded on receipt in the laboratory in accordance with
laboratory SOP ENV-SOP-GBAY-0006 Sample Management (most recent revision or replacement).
Chemical preservation is checked and recorded at time of receipt or prior to sample preparation.
Shipments of soil and water samples to the laboratory require thermal preservation in the form of
cubed, block or dry ice. At the time of laboratory receipt, proper thermal preservation is checked by
measuring the temperature of melt water or when provided the temperature blank. The Pace
Analytical acceptable temperature range is 0 to 6°C (or 5.-10 for dry ice for biota samples). All QAPjP
and regulatory authority requirements become priority over this requirement.
After receipt, aqueous samples are stored at room temperature, solid samples are stored at 0 - 6°C,
and biota samples are stored at -10°C or less until sample preparation. Prepared samples
(digestates)are stored at room temperature until sample analysis.
After analysis, unless otherwise specified in the analytical services contract, samples are retained for
21 days from date of final report and then disposed of in accordance with Federal, State, and Local
regulations.
Anyprinted copyof this SOP andall copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
7 of 42

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
7.0 EQUIPMENT AND SUPPLIES
7.1 Equipment
Equipment* Manufacturer* Model(s)* Serial Number Model(s)* Serial Number
Thermo XSeries ThermoFisher XSeries 2 01301C XSeries 2 01780C
2 ICPMS Scientific
Rough Pump Sogevac SV40B1 31001133096 SV40B1 31001001928
Computer Lenovo ThinkCentre 1S3133A3UMJ ThinkCentre 00186046357407
GPFVE
Autosampler CETAC ASX520 101016A520 ASX520 0610120A520
Refrigerated NESLAB ThermoFlex 2500 111835101171 ThermoFlex 11223001011810
Recirculator 108 2500 04
Uninterruptible Toshiba 1600 XP Series 15701152 Xtreme TX99150400005
Power Supply UPS Power
(UPS) Conversion
Hot Block Environmental SC100 526CEC0714 SC100 526CEC0714
Express
Analytical Denver XE-310 718860 XE-310 718860
Balance Instrument
Note: Equivalent substitutes may be used. Examples include Analytical West for the nebulizer, torch, and the
screen/bonnet. There are 3 possible autosamplers for these instruments. Any change due to a broken part will
be recorded in the maintenance log.
7.2 Supplies
Supplies* Manufacturer* Vendor* Catalog
number*
Sample Peri-Pump Tubing Analytical West Analytical West PT-2100P
Internal Standard Peri-Pump Tubing Analytical West Analytical West PT-2100P
Waste Peri-Pump Tubing Analytical West Analytical West PT-2160P
Quartz T Connecter Glass Expansion Glass Expansion 60-808-1185
Concentric Nebulizer Thermo Electron Corp. Thermo Electron Corp. 4600294-03
Quartz Torch Thermo Electron Corp. Thermo Electron Corp. 3601145
Screen and Bonnet Thermo Electron Corp. Thermo Electron Corp. 3601219
Ni Sample Cone Thermo Electron Corp. Thermo Electron Corp. 3600812
Ni Skimmer Cone Thermo Electron Corp. Thermo Electron Corp. 3600811
Graphite Sample Cone Seal Thermo Electron Corp. Thermo Electron Corp. 3004382
15 mL Polypropylene Test Tubes Fisher Scientific Fisher Scientific 14-956-7E
50-mL Disposable Digestion Cups Environmental Express Environmental Express SC475
Calibrated Pipette 1000 pL Eppendorf Fisher Scientific 21-371-13
Calibrated Pipette 10-50 pL Thermo Thermo 21-377-193
Calibrated Pipette 100-1000 pL Eppendorf Fisher Scientific 05-402-50
Calibrated Pipette 1000-5000 pL Eppendorf Fisher Scientific 05-402-91
Trace Metal Grade Pipette Tips 1 Eppendorf Fisher Scientific 21-372
mL
Trace Metal Grade Pipette Tips 5 Eppendorf Fisher Scientific 21-381-198
mL
1 N-DEX Nitrile Gloves Best Fisher Scientific 6005 PFM
pH Indicator Sticks Whatman MG Scientific P114-26
*Or equivalent
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
Rnf42

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020E and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY I
COPYRIGHT©2021 Pace Analytical Services, LLC
8.0 REAGENTS AND STANDARDS
8.1 Standards are used in the tuning of the instrument through the calibration, calibration verification,
sample analysis, and continuing calibration verification. Standard solutions include: instrument
tuning solutions, calibration and calibration check standards, ICSA/AB, internal standards, low
level check standards (LLC, CRI, or CRDL), and spike standards. Please see Table 8.7 for a
list of working standards. Table 8.6 lists the directions to making intermediate standards
from the stock standards listed in Table 8.5.
8.1.1 Mass Spectrometer Tuning Solution: A solution containing elements representing all of the
mass regions of interest (for example, 10 pg/L of 23, 24, 25Mg and 206, 207, 208Pb) must be
prepared to verify that the mass resolution and mass calibration of the instrument are within
the required specifications. This solution is also used to verify that the instrument has
reached thermal stability.
8.1.2 Cross Calibration Solution (X Cal): contains 50 ppb of all method analyte elements (with the
exception of Li, at 100ppb). This solution is used to calculate the concentration when the
detector changes from pulse mode to analog mode. This enables a large linear range
while protecting the detector.
8.1.3 Calibration Standards: These are an increasing gradient of concentration for the analytes of
interest. These can be made in the laboratory or purchased from commercial suppliers.
8.1.4 Linear Range (LR): These standards may be a mix or single element standard used to
verify the upper limit of the instrument's working range. 6020B requires that the upper limit
of the range be verified every calibration. If the LDR is not verified above the high point of
the calibration, it defaults to the high point of the calibration. This procedure will be
followed for all sample analysis.
8.1.5 Initial Calibration Verification (ICV): The quality control standard is the initial calibration
verification solution (ICV), which must be prepared in the same acid matrix as the
calibration standards. This solution must be an independent standard at approximately half
(or less than) of the concentration of the high standard used for instrument calibration. An
independent standard is defined as a standard composed of the analytes from a source
different from those used in the standards for instrument calibration.
8.1.6 Reporting Limit Verification Standard (RLVS / CRDL): With every Initial Calibration, a
standard corresponding to the Pace reporting limit (PRL), or lower, must also be analyzed
and meet established acceptance criteria. The RLVS is analyzed prior to any samples
being analyzed. It is also analyzed at the end of the analytical sequence when following
6020B quality control samples (LOD sets and DOC sets) or by client request. Additional
RLVSs may be analyzed throughout the analytical sequence at the analyst's discretion.
These standards are the first calibration point for the analytes of interest. The analysis of
this standard demonstrates the instruments ability to report down to the reporting limit with
known accuracy.
8.1.7 ICS LDR 1, 2, and 3: These standards are analyzed to establish the linear range with each
calibration. The set is essentially all of the major cations in 3 separate standards since
combining all of them in one standard would cause problems with the internal standard
recoveries due to the total amount of dissolved solids present. It is known that the single
element Al and Ca standards contain a background of Sr above the first calibration point at
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
n ..r A

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
the concentrations used and is not a polyatomic interference that requires a correction
equation. The control limit for Sr in these 2 standards (LDR 1 & 2) is < RL above the mean
background concentration.
8.1.8 Interference Check Solutions (ICSA and ICSAB): The ICSA and ICSAB are prepared to
contain known concentrations of interfering elements that will demonstrate the magnitude
of interferences and provide an adequate test of any corrections. The ICSA and ICSAB are
analyzed prior to any samples. They are also analyzed at the end of the analytical
sequence by client request. Chloride in the ICS provides a means to evaluate software
corrections for chloride-related interferences such as 35CI 160 on 51V. Iron is used to
demonstrate adequate resolution of the spectrometer for the determination of manganese.
Molybdenum serves to indicate oxide effects on cadmium isotopes. The other components
are present to evaluate the ability of the measurement system to correct for various
polyatomic isobaric interferences. The ICS is used to verify that the interference levels are
corrected by the data system to within quality control limits. Table D provides a summary
of the ICS-A and ICS-AB solution concentrations used.
8.1.9 Continuing Calibration Verification (CCV): This standard is near (or less than)the midpoint
of the curve and used to verify that the instrument is still in calibration. This standard is
from the same source as the calibration standards.
8.2 Reagents: Please see Table 8.4 for a list of reagents.
8.2.1 All standards, reagents, and spiking solutions are kept at room temperature. Stock
standards and reagents can be used until they expire. Refer to the most recent version of
ENV-SOP-GBAY-00145 Laboratory Supply Procedures for stock standard and reagent
expiration rules. Intermediate and working standards are given a six-month expiration date.
However, the expiration date may not extend past the earliest expiration date of any stock
standard used to create the solution. The use of any standard or reagent will be terminated
if any contamination or problems arise prior to the expiration date.
8.3 Log-in of Standards, reagents, and spike solutions are logged as follows:
8.3.1 Stock standards have a copy of their certificate of analysis logged into the LIMS (Epic Pro).
Please see the SOP T-ALL-IT-010 (most recent revision or equivalent).
8.3.2 Reagents are logged in the same manner.
8.4 Reagents
Purchased Catalog Concentration/ Expiration Storage
Reagent* Alias From* Number* Purity*
Reagent Water Water In House NA >_18 Mega ohm Generated for use
Hydrochloric Acid HCI Fischer A508-P212 Trace Metal Manufacturer's
Scientific Grade 34-37% recommended
Nitric Acid HNO3 Fischer A509-P212 Trace Metal expiration date or 2 Room
Scientific Grade 67-70%, years from Temp
ACS receipt/made date,
Hydrogen H202 Fischer H325-4 Trace Metals whichever is sooner
Peroxide Scientific Grade 30%
*Or equivalent
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
Innfd9

'ace Analytical
i
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV-Green Bay Quality-GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
8.5 Stock Standards
Standard Type Manufacturer Part# Conc. Analyte Used In Exp.
200 mg/L As,Ba,Be,Cd,Co,Cr,Cs,Cu,Li,
SPEX CertiPrep XPACEMN-76 Mn,Ni,Pb,Se,Sr, U,V,Zn
100 mg/L Ag,TI
SPEX CertiPrep XPACEMN-77 200 mg/L B,Mo, Pd, Pt,Sb,Sn,Ti,Zr
1,000 mg/L AI,Ca, K,Mg,Na,S
SPEX CertiPrep XPACEMN-75 500 mg/L Fe,P,Si
SPEX CertiPrep PLB9-2Y 1,000 mg/L B
Calibration SPEX CertiPrep PLCA2-2Y 10,000 mg/L Ca
Stocks SPEX CertiPrep PLFE2-2Y 10,000 mg/L Fe ICAL,
SPEX CertiPrep PLK2-3Y 10,000 mg/L K CCVs
SPEX CertiPrep PLHG4-2Y 1,000 mq/L Hg
SPEX CertiPrep PLP9-3Y 10,000 mg/L P
SPEX CertiPrep PLSI9-3Y 10,000 mg/L Si
SPEX CertiPrep PLTI-2Y 1,000 mg/L Ti
SPEX CertiPrep PLTL2-2Y 1,000 mg/L TI
SPEX CertiPrep PLZN2-2Y 1,000 mg/L
g Zn
High Purity Standards 100063-3-100 1,000 mg/L W
High Purity Standards HP7375-500 1,000 mg/L AI,Ca,K,Mg, Na,S
500 mg/L Fe,P,Si
High Purity Standards HP7376-500 200 mg/L B,Mo,Pd, Pt,Sb,Sn,Ti,Zr
200 mg/L As,Ba,Be,Cd,Co, Cr,Cs,Cu,Li,
High Purity Standards HP7379-500 Mn,Ni,Pb,Se,Sr,U,V,Zn
ICV/Spike 100 mg/L Ag,TI ICV/
Stocks HP100033- Spike
High Purity Standards 1100 1000 mg/L Hg
Agilent ICP-126 10,000 mg/L Fe 1
Agilent ICP-115 10,000 mg/L P
Agilent 5190-8450 10,000 mg/L Si
Agilent ICP-081 1,000 mg/L TI
Internal Environmental Express HP-ICP-MS- ISTD,
Standard Stocks IS-3-500 10 ug/mL Li6,Bi,Ge, In,Sc,Tb,Y Tune
Agilent ICP-112 10,000 mg/L Mg Tune/Int
Agilent ICP-056 1,000 mg/L Ba Tune
Aqilent ICP-005 1,000 mg/L B Tune
Agilent ICP-004 1,000 mg/L Be Tune
Agilent ICP-058 1,000 mg/L Ce Tune
Agilent ICP-027 1,000 mg/L Co Tune
Single Element Inorganic Ventures CGLI10-5 10,000 mg/L _Li Tune
Stocks Aqilent ICP-028 _ 1,000 mg/L Ni Tune
Agilent ICP-082 1,000 mg/L Pb Tune
Agilent ICP-092 1,000 mg/L U Tune
Agilent ICP-055 1,000 mg/L _ Cs MDL
Agilent 5190-8547 1,000 mg/L W ICV/
Spike
High Purity Standards 100033-1 1,000 mg/L Hg ICV/
Spike
1,000 pg/mL AI,Ca, Fe,K,Mg,Na,P,S
ICSA High Purity Standards HP7311-500 2 000 Ng/mL C ICSA&
10,000 pg/mL CI ICSAB
20 pg/mL _ Mo,Ti
Note: Equivalent substitutes may be used.
Note:Single element standards may be used.
1.Not to exceed manufacturers specifications.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
8.6 Intermediate Standards
Intermediate Name Stock Concentration Elements Amount Acid Used Final Volume Final
Type Standard(s) Used (W/Nanopure Concentration
Used(Part#) H20)
3 mL
Mg Tune Int ICP-112 10,000 ppm Mg 0.1 mL HNO3 100 mL 10 ppm
Mg Tune Int 10 ppm Mg 10 mL
HP-ICP-MS-IS- Lib,Bi,Ge,In,
3-500 10 ppm Sc,Tb,Y 10 mL
ICP-056 1,000 ppm Ba 0.1 mL
Tune Solution ICP-005 1,000 ppm B 0.1 mL
Intermediates Tune Int ICP-004 1,000 ppm Be 0.1 mL 2 mL 100 mL 1 ppm ICP-058 1,000 ppm Ce 0.1 mL HNO3
ICP-027 1,000 ppm Co 0.1 mL
CGLI10-5 10,000 ppm Li 0.01 mL
ICP-028 1,000 ppm Ni 0.1 mL
ICP-082 1,000 ppm Pb 0.1 mL
ICP-092 1,000 ppm U 0.1 mL
PLHG4-2Y Hg
3 mL
Hg Int HP1000021- 1,000 ppm Au 0.1 mL HNO3 100 mL 1 ppm
2500 (preservative)
As,Ba,Be,Cd,
200 ppm Co,Cr,Cs,Cu,
XPACEMN-76 Li,Mn,Ni,Pb, 1.25 mL
Se,Sr,U,V,Zn 20 mL 1.25 ppm
T Int 100 ppm Ag,TI HNO3 200 mL 0.625 ppm
B,Mo, Pd,Pt, 10 mL HCI
XPACEMN-77 200 ppm 1.25 mL
Sb,Sn,Ti,Zr
PLTL2-2Y 1000 ppm TI 0.125 mL
100063-3-100 1000 ppm W 0.25
Calibration AI,Ca, K,Mg,
Intermediates XPACEMN-75 1,000 ppm Na,S 50 mL
500 ppm Fe, P,Si
M Int PLFE2-2Y 10,000 ppm Fe 2.5 mL 100 mL 500 ppm
PLP9-3Y 10,000 ppm P 2.5 mL
PLSI9-3Y 10,000 ppm Si 2.5mL 3 mL
PLB9-2Y HNO3
B,Zn INT PLZN2-2Y 1,000 ppm B,Zn 0.225 50 mL 4.5 ppm
K,Ca INT PLK2-3Y 10,000 ppm K,Ca 0.1 mL 50 mL 20 ppm
PLCA2-2Y
Ti INT PLTI-2Y 1,000 ppm Ti 0.05 mL 50 mL 1 ppm
ICV Hg ICV Int HP100033- 1,000 ppm Hg 1.0 mL 1 mL 100 mL 10 ppm
Intermediate 1100 HNO3
5 mL
XCAL Int Li XCAL Int CGLI10 1,000 ppm Li 0.1 mL HNO3 50 mL 20 ppm
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
10 of A')

(/ eAnaIYticaI
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
8.7 Working Standards
Stock or Intermediate Final Volume
Amount Final
Standard Conc. Elements (W/Diluent) Conc. Elements
Standard Used(mL)
Al,As, Ba, Be,Bi,B, Cd,Ca,
Ce,Cs,Cr,Co,Cu, Dy, Er,Eu,
ICP-MS-68A Solution Gd,Ga,Ho, In, Fe,La, Pb, Li,
Cross A Lu, Mg, Mn, Nd, Ni, P,K, Pr, 0.5
Calibration 10 ppm Re,Rb,Sm,Sc,Se, Na,Sr, 100 mL 50 ppb All Elements except Li
(XCal) Tb,TI,Th,Tm, U,V,Yb,Y,Zn Li 100ppb
ICP-MS-68A Solution
B Sb,Ge, Hf, Mo, Nb,Si,Ag,Ta, 0.5
Li XCAL Int 20 ppm Te,Sn,Ti,W,Zr
0.25
—
Tune Solution Tune Int 1 ppm
Mg, Bi,Ge, In,Sc,Tb,Y,Ba, 5 500 mL 10 b
B,Be, Ce, Co, Li,Ni, Pb, U pp All Elements
ICB Same as Cal.Level 0
CCB Same as Cal.Level 0
Calibration Cal 0 --- ---- 50 mL
Level 0 and _
Diluent/Blank Diluent/Blank ---- ---- ---- 1000 mL ----
Solution
Hg Int 1 ppm Hg 0.010 0.2 ppb Hg
As, Ba,Be,Cd, Co,Cr,Cs,Cu,
1.25 ppm Li, Mn,Ni, Pb,Se,Sr, U,V,Zn,
TI,B, Mo, Pd, Pt,Sb, Sn,Ti, 1 ppb All Elements(not Ag)
Calibration T Int Zr,W .04
Level 1 and
RLVS as 0.625 ppm Ag 50 mL 0.50 ppb Ag
applicable(See
Sec.9.1.2) M Int 500 ppm AI,Ca, Fe,K, Mg,Na,Si,P,S 0.010 100 ppb AI, Na, Mg,Si, P,Fe, K,Ca
B,Zn INT 4.5 ppm B,Zn 0.1 9 ppb B,Zn
K,Ca INT 20 ppm K, Ca 0.375 150 ppb K,Ca
Ti INT 1 ppm Ti 0.075 1.5 ppb Ti
Hg Int 1 ppm Hg 0.025 0.5 ppb Hg
As,Ba, Be,Cd,Co,Cr,Cs,Cu,
1.25 ppm Li, Mn, Ni, Pb,Se,Sr,U,V,Zn,
T Int TI, B,Mo, Pd, Pt,Sb,Sn,Ti, 0.2
5 ppb All Elements(not Ag)
Calibration Zr,W
Level 2 0.625 ppm Ag 50 mL 2.5 ppb Ag
M Int 500 ppm Al,Ca, Fe, K,Mg, Na,Si, P,S 0.05 500 ppb AI,Ca, Fe, K, Mg,Na,Si,P,S
B,Zn INT 4.5 ppm B,Zn 0.25 22.5 ppb B,Zn
Ti INT 1 ppm Ti 0.25 5 ppb Ti
Hg Int 1 ppm Hg 0.05 1 ppb Hg
As,Ba,Be,Cd,Co,Cr,Cs,Cu, As, Ba,Be,Cd,Co,Cr,Cs, Cu,
Li,Mn,Ni, Pb,Se,Sr,U,V,Zn,
Li, Mn,Ni, Pb, Se,Sr, U,V,Zn,
1.25 ppmT Int TI,B,Mo, Pd,Pt,Sb, Sn,Ti, 2.0 50 ppb TI B, Mo, Pd,Pt,Sb,Sn,Ti,Zr,
Calibration Zr,W W
Level 3 0.625 ppm Ag 50 mL 25 ppb Ag
M Int 500 ppm Al,Ca, Fe, K,Mg, Na,Si, P,S 0.25 2,500 ppb Al,Ca, Fe, K, Mg,Na
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

79ceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Stock or Intermediate Amount Final Volume Final
Standard Standard Conc. Elements Used(mL) (W/Diluent) Conc. Elements
Hg Int 1 ppm Hg 0.5 10 ppb Hg
As, Ba,Be, Cd,Co,Cr,Cs,Cu, As, Ba, Be, Cd, Co, Cr, Cs, Cu,
1.25 ppm Li, Mn, Ni, Pb,Se,Sr, U,V,Zn, Li, Mn, Ni, Pb, Se, Sr, U, V, Zn,
TI,B,Mo,Pd,Pt,Sb,Sn,Ti,Zr, 250 ppb
Calibration T Int W 10 50 mL TI, B, Mo, Pd, Pt, Sb, Sn, Ti, Zr,
W
Level 4
0.625 ppm Ag 125 ppb Ag
M Int 500 ppm Al,Ca,Fe,K,Mg,Na,Si,P,S 1.25 1 ppb0 Al,Ca,Fe,K,Mg,Na,Si,P,S
Hg Int 1 ppm Hg 1.25 25 ppb Hg
As, Ba,Be, Cd,Co,Cr,Cs,Cu, As, Ba, Be, Cd, Co, Cr, Cs, Cu,
Li, Mn, Ni,Pb,Se,Sr, U,V,Zn, 500ppb Li, Mn, Ni, Pb, Se, Sr, U, V, Zn,
1.25 ppm TI,B,Mo,Pd,Pt,Sb,Sn,Ti,Zr, TI, B, Mo, Pd, Pt, Sb, Sn, Ti, Zr,
Calibration T Int W 20 50 mL W
Level 5
0.625 ppm Ag 250 ppb Ag
M Int 500 ppm Al,Ca, Fe,K,Mg,Na,Si,P,S 5.0 5p'pb0 Al,Ca, Fe, K,Mg,Na,Si,P,S
Hg Int 1 ppm Hg 0.25 5 ppb Hg
As, Ba,Be, Cd,Co,Cr,Cs,Cu, As, Ba, Be, Cd, Co, Cr, Cs, Cu,
Li, Mn, Ni,Pb,Se,Sr, U,V,Zn, 200 b Li, Mn, Ni, Pb, Se, Sr, U, V, Zn,
T Int 1.25 ppm TI,B,Mo,Pd,Pt,Sb,Sn,Ti,Zr, pp TI, B, Mo, Pd, Pt, Sb, Sn, Ti, Zr,
CCV W 16 100 mL W
0.625 ppm Ag 100 ppb Ag
M Int 500 ppm Al,Ca,Fe,K,Mg,Na.Si,P,S 2.0 1 Ppbo AI,Ca, Fe,K,Mg,Na,Si,P,S
High Purity Standards 1000 ppm AI,Ca,K,Mg,Na,S 3.1 15500 ppb Al,Ca,K,Mg, Na,S
500 ppm Fe,P,Si 7750 ppb Fe,P,Si
High Purity Standards 200 ppm B,Mo,Pd,Pt,Sb,Sn,Ti,Zr 0.15 150 ppb B, Mo,Pd,Pt,Sb,Sn,Ti,Zr
As, Ba, Be, Cd, Co, Cr, Cu, Li, As, Ba, Be, Cd, Co, Cr, Cu, Li,
High Purity Standards 200 ppm Mo,Ni,Pb,Se,Sr, U,V,Zn 0.15 150 ppb Mo,Ni, Pb,Se,Sr,U,V,Zn
ICV 100 ppm Ag,TI 200 mL 75 ppb Ag,TI
Agilent 10000 ppm Si 0.155 7750 ppb Si
Agilent 10000 ppm P 0.155 7750 ppb P
Agilent 10000 ppm Fe 0.155 7750 ppb Fe
Agilent 1000 ppm TI 0.155 75 ppb TI
Agilent 1000 ppm W 0.03 150 ppb W
Hg ICV Int 10 ppm Hg 0.08 4 ppb Hg
1000 ppm AI,Ca,Fe,K,Mg,Na,P,S 50 ppm Al,Ca,Fe,K,Mg,Na,P,S
2000 ppm C 5.0 100 ppm C
High Purity Standards 10000 ppm CI 500 ppm CI
20 ppm Mo,Ti 1 ppm Mo,Ti
Agilent 10000 ppm Na 2 200 ppm Na
ICSA(6020B Agilent 10000 ppm Mg 0.5 50 ppm Mg
LDR) Agilent 10000 ppm Al 0.5 100 mL 50 ppm Al
Agilent 10000 ppm Si 1 100 ppm Si
Agilent 10000 ppm P 1 100 ppm P
Agilent 10000 ppm K 1 100 ppm K
Agilent 10000 ppm Ca 2 200 ppm Ca
Agilent 10000 ppm Fe 1 100 ppm Fe
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Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
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4 A ..F A')

.ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Standard Stock Standard Conc. Elements Amount Final Volume Final Elements
Used(mL) (W/Diluent) Conc.
1000 ppm Al,Ca, Fe,K, Mg,Na,P,S 50 ppm Al,Ca, Fe,K, Mg,Na,P,S i
High Purity Standards 2000 ppm C 5.0 100 ppm C
10000 ppm CI
500 ppm CI
20 ppm Mo,Ti 1 ppm Mo,Ti
Agilent 10000 ppm Na 2 200 ppm Na
Agilent 10000 ppm Mg 0.5 50 ppm Mg
Agilent 10000 ppm Al 0.5 50 ppm Al
Agilent 10000 ppm Si 1 100 ppm Si
ICSAB(6020B
LDR) Agilent 10000 ppm P 1 100 mL 100 ppm P
Agilent 10000 ppm K 1 100 ppm K
Agilent 10000 ppm Ca 2 200 ppm Ca
Agilent 10000 ppm Fe 1 100 ppm Fe
Agilent 1000 ppm W 0.005 50 ppb W
High Purity Standards 200 ppm B,Mo,Pd, Pt,Sb,Sn,Ti,Zr B,Mo,Pd,Pt,Sb,Sn,Ti,Zr
200 m As, Ba, Be, Cd, Co, Cr, Cu, Li, 50 ppb As, Ba, Be, Cd, Co, Cr, Cu, Li,
pp Mo,Ni, Pb,Se,Sr,U,V,Zn 0.025 Mo, Ni,Pb,Se,Sr,U,V,Zn
High Purity Standards 100 ppm Ag,TI 25 ppb Ag,TI
1 ppm Hg 0.50 5 ppb Hg
Biota SPKB, 200 m As, Ba, Be, Cd,Co,Cr,Cs,Cu, As, Ba, Be, Cd, Co, Cr, Cs, Cu,
Biota SPKB3, HP7379-500 pp Li,Mn,Ni,Pb,Se,Sr, U,V,Zn 10 ppm Li,Mn,Ni,Pb,Se,Sr, U,V,Zn _
Biota SPKB2 100 ppm Ag,Ti 5 5 ppm Ag,TI
(project g
HP7376-500 200 ppm B,Mo,Pd,Pt,Sb,Sn,Ti,Zr _ 10 ppm B, Mo,Pd,Pt,Sb,Sn,Ti,Zr
specific)I 1000 ppm Al,Ca,K,Mg, Na,S 500ppm Al,Ca, K, M Na,S HP7375-500 500 ppm Fe,P,Si 25 g, -
100 mL 250 ppm Fe, P,Si
Agilent 10,000 ppm P 7.5 750 ppm P
Agilent 10,000 ppm K 15 2000 ppm K
Agilent 10,000 ppm Fe 2.5 250 ppm Fe
Agilent 1000 ppm TI 0.5 5 ppm TI
High Purity Standards 1000 ppm Hg 0.025 250 ppm Hg
Conc.HNO3 69-70% HNO3 10.0 10% HNO3
Water/Soil 200 m As, Ba, Be, Cd,Co,Cr,Cs,Cu, As, Ba, Be, Cd, Co, Cr, Cs, Cu,
6000 SPK, HP7379-500 pp Li, Mn, Ni,Pb,Se,Sr,U,V,Zn 12.5 ppm Li,Mn, Ni, Pb,Se,Sr, U,V,Zn
6000 SPK2 2 100 ppm Ag,TI 6.25 6.25 ppm Ag,TI
HP7376-500 200 ppm B, Mo, Pd,Pt,Sb,Sn,Ti,Zr 12.5 ppm B,Mo, Pd, Pt,Sb,Sn,Ti,Zr
1000 ppm Al,Ca, K,Mg, Na,S 50 500 ppm Al,Ca, K,Mg,Na
HP7375-500
500 ppm Fe, P,Si 250 pm Fe, P,Si
HP100033-1100 1,000 ppm Hg 0.025 100 mL 0.25 ppm Hg
ICP-081 1,000 ppm TI 0.625 6.25 ppm TI
ICP-126 10,000 ppm Fe 2.5 250 ppm Fe
ICP-115 10,000 ppm P 2.5 250 ppm P
5190-8450 10,000 ppm Si 2.5 250 ppm Si
5190-8547 1,000 ppm W 1.25 12.5 ppm W
Internal HP-ICP-MS-IS-3-500 10 ppm Li6,Bi,Ge, In,Sc,Tb,Y 20 100 ppb Bi,Ge,In,Sc,Tb,Y,Li6
Standards Conc.HNO3 69-70% NA 60 2000 mL 3% HNO3
(ISTD) HP1000021-2500 1,000ppm Au 4.0 2 ppm Au
HP1000021-2500 1,000ppm Au 2.5 1 ppm Au
Probe Rinse 3 Conc.HNO3 69-70% NA 250 2500 mL 10% HNO3
Conc.HCI 34-37% NA 125 5% HCI
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
e r_ ...e A"

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Al 1 100 ppm
Si 1 100 ppm Matrix Matched ICS LDR 1 Al,
ICS LDR 1 Agilent 10000 ppm K 1.5 150 ppm Ca,Si
HNO3 10 10%
HCI 5 5%
Ca 2.5 250 ppm
ICS LDR 2 Agilent 10000 ppm Fe 1.5 100 mL 150 ppm Matrix Matched ICS LDR 2 Ca,
Fe
HNO3 10 10%
HCI 5 5%
P 1 100 ppm
Mg 1 100 ppm Matrix Matched ICS LDR 3 P,
ICS LDR 3 Agilent 10000 ppm Na 2.5 250 ppm Mg, Na
HNO3 10 10%
HCI 5 5%
Note:Equivalent substitutes may be used.
Note:Spikes may be altered as a result of client specific requirements.
Note:Final mixes used may be altered due to mix compatibility and stability.
1 =1 mL added to LCS/LCSD and MS/MSD
2=1 mL added to LCS/LCSD and MS/MSD,(0.5 mL for Aqueous Digest),0.2 mL to PS of 10 mL
3=All on instrument Matrices contain 10%HNO3 and 5%HCI
9.0 PROCEDURE
9.1 Calibration and Standardization: The instrument is calibrated daily at a minimum when
analyzing samples. High solids and complex matrices can and do result in more frequent
calibration.
9.1.1 Calibration Curve: Demonstration and documentation of acceptable initial calibration is
required before any samples are analyzed and is required periodically throughout sample
analysis as dictated by the results of the continuing calibration verification standards.
Calibration consists of a calibration blank and four or five non-zero standards (analyte
dependent) analyzed after a calibration blank. The ICPMS software creates a curve based
on this data which is linear regression using Absolute Standard Deviation weighting
inclusive of the calibration blank with a calculated intercept and uses the following equation:
Y=a(x)+b. In calculating x (concentration)from y (response)the b (intercept) is subtracted.
The b represents the intercept of the regression line. The correlation coefficient must be
4.998. If the correlation coefficient is not within criteria, the issue must be resolved, and
the instrument recalibrated with passing criteria prior to analyzing samples. To satisfy
6020B calibration criteria the following must be met. The calculated concentration for the
lowest calibration point used must have a recovery of+/-20% (i.e. a relative error of<_20%).
The calculated concentration midpoint calibration standard must have a recovery of+/-10%
(i.e. a relative error of 510%). The calculated concentration highpoint calibration standard
must have a recovery of+/-10% (i.e. a relative error of<_10%)for LDR in 6020B.
9.1.2 Calibration Levels: Please see Table Below for directions on making the calibration
standards and the calibration levels used in the calculations.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
is ..f AO

'aceAnalytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Element Cal 0 Calibration Standard 1 Calibration Calibration Calibration Calibration
Blank and RLVS as applicable Standard Standard 3 Standard 4 Standard 5
Aluminum 0 ppb 100 ppb 500 ppb 2,500 ppb 12,500 ppb 50,000 ppb
Antimony 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Arsenic 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Barium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Beryllium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Boron 0 ppb 10 ppb 27.5 ppb 50 ppb 250 ppb 500 ppb
Cadmium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Calcium 0 ppb 250 ppb 500 ppb 2,500 ppb 12,500 ppb 50,000 ppb
Cesium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Chromium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb _ 500 ppb
Cobalt 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Copper 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb _ 500 ppb
Iron 0 ppb 100 ppb 500ppb 2,500 ppb 12,500 ppb 50,000 ppb
Lithium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Lead 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Magnesium 0 ppb 100 ppb 500 ppb 2,500 ppb 12,500 ppb 50,000 ppb
Manganese 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Mercury 0 ppb 0.2 ppb 0.5 ppb 1.0 ppb 10 ppb _ 25 ppb
Molybdenum 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Nickel 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Palladium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Phosphorus 0 ppb 100 ppb 500 ppb 2500 ppb 12500 ppb 50,000 ppb
Platinum 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Potassium 0 ppb 250 ppb 500 ppb 2,500 ppb 12,500 ppb 50,000 ppb
Selenium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Silicon 0 ppb 100 ppb 500 ppb 2500 ppb 12500 ppb 50,000 ppb
Silver 0 ppb 0.5 ppb 2.5 ppb 25 ppb 125 ppb 250 ppb
Sodium 0 ppb 100 ppb 500 ppb 2,500 ppb 12,500 ppb 50,000 ppb
Strontium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Thallium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Tin 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Titanium 0 ppb 2.5 ppb 10 ppb 50 ppb 250 ppb 500 ppb
Tungsten 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Uranium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Vanadium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Zinc 0 ppb 10 ppb 27.5 ppb 50 ppb 250 ppb 500 ppb
Zirconium 0 ppb 1 ppb 5 ppb 50 ppb 250 ppb 500 ppb
Internal
Standards, 50 ppb each 50 ppb each 50 ppb each 50 ppb each 50 ppb each 50 ppb each
Note: Calibration levels may change if noted. All solutions in 10% HNO3 and 5%HCI. Sulphur is contained in the Primary solutions but are
not quantified analytically.
1 =The Internal Standard Concentration is a result of a 2X Dilution via a T adapter in the delivery lines to the nebulizer.
9.1.3 Internal Standards:
9.1.3.1 Internal standardization must be used in all analyses to correct for instrument
drift and physical interferences. For full mass range scans, a minimum of six
internal standards must be used. Procedures described in this SOP for general
applications detail the use of seven internal standards; 6Li, 45Sc-CCT, 45Sc-KED,
72Ge, 89Y, 115ln, 159Tb, and 209Bi. The interpolation between 2 internal standards
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
17nfA')

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
is done when a reported element mass is bracketed by two internal standards.
See Table below for a list of acceptable internal standards and their
suggested associated elements. (Multiple listing indicates interpolation
between the surrounding Internal Standards):
ISTD Analytes
6L1 Li, Be, B
45Sc-KED 72Ge Na— Zn
72Ge 89Y As— Sr
89Y 115ln Me— Cd
115In 159Tb Sn—Ba
159Tb 209Bi Hg—Pb
209Bi U
9.1.3.2 Internal standards must be present in all samples, standards, and blanks at
identical levels. This is achieved by directly adding the internal standard stock
solution (100ppb in 3% HNO3) to all samples, standards, and blanks by on-line
addition prior to nebulization using a second channel of the peristaltic pump and
a mixing T-connector. The concentration of the internal standard should be
sufficiently high that good precision is obtained in the measurement of the
isotope used for data correction and to minimize the possibility of correction
errors if the internal standard is naturally present in the sample. A final
concentration at the nebulizer of approximately 50 ppb will result from the
addition of a 100 ppb solution.
9.1.3.3 Due to matrix interferences one or more of the internal standards may not be
suitable. It is up to the analyst to recognize and correct the problem by diluting
the sample(s) for reanalysis. This procedure may result in some analytes being
diluted below the PRL and must be appropriately flagged.
9.1.3.4 During the determination, the software uses the ratio of analyte and internal
standard intensities to adjust the final concentration values. Ratios are based on
the intensities in the sample vs. the calibration blank intensities.
9.1.3.5 An internal standard without Li must be used if Li is an analyte of interest. If Li is
to be used as an internal standard, and Li is an analyte of interest, an isotopically
enriched Li standard must be used such that the analyte can be differentiated
from the internal standard. (i.e. 6Li enriched internal standard to report 7Li in
samples.)
9.1.4 Interference Calculations: Interference equations are used to correct for isobaric elemental
and polyatomic interferences. All equations can be adjusted if necessary or added if the
analyst determines that any particular correction is insufficient or if an equation is over
correcting the data. The Equations Table below shows the recommended Elemental
Interference Equations.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
A(1 -t .1 1

eAnaIicaI®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV-Green Bay Quality-GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Recommended Elemental Recommended Elemental
Analyte Interference Equations Analyte Interference Equations
6Li -0.03531*7Li 72Ge -0.00015*54Fe
43Ca 2 -0.00135*88Sr 75As -0.00001*59Co
45Sc-KED3 -0.0399*31P 78Se -0.03065*83Kr
0.00025*90Zr
0.00355*27Si 90Zr -0.00154*73Ge
47Ti3 -0.00030*90Zr 95Mo3 -0.00027*90Zr
-0.00162*31 P
-0.00001 *95Mo
51U1 -2.0995*53CIO 107Ag3 -0.00055* 105Pd
-0.00061 *90Zr
53C10 -0.11400*52Cr 111Cd3 -0.00020*105Pd
-0.00025*95Mo
-0.00003*90Zr
52Cri -0.00015*35CI 1151n -0.01416*118Sn
55Mn -0.00020*54Fe 121Sb -0.00025*118Sn
54Fe -0.03613*52Cr 137Ba -0.00008*121Sb
59Co -0.00010*54Fe 201Hg -0.00055* 184W
60Ni -0.00020*43Ca 208Pb 1.00000*206Pb+ 1.00000*207Pb
-0.00059*59C0
-0.00001 *54Fe
-0.00005*118Sn
63Cu -0.00010*60Ni 209Bi -0.00135*195Pt
66Zn -0.00005*54Fe
-0.00030*137Ba
1 -The equation may require periodic adjustment based on the KED add gas and tuning
parameters. The mean value in counts per second (cps)for the calibration blank MUST be
> 0 cps (ideally, all replicates should be > 0 cps). The normal operating range in cps is 0- 1
1000cps for the calibration blank and must be inspected by the analyst.
2-The ICSA/AB and the LCS sample are used in the evaluation of this equation. Ca is
affected by doubly charged strontium and can vary from day to day plasma conditions. The
ICSA&AB will not fully identify doubly charged conditions based on the ratio of Ca to Sr,
whereas the LCS sample for waters and soils have sufficiently large Sr concentrations
compared to Ca and will assist in identification of adjustment requirements for the Ca
interference equation.
3-Zirconium must be less than the previously established linear dynamic range (LDR) of
10,000 pg/L on instrument for proper correction of polyatomic and doubly charged
interferences.
9.1.5 Acquisition Mode:
Points per Mass: 1
Number Replicates: 3
Dwell Time: 10 ms for all elements except Na, As, Se, Kr; 5 ms for
Na, and 50 ms for As, Se, Kr.
9.1.6 Example Peristaltic Pump Program:
Uptake time: 20 sec
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
1Qnfd7

ace Analytical°
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Neb Settle Time: 20 sec
Stabilization Time (KED Changeover): 40 sec
Acquisition masses and Dwell times can be found in Table Below.
Mass Element Resolution Dwell Time Per Mass Element Resolution Dwell Time Per
Mode Mass (mSec) Mode Mass(mSec)
6 Li Standard 10 78 Se Standard 50
7 Li Standard 10 83 Kr Standard 50
9 Be Standard 10 89 Y Standard 10
10 B Standard 10 95 Mo Standard 10
23 Na High 5 105 Pd Standard 10
25 Mg Standard 10 107 Ag Standard 10
27 Al Standard 10 111 Cd Standard 10
28 Si Standard 10 115 In Standard 10
31 P Standard 10 118 Sn Standard 10
34 S High 10 121 Sb Standard 10
35 CI High 10 133 Cs Standard 10
39 K High 10 137 Ba Standard 10
43 Ca Standard 10 159 Tb Standard 10
45 Sc-KED Standard 10 182 W Standard 10
184 W Standard 10
47 Ti Standard 10 195 Pt Standard 10
47 V Standard 10 201 Hg Standard 10
51 Cr Standard 10 205 TI Standard 10
52 Fe Standard 10 206 Pb Standard 10
54 Mn Standard 10 207 Pb Standard 10
55 Co Standard 10 208 Pb Standard 10
59 Ni Standard 10 209 Bi Standard 10
60 Cu Standard 10 238 U Standard 10
63 Zn Standard 10 209 Bi Standard 10
66 Ge Standard 10 238 U Standard 10
75 As Standard 50
9.2 Analytical Procedure:
9.2.1 Solubilization and digestion procedures are in the Metals Digestion SOPs (e.g. Methods
200.8, 3010A and 3050B for both Solids and Biota).
9.2.2 Instrument Startup:
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

aceAnalytical0
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
9.2.2.1 Verify argon supply and pressure.
9.2.2.2 Turn on water chiller and exhaust fan.
9.2.2.3 Ensure that the internal standard solution bottle is adequately full.
9.2.2.4 Verify contents of auto-sampler rinse port reservoir.
9.2.2.5 Empty the waste reservoir.
9.2.2.6 Ignite the plasma and allow at least 25 minutes of warm-up. The tuning
procedures may then be carried out.
9.2.2.7 Ensure that all peristaltic pump tubes are in good condition and correctly
clamped into the peristaltic pumps. Verify that the flow of sample and internal
standard solutions through the uptake lines and into the nebulizer are free from
extreme pulsations by introducing a bubble into each line and observing its
progress.
9.2.3 Mass Tuning: Allow 25 minutes for the Instrument to achieve thermal stability. Aspirate the
10ppb Tuning Solution by inserting both the sample and internal standard delivery lines into
the tune solution, so as not to dilute the tune solution. Run each of the following
performance reports, print the passing report, and save the mode by month, day, year (no
commas) into the configurations list by type (e.g. Standard Mode 01152021, CCT Mode
01152021, and CCTKED Mode 01152021).
9.2.3.1 EPA Performance Report (Xt Standard Mode)
9.2.3.1.1 Mass Resolution (10 Sweeps, 5 Reps)
Acquisition Parameters: Peak width measured at 5% peak
maximum.
Dwell Time (mSec): 10
Point Spacing: 0.05amu
Mass Limits: 0.65—0.85 amu (Max error 0.10 amu)
Defined Masses: 24Mg, 25Mg, 26Mg, 206Pb, 207Pb, 208Pb
9.2.3.1.2 Sensitivity and Stability(35 Sweeps, 5 Reps)
Mass: Dwell (mSec): %RSD: Counts
(NA=Not Applicable)
5Bkg 500.0: NA: <1
7Li 10.0: 2.0 : >60,000
24Mg 10.0 : 2.0 : >10,000
25Mg 10.0 : 2.0 : >10,000
26Mg 10.0 : 2.0 : >10,000
59Co 10.0 : 2.0 : >150,000
137Ba++ 10.0 : NA : NA
1151 n 10.0 : 2.0 : >400,000
137Ba 10.0 : NA : NA
138Ba 10.0 : NA : NA
1400e 10.0 : NA : NA
156CeO 100.0 : NA: NA
206Pb 10.0 : 2.0 : >10,000
207Pb 10.0 : 2.0 : >10,000
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use. 1
91 nfd7

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
208Pb 10.0 : 2.0 : >10,000
220Bkg 500.0 : NA : <1
238U 10.0 : 2.0 : >800,000
9.2.3.1.30xides and Doubly Charged (Ratio Results).
137Ba++/137Ba: <0.0300
156Ce0/140Ce: <0.0200
9.2.3.2 CCT Performance Report (Xt CCT).
Sensitivity and Stability (35 Sweeps, 5 Reps)
Acquisition Parameters: Mass: Dwell (mSec) : %RSD : Counts
7Li 10.0: 2.0: >10,000
'Be 10.0: 2.0: >2,000
11B 10.0: 2.0: >2,000
9.2.3.3 KED Performance Report (Xt CCT-KED)
9.2.3.3.1 Sensitivity and Stability (35 Sweeps, 5 Reps)
Acquisition Parameters: Mass: Dwell (mSec): %RSD: Counts
78Se 100.0: NA: <20
1151n 10.0: 2.0: >100,000
140Ce 10.0: NA: NA
156Ce0 50.0: NA: NA
9.2.3.3.2Ratio Results
156Ce0/140Ce <0.0200
9.2.3.4 The Xcal solution does not need to be run unless a deviation between the pulse
counting and analog counting methods is observed in the spectra. The analog
counting will appear to sit significantly above the pulse baseline in an observed
spectra from the scan acquisition and indicates that the cross calibration needs
to be performed. Also, an indication of when the Xcal needs to be reset is when
the calibration loses its linearity (this will likely occur first with High Resolution
Mineral elements like Na and K or high concentration elements like Fe. A
deviation can also be observed for the heavy elements TI, Pb, and U). Aspirate
the Xcal solution in Standard Mode, with both the sample delivery and internal
standard lines (so as to not dilute the Xcal solution).
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
nn _r nn

eAnaIicaI®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
9.2.3.4.1 Cross Calibration Only. This is done when the deviation between
the pulse and analog counting methods is observed (from spectra or
from linearity observations) and the minimum counts per second
listed in the tuning section are achievable. Run the Instrument
Calibration wizard in PlasmaLab when deviation of the analog
spectra is observed. The detector cross calibration is selected by
default in the wizard. This will reset the detector-gating plateau
such that the analog spectra (dashed line in the spectra) will sit
directly on top of the pulse baseline (solid line in the spectra).
9.2.3.4.2 Detector Setup and Cross Calibration. This is done when the
minimum counts per second listed in the tune section are not
achievable. Thus, the detector dynode value will be adjusted, and a
new cross calibration will be performed with the new detector
voltage setting. Launch the Instrument Calibration wizard in
PlasmaLab and select detector set up. The detector cross
calibration will be checked by default, also select the detector set up
portion in the wizard. The voltage applied to the detector will be set
first to achieve acceptable sensitivity followed by a detector cross
calibration with the new detector setting.
9.2.3.4.3 Dead Time Experiment: This experiment must be and is only
performed after a detector is replaced. The dead time experiment
will identify the delay or "dead time" associated with a particular
detector. The dead time is the delay between the pulse
measurement and analog measurement when the detector gate is
dropped. In the experiment a 1 ppb and 10ppb solution of Uranium
is run, and the ratios between 235U and 238U are calculated for both
concentrations. The values for the ratios are adjusted such that the
ratio values are as close to identical as possible and that value
(dead time in nanoseconds) is entered into PlasmaLab software via
the Advanced Page.
9.2.3.5 Tune Procedure Summary (Use this order of events, some adjustments may be
required after an auto tune). Save each passing configuration with the Mode
followed by the Date (e.g. Standard Mode, CCT Mode, and KED Mode
09052020). The tunes for passing performance reports are valid for 36 hours.
Introduce the internal standard and aspirate a new rinse blank for 5-10 minutes
to eliminate any carry-over into the calibration blank.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
9'1 of a9

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
9.2.3.5.1 Torch Box Alignment
9.2.3.5.2 Xt Standard Mode Autotune or X Series II Factory auto tune, or
manually adjust the previous standard mode settings.
9.2.3.5.3 Detector X Calibration
9.2.3.5.4 Mass Calibration
9.2.3.5.5 EPA Performance Report
9.2.3.5.6 XT CCT Mode Auto tune
9.2.3.5.7 XT CCT Mode Performance Report
9.2.3.5.8 XT CCT/KED Auto tune
9.2.3.5.9 XT CCT/KED Performance Report
9.2.4 Automated Calibration, Quality Control and Sample Analysis:
9.2.4.1 Prepare calibration standards, blanks, spikes, samples, and QC samples.
Directions to make up the standards can be found in Tables 8.6 and 8.7.
9.2.4.2 Build a sequence in the sequence table and apply the repeat run rules to insert
the CCV and CCB for every 10 unknowns. A typical sequence will consist of a
calibration blank and calibration points 0 through 5, followed by an ICV, ICB,
CRDL, ICSA, ICSAB, CCV, CCB and then batch samples and QC. The repeat
rules set above will insert a CCV, CCB combo every 10 analyses and at the end
of the sequence.
9.2.4.3 Ensure the RLVS / CRDL standard bracket the sample list for analysis by 6020B
for LOD and DOC analysis. The bracketing check may be by Client specific
criteria and refer to any applicable requirements if there is uncertainty.
9.2.4.4 When the sample list and QC checks have been verified for accuracy, queue the
experiment to the Technician Queue. Each experiment will require a unique
code (e.g. 0905220A, 0905220B, for 401CM2, and add _3 after the name for
401CM3, etc.).
9.2.4.5 Expected values and limits for ICV, CCV, ICS LDR (1,2,&3), ICS-A, and ICS-AB
can be found in Attachment II.
10.0 DATA ANALYSIS AND CALCULATIONS
10.1 The Plasma Lab software performs all calculations necessary to convert raw counts per second
data into quantitative concentration results.
10.2 Consideration should be given to the interference equations that are in the method. As a result
of changing tune parameters over time, the equations may require adjustment periodically to
ensure they are not overcompensating or under compensating for the polyatomic or isobaric
interferences. This is especially true of 52Cr and 51V as the CCT-KED tune can vary slightly from
day to day operation. This variation (primarily in the add gas for the collision cell) will change
the counts per second acquired for CI and CIO ions. This can make the counts per second in
the calibration blank for these isotopes artificially high or low (See Section 9.1.4). In the case
of Lead, quantitation is based on the sum of isotopes 206, 207, and 208 to compensate for any
variation in naturally occurring isotope ratios. This is accomplished through the use of the
interference correction equation for lead.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
.r nn

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
10.3 Liquid Calculation
Raw Data Value (ug/L)x DF x VF = Final Result (pg/L)
Vi
Where:
DF = Dilution Factor
VF = Final Volume (L)
Vi = Initial Sample Volume (L)
10.4 Soil Calculation
Raw Data result(uq/L) * DF * VF = Final Result (mg/kg dry weight)
Ws X%S
Where:
DF = Dilution Factor
VF = Final Volume (L)
Vi = Initial Sample Volume (L)
Ws = Sample weight (grams)
%S = Percent solids/ 100
Example: For a sample that is 97.6% solid use 0.976
10.5 Biota Sample Calculation:
Raw Data result (ug/L) * DF * VF = Final Result (mg/kg)
Ws
Where:
DF = Dilution Factor
VF = Final Volume (L)
Vi = Initial Sample Volume (L)
Ws= Sample weight(grams)
NOTE: Results for biological samples are routinely reported on an "as is" or wet weight basis. Dry
weight correction is available on request when sufficient sample has been provided.
10.6 Hardness as CaCO3 in mg/L = 2.497 * [Ca in mg/L] + 4.118 * [Mg in mg/L]
10.7 Silica (Si02) (pg/L) = Silicon (Si) (pg/L) * DF * 60.09 amu (SiO2 molecular weight) / 28.09 amu
(Si atomic weight)
Where: DF is the sample Dilution Factor
10.8 Relative Standard Error:
(Standard Readback after Linear Regression (Cal 1 & 4)/ Standard Theoretical) / * 100% =
Relative Standard Error
Cal 1 must be 80-120%
Cal 2 & 3 must be 85-115%
Cal 4 & 5 must be 90-110% (Cal5 for 6020B LDR purposes).
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
7F l,f A')

0
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
11.0 QUALITY CONTROL AND METHOD PERFORMANCE
11.1 Quality Control: There are three levels of quality control utilized in this SOP. They consist of
Method QC, Instrument QC, and Prep/Batch QC.
11.2 Method QC consists of the instrument detection limits, linear ranges, method detection limits,
the lower limit quantitation check, and demonstrations of capability. This QC must be
completed prior to analyzing any samples.
11.2.1 Instrument Detection limits (IDLs): IDLs in pg/L are estimated as the mean plus the
average of the standard deviations of the three runs on three non-consecutive days
from the analysis of a reagent blank solution with ten consecutive measurements per
day. Each measurement must be performed as though it were a separate analytical
sample (i.e., each measurement must be followed by a rinse and/or any other
procedure normally performed between the analysis of separate samples). IDLs
must be determined quarterly.
11.2.2 Linear Dynamic Ranges (LDR): The LDR for each element is determined by
analyzing a standard series ending at a concentration expected to be near the high
end of the instruments range. The result must be within ± 10% of the expected
concentration, or a lesser concentration tested until acceptable results are obtained.
This procedure is done with each new instrument to determine the LDR of a
particular model of Instrument and methodology. This is critical to the determination
of any doubly charged, polyatomic and memory interferences. Once established,
6020B methodology will be followed. For 6020B the LDR is verified for each
calibration. If the ICS solutions for the higher concentration elements does not
recover within the 90-110% acceptance range, the high point of the calibration sets
the high end of the instrument working range and is the highest reportable
concentration for that element. The 6020B criteria is more stringent than 200.8 and
will be followed for both methods.
11.2.3 Method Detection Limits (MDLs): Method detection limits, at a minimum, are
obtained by multiplying 3.143 by the standard deviation of seven spikes. The spikes
went through the digestion procedures and were spiked at a concentration suspected
to be within a factor of ten greater than the MDL. The most recent version of the
MDL SOP, S-ALL-Q-004, must be followed when determining MDLs. Note: The MDL
determined by the MDL study is the theoretical MDL. The MDL used for reporting
purposes may be higher than the theoretical MDL.
11.2.4 Lower Limit of Quantitation Check Standard (LLOQ): The LLOQ is a standard at the
reporting limit concentration that has gone through all the preparation procedures.
For the purposes of 6020B, the acceptance criteria is ± 35% for the LLOQ sample.
The Percent RSD for the acquired LLOQ replicates should be <_ 20%. It is analyzed
to establish the lower limit of quantitation, verified quarterly using the data from the
LOD studies collected throughout the year, and whenever new limits are established.
If an element repeatedly does not meet criteria at a certain level, it should be re-
evaluated to determine if that level is realistic.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
_rA

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
11.3 Instrument QC: Prior to the analysis of samples, and in some cases during the analysis run,
the following quality control must be generated and within limits: Performance Report for each
mode of operation generated (up to 36 hours since previous or a nonconformance filed when
the window is exceeded), Internal Standards, ICS LDR (1,2,&3), Interference Correction
Solutions A and B (ICSA and ICSAB), Initial Calibration Verification (ICV), Continuing
Calibration Verification (CCV), RLVS / CRDL standards, and Initial and Continuing Calibration
Blanks (ICB and CCB).
11.3.1 The intensities of all internal standards must be monitored for every analysis. When the
intensity of any required internal standard fails to fall between 60 and 125 percent of the
intensity of that internal standard in the blank of the calibration, one of the following
procedures is followed'. The sample is diluted appropriately and reanalyzed with the
addition of appropriate amounts of internal standards. This procedure must be repeated
until the required internal standard intensities fall within the prescribed window. If
significant deviation cannot be overcome by dilution of the sample in the same analytical
run, then recalibration is required. Sudden increases in internal standard recoveries of 10
or more percent may also indicate that dilutions are necessary. The presence of high
levels of dissolved solids in samples can result in instrument drift. A sequence with high
solids samples will have recoveries drift down. Should the internal standards drift outside
of the acceptance range; these samples will need to be re-analyzed at a dilution. If a
subsequent batch is clean (samples with low dissolved solids present) the instrument may
see an increase in signal and internal standard recovery. Unless the internal standards are
actually present in the samples, these can be re-analyzed at the same dilution after a
passing recalibration. 16020B allows for the lower limit of the internal standard recovery to
be set at 30%.
11.3.2 The ICSA, ICSAB, and ICS LDR solutions are used to verify the magnitude of elemental
and molecular-ion isobaric interferences and the adequacy of any corrections. They are
analyzed after the CRDL, prior to the analysis of any samples. For 200.8, additional ICSA
and ICSABs are not analyzed, as sequences do not reach 12 or more hours in duration.
By client request, the ICSA and ICSAB will be analyzed at the end of the analytical
sequence. The analyst should be aware that precipitation from solution AB may occur with
some elements, specifically silver. The control limits for the elements in the ICSA and
ICSAB solutions is 80 to 120% for 200.8 and those elements not being used for linear
range purposes. For 6020B the recovery of the elements with concentrations to establish
the linear range is 90-110% (specifically for Ti and Mo). Elements that are not spiked in the
ICSA, must have a measurement lower than the LOQ. If an element of interest does not
meet these limits, then the problem must be corrected, the instrument recalibrated, and the
run reanalyzed.
11.3.3 The ICV is analyzed to check the accuracy of the curve. It must be evaluated after each
calibration and before any samples are analyzed. The ICV should be at or near (or lower
than) the midpoint of the calibration curve, derived from a source independent of the
calibration standards, and must quantitate within ± 10% of the expected value. If these
limits are not met for an element of interest, the problem must be corrected, the instrument
recalibrated, and the run reanalyzed. If the ICV fails high and the samples are non-detects,
then they may be reported.
11.3.4 Reporting Limit Verification Standard (RLVS / CRDL): With every Initial Calibration, a
standard corresponding to the Pace reporting limit (PRL) or lower than the derived LLOQ
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
97 of A9

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
must also be analyzed and meet established acceptance criteria. The RLVS is analyzed
prior to any samples being analyzed. By client request it will also be analyzed at the end of
the analytical sequence. Additional RLVSs may be analyzed throughout the analytical
sequence at the analyst's discretion. The limits for the RLVS are ± 30% of the true
concentration. These standards are the first calibration standard for the analytes of interest.
The analysis of this standard demonstrates the instruments ability to quantify down to the
reporting limit with known accuracy. If an element fails the CRDL, but the CCV passes and
the samples are greater than the CCV concentration or if the samples are <LOD/ ND, then
the sample data may be reported with the filing of a non-conformance report with the data.
Results >LOD but<CCV must be re-analyzed under passing criteria.
11.3.5 The CCV is analyzed to check for calibration drift. The CCV is run prior to any samples,
after every 10 samples and again at the end of samples. It must quantitate within 10% of
the expected value. Any sample analyzed under out-of-control calibration must be
reanalyzed, following the successful re-calibration of the instrument. If the CCV fails high
and the samples are non-detects, then they may be reported. All others must be re-
analyzed under passing criteria.
11.3.6 The ICB is analyzed to check the accuracy of the curve. The CCBs are analyzed to
check for calibration drift and memory from high concentration samples. In the absence of
Project specificreportinglimits, 1/2the results of the calibration blanks must be less than the
LLOQ (<1/2 the concentration in Cal 1). For the ICB result must be less than one half the
reporting limit (for ease in identifying an issue, reference the first non-zero standard). The
ICB is run after the ICV and the CCBs are run after the CCVs. If the CCB fails high for an
analyte and the samples are non-detects or are greater than 10x the blank value, then they
may be reported. All others must be re-analyzed under passing criteria.
11.4 A batch will consist of 20 or fewer samples. Batch Quality Control will include a Method Blank
(MB), Chicken Blank (CB) (Biota only), Laboratory Control Spike (LCS), Matrix Spike (MS),
Matrix Spike Duplicate (MSD), Post Digestion Spike (PDS), and a Serial Dilution (SD). It may
also include a Laboratory Control Spike Duplicate (LCSD) and/or Standard Reference Material
(SRM).
11.4.1 The Method Blank is used to verify that interferences caused by contaminants in the
solvents, reagents, glassware, etc. are known and minimized. The method blank is
processed through all clean-ups, etc., which were performed on the samples in the batch.
For a method blank to be acceptable, in the absence of project specific criteria, the
concentration shall not be higher than the highest of the following: The reporting limit, or ten
percent of the regulatory limit of concern for that analyte, or ten percent of the measured
concentration in a particular sample of interest. Each sample in the batch is assessed
against the above criteria to determine if the sample results are acceptable. Any sample
associated with an unacceptable blank is either flagged, re-prepped for analysis, or if re-
prepping is not an alternative, the results are reported with the appropriate data qualifying
codes.
11.4.2 The Chicken Blank (CB) must be prepared with every biota batch, and is processed
through all clean-ups, etc., which were performed on the samples. It consists of a control
matrix (ground chicken) to verify the interferences in the biological tissue is known and
minimized. The CB will contain detectable amounts of elements such as K, Ca, Na, Mg,
and P etc., and is used to ensure acceptable performance of the laboratory control spike.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
no -cen

aceAnalytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Any detections in the CB greater than the 40CFR Part 136 statistically derived MDL is
subtracted from the LCS/LCSD before recovery limits are evaluated.
11.4.3 A laboratory control sample (LCS) consists of a control matrix, which has been spiked,
with the analytes(s) of interest or compounds representative of those analytes. Laboratory
Control Samples are analyzed at a minimum of 1 per batch of 20 or fewer samples or
preparation method. Results of the LCS are expressed in terms of percent recovery and
are used to determine batch acceptance. Acceptance limits 6020B are 80 to 120% of the
expected concentration. Acceptance limits for 200.8 are 85 to 115% of the expected
concentration. If these limits are not met with the instrument in control, then the entire
batch will be re-digested and re-analyzed.
11.4.4 An LCS Duplicate may be analyzed to evaluate laboratory precision. The LCSD must
also meet the criteria for the LCS. The Relative Percent Difference (RPD)will be calculated
between the LCS and LCSD. The RPD is calculated as outlined below:
RPD = I Di - D2 [ x 100
(Di, + D2,)/2
Where:
RPD = relative percent difference.
Di =first sample value.
D2 = second sample value (duplicate)
The control limit for RPD is 20% or is based on laboratory generated data and not to
exceed 20%. If outside this limit, all associated results are given a R1 data qualifier.
Data generated with LCS samples that fall outside the established acceptance criteria
are judged to be out-of-control. These data are considered suspect and the
corresponding samples are reanalyzed or reported with qualifiers.
For the biota matrix, any detections greater than the MDL must be subtracted from the
LCS/LCSD on-instrument value before calculating the recovery limits.
NOTE: In the event where adequate sample is not supplied by the client to
perform a Matrix Spike/ Matrix Spike Duplicate, the LCS and duplicate can lend
insight on the precision of the analysis.
11.4.5 Matrix spikes (MS and MSD) are performed to evaluate the effect of the sample matrix
upon analytical methodology. A separate aliquot of sample is spiked with the analyte of
interest and analyzed with the sample. For 6020B an MS and MSD are performed at a
minimum frequency of 5% per batch. One pair in 20 samples, per matrix type, per sample
preparation method and are performed more frequently where regulations require. For
200.8, an MS/MSD pair, are performed at a 10% frequency per batch. Matrix spike
recoveries are evaluated against in-house control limits. The recovery must not exceed 75
to 125% of the expected recovery. If outside this recovery, the parent is flagged with an
appropriate data qualifier. If the recovery of an analyte is outside this range but the spike
level in not at least 25% the background concentration in the parent sample, the data is
flagged with an appropriate data qualifier. The RPD between the MS and MSD must be
less than or equal to 20%. If outside this limit, the parent is given an appropriate data
qualifier. The parent sample for the MS/MSD is chosen at random unless specified by a
client. Poor performance in a matrix spike generally indicates a problem with the sample
composition, and not the laboratory analysis, and results are used to assist in data
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
0a „fn',

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
assessment. A matrix effect is indicated if the LCS data are within acceptance criteria, but
the matrix spike data exceed the acceptance criteria. Prior to calculating recovery, the
parent sample concentration (results <Reporting MDL = 0) is subtracted from the spike
aliquot concentrations.
11.4.6 The Post Digestion Spike (PDS) is run to verify matrix interferences. A spike is added to
a portion of a prepared sample, or its dilution and must be recovered to within 80 to 120
percent of the known value. If the spike is not recovered within the specified limits with the
instrument in control, then the sample has a confirmed matrix effect. Dilute the parent and
re-spike the diluted sample until the PDS recovers within acceptance criteria.
11.4.7 The Serial Dilution (SD) is run to check for matrix interferences. If the analyte
concentration is within the linear dynamic range (LDR) of the instrument and sufficiently
high (minimally, a factor of at least 10 times greater than the lower limit of quantitation for
the diluted sample, 50 times the RLVS standard for the parent sample, or by project/client
specific criteria) an analysis of a fivefold (1+4) dilution must agree within ± 10% of the
original determination for 200.8. For the analysis of 6020B the limit is 25 times the RLVS
standard with the fivefold dilution agreement ± 20%. If these limits are not met, then an
interference effect must be suspected, and the data qualified with an SD data qualifier. If
the analytes of interest are greater than the LDR in the parent sample, the sample can be
diluted, and an SDL done from the dilution. Client specific requirements may require
different reference concentrations and limits.
11.4.8 The type of SRM is typically prepped and analyzed upon client request. It is a sample of
known concentration chosen to resemble the matrix being analyzed. Unless an alternative
is provided and specified by the client, the default SRM used for all Biota batches is TORT-
3 (Lobster Hepatopancreas) as it contains 15 commonly requested elements.
11.5 Data Assessment and Acceptance Criteria for QC Measures
Analytical Frequency
Method b
Quality Control
Measure 41 Acceptance Criteria
Method Blank One per batch, not to exceed 20samples. < LOD
<LOQ
Laboratory One LCS per batch, not to exceed 20samples. 6020B: ±20% recovery of the true value.
Control Spike LCSD performed by client request or if 200.8: ±15% recovery of the true value.
and Duplicate insufficient sample volume for MS/MSD. 520% RPD
Matrix Spike/ 200.8-one pair at 10%sample frequency. ±25%recovery of the true value.
Matrix Spike 6020B-one pair at 5%sample frequency. _<20% RPD
Duplicate
Post Digestion Once per batch of 20 or fewer samples. ±20%recovery of the true value.
Spike
Serial Dilution Once per batch of 20 or fewer samples. ±10% RPD referenced to the parent for
200.8
±20% RPD referenced to the parent for
6020B
DUP By client request. 5_20% RPD
SRM One per batch of 20 or fewer biota samples. Internally generated statistical limits.
Additional SRMs can be performed by client Client specific acceptance criteria.
request.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Initial Once per day at minimum. ?0.998 correlation coefficient(Calculated
Calibration Intercept,Absolute SD weighted)
Standard Error Call, Cal 2, Cal 3, Cal4, &Cal5(LDR 6020B) Call ±20%, Cal 2&3±15%, Cal4&5
readback after Linear Regression ±10%
ICV Once right after calibration. ±10% recovery of the true value.
ICB Once right after ICV. < <1/2 LLOQ(<1/2 Cal 1)
ICSA Prior to any samples,typically after the CRDL ±20%recovery of the true value.
and bracketing the samples by client request. <LOQ for non-spiked elements
ICSAB After the ICSA and bracketing samples by ±20% recovery of the true value.
client request. To use as the LDR check for 6020B
±10% recovery(elements> Cal5
specifically Ti and Mo)
CRDL/RLVS Prior to samples being analyzed,typically after ±30% recovery of the true value.
the ICB for 200.8, and bracketing the samples
for 6020B LOD and DOC sets or if requested
by client.
CCV Prior to any samples. Bracket every 10 or ±10% recovery of the true value.
fewer samples. At the end of the sequence.
CCB Right after CCVs. < LLOQ and client specific
11.6 Method Performance
11.6.1 Detection Limits
11.6.1.1 Detection limits (DL) and limits of quantitation (LOQ) are established at initial
method setup and verified on an on-going basis thereafter. Refer to Pace ENV
corporate SOP ENV-SOP-CORQ-0011 Method Validation and Instrument
Verification and to the laboratory's SOP ENV-SOP-GBAY-0106 Determination of
LOD and LOQ (most recent revision or replacement)for these procedures.
11.6.1.2 The LOD and LOQ are always adjusted to account for actual amounts used and
for dilution.
11.6.1.3 Current LOD and LOQ can be found in the Laboratory Information Management
System (LIMS)— EpicPro and is subject to change.
11.6.1.4 Level of Detection (LOD): The LOD is determined by the 40CFR Part 136B MDL
study. Once the 40CFR Part 136B MDL is determined it may be elevated if
deemed unrealistic as demonstrated using method blank evaluations.
11.6.2 Periodic performance evaluation (PE) samples are analyzed per ENV-SOP-
GBAY-0107, PE/PT Program (current revision or replacement), to
demonstrate continuing competence. All results are stored in the QA office.
At a minimum, these are performed twice a year for the aqueous and soil
matrices
11.6.3 A linear dynamic range study must be conducted at least once. The study is
conducted for each element by analyzing increasing concentrations (at least
3 levels) until the results generated exceed ±10% difference from the true
value, or another reason the data becomes of unacceptable quality (e.g.
Internal Standard Recovery failure or excessive memory effect). The highest
concentration within the 10% criteria is the maximum of the linear range for
that element. Once the linear dynamic range study determination is
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
'11 ofA7

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
performed, keep the data, as it is useful for the determination of memory
effects from samples and any polyatomic or doubly charged interferences
resulting from a high element concentration in a sample. For the analysis of
samples, the highest standard used in the same calibration event must be
used for the linear range within that analysis set. If the ICS LDR standards at
levels higher than the upper calibrations standard do not meet± 10% the true
value of the standard, then the linear range becomes the same concentration
as the highest calibration standard provided the readback after the linear
regression is 90-100% the expected value. All samples will be diluted and
reanalyzed that are over the linear calibration range.
11.7 Analyst Qualifications and Training
Employees that perform any step of this procedure must have a completed Read and
Acknowledgment Statement for this version of the SOP in their training record. In addition, prior
to unsupervised (independent) work on any client sample, analysts that prepare or analyze
samples must have successful initial demonstration of capability (IDOC) and must successfully
demonstrate on-going proficiency on an annual basis. Successful means the initial and on-going
DOC met criteria, documentation of the DOC is complete, and the DOC record is in the
employee's training file. Refer to laboratory SOP ENV-SOP-GBAY-0094 Orientation and
Training Procedures (most recent revision or replacement)for more information.
12.0 DATA REVIEW AND CORRECTIVE ACTION
12.1 Data Review
Pace's data review process includes a series of checks performed at different stages of the
analytical process by different people to ensure that SOPs were followed, the analytical record is
complete and properly documented, proper corrective actions were taken for QC failure and
other nonconformance(s), and that test results are reported with proper qualification.
The review steps and checks that occur as employee's complete tasks and review their own
work is called primary review.
An experienced peer or supervisor also reviews all data and results. Secondary review is
performed to verify SOPs were followed, that calibration, instrument performance, and QC
criteria were met and/or proper corrective actions were taken, qualitative ID and quantitative
measurement is accurate, all manual integrations are justified and documented in accordance
with the Pace ENV's SOP for manual integration, calculations are correct, the analytical record is
complete and traceable, and that results are properly qualified.
Reporting performs a third-level review, called a completeness check, or project management
staff to verify the data report is not missing information and project specifications were met.
Refer to laboratory SOP ENV-SOP-GBAY-0120 Data Review and Final Report Processes (most
recent revision or replacement) for specific instructions and requirements for each step of the
data review process.
Draw a single-line strikethrough for any unacceptable or changed data, then DATE and INITIAL
and provide a written explanation of the reason for the change.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
'2') of A')

m
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Data are validated and peer reviewed by lab personnel using a batch cover sheet attached to
the raw data and filed.
Any discrepancies and issues occurring with each batch should be included on the cover sheet
to be incorporated into a narrative.
To assist the primary and secondary reviewer of the data, a spreadsheet (ENV-FRM-GBAY-
0428) was created to copy and paste the calibration curve and initial QC samples into from the
LIMS Link generated bench sheet. This spreadsheet will automatically flag any non-compliant
quality control samples and QC checks.
12.2 Corrective Action
Corrective action is expected any time QC or sample results are not within acceptance criteria.
If corrective action is not taken or was not successful, the decision/outcome must be
documented in the analytical record. The primary analyst has primary responsibility for taking
corrective action when QA/QC criteria are not met. Secondary data reviewers must verify that
appropriate action was taken and/or that results reported with QC failure are properly qualified.
Corrective action is also required when carryover is suspected and when results are over range.
Samples analyzed after a high concentration sample must be checked for carryover and
reanalyzed if carryover is suspected. Carryover is usually indicated by low concentration detects
of the analyte in successive samples analyzed after the high concentration sample.
Sample results at concentrations above the upper limit of quantitation must be diluted and
reanalyzed. The result in the diluted samples should be within the upper half of the calibration
range. Results less than the mid-range of the calibration indicate the sample was over diluted
and analysis should be repeated with a lower level of dilution. If dilution is not performed, any
result reported above the upper range is considered a qualitative measurement and must be
qualified as an estimated value.
12.2.1 DATA ASSESSMENT/CORRECTIVE ACTION
Data Assessment Measure If these conditions are not achieved
MB ! 1
LCS/LCSD ! 2
MS/MSD ! 3
PS ! 4
SD ! 5
DUP ! 6
SRM ! 7
Initial Calibration ! 8
ICV ! 9
ICB ! 10
ICSA ! 11
ICSAB ! 12
CRDL ! 13
CCV ! 14
CCB ! 15
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
nf t7

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
1. If not<LOQ,verify by second analysis. If second analysis confirms contamination for target analyte at
or greater than the LOQ, re-digest sample batch and batch QC provided sufficient sample volume
remains. If insufficient sample volume remains, consult with project manager and client on how to
proceed. For MB detections greater than or equal to the LOD, but less than the LOQ; qualify applicable
sample results. For negative measurements more negative than the LOD, applicable data is given the
following data qualifier: "Analyte was measured in the associated method blank at a concentration of-
#.#units."
*For positive MB failures, samples that are non-detection need not be qualified. In addition,samples
that are greater than 10 times the MB detection, need not be qualified.
* For negative MB failures samples that are greater than 10 times the absolute value of the negative MB
measurement, need not be qualified.
2. Verify failure by second analysis. If second analysis confirms LCS(LCSD)failure, re-digest sample
batch and batch QC provided sufficient sample volume remains. If insufficient sample volume remains,
consult with project manager and client on how to proceed.
3. If the parent, MS, or MSD is greater than the reportable linear dynamic range, dilute and reanalyze the
parent, MS, and MSD. If the concentration of the spike is less than 25%of the concentration of the
parent,the MS and MSD recoveries are not evaluated. Any failures resulting from this are qualified
appropriately with a P6 qualifier. If the concentration of the spike is greater than 25%of the
concentration of the parent, appropriately qualify(MO)the parent sample if either the MS and/or MSD
fail accuracy. If the MS and MSD fail precision control limits flag the parent with the appropriate
precision data qualifier(R1).
4. If the spike is not recovered within the specified limits with the instrument in control, dilute the parent
and re-spike the diluted sample until the PS recovers within acceptance criteria.
5. If these limits are not met(as listed in Table 11.5),then an interference effect must be suspected, and
the data qualified with an appropriate data qualifier. If the analytes of interest are greater than the LDR
in the parent sample,the sample can be diluted, and an SDL done from the dilution.
6. If the DUP fails precision control limits flag the parent with the appropriate precision data qualifier
7. For Biota analysis only. Outside of client specific criteria,the SRM is digested and analyzed only to
demonstrate analyte recovery in a standard reference material. When the recovery is outside the lab
generated statistical limits,the element that failed recovery will be flagged in the samples for the
element that failed.Client specific action may also exist.
8. Correct the issue and recalibrate.
9. Verify failure by second analysis. If second analysis confirms ICV failure, correct the issue and
recalibrate the instrument. No data may be reported unless there is a passing ICV for that target
element. If verification passes criteria,then proceed with the analytical sequence.
10. Verify failure by second analysis when possible. If second analysis confirms ICB failure, correct the
issue and recalibrate the instrument. No data may be reported unless there is a passing ICB for that
target element.
11. Verify failure by second analysis. If second analysis confirms ICSA failure,the system is out of control.
Correct the issue and recalibrate the instrument. No data may be reported unless there is a passing
ICSA for that target element.
12. Verify failure by second analysis. If second analysis confirms ICSAB failure,the system is out of
control. Correct the issue and recalibrate the instrument. No data may be reported unless there is a
passing ICSAB for that target element.
13. Verify failure by second analysis when possible. If second analysis confirms CRDL failure,the system
is out of control. Correct the issue and recalibrate the instrument. No data may be reported unless
there is a passing CRDL for that target element. Exceptions; if the sample element concentration is
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
)A i A')

aceAnalytical®
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
greater than the CCV concentration and the bracketing CCVs are within control,that sample data may
be reported.
14. Verify failure by second analysis. If second analysis confirms CCV failure,correct the issue and
recalibrate the instrument. On unattended sequence, CCVs may fail and then pass later in the
sequence, but no data may be reported unless bracketed by passing CCVs for that target element.
15. Verify failure by second analysis when possible. If second analysis confirms CCB failure, correct the
issue and recalibrate the instrument. On unattended sequence, CCBs may fail and then pass later in
the sequence, but no data may be reported unless bracketed by passing CCBs. Exceptions;if the
failure is biased high and the sample is a non-detection, or the sample concentration is greater than 10
times the detection in the CCB for that target element. High concentration samples are the likely cause
of a CCB failure. The memory in the sample introduction system was not high enough to cause a CCV
failure, but enough to cause a CCB to fail high.
13.0 POLLUTION PREVENTION AND WASTE MANAGEMENT
Pace proactively seeks ways to minimize waste generated during our work processes. Some
examples of pollution prevention include but are not limited to: reduced solvent extraction, solvent
capture, use of reusable cycletainers for solvent management, and real-time purchasing.
The EPA requires that laboratory waste management practice to be conducted consistent with all
applicable federal and state laws and regulations. Excess reagents, samples and method process
wastes must be characterized and disposed of in an acceptable manner in accordance with Pace's
Chemical Hygiene Plan / Safety Manual.
For further information on waste management, consult ENV-SOP-GBAY-0125 Waste Handling and
Management(most recent revision or replacement).
14.0 MODIFICATIONS
A modification is a change to a reference test method made by the laboratory. For example, changes
in stoichiometry, technology, quantitation ions, reagent or solvent volumes, reducing digestion or
extraction times, instrument runtimes, etc., are all examples of modifications. Refer to Pace ENV
corporate SOP ENV-SOP-CORQ-0011 Method Validation and Instrument Verification for the
conditions under which the procedures in test method SOPs may be modified and for the procedure
and document requirements.
14.1 When there is insufficient volume provided by the client for the method specified matrix
spike/matrix spike duplicate (MS/MSD), a laboratory control spike duplicate will be analyzed to
demonstrate precision criteria. Laboratory batches will be qualified with the appropriate "M5"
data qualifier. When performing this analysis on paint chip samples, a MS/MSD will not be
completed on the samples due to high levels of elements present in the native sample.
15.0 RESPONSIBILITIES
Pace ENV employees that perform any part this procedure in their work activities must have a signed
Read and Acknowledgement Statement in their training file for this version of the SOP. The
employee is responsible for following the procedures in this SOP and handling temporary departures
from this SOP in accordance with Pace's policy for temporary departure.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
'2F of A',

0
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Pace supervisors/managers are responsible for training employees on the procedures in this SOP
and monitoring the implementation of this SOP in their work area.
16.0 ATTACHMENTS
Attachment I: Flowchart ICPMS Determinative Method
Attachment II: Instrument QC Limits
Attachment III: Aqueous Batch QC, On Instrument Concentrations and Limits
Attachment IV: Solid Batch QC, On Instrument Concentrations and Limits
Attachment V: Biota Batch QC, On Instrument Concentrations and Limits
17.0 REFERENCES
17.1 Pace Quality Assurance Manual (most recent revision or replacement).
17.2 The NELAC Institute TNI ; Volume 1 Module 2 "QualitySystems" TNI Standard, Management
( )>
and Technical Requirements for Laboratories PerformingEnvironmental Analyses, EL-V1-
q Y
2016-Rev2.1 (most recent revision or replacement).
17.3 USEPA, SW-846, Method 6020A"Inductively Coupled Plasma — Mass Spectrometry", February
2007.
17.4 USEPA, SW-846, Method 6020B "Inductively Coupled Plasma — Mass Spectrometry", Rev.2
July 2014.
17.5 USEPA, SW-846, Method 3010A, "Acid Digestion of Aqueous Samples and Extracts for Total
Metals for Analysis by FLAA or ICP Spectrometry", December 1996.
17.6 USEPA, SW-846, Method 3050B, "Acid Digestion of Sediments, Sludges, and Soils",
December 1996.
17.7 USEPA, 200.8 Revision 5.4, "Determination of Trace Elements in Water and Wastes by
Inductively Coupled Plasma-Mass Spectrometry", 1994
18.0 REVISION HISTORY
This Version: ENV-SOP-GBAY-0010-Rev.03
Section Description of Change
NA Update to Corporate Format
All Added additional 6020B Requirements, removed 6020 and 6020A references. Added
Cs and W.
9.1.3 Added Internal Standard
10.8 Added Relative Standard Error Calculation and limits
Tables Calibration and Spike tables have concentration changes, source standards, Internal
Standard
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
nr_ .,C An

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
This document supersedes the following document(s):
Document Number Title Version
ENV-SOP-GBAY-0010 Metals by ICPMS by EPA 6020/6020A and 200.8 01
ENV-SOP-GBAY-0010 Metals by ICPMS by EPA 6020/6020A and 200.8 02
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies,
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
37 of 42

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Attachment I: Flowchart
4110
Calibrate the
Appropriate instrument for
analytes of
Sample
interest
Preparation
Steps
•
Initial Calibration
Verification (ICV) and
Instrument Blank (ICB<1/2 LLOQ),
Warm up and RLVS, Linear Range
Tune Standards, ICSA, ICSAB
1 L
Continuing
Analyze Daily Calibration
ReportsPerfor in Verification ► Analyze
(CCV) and
Tune Solution Blank Samples
(CCB<LLO
Q) every 10
Does
response Yes Dilute
exceed LDR extract
range?
No
Take No • Yes Report
appropriate i QA/QC ► Results
corrective Passes?
action
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
38 of 42

ace Analytical
I
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV-Green Bay Quality-GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Attachment II: Instrument QC Limits
Element ICV CCV ICV/CCV ICS LDR ICSA ICSAB ICSAB Limits RLVS&Cal RLVS/ Cal 1 Cal 4 Cal 4
(ppb) (ppb) Limits 1,2,3 (ppb) (ppb) 1 (ppb) CRDL Relative (ppb) Relative
Limit Standard Standard
Error Error
Aluminum 15500 10,000 90%-110% 100,000 50,000 50,000 80%-120% 100 70-130% ±20% 12,500 ±10%
Antimony 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Arsenic 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Barium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Beryllium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Boron 150 200 90%-110% 50 _80%-120% 10 70-130% ±20% 250 ±10%
Cadmium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Calcium* 15500 10,000 90%-110% 250,000* 50,000 _ 50,000 80%-120% 250 70-130% _ ±20% 12,500 ±10%
Cesium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Chromium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Cobalt 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Copper* 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Iron 15500 10,000 90%-110% 150,000* 50,000 50,000 80%-120% 100 70-130% ±20% 12,500 ±10%
Lithium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Lead 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Magnesium* 15500 10,000 90%-110% 100,000* 50,000 50,000 80%-120% 100 70-130% ±20% 12,500 ±10%
Manganese* 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Mercury 4 5 90%-110% 5 _ 80%-120% 0.2 70-130% ±20% 250 ±10%
Molybdenum 150 200 90%-110% 1,000 1,050* 80%-120% 1 70-130% ±20% 250 ±10%
Nickel 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
1 Water ±20% ±10%
Palladium 150 200 90%-110% 50 80%-120% only 70-130% 250
Phosphorus* 15500 10,000 90%-110% 100,000* 50,000 50,000 80%-120% 100 70-130% ±20% 12,500 ±10%
1 Water ±20% ±10%
Platinum 150 200 90%-110% 50 80%-120% only 70-130% 250
Potassium* 15500 10,000 90%-110% 150,000* 50,000 50,000 80%-120% 250 70-130% ±20% 12,500 ±10%
Selenium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% ±10%
100,000* 100 Water ±20% ±10%
Silicon 15500 10,000 90%-110% 50,000 50,000 80%-120% only 70-130% 250
Silver 75 100 90%-110% 25 80%-120% 0.5 70-130% ±20% 125 ±10%
Sodium* 15500 10,000 90%-110% 50,000 50,000 80%-120% 100 70-130% ±20% 12,500 ±10% _
Strontium* 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Thallium 150 200 90%-110% 25 80%-120% 1 70-130% ±20% 250 ±10%
Tin 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Titanium* 150 200 90%-110% 1,000 1,050* 80%-120% 2.5 70-130% ±20% 250 ±10%
Tungsten 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Uranium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Vanadium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Zinc 150 200 90%-110% 50 80%-120% 10 _70-130% ±20% 250 ±10%
Zirconium 150 200 90%-110% 50 80%-120% 1 70-130% ±20% 250 ±10%
Elements indicated are subject to the latest LOD and LOQ studies and will likely be different in
liquid vs.solid matrices. The listed RLVS values are the lowest evaluated level.The RSE for Cal 2
&3 is set at 85-115%.
X For the purposes of Linear Dynamic Range in 6020B, these Recovery Limits are 90-110%.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
`2onfA9

( eAnaIicaI®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Attachment III: Aqueous Batch QC, On Instrument Concentrations and QC Limits
Element LCS/LCSD LCS/LCSD Limits MS/MSD MS/MSD Limits PS Amount PS Limits(%)
(ppb) (%)" Amount (%) (ppb)
(ppb)
Aluminum 10,000 80-120 10,000 75-125 10,000 80-120
Antimony 250 80-120 250 75-125 250 80-120
Arsenic 250 80-120 250 75-125 250 80-120
Barium 250 80-120 250 75-125 250 80-120
Beryllium 250 80-120 250 75-125 250 80-120
Boron 250 80-120 250 75-125 250 80-120
Cadmium 250 80-120 250 75-125 , 250 80-120
Calcium 10,000 80-120 10,000 75-125 10,000 80-120
Cesium 250 80-120 250 75-125 250 80-120
Chromium 250 80-120 250 75-125 250 80-120
Cobalt 250 80-120 250 75-125 250 80-120
Copper 250 80-120 250 75-125 250 80-120
Iron 10,000 80-120 10,000 75-125 10,000 80-120
Lithium 250 80-120 250 75-125 250 80-120
Lead 250 80-120 250 75-125 250 80-120
Magnesium 10,000 80-120 10,000 75-125 10,000 80-120
Manganese 250 80-120 250 75-125 250 80-120
Mercury 5 80-120 5 75-125 5 80-120
Molybdenum 250 80-120 250 75-125 250 80-120
Nickel 250 80-120 250 75-125 250 80-120
Palladium 250 80-120 250 75-125 250 80-120
Phosphorus 10,000 80-120 10,000 75-125 10,000 80-120
Platinum 250 80-120 250 75-125 250 80-120
Potassium 10,000 80-120 10,000 75-125 10,000 80-120
Selenium 250 80-120 250 75-125 250 80-120
Silicon 10,000 80-120 10,000 75-125 10,000 80-120
Silver 125 80-120 125 75-125 125 80-120
Sodium 10,000 80-120 10,000 75-125 10,000 80-120
Strontium 250 80-120 250 75-125 250 80-120
Thallium 250 80-120 250 75-125 250 80-120
Tin 250 80-120 250 75-125 250 80-120
Titanium 250 80-120 250 75-125 250 80-120
Tungsten 250 80-120 250 75-125 250 80-120
Uranium 250 80-120 250 75-125 250 80-120
Vanadium 250 80-120 250 75-125 250 80-120
Zinc 250 80-120 250 75-125 250 80-120
Zirconium 250 80-120 250 75-125 250 80-120
* For 200.8 the recovery limits for the LCS/ LCSD are 85—115%
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
A 11.,f A')

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'ace Analytical
I
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020B and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Attachment IV: Solid Batch QC, On Instrument Concentrations and QC Limits
Element LCS/ LCS/LCSD MS/MSD MS/MSD Limits PS PS Limits(%)
LCSD Limits(%) Amount (%) Amount
(PPb) (PPb) (PPb)
Aluminum 10,000 80-120 10000 75-125 10,000 80-120
Antimony 250 80-120 250 75-125 250 80-120
Arsenic 250 80-120 250 75-125 250 80-120
Barium 250 80-120 250 75-125 250 80-120
Beryllium 250 80-120 250 75-125 250 80-120 _
Boron 250 80-120 250 75-125 250 80-120
Cadmium 250 80-120 250 75-125 250 80-120
Calcium 10,000 80-120 10,000 75-125 10,000 80-120
Cesium 250 80-120 250 75-125 250 80-120
Chromium 250 80-120 250 75-125 250 80-120
Cobalt 250 80-120 250 75-125 250 80-120
Copper 250 80-120 250 75-125 250 80-120
Iron 10,000 80-120 10,000 75-125 10,000 80-120
Lithium 250 80-120 250 75-125 250 80-120
Lead 250 80-120 250 75-125 250 80-120
Magnesium 10,000 80-120 10,000 75-125 10,000 80-120
Manganese 250 80-120 250 75-125 250 80-120
Mercury 5 80-120 5 75-125 5 80-120
Molybdenum 250 80-120 250 75-125 250 80-120
Nickel 250 80-120 250 75-125 250 80-120
Phosphorus 250 80-120 250 75-125 250 80-120
Potassium 10,000 80-120 10,000 75-125 10,000 80-120
Selenium 250 80-120 250 75-125 250 80-120
Silicon 2500 80-120 2500 75-125 2,500 80-120
Silver 125 80-120 125 75-125 125 80-120
Sodium 10,000 80-120 10,000 75-125 10,000 80-120
Strontium 250 80-120 250 75-125 250 80-120
Thallium 250 80-120 250 75-125 250 80-120
Tin 250 80-120 250 75-125 250 80-120
Titanium 250 80-120 250 75-125 250 80-120
Tungsten 250 80-120 250 75-125 250 80-120
Uranium 250 80-120 250 75-125 250 80-120
Vanadium 250 80-120 250 75-125 250 80-120 l
Zinc 250 80-120 250 75-125 250 80-120
Zirconium 250 80-120 250 75-125 250 80-120
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
Al nfA.9

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Determination of Trace Metals in Waters and Wastes By Inductively Coupled
Plasma Mass Spectroscopy
TEST METHOD SW-846 6020E and EPA 200.8
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2021 Pace Analytical Services, LLC
Attachment V: Biota Batch QC, On Instrument Concentrations and QC Limits
Element LCS/ LCS/LCSD MS/MSD MS/MSD Limits PS PS Limits(%)
LCSD Limits(%) Amount (%) Amount
(PPb) (PPb) (PPb)
Aluminum 10,000 80-120 10,000 75-125 10,000 80-120
Antimony 200 80-120 200 75-125 200 80-120
Arsenic 200 80-120 200 75-125 200 80-120
Barium 200 80-120 200 75-125 200 80-120
Beryllium 200 80-120 200 75-125 200 80-120
Boron 200 80-120 200 75-125 200 80-120
Cadmium 200 80-120 200 75-125 200 80-120
Calcium 10,000 80-120 10,000 75-125 10,000 80-120
Chromium 200 80-120 200 75-125 200 80-120
Cobalt 200 80-120 200 75-125 200 80-120
Copper 200 80-120 200 75-125 200 80-120
Iron 10,000 80-120 10,000 75-125 10,000 80-120
Lithium 500 80-120 500 75-125 500 80-120
Lead 200 80-120 200 75-125 200 80-120
Magnesium 10,000 80-120 10,000 75-125 10,000 80-120
Manganese 200 80-120 200 75-125 200 80-120
Mercury 5 80-120 5 75-125 5 80-120
Molybdenum 200 80-120 200 75-125 200 80-120
Nickel 200 80-120 200 75-125 200 80-120
Phosphorus 20,000 80-120 20,000 75-125 20,000 80-120
Potassium 40,000 80-120 40,000 75-125 40,000 80-120
Selenium 200 80-120 200 75-125 200 80-120
Silver 100 80-120 100 75-125 100 80-120
Sodium 10,000 80-120 10,000 75-125 10,000 80-120
Strontium 200 80-120 200 75-125 200 80-120
Thallium 200 80-120 200 75-125 200 80-120
Tin 200 80-120 200 75-125 200 80-120
Titanium 200 80-120 200 75-125 200 80-120
Uranium 200 80-120 200 75-125 200 80-120
Vanadium 200 80-120 200 75-125 200 80-120
Zinc 200 80-120 200 75-125 200 80-120
Note: Biota spikes are fortified for P and K as a result of its natural presence in the Chicken blank.
These spike levels are also subject to project or client specific requirements, but the acceptance
criteria remain the same.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
A') .,f A')

-.'lace.AAnalytical
ENVIRONMENTAL SCIENCES
Document Information
Document Number: ENV-SOP-GBAY-0014 Revision: 01
Document Title: Determination of Mercury in Biological Samples by Cold Vapor Atomic Absorption
Spectroscopy-CETAC M-7500 (245.6)
Department(s):
Metals
Date Information 1
Effective Date: 09 Nov 2020
Notes
Document Notes:
All Dates and Times are listed in: Central Time Zone
1 of 26

Signature Manifest
Document Number: ENV-SOP-GBAY-0014 Revision: 01
Title: Determination of Mercury in Biological Samples by Cold Vapor Atomic Absorption Spectroscopy- CETAC
M-7500 (245.6)
All dates and times are in Central Time Zone.
ENV-SOP-GBAY-0014-Rev.01 Mercury in Biological Samples CVAAS_245.6
QM Approval
Name/Signature Title Date Meaning/Reason
Kate Verbeten(007119) Manager-Quality 05 Nov 2020,03:26:18 PM Approved
Management Approval
Name/Signature Title Date Meaning/Reason
Nils Melberg(007142) General Manager 2 05 Nov 2020, 03:35:54 PM Approved
Chad Rusch(007163) Manager 06 Nov 2020, 07:55:18 AM Approved
9rf7F

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
1.0 SCOPE AND APPLICATION
This standard operating procedure (SOP)describes the laboratory procedure for the determination of
mercury in biological tissue samples using the CETAC M-7500 instrument.
1.1 Target Analyte List and Limits of Quantitation (LOQ)
Element Symbol CAS# Biota LOQ
(mg/kg)'
Mercury Hg 7439-97-6 0.0188
' Values in place as of effective date of this SOP and are subject to change. For the most up to date LOQ, refer to the
LIMS or contact the laboratory.
LOQ are established in accordance with Pace policy and SOPs for method validation and for the
determination of detection limits (DL) and quantitation limits (LOQ). DL and LOQ are routinely
verified and updated when needed.
The reporting limit (RL) is the value to which analytes are reported as detected or not detected in
the final report. When the RL is less than the lower limit of quantitation (LLOQ), all detects and
non-detects at the RL are qualitative. The LLOQ is the lowest point of the calibration curve used
for each target analyte.
DL, LOQ, and RL are always adjusted to account for actual amounts used and for dilution.
1.2 Applicable Matrices- EPA 245.6 applies biological tissue samples.
1.3 Personnel: The policies and procedures contained in this SOP are applicable to all personnel
involved in the analytical method or non-analytical process.
2.0 SUMMARY OF METHOD
2.1 Cold vapor atomic absorption utilizes the volatile property of elemental mercury at the 253.7
nm wavelength. To release mercury from organic complexes, the sample is digested with
oxidizing reagents and acids in a hot block digester at 58°C, followed by overnight oxidation
with potassium permanganate and potassium per-sulfate at room temperature.
2.2 After digestion, the oxidizing reagents are neutralized by adding hydroxylamine
hydrochloride. The Flow Injection Analysis System sweeps the volatile elemental mercury
out of the sample and into the cell of an atomic absorption spectrophotometer. The
absorbance signal is proportional to the amount of mercury in the sample.
2.3 Results are reported in parts per million (mg/kg).
3.0 INTERFERENCES
3.1 Biota samples can contain diverse matrix types, each of which may present analytical
challenges. Spiked samples and Laboratory Control Samples are important for determining
digestion efficiency.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
..tnc

aceAnaIicaI®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
3.2 During the oxidation step, chlorides are converted to free chlorine, which also absorbs
radiation at 253.7 nm. Care must therefore be taken to ensure that free chlorine is absent
before the Mercury is reduced and swept into the cell. This may be accomplished by using
an excess of hydroxylamine hydrochloride reagent.
3.3 Certain volatile organic materials that absorb at this wavelength may also interfere. A
preliminary run without reagents may be used to determine if this type of interference is
present.
4.0 DEFINITIONS
Refer to the Laboratory Quality Manual for a glossary of common lab terms and definitions.
4.1 Biota Control Blank (Matrix Blank): A sample of a matrix that is used for the control spike.
The biota control blank will either be catfish, tilapia, chicken, or other tissue whichever is
available at the time of analysis. The biota control blank should be "farm-raised" to minimize
background mercury levels. The concentration in the biota control blank will be subtracted
from the concentration of the laboratory control spike when the biota control blank
concentration is greater than/equal to the MDL. This is done because the biota control blank
is known to have some contamination. This SOP will reference biota control blank for ease.
Note: For plant material analysis, alfalfa can be used as the biota control blank matrix.
4.2 Standardized Reference Material (SRM): A certified reference material produced by the U.S.
National Institute of Standards and Technology or other equivalent organization and
characterized for absolute content, independent of analytical method. A SRM is analyzed
with each analytical batch of biota samples.
5.0 HEALTH AND SAFETY
The toxicity or carcinogenicity of each chemical material used in the laboratory has not been fully
established. Each chemical should be regarded as a potential health hazard and exposure to these
compounds should be as low as reasonably achievable.
The laboratory maintains documentation of hazard assessments and OSHA regulations regarding the
safe handling of the chemicals specified in each method. Safety data sheets for all hazardous
chemicals are available to all personnel. Employees must abide by the health, safety and
environmental (HSE) policies and procedures specified in this SOP and in the Pace Chemical Hygiene
/Safety Manual.
Personal protective equipment (PPE) such as safety glasses, gloves, and a laboratory coat must be
worn in designated areas and while handling samples and chemical materials to protect against
physical contact with samples that contain potentially hazardous chemicals and exposure to chemical
materials used in the procedure.
Concentrated corrosives present additional hazards and are damaging to skin and mucus membranes.
Use these acids in a fume hood whenever possible with additional PPE designed for handing these
materials. If eye or skin contact occurs, flush with large volumes of water. When working with acids,
always add acid to water to prevent violent reactions. Any processes that emit large volumes of
solvents (evaporation/concentration processes) must be in a hood or apparatus that prevents
employee exposure.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
A of 7R

aceAnaIicaI®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
Extreme caution must be used when preparing rodents for digestion. The samples must undergo a
special procedure to destroy any Hantavirus, which may be present. Refer to the most recent version
of SOP ENV-SOP-GBAY-0130 Small Rodent Handling and Homogenization for details.
Contact your supervisor or local HSE coordinator with questions or concerns regarding safety protocol
or safe handling procedures for this procedure.
6.0 SAMPLE COLLECTION, PRESERVATION, HOLDING TIME, AND STORAGE
Samples should be collected in accordance with a sampling plan and procedures appropriate to
achieve the regulatory, scientific, and data quality objectives for the project.
The laboratory does not perform sample collection or field measurements for this test method. To
assure sample collection and field checks and treatment are performed in accordance with applicable
regulations Pace project managers will inform the client of these requirements at the time of request
for analytical services when the request for testing is received prior to sample collection. If samples
were already collected, the laboratory will record any nonconformance to these requirements in the
laboratory's sample receipt record when sufficient information about sample collection is provided with
the samples.
The laboratory will provide containers for the collection of samples upon client request for analytical
services. Bottle kits are prepared in accordance with laboratory SOP ENV-SOP-GBAY-0007 Bottle
Preparation (current revision or replacement).
6.1 Where applicable, the bottle ware is demonstrated to be fee of target analytes. When bottle
ware not originating from the lab is used, the data may be qualified with either one or both of
the following data qualifiers:
6.1.1 Sample field preservation does not meet EPA or method recommendations for this
analysis.
6.1.2 Sample container did not meet EPA or method requirements.
Requirements for container type, preservation, and field quality control (QC)for the common list of test
methods offered by Pace are included in the laboratory's Quality Manual.
6.2 General Requirements
Matrix Routine Minimum Preservation Holding Time
Container Sample Amount
Biological 4oz amber glass,aluminum 30 Thermal:<_-10°C Collection to Analysis: 28 days after
Tissue foil or zip top bags g _ Chemical:None removal from freezer.
'Minimum amount needed for each discrete analysis.
Thermal preservation is checked and recorded on receipt in the laboratory in accordance with
laboratory SOP ENV-SOP-GBAY-0006 Sample Management (current revision or replacement).
Chemical preservation is checked and recorded at time of receipt or prior to sample preparation.
After receipt, biota samples large enough to sub-sample are homogenized using normal biota
preparation procedures (See the current version of ENV-SOP-GBAY-0129 Sample Homogenization,
Compositing and Sub-sampling). After homogenization, samples are stored frozen at <-10°C in an
acid-cleaned glass fluoropolymer jar. Biological tissue samples received lyophilized (freeze dried)may
be stored at ambient temperature.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
r_

Frixtf .• 7'"
6ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services,LLC
After analysis, unless otherwise specified in the analytical services contract, samples are retained for
21 days from date of final report and then disposed of in accordance with Federal, State, and Local
regulations.
7.0 EQUIPMENT AND SUPPLIES
7.1 Equipment
Equipment* Pace Name Manufacturer/Vendor* Model(s)*
Quick Trace Mercury Analyzer 40HG2 CETAC M-7500
Auto-Sampler 40HG2 CETAC ASX-260
Analytical Balance 40BAL2 Ohaus AV213
Hot Block 40HB03 Environmental Express SC100
10 Fixed Pipette 40PPT02 Fisherbrand F1226505
20-200 pL Adjustable Pipette 4OPPT11 Eppendorf G1111396
100—1000 pL Adjustable Pipette 40PPT68 Eppendorf 030571G
1000-5000 pL Adjustable Pipette 40PPT71 Eppendorf R40811 G
*Or equivalent
7.2 Supplies
Supply Vendor* Model/ID* Catalog# Description
Tubing (Pump) Cetac Technologies Yellow-Yellow SP5705A 1.42 mm ID
Tubing (Pump) Cetac Technologies Blk-Blk SP5075B 0.76 mm ID
Tubing (GLS) Cetac Technologies GLS SP5812 Tubing
Tubing (Waste) Cetac Technologies Waste SP5706 Tubing
Cartridge Cetac Technologies Nafion Dryer SP5894 NA
Instrument Lamp Cetac Technologies Lamp SP5603 Replacement Lamp
SnCl2 Capillary Cetac Technologies SnCl2 Capillary SP8049 NA
Probe Cetac Technologies Autosampler SP6033 1.0 mm ID
Rinse Station Cetac Technologies Rinse Station SP7027 NA
Liquid Mix Line Cetac Technologies Liquid Mix Line SP5812 NA
Gas Liquid Separator Cetac Technologies GLS SP6041 NA
GLS Drain Tube Cetac Technologies Drain Tube SP6042 NA
Peri-Pump Fittings Cetac Technologies Peri-Pump SP6036 NA
Chicken Local Vendor NA NA Kept at 5-10°C
Pipette Tips Eppendorf 1 mL 21-372 Fisher Scientific
Pipette Tips Eppendorf 5 mL 21-381-198 Fisher Scientific
pH Strips EMD Millipore NA M1095400001 Fisher Scientific
Digestion Vial SCP Science 15 mL M115PB NA
Digestion Vial Mold Pro 50 mL 010-500-263 Fisher Scientific
250 mL Graduated Cylinder Pyrex 250 mL 07-250-070 Class A
Volumetric Flask Fisher Scientific 100, 1000,2000 mL 1025-C, FB400200,10-205F Class A
*Or equivalent
7.3 All reusable lab ware (glass, quartz, polyethylene, PTFE, FEP, etc.) should be sufficiently
clean for the task objectives following current revision of SOP: ENV-SOP-GBAY-0143,
Labware Cleaning Procedure.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
G ..$')G

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
7.4 Digestion tubes— Each lot of digestion tubes has its volumetric increments validated prior to
use.
7.4.1 Each digestion tube is evaluated at the 5.0, 25, and 50 mL increments.
7.4.2 The digestion tube is first tarred and then filled to the increment to be tested and then
weighed. The weight is documented.
7.4.3 The RSD is calculated between of the average of the 4 digestion tubes for that volume
increment and the expected mass.
7.4.4 The RSD must be <2% to be acceptable for that lot and used as a measurement tool.
I 7.4.5 This is documented in the Metals Support Supplies Verification Logbook.
8.0 REAGENTS AND STANDARDS
8.1 Expiration dates listed in tables are the maximum that may be used. The expiration date
cannot exceed that of the material used to make a standard and/or reagent.
8.2 Reagent and Stock Standard(s)
Purchased Catalog Concentration/
Reagent or Stock* Alias From* Number* Purity* Expiration Storage
Reagent Water Water In House NA >_18 Mega ohm se erated for Room Temp
DORM-4 DORM-SRM NRC CNRC DORM-4 0.41 mg/Kg 05/31/2022 Desiccator @
Room Temp
Potassium KMnO4 Fisher Scientific P279-500 Neat/Certified A.C.S
Permanganate
Potassium Persulfate K2S208 J.T. Baker 3238-01 Neat/Certified A.C.S
Hydroxylamine NH2OH• Neat/Certified Manufacturer's
Fisher H330-500
Hydrochloride HCI A.C.S. recommended
Stannous Chloride SnCl2 Fisher T142-500 Neat/Certified expiration date or
A.C.S. 2 years from Room Temp
Rinse 36.5-38%Trace receipt date,
Hydrochloric Acid HCI JT Baker 9530-33 Metal Grade whichever is
Hydrochloric Acid HCI SCP Science 250-038-155 34-37% PlasmaPure sooner
Nitric Acid Rinse JT Baker 9598 34 67-70%Trace Metals
HNO3 Grade
Nitric Acid HNO3 SCP Science 250-038-175 67-70% PlasmaPure
Manufacturer Mini-Bulk
Argon—Grade 5.0 Ar2 Air Gas Ultra-High Purity Date Tank
Mercury Standard Hg-STK High Purity 100033-1 1000 pg/mL Manufacturer's
primary recommended Room Temp
Mercury Standard Hg-SPK Inorganic CGHG1-1 1000 pg/mL expiration date
second source Ventures
*Or equivalent
Anyprinted copyof this SOP and all copies of this SOP outside
p of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
7nf7R

o
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services,LLC
8.3 Working Standard Solutions
Stock or Inter- Amount Final Volume Final
Standard Alias mediate Used W/Diluent Diluent Conc. Expiration Storage
CVAA Hg Primary CVAA Hg Hg Calibration 20 pL 200 mL Water 100 ppb 1 Month
Intermediate Cal Stock
HNO3 6.0 mL
CVAA Hg Secondary CVAA Hg Hg ICV Stock 20 pL
Intermediate(ICV) Spk(ICV) 200 mL Water 100 ppb 1 Month
HNO3 6.0 mL
CVAA Hg Secondary CVAA Hg Hg ICV Stock 20 pL 200 mL Water 1000 ppb 1 Month
Intermediate(Spike) Spk(Spike) HNO3 6.0 mL
5%Potassium 5% KMnO4 KMnO4 50.0 g 1000 mL Water 5% 1 Month Room
Permanganate solution
5% Potassium Temp
Persulfate 5% K2S2O8 K2S2O8 50.0 g 1000 mL Water 5% 1 Month
12% Hydroxylamine 12% NaCI 120 g 1000 mL Water 12% 1 Month
Hydrochloride NH2OH•HCI NH2OH•HCI 120 g
Stannous Chloride SnCl2 SnCl2 100.0 g 1000 mL Water 10% 1 Week
Solution Solution HCI 70 mL
Acid Rinse Solution Acid Rinse HCI 125 mL 2,500 mL Water 5% 6 Months
HNO3 125 mL
*Or Equivalent
8.4 Stannous Chloride Solution —Discard if oxidized or precipitate forms.
8.5 Diluent—Each digest has 1-12 extra digested blanks made as diluent.Amount is determined
as needed and assigned a one-week expiration date.
8.6 Biota Calibration and Verification Standards
Standard Alias Stock or Amount Final Volume Diluent Final Expiration Storage
Intermediate Used (W/Diluent) Concentration
Hg Cal.0 CVAA-CALO - - 50 mL Water 0.0 ppb
Hg Cal. 1 and CRDL CVAA-CAL1 100 pL 50 mL Water 0.2 ppb
Hg Cal.2 CVAA-CAL2 500 pL 50 mL Water 1.0 ppb
Hg Cal.3 CVAA-CAL3 1250 pL 50 mL Water 2.5 ppb
Hg Cal.4 CVAA-CAL4 2500 pL 50 mL Water 5.0 ppb
Hg Cal. Made Per Room Temp
Hg Cal.5 CVAA-CAL5 Intermediate 5000 pL 50 mL Water 10.0 ppb Use
Hg ICV CVAA-ICV 2000 pL 50 mL Water 4.0 ppb
Hg CCV CVAA-CCV 2500 pL 50 mL Water 5.0 ppb
Hg ICB/CCB CVAA-CALO - - 50 mL Water 0.0 ppb
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
n _r nn

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
8.7 Standards will have a label attached to the bottle identifying the following (due to the limited
amount of space on some standard vials (i.e., 2 mL autosampler vials), an EpicPro standard
label will be attached which does not contain all the following):
8.7.1 Name of Solution.
8.7.2 Pace, LLC. Standard ID Number
8.7.3 Pace, LLC. Lab Lot ID (for Stock standards and reagents)
8.7.4 Preparation Date
8.7.5 Preparer's initials
8.7.6 Concentration
8.7.7 Expiration Date
9.0 PROCEDURE
9.1 Analytical Balance Procedures:
9.1.1 Annual Calibration:The balance must be calibrated at least annually by an outside agency
and checked daily before each use using Class 1 or 2 weights. Refer to Pace SOP ENV-
SOP-GBAY-0115 Support Equipment(most recent revision or replacement.
9.1.2 Daily Calibration Check:
9.1.2.1 Clean the balance and surrounding area prior to starting the daily calibration
check.
9.1.2.2 Check the sight level on the balance. If it needs adjusting, level the balance.
9.1.2.3 The weight set ID indicated in the logbook is used as the primary set. If an
alternate weight set ID is used, that ID must be recorded in the comment section
of the balance calibration logbook for that day.
9.1.2.4 Tare the balance before weighing the NIST certified weights.
9.1.2.5 Use forceps or other means to lift each weight (Do not touch the weights with
fingertips as the residue may artificially adjust the true value of the weights).
Record the date of the calibration check, the true value of the weight, and the
actual measured weight in the logbook. Repeat this procedure for the other
certified weights. If calibration weights differ from the certified weights by more
than specified in the balance calibration logbook, corrective action must be taken.
9.1.3 Corrective Action Procedures:
9.1.3.1 Clean the balance and balance pan. Check the sight level on the balance and
adjust if necessary. Re-tare and reweigh all the certified weights.
9.1.3.2 The internal calibration function (if available) of the balance may be used as a
means of corrective action.
9.1.3.3 Utilize the internal calibration function and diagnostics. Refer to instrument
manual.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use. I
CI.,f')
I[

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
9.1.3.4 Contact the QA office for assistance if the balance does not meet the calibration
tolerances.
9.1.3.5 If the above action does not correct the problem, the balance should be taken out
of service and appropriately labeled to avoid improper usage. A service
technician should be contacted.
9.1.3.6 Record any corrective action. Initial and date all entries in the logbook.
9.2 Thermometer: See the most recent revision of the SOP ENV-SOP-GBAY-0115, Support
Equipment for thermometer calibration and validation.
9.3 Pipette/Bottle Top Dispenser: See the most recent revision of the SOP ENV-SOP-GBAY-
0115, Support Equipment for volumetric dispensing device calibration and validation.
9.4 CETAC M-7500 Operating Parameters: In the Method Editor Page the default parameters
should be set as the following.
Operating Condition* Setting
Gas Flow(mL/min) 100
Pump Speed (%) 50
Sipper Depth (mm) 145
Sample Uptake Time (s) 35
Rinse Time (s) 95
Read Delay Time (s) 57
Replicate Read Time (s) 1.5
Replicates 4
*Or Equivalent
9.5 CETAC M-7500 Calibration and Standardization.
9.5.1 Calibration requires analysis of a minimum of 5 standards plus a blank due to the linear
regression calibration used. The working range is from the current MDL to the highest
standard in the calibration curve. The lowest calibration concentration is used to validate
the pace reporting limit.
9.5.2 The typical batch for initial calibration should include:
CALO-0 pg/L
CAL1 -0.2pg/L
CAL2-1.0 pg/L
CAL3-2.5 pg/L
CAL4-5.0 pg/L
CAL5- 10.0 pg/L
Initial Calibration Verification (ICV)—4.0 pg/L
Initial Calibration Blank(ICB)
CRDL
9.5.3 Frequency: A digested calibration curve is made up every day samples are prepared. The
curve is associated to the sample batch(es) it is prepped with.
9.5.4 Acceptance Criteria:
9.5.4.1 The resulting correlation coefficient for the curve must be 0.995 or better.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

aceAnalj4ical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
9.5.4.2 The %RE of the lowest calibration points must be within ±40% of the true value.
9.5.4.3 The %RE of the remaining calibration points must be within ±10% of their true
value.
9.5.5 Corrective action: The instrument must be recalibrated and or the calibration curve and
the associated samples must be re-prepped.
9.5.6 Calibration Verification: The calibration curve must be validated by acceptable analysis of
applicable instrument QC. At a minimum these included ICV, ICB, CRDL, CCV(s), and
CCB(s). See section 11 for more details on calibration verification QC.
9.5.7 See Attachment I: QC Summary and laboratory SOP: ENV-SOP-GBAY-0138, Calibration
Procedures (most recent revision or replacement)for additional guidance.
9.6 Biological Tissue Sample Digestion (EPA 245.6):
9.6.1 50 mL digestion vials are used for Biota samples.
9.6.2 Prior to analysis the samples and calibration curve must be digested.
9.6.3 Turn on the hot block and set the temperature to maintain a sample temperature of 58±3°C.
Before placing samples in the hot block to digest, use a temperature blank to verify that
the block temperature is correct and adjust as required. Record the temperature in the
electronic prep log. Verify that the hood is functioning.
9.6.4 Add 2.5 mL of Nano-Pure water and add the appropriate amounts (as shown in Section
8.3) of Hg Calibration Intermediate and Hg ICV Intermediate to digestion vials for the curve,
ICV, CCV, ICB, and CCB. Additional blanks (and standards) may be prepared to be used
as continuing calibration blanks and calibration check standards and to be used as diluent
in cases where the sample concentration exceeds the high point of the calibration curve or
matrix interferences are observed.
9.6.5 Prepare one Method Blank. For biota analysis, leave the Method Blank empty. A Biota
Control Blank is also prepared by weighing 0.6 g of homogenized biota control blank tissue
(chicken) into a digestion vial.
9.6.6 Prepare the LCS for biota samples by weighing 0.6 g of homogenized biota control blank
1 into the digestion vial. Add 2.5 mL of Hg ICV Intermediate (100 pg/L CVAA Hg Spk) the
vial. Only prep a Laboratory Control Spike Duplicate (LCSD) if requested by client or there
is not enough sample to run a MS/MSD. Prepare the LCSD in the same fashion as the
LCS.
9.6.7 For biota samples, weigh approximately 0.05 g of Standard Reference Material into a
labeled digestion vial (DORM-4 or equivalent).
9.6.8 Weigh 0.6 g of homogenized sample into a labeled digestion vial. Record the weight to
the nearest 0.01 g in the digestion prep log. Try to minimize any thawing of the sample
during the weighing process to prevent fluid migration within the tissue.
9.6.9 To prepare a Matrix Spike and Matrix Spike Duplicate, a sample with sufficient volume is
chosen at random. Weigh 2 additional 0.6g aliquots into digestion vials. Add 2.5 mL of Hg
ICV Intermediate (100 pg/L CVAA Hg Spk)to each vial.
9.6.10 To each digestion vial add 2.0 mL of concentrated sulfuric acid and 0.5mL of concentrated
nitric acid and cap loosely. Swirl digestion vials to gently mix.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
11 of 26

aeAnalWcal®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
9.6.11 Heat the samples, standards and SRM for 1 hour on a hot block set to reach 58±3°C (soft
tissue should be completely dissolved).
9.6.12 Remove the vessels from the hot block and cool in an ice bath, or pack ice around the
samples for at least one hour.
9.6.13 Slowly add 7.5 mL of 5%KMnOato all samples and batch QC. Samples may react violently
if added too quickly.
9.6.14 To each sample, including QC, add 4 mL of potassium persulfate solution, cap loosely, and
allow the samples to sit overnight at room temperature.
9.6.15 To each sample, including QC, add 3 mL of hydroxylamine solution to decolorize it and let
sit for about two hours (capped)to allow gases to diffuse out of solution.
9.6.16 Bring to a final volume of 50 mL with water.
9.6.17 All samples and QC need to be diluted by a dilution factor of 5. Add 2.0 mL of sample to
a digestion vessel. Dilute the sample by adding 8.0 mL of blank water that has been
digested by the EPA 245.6 method.
9.7 Dry Ice Blank and Blender Blank Preparation:
9.7.1 Dry Ice Blank-Add 50 mL of DI water and 1.0 mL of nitric acid to Dry Ice Blank jar sent by
sampler.
9.7.2 Blender Blank — Rinse blender with 50 mL of DI water acidified with 1 mL of nitric acid.
Collect in sample container and label as Blender Blank.
9.7.3 Close each sample jar, shake well, and let stand for at least 30 minutes.
9.7.4 Pipette a 25 mL aliquot of the prepared sample into a sample digestion vessel. This
procedure will allow enough sample digestate for one re-analysis, if necessary.
9.7.5 Digest the dry ice blank and blender blank.
9.7.6 See Section 10 for calculation of results for dry ice blanks and blender blanks.
9.8 Dilutions: All reported results must be within the range of the calibration curve. Dilute when
results are greater than the high standard in the curve. Dilutions on sample extracts must be
prepared in a volumetric fashion. Sample aliquots should be taken with a calibrated pipette
and brought to an appropriate final volume. In the event a dilution is made to bring a target
analyte into calibration range, the analyst should make a dilution such that the target analyte
is roughly the equivalent of the mid calibration point whenever possible.
9.9 CETAC M-7500 Basic System Operation (Analytical): This portion of the SOP is designed
to allow the user to set up and run a method, print a sample report, then shut down using the
more basic software functions. For a more detailed explanation of the many other options,
the user should refer to the Reference Manual.
9.9.1 Verify the carrier argon gas supply is on.
9.9.2 Switch on the CETAC M-7500.
9.9.3 Verify the computer is on. If not, switch on the computer and enter network password and
click on Start.
9.9.4 Go to programs, CETAC QuickTrace, and click on QuickTrace.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
4 n

®
aceAnalytical 2
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
9.9.5 To create a new worksheet from a Template, Click on File, New From. Click on the browse
button to select a Template worksheet, then enter the new File name (ex. Naming file
0713111AJT denotes the month, date, year, and analyst. The number at the end of the
date signifies each run within a day's output.). Click Save. Click ok.
9.9.6 To open an existing worksheet, select Open, and select the desired worksheet. The
worksheet will open to the sequence page.
9.9.7 To enter sample information, go to the sequence page. Follow the Template to fill in Ids
for the Calibration QC and samples, under the sample label column.
9.9.8 A typical sequence will consist of the following in order: a calibration curve (5 standards
plus a blank), an ICV immediately followed by an ICB, a CRDL, a CCV immediately
followed by a CCB. At this point a batch consisting of samples and batch QC can be
analyzed. At a maximum of every 10 batch injections a CCV immediately followed by a
CCB must be analyzed. The batch must also end with CCV immediately followed by a
CCB.
ICAL Standards
ICV/ICB
CRDL
CCV/CCB
MB
LCS/LCSD
Samples (Up to 10 Injections)
CCV/CCB
Samples(Up to 10 Injections)
MS/MSD
CCV/CCB
9.9.9 Go to File, Save to ensure changes to the worksheet are saved.
9.9.10 Under Method editor, click QC Tests to Set the QC concentration and the control limits.
9.9.11 On the Sequence Parameters page hit the control button to set up when the QC will be
• analyzed, i.e. after calibration, after 10 samples, and at the end. IF re-calibration occurs
the QC must be analyzed at the same frequency. This page also allows you to put the
system into standby mode. The options allow you turn the pump on "slow" or"off. It also
allows you to turn the Lamp off and Gas off.
9.9.12 The Sequence Parameters under the reports button allows you to customize the report
printout by selecting solution information, report contents, and default number format.
9.9.13 Under the Sequence Editor page click on Manual QC, specify what to do if calibration QC
fails, for example stop analysis, flag and continue, repeat-flag and continue, recalibrate
and repeat, recalibrate and repeat with samples, or reslope and repeat.
9.9.14 On the Auto QC page of the Sequence Editor, specify what QC to run at the end of a run
and corrective action if QC fails.
9.9.15 Under the Sequence Editor click Sequence; This is where you determine the number of
samples in the analysis and how often calibrations will be performed.
9.9.16 The analysis screen is accessed by clicking on the analysis button, from the main toolbar.
This screen is where analysis controls and displays are located.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
12tnf9R

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
9.10 CETAC M-7500 Starting the Analysis:
9.10.1 Prepare the required reagents: Acid Rinse solution and reducing agent.
9.10.2 Turn on the lamp and carrier gas. A minimum 15-minute warm-up time is required.
9.10.3 Put peristaltic tubing in place, and clamp in place.
9.10.4 Place the auto-sampler rinse tubing into the Acid Rinse bottle. If rinse pump is not on make
sure it is on by clicking on the instrument page and clicking "pump on". Make sure to have
probe down at this time as well.
9.10.5 Place the SnCl2 line in a bottle of reagent water and start the peristaltic pump. Inspect flow
to make sure lines are flowing correctly and not pulsing.
9.10.6 Wet the GLS (Gas Liquid Separator) center post. In the software click on the instrument
icon, click analyzer, set gas flow to 350-mL/min and change pump speed to 100%. Pinch
the drain line until 2 or 3 bubbles go to the top of the GLS center post. Then release the
drain line and allow liquid to restore itself.
9.10.7 Attach GLS exhaust tube to GLS center post and close the optical cabinet door. Place
reagent capillaries in appropriate reagent bottles.
9.10.8 Open the appropriate worksheet and verify that the gas flow and pump speed in the
worksheet matches what is listed in instrument/analyzer, if the flow and the speed is not
the same make the necessary change or click the auto set icon on the menu bar. This will
stabilize the instrument before auto-zeroing and running a peak profile.
9.10.9 Record the Lamp's mA value in a daily instrument logbook by clicking on the instrument
icon, clicking on analyzer, "status of lamp".
9.10.10 Peak profile the high standard of the calibration. To do this click on Method Editor, read a
sample icon, and then choose the location of high standard. Record the concentration of
the peak profile standard in a daily instrument logbook. The read delay time is adjusted
here as well.
9.10.11 Hit the GO icon to start the calibration. Once the calibration is complete a dialog window
will generate stating, "Continue with Analysis" Click YES if satisfied with Calibration or
click NO to re-analyze Calibration.
9.10.12 Hit the STOP icon to immediately end an analysis that is currently running. The auto-
sampler probe will immediately return to the rinse station.Stopping an analysis in progress
will prevent data from being saved for that sample.
9.10.13 To stop the analysis after the current sample, select the Stop/After solution item from the
analyze menu.
Note: If you stop during sample uptake, or before the rinse has been completed, make sure you
allow sufficient time in the rinse station before re-starting the analysis.
9.10.14 If you stopped the analysis, you can simply restart by clicking the GO button. The analysis
will begin at the next un-analyzed solution within the sequence.
9.10.15 To restart the analysis from the beginning you will need togenerate the sequence again.
Y g 9q g
Open the Sequence Editor, make any desired changes, click on Generate Sequence.
Then click GO to start analysis over.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
44 ..f')G

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
9.10.16 To read a single sample, click on the icon, analyze single sample. A dialog window will
be brought up where you will enter the tube position, sample label, sample type, and other
information if desired.
Note: Using the read sample feature may invalidate your QC setup. If you have stopped
during a batch analysis to read a single sample, it will be inserted into the sequence after
the last analyzed sample.
9.10.17 When the run is complete the instrument will automatically go into standby mode.
Depending what options, you have selected from sequence parameters, this may turn off
or slow the pump, turn off the lamp, and/or the carrier gas flow.
9.10.18 To export the data,go to File then Export.Go to K:\Metals\CVAA\40HG2\, enter file name,
and click Save.
9.11 CETAC M-7500 System Shutdown:
9.11.1 Place the inlet of the SnCl2 line in a container of 10% nitric acid rinse (use a 500mL
container; use 50mL of Nitric acid and dilute to 500 with Nanopure water))for 10 minutes.
9.11.2 Once the SnCl2 is rinsed with 10% nitric acid rinse, place the SnCl2 line into DI water for 1
minute to rinse system.
9.11.3 Remove the SnCl2 line from the DI water and raise lines out of rinse solution. Run the pump
until the lines are dry.
9.11.4 Raise the probe from the rinse station by clicking on the instrument icon and by clicking
the Move Sipper Up button. Turn off peristaltic pump by clicking the Pump Off button.
9.11.5 Release all four peristaltic pump channel clamps and remove the tubing from the channel.
9.11.6 Remove the GLS exhaust tube from the GLS center post.
9.11.7 Turn off the gas and lamp by clicking on the instrument icon, then click analyzer. Turn the
Lamp Off and set the gas to O.
9.11.8 Close out of the software.
10.0 DATA ANALYSIS AND CALCULATIONS
10.1 Biota Samples:
Final Result(mg/kg dry weight corrected)
(Raw Result µg/L)* (Final Volume L)* (Dilution Factor)
(Sample Wt g) * (Dry Wt for soil/solid)
Biota results can be reported on an as-is wet weight basis.The dry weight correction in the formula
is then not applicable. Results in pg/g are equivalent to results in mg/kg
10.2 Dry Ice and or Blender Blank Samples:
Final Result(Total ig) = (Raw Result µg/L)* (0.05 L) * (2 Dilution Factor)
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
15 of 26

aceAna/ icaI®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
1 10.3 Quality Control Results: Calculate recoveries for the spiked analytes in LCS/LCSD and
MS/MSD samples; and Relative Percent Differences (RPD) for duplicate and MS/MSD
samples. See current revision or replacement of SOP ENV-SOP-GBAY-0153, Laboratory
Calculations for additional information.
11.0 QUALITY CONTROL AND METHOD PERFORMANCE
11.1 Initial Calibration (ICAL):
11.1.1 Frequency: A calibration must be performed daily with samples when they are prepared.
11.1.2 Acceptance Criteria: The resultant correlation coefficient must be greater than 0.995.
The calculate concentration of the low point of the calibration curve must be within ±40%
of the true value (relative error<_40%). The calculate concentration of the remainder of the
calibration curve must be within ±10% of their true value (relative error<_10%).
11.1.3 Corrective Action: If outside acceptance criteria, the problem must be corrected, the
instrument re-calibrated, and quality control within criteria achieved before continuing and
the affected samples reanalyzed.
11.2 Instrument Quality Control: Instrument QC consists of an ICV ICB, CRDL, and CCV(s)
and CCB(s).
11.2.1 Initial Calibration Verification (ICV): The ICV is a second source standard used to verify
the calibration, also known as the Quality Control Sample (QCS).
11.2.1.1 Frequency: Immediately after the ICAL and prior to sample analysis.
11.2.1.2 Acceptance Criteria: The result of the ICV must fall within the range of 90%-
110% of the true value.
11.2.1.3 Corrective Action: If outside acceptance criteria, the problem must be
corrected,the instrument re-calibrated, and quality control within criteria achieved
before continuing and the affected samples reanalyzed.
11.2.2 Continuing Calibration Verification (CCV): The CCV is the same source as the ICAL at
the midpoint of the calibration curve used to verify the calibration throughout the analytical
run.
11.2.2.1 Frequency: A CCV is analyzed prior to sample analysis, every 10 injections and
at the end of the analytical sequence.
11.2.2.2 Acceptance Criteria: CCV limits are± 10% of their expected values.
11.2.2.3 Corrective Action: If a CCV is outside of the control limits, a verification I CCV
can be immediately analyzed. If the verification CCV is outside of control limits,
the problem must be corrected, and the instrument recalibrated prior to any
reportable samples being analyzed.
11.2.3 Calibration Blanks: Calibration blanks (ICB and CCB)
11.2.3.1 Frequency: The ICB is analyzed immediately following the ICV and a CCB is
analyzed immediately following any CCV.
1 11.2.3.2 Acceptance Criteria: ICB and CCBs may not contain concentrations in excess
of the LOQ.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
1 F ,,F O

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
11.2.3.3 Corrective Action: If a blank is outside of the control limits, a verification blank
can be immediately analyzed. If the verification blank is outside of control limits,
the problem must be corrected, and the instrument recalibrated prior to any
reportable samples being analyzed.
11.2.4 Pace Reporting Limit Standard (CRDL): A standard prepared at the concentration of the
lowest calibration point.
11.2.4.1 Frequency: It is analyzed after the ICV/ICB.
11.2.4.2 Acceptance Criteria: The recovery must be within 60-140% recovery of the true
value.
11.2.4.3 Corrective Action: If a CRDL is outside of the control limits, a verification CRDL
can be immediately analyzed. If the verification CRDL is outside of control limits,
the problem must be corrected, and the instrument recalibrated prior to any
reportable samples being analyzed.
11.3 Batch Quality Control: Batch QC consists typically of a MB, LCS(LCSD), MS/MSD, and
SRM. These are prepared and analyzed with each batch of samples. A batch will consist of
up to 20 samples. In some cases, a DUP may be analyzed in a batch.
11.3.1 Method Blank: The MB is laboratory grade water and is carried through all preparation
procedures . The MB is used to verify that interferences caused by contaminants in the
solvents, reagents, glassware, etc. are known and minimized. For dissolved samples
filtered in-house, a filter blank is created. The filter blank is evaluated and qualified the
same as a method blank.
11.3.1.1 Frequency: A MB must be analyzed with each batch of samples or every 20
samples, whichever is more frequent.
11.3.1.2 Acceptance Criteria: The MB is evaluated for both positive and negative bias
and must have an absolute value less than the LOQ. For samples reporting down
to the LOD, the MB measurements are evaluated to the LOD. In these cases,
qualify applicable samples for MB measurements from >LOD to <LOQ.
11.3.1.3 Corrective Action: If the MB is greater than the LOQ, perform the following:
11.3.1.3.1 Check for errors in calculations. If an error or problem is found and
can be corrected by amending the calculations and the result falls
within the limits, accept the data and report without a qualifier flag.
11.3.1.3.2 If there is sufficient sample available and hold time remaining, re-
prepare the MB and all associated. If the MB is less than the LOQ in
this analysis, accept the second set of data. If the MB is still outside
the RL after re-analysis, contact the PM to determine the resolution.
If the client does not require additional work, report the data, applying
an appropriate flag to the samples associated with the non-compliant
MB.
11.3.1.3.3 If sufficient sample volume is not available, report the sample data
with a qualifier flag on each of the samples associated with the non-
compliant MB. Contact the project manager regarding the
occurrence.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
17nf7R

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
11.3.1.4 MB data qualifying:
11.3.1.4.1 In the absence of project specific requirements, samples with
concentrations greater than 10 times the absolute blank
measurement may be reported unqualified.
11.3.1.4.2 In the absence of project specific requirements, samples that are non-
detect may be reported unqualified if the blank measurement
demonstrates a positive bias.
11.3.1.4.3 In the absence of project specific requirements,samples that are non-
detect must be qualified if the blank measurement demonstrates a
negative bias between and including the LOD and LOQ. Non-detect
samples may not be reported with a blank negative bias greater than
the LOQ.
11.3.1.4.4 For samples that need qualification resulting from MB measurements
that are positive, apply a B data qualifier to the analyte. B = "Analyte
was detected in the associated method blank."
11.3.1.4.5 For samples that need qualification resulting from MB measurements
that are negative, apply a hand entered qualifier with the
measurement and the units. "Analyte was measured in the
associated method blank at a concentration of-#.# units."
11.3.2 Laboratory Control Spike/ Laboratory Control Spike Duplicate(LCS/LCSD):The LCS
is carried through all preparation procedures and is made from a standard different from
that of the calibration curve.
11.3.2.1 LCS Frequency: The LCS is performed at a frequency of 5%, or one per batch
of up to 20 environmental samples. An LCSD must be analyzed if there is
insufficient sample volume to perform a MS/MSD or if the client requests one.
11.3.2.2 Acceptance Criteria: For method 245.6 the acceptance criterion is 85-115%
recovery. The acceptance criterion for precision is 520% RPD.
11.3.2.3 Corrective Action: If the LCS or LCSD is outside of acceptance criterion,
reanalyze once to verify failure. If still outside the limits, determine/correct the
problem, re-digest and re-analyze the entire batch.
11.3.3 Matrix Spike/Matrix Spike Duplicate (MS/MSD): The sample used for the MS/MSD pair
is either determined by the client or selected at random from client samples as sample
volume allows. No field, filter, trip, or equipment blanks can be used for MS/MSD.
11.3.3.1 Frequency: One matrix spike and matrix spike duplicate are analyzed at a
frequency of 10% for EPA 245.6.
11.3.3.2 Acceptance Criteria: For method 245.6 the accuracy acceptance criterion is 70-
130%. The precision acceptance criterion is 520% RPD.
11.3.3.3 Corrective Action: If the MS/MSD accuracy and/or precision recoveries are
outside control limits, qualify the parent sample and MS/MSD results with an
appropriate data qualifier.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
1Rof )G

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
11.3.4 Sample Duplicate (DUP):
11.3.4.1 Frequency: Typically, the method requirements for duplicate sample analysis
are met with the use of an MSD or LCSD but based on client request a DUP(s)
may also be prepared and analyzed. Parent sample is chosen at random or
assigned by the client.
11.3.4.2 Acceptance Criteria: The precision acceptance criterion is _. 20% RPD.
11.3.4.3 Corrective Action: If the RPD is outside of acceptance criterion, then the parent
sample and DUP are given an appropriate data qualifier.
11.3.5 Standard Reference Material (SRM): An SRM is a purchased standard reference with a
documented concentration from a similar matrix (Biota) and is carried through all
preparation procedures with the samples.
11.3.5.1 Frequency: An SRM must be analyzed with each batch of samples or every 20
samples, whichever is more frequent.
11.3.5.2 Acceptance Criteria: The default acceptance criteria is±20% recovery from the
certificate of analysis provide for the SRM.
11.3.5.3 Corrective Action: The SRM is given a data qualifier stating that it the recovery
exceeds the default limits.
11.4 Hold Time:When preparation of a sample exceeds 28 days past the time of collection, notify
the project manager before proceeding. If a sample is run past 28 days after collection, flag
the result with appropriate data qualifier.
11.5 Dilution: If a sample was diluted due to matrix effects and the result is a non-detect, the
result must be qualified with appropriate data qualifier.
11.6 Method Performance
11.6.1 Method Validation
11.6.1.1 Detection Limits
Detection limits (DL) and limits of quantitation (LOQ) are established at initial
method setup and verified on an on-going basis thereafter. Refer to Pace ENV
corporate SOP ENV-SOP-CORQ-0011 Method Validation and Instrument
Verification (current revision or replacement) and to the laboratory's SOP ENV-
SOP-GBAY-0106 Determination of the LOD and LOQ (current revision or
replacement)for these procedures.
The LOD and LOQ are always adjusted to account for actual amounts used and
for dilution.
Current LOD and LOQ can be found in the Laboratory Information Management
System (LIMS) - EpicPro.
Level of Detection (LOD): The LOD is determined by the 40CFR Part 136B MDL
study. Once the 40CFR Part 136B MDL is determined it may be elevated if
deemed unrealistic as demonstrated using method blank evaluations.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
1 0 .,f 0P

®
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services,LLC
11.6.1.2 Linear Dynamic Range: This method is for determination of Hg in the range of
0.2-10 pg/L. Application may be extended to higher levels by selection of a
smaller sample size or by calibration of the analytical system across a higher
range. Since the calibration used only extends to 10 pg/L, the reportable linear
range will not exceed 10 pg/L.
11.6.1.3 Periodic performance evaluation (PE) samples
Periodic performance evaluation (PE) samples are analyzed per ENV-SOP-
GBAY-0107, PE/PT Program (most recent revision or replacement), to
demonstrate continuing competence. All results are stored in the QA office.
1 11.6.2 Analyst Qualifications and Training
Employees that perform any step of this procedure must have a completed Read and
Acknowledgment Statement for this version of the SOP in their training record. In addition,
prior to unsupervised (independent) work on any client sample, analysts that prepare or
analyze samples must have successful initial demonstration of capability (IDOC) and must
successfully demonstrate on-going proficiency on an annual basis. Successful means the
initial and on-going DOC met criteria, documentation of the DOC is complete, and the DOC
record is in the employee's training file. Refer to laboratory SOP ENV-SOP-GBAY-0094
Employee Orientation and Training Procedures (current revision or replacement)for more
information.
12.0 DATA REVIEW AND CORRECTIVE ACTION
12.1 Data Review
Pace's data review process includes a series of checks performed at different stages of the
analytical process by different people to ensure that SOPs were followed, the analytical record is
complete and properly documented, proper corrective actions were taken for QC failure and other
nonconformance(s), and that test results are reported with proper qualification.
The review steps and checks that occur as employees complete tasks and review their own work
are called primary review.
All data and results are also reviewed by an experienced peer or supervisor. Secondary review
is performed to verify SOPs were followed, that calibration, instrument performance, and QC
criteria were met and/or proper corrective actions were taken, qualitative ID and quantitative
measurement is accurate, all manual integrations are justified and documented in accordance with
the Pace ENV's SOP for manual integration, calculations are correct, the analytical record is
complete and traceable, and that results are properly qualified.
A third-level review, called a completeness check, is performed by reporting or project
management staff to verify the data report is not missing information and project specifications
were met.
Draw a single-line strikethrough for any unacceptable or changed data, then DATE and INITIAL
and provide a written explanation of the reason for the change.
Any discrepancies and issues occurring with each batch should be included on the cover sheet to
be incorporated into a narrative.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
on ,-,FO2

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
Refer to laboratory SOP ENV-SOP-GBAY-0120 Data Review and Final Report Processes (most
recent revision or replacement)for specific instructions and requirements for each step of the data
review process.
12.2 Corrective Action
Corrective action is expected any time QC or sample results are not within acceptance criteria. If
corrective action is not taken or was not successful, the decision/outcome must be documented
in the analytical record. The primary analyst has primary responsibility for taking corrective action
when QA/QC criteria are not met. Secondary data reviewers must verify that appropriate action
was taken and/or that results reported with QC failure are properly qualified.
Corrective action is also required when carryover is suspected and when results are over range.
Samples analyzed after a high concentration sample must be checked for carryover and
reanalyzed if carryover is suspected. Carryover is usually indicated by low concentration detects
of the analyte in successive samples analyzed after the high concentration sample.
Sample results at concentrations above the upper limit of quantitation must be diluted and
reanalyzed. The result in the diluted samples should be within the upper half of the calibration
range. Results less than the mid-range of the calibration indicate the sample was over diluted and
analysis should be repeated with a lower level of dilution. If dilution is not performed, any result
reported above the upper range is considered a qualitative measurement and must be qualified
as an estimated value.
13.0 POLLUTION PREVENTION AND WASTE MANAGEMENT
Pace proactively seeks ways to minimize waste generated during our work processes. Some
examples of pollution prevention include but are not limited to: reduced solvent extraction, solvent
capture, use of reusable cycletainers for solvent management, and real-time purchasing.
Regulated soil samples are to be handled in accordance with Pace SOP: ENV-SOP-GBAY-0121,
Regulated Soil Handling (current revision or replacement).
The EPA requires that laboratory waste management practice to be conducted consistent with all
applicable federal and state laws and regulations. Excess reagents, samples and method process
wastes must be characterized and disposed of in an acceptable manner in accordance with Pace's
Chemical Hygiene Plan/Safety Manual.
14.0 MODIFICATIONS
A modification is a change to a reference test method made by the laboratory. For example, changes
in stoichiometry, technology, quantitation ions, reagent or solvent volumes, reducing digestion or
extraction times, instrument runtimes, etc. are all examples of modifications. Refer to Pace ENV
corporate SOP ENV-SOP-CORQ-0011 Method Validation and Instrument Verification(current revision
or replacement)for the conditions under which the procedures in test method SOPs may be modified
and for the procedure and document requirements.
EPA method 245.6 Rev.2.3 1991; throughout the document equipment and supplies are mentioned
that have had advances in technology. This has resulted in differences in descriptions (11.2 circulating
pump) and procedures (11.6.1 Placing the aspirator inside the BOD bottle)from the method.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
21 of 26

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
EPA method 245.6 Rev.2.3 1991 Section 7.7 lists the stannous chloride solution as being made using
H2SO4. The lab uses a 10 % SnCl2 solution made up with a final acid concentration of 7% HCI. This
is based on Section 4.1.2 of Quicktrace M-7500 Automated Mercury Analyzer.
According to Method 200.3, section 8; Samples should be placed in plastic bag, sealed, and placed
on ice or refrigerated at 4 degrees Celsius. The lab practice is to have thermal preservation at 5_6°C.
The lab bases this on 40CFR Part 136, page 29808, footnote 18. While Biota is not listed as a matrix,
this is consistent with temperature references of EPA methods at 4 degrees Celsius.
According to Method 200.3, section 8; Dissection should be performed within 24 hours of collection.
This is not practical as sampling events take days or even weeks to complete. This is why the lab
prefers to have samples frozen and shipped to the lab frozen.
According to Method 200.3, section 8; Tissue can also be frozen at < -20 degrees Celsius. The lab
uses the criteria of< -10 degrees Celsius for storage of frozen biota samples.
The preparation of Stannous Chloride solution differs from EPA 245.1: automated mercury analyzers
with reduced concentration of stannous chloride have been deemed equivalent.
Prepare calibration standards as liquid standards. (This is different from Method 245.6 which specifies
preparing calibration tissues directly in a tissue matrix).
EPA 245.6 Rev.2.3 1991, section 6.10 describes a water bath as follows: The water bath should have
a covered top and capacity to sustain a water depth of 2-in. to 3-in. at 95°C+1°C. Nowhere in the
document is a temperature acceptance range given for the operating temperature of 58°C. The lab
follows the criteria of +3°C from similar methodology of SW846 7471 B Rev.2 2007 and also uses a
hot block.
For EPA 245.6 Rev.2.3 1991, the lab has chosen to use a 0.6g sample volume instead of the method
specified 0.2-0.3g in section 8.3. In section 11.1, 4 mL of conc. H2SO4 and 1 mL of conc. HNO3 are
added. The lab uses 2.0 mL of conc. H2SO4 and 0.5 mL of conc. HNO3. In section 11.2 5 mL of
potassium permanganate and 8 mL of potassium persulfate are added. The lab uses 7.5 mL of
potassium permanganate and 4 mL of potassium persulfate. The lab has established this procedure
for re-occurring project work with many years of historical.
15.0 RESPONSIBILITIES
Pace ENV employees that perform any part this procedure in their work activities must have a signed
Read and Acknowledgement Statement in their training file for this version of the SOP. The employee
is responsible for following the procedures in this SOP and handling temporary departures from this
SOP in accordance with Pace's policy for temporary departure.
Pace supervisors/managers are responsible for training employees on the procedures in this SOP and
monitoring the implementation of this SOP in their work area.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
22 of 26

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
16.0 ATTACHMENTS
16.1 Attachment I: Quality Control
16.2 Attachment II: Analyst/Technician Data Assessment
16.3 Attachment III: Flow Chart
17.0 REFERENCES
17.1 Pace Analytical Services, LLC—Green Bay, WI Quality Assurance Manual- current version.
17.2 TNI Standard, Management and Technical Requirements for Laboratories Performing
Environmental Analyses, EL-VI-2016-Rev.2.1.
17.3 EPA Method 245.1 Revision 3.0, Determination of Mercury in Water Cold Vapor Atomic
Absorption Spectrometry, 1994.
17.4 EPA Method 245.6, Revision 2.3, Determination of Mercury in Tissues by Cold Vapor Atomic
Absorption Spectrometry, April 1991.
17.5 National Research Council of Canada, Institute for National Measurement Standards,
Montreal Road, Ottawa, Ontario K1A 0R9, Canada: Dogfish Liver(DOLT-3).
18.0 REVISION HISTORY
This Version: ENV-SOP-GBAY-0014-Rev.01
Section Description of Change
ALL Updated to current corporate format.
This document supersedes the following document(s):
Document Number Title Version
ENV-SOP-GBAY-0014 Mercury Analysis of Biological Tissue Samples by Cold- 00
Vapor Atomic Absorption Spectroscopy CETAC M-7500
(EPA 245.6)
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
7' nf`IR

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services,LLC
Attachment I: Quality Control
Analytical Method i* EPA 245.6
Quality Control Measure b Frequency-5 Acceptance Criteria-5
Initial Calibration -Analyzed daily before samples -Correlation Coefficient of 0.995
-Minimum 5 standards plus a blank -%RE±40%&±10%
Initial Calibration Verification(ICV) Analyzed after calibration at a Recovery must be between 90—
concentration midway through the 110%
calibration.
Initial Calibration Blank(ICB) Analyzed after ICV pair but before Project specific or less than RL
samples. (LOWEST STANDARD IN
CURVE)
CRDL Standard Analyzed after ICV/ICB, but before 60-140%
samples.
Continuing Calibration Verification Analyzed after every 10 samples at a Project specific or recovery
(CCV) concentration midway through the between 90—110%
calibration.
Continuing Calibration Blank(CCB) After each CCV pair but before Project specific or less than RL
samples. (LOWEST STANDARD IN
CURVE)
Method Blank One per batch of samples, up to 20 Project Specific or less than the
environmental samples,whichever is LOQ(LOWEST STANDARD IN
more frequent. CURVE)
Laboratory Control Spike and -One LCS per batch of samples, up Project Specific or 85—115%
Duplicate to 20 environmental samples, with 20% RPD
whichever is more frequent.
-A LCSD is required if MS/MSD is not
performed or if requested by the
client.
Matrix Spike/Matrix Spike Duplicate One pair per batch of samples, up to Project Specific or 70—130%
10 environmental samples, with 20% RPD
whichever is more frequent.
Duplicate Upon client request or if insufficient 20% RPD
sample volume for MSD.
Standard Reference Material(SRM) One per batch of samples, up to 20 Default Limits of 80-120%
environmental samples,whichever is recovery
more frequent.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
on , F7G

(//7 'ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
Attachment II: Analyst/Technician Data Assessment
Analytical Method EPA 245.6
Data Assessment Measure . Data Assessment Corrective Action.
Initial Calibration 1
Initial/Continuing Calibration Verification 2
Initial/Continuing Calibration Blank 3
CRDL/RLVS 4
Method Blank 5
Accuracy & Precision Laboratory Control 6
Spikes
Accuracy& Precision Matrix Spike Samples 7
Precision Duplicate Sample 8
Standard Reference Material 9
Holding Time Compliance 10
1. If calibration criteria are not met, perform maintenance and recalibrate.
2. If ICV/CCV is outside the control limits reanalyze the ICV/CCV to verify the instrument is out of control. If the 2nd
analysis is outside control limits, perform maintenance and recalibrate. Samples that bracket the out of control
standards must be reanalyzed.
3. If ICB/CCB is outside the control limits reanalyze the ICB/CCB to verify the instrument is out of control. If the 2nd
analysis is outside control limits, perform maintenance and recalibrate. Samples that bracket the out of control
standards must be reanalyzed.
4. If CRDL is outside the control limits reanalyze the CRDL to verify the instrument is out of control. If the 2nd analysis
is outside control limits, perform maintenance and recalibrate.All applicable samples must be reanalyzed.
5. If not<LOQ,verify by second analysis. If second analysis confirms contamination for target analyte at or greater
than the LOQ, re-digest sample batch and batch QC provided sufficient sample volume remains. If insufficient
sample volume remains, consult with project manager and client on how to proceed. For MB detections greater
than or equal to the LOD, but less than the LOQ;qualify applicable sample results. For negative measurements
more negative than the LOD, applicable data is given the following data qualifier: "Analyte was measured in the
associated method blank at a concentration of-#.#units."
**For positive MB failures, samples that are non-detection need not be qualified. In addition, samples that are
greater than 10 times the MB detection need not be qualified.
**For negative MB failures samples that are greater than 10 times the MB detection need not be qualified.
6. Verify failure by second analysis. If second analysis confirms LCS (LCSD) failure, re-digest sample batch and
batch QC provided sufficient sample volume remains. If insufficient sample volume remains, consult with project
manager and client on how to proceed.
7. If the parent, MS,or MSD is greater than the reportable linear dynamic range, dilute and reanalyze the parent, MS,
and MSD. If the concentration of the spike is less than 25%of the concentration of the parent,the MS and MSD
recoveries are not evaluated. Any failures resulting from this are qualified appropriately. If the concentration of
the spike is greater than 25% of the concentration of the parent,appropriately qualify the parent sample if either
the MS and/or MSD fail accuracy. If the MS and MSD fail precision control limits flag the parent with the appropriate
precision data qualifier.
8. If the precision control exceeds limits flag the DUP and parent with the appropriate precision data qualifier.
9. The SRM is given a data qualifier stating that it the recovery exceeds the default limits.
10. Notify Project Manager by submitting a LabTrack Ticket and flag with the appropriate data qualifier.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
25 of 26

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Mercury Analysis of Biological Samples by CVAAS CETAC M-7500
TEST METHOD EPA 245.6
ISSUER: Pace ENV—Green Bay—GBAY
COPYRIGHT©2020 Pace Analytical Services, LLC
Attachment HI: Flow Chart
Start
t
Digest Samples, QC
Samples.
Calibrate
instrument with
I Digested Curve
Standards.
v
Analyze Samples
& QC Samples.
1
Dilute Sample No
Results
Within
Calibration
Curve?
Yes
Calculate Sample Results
CStop
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
26 of 26

aceAnaij4.ical ®
ENVIRONMENTAL SCIENCES
Document Information
Document Number: ENV-SOP-GBAY-0018 Revision: 02
Document Title: Acid Digestion of Biological Tissue by EPA 3050B Modified
Department(s):
Metals
I
Date Information
Effective Date: 09 Feb 2021
Notes
Document Notes:
All Dates and Times are listed in: Central Time Zone
,
1 of 20

Signature Manifest
Document Number: ENV-SOP-GBAY-0018 Revision: 02
Title: Acid Digestion of Biological Tissue by EPA 3050B Modified
All dates and times are in Central Time Zone.
ENV-SOP-GBAY-0018-Rev.02 Acid Digestion of Biological Tissue by EPA 3050B Modified
QM Approval
Name/Signature Title Date Meaning/Reason
Kate Verbeten (007119) Manager-Quality 08 Feb 2021,07:50:26 PM Approved
Management Approval
Name/Signature Title Date Meaning/Reason
Chad Rusch(007163) Manager 09 Feb 2021,07:25:02 AM Approved
Nils Melberg(007142) General Manager 2 09 Feb 2021,08:40:29 AM Approved
2 of 20

ace Analytical m
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
1.0 SCOPE AND APPLICATION
This standard operating procedure (SOP) describes the laboratory procedure for the acid digestion
of biological tissue and vegetation samples by method EPA 3050B Inductively Coupled Plasma
Mass Spectrometry (ICPMS).
1.1 Target Analyte List
Isotope Element Symbol Chemical Abstracts Service
Registry Number(CASRN)
27 Aluminum Al 7429-90-5
121 Antimony Sb 7440-36-0
' 75 Arsenic As 7440-38-2
137 Barium Ba 7440-39-3
9 Beryllium Be 7440-41-7
10 Boron B 7440-42-8
111 Cadmium Cd 7440-43-9
43 Calcium Ca 7440-70-29
52 Chromium Cr 7440-47-3
59 Cobalt Co 7440-48-4
63 Copper Cu 7440-50-8
54 Iron Fe 7439-89-6
7 Lithium Li 7439-93-2
208 Lead Pb 7439-92-1
25 Magnesium Mg 7439-95-4
55 Manganese Mn 7439-96-5
201 Mercury Hg 7439-97-6
95 Molybdenum Mo 7439-98-7
60 Nickel Ni 7440-02-0
31 Phosphorous P 7723-14-0
39 Potassium K 7440-09-7
78 Selenium Se 7782-49-2
107 Silver Ag 7440-22-4
23 Sodium Na 7440-23-5
88 Strontium Sr 7440-24-6
205 Thallium TI 7440-28-0 _
118 Tin Sn 7440-31-5
47 Titanium Ti 7440-32-6
238 Uranium U 7440-61-1
51 Vanadium V 7440-62-2
66 Zinc Zn 7440-66-6
1.2 Applicable Matrices: This SOP is applicable to biological tissue and vegetation samples.
1.3 Personnel: Use of this method is restricted to analysts who involved in the digestion process.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
3 of 20

J
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services,LLC
2.0 SUMMARY OF METHOD
2.1 An aliquot (0.500g to 0.575g) of sample is weighed into a digestion tube. Applicable analytes
are listed in the Target Analyte List.
2.2 The sample is acidified with nitric acid and heated on an apparatus with additions of nitric acid,
hydrogen peroxide, and hydrochloric acid.
2.3 The digestate is brought to a 50 mL final volume with reagent water, and either centrifuged,
allowed to settle, or filtered.
2.4 This process is to extract the metals from the biota matrix so it can go through multi-element
analysis by ICPMS.
3.0 INTERFERENCES
3.1 Cross contamination from standards and samples containing high concentrations is possible. It
is critical that the metals digestion (prep) lab is kept in a clean organized manner to minimize
any possible cross contamination.
3.2 Isobaric Polyatomic Interferences — Isobaric polyatomic interferences result when ions
containing more than one atom have the same nominal mass-to-charge ratio as an analyte of
interest and cannot be resolved by the instrument's spectrometer. An example includes CIO+
(mass 51), which interferes with V, and must be corrected by measuring CIO+ at mass 53.
When possible, an interference free isotope should be chosen for measurement.
3.3 Chromic acid should never be used to clean any container used in metals analysis.
3.4 Borosilicate glass in sample containers can lead to interference of Boron concentrations in
samples. This is also true of volumetric flasks, thus when dilution in the flask is complete the
standards must be removed as soon as possible from the dilution container and placed into a
clean plastic container.
4.0 DEFINITIONS
Refer to the Laboratory Quality Manual for a glossary of common lab terms and definitions.
5.0 HEALTH AND SAFETY
The toxicity or carcinogenicity of each chemical material used in the laboratory has not been fully
established. Each chemical should be regarded as a potential health hazard and exposure to these
compounds should be as low as reasonably achievable.
The laboratory maintains documentation of hazard assessments and OSHA regulations regarding
the safe handling of the chemicals specified in each method. Safety data sheets for all hazardous
chemicals are available to all personnel. Employees must abide by the health, safety and
environmental (HSE) policies and procedures specified in this SOP and in the Pace Chemical
Hygiene /Safety Manual.
Personal protective equipment (PPE) such as safety glasses, gloves, and a laboratory coat must be
worn in designated areas and while handling samples and chemical materials to protect against
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
4 of 2u

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
physical contact with samples that contain potentially hazardous chemicals and exposure to
chemical materials used in the procedure.
Concentrated corrosives present additional hazards and are damaging to skin and mucus
membranes. Use these acids in a fume hood whenever possible with additional PPE designed for
handing these materials. If eye or skin contact occurs, flush with large volumes of water. When
working with acids, always add acid to water to prevent violent reactions. Any processes that emit
large volumes of solvents (evaporation/concentration processes) must be in a hood or apparatus that
prevents employee exposure.
Contact your supervisor or local HSE coordinator with questions or concerns regarding safety
protocol or safe handling procedures for this procedure.
6.0 SAMPLE COLLECTION, PRESERVATION, HOLDING TIME, AND STORAGE
Requirements for container type, preservation, and field quality control (QC) for the common list of
test methods offered by Pace are included in the laboratory's quality manual.
Samples should be collected in accordance with a sampling plan and procedures appropriate to
achieve the regulatory, scientific, and data quality objectives for the project.
The laboratory will provide containers for the collection of samples upon client request for analytical
services. Bottle kits are prepared in accordance with laboratory SOP ENV-SOP-GBAY-0007 Bottle
Preparation.
6.1 All sample containers must be HDPE, glass, or Teflon. The containers are purchased pre-
cleaned and documented to be contaminant free. Where applicable, the bottle ware is
demonstrated to be free of target analytes. When bottle ware not originating from the lab is
used, the data may be qualified with either one or both of the following data qualifiers:
6.1.1 Sample field preservation does not meet EPA or method recommendations for this
analysis.
6.1.2 Sample container did not meet EPA or method requirements.
6.2 General Requirements
Matrix Routine Minimum
Container Sample Amount' Preservation Holding Time
Glass, Plastic,
Plastic Zip-top Thermal:�6°C;<_-10°C when frozen Removal from freezer:
Biota bags, or 5g Chemical:None 6 months,excluding Hg.
aluminum foil 28 Days if Hg requested.
'Minimum amount needed for each discrete analysis.
Thermal preservation is checked and recorded on receipt in the laboratory in accordance with
laboratory SOP ENV-SOP-GBAY-0006 Sample Management (most recent revision or replacement).
Chemical preservation is checked and recorded at time of receipt or prior to sample preparation.
Shipments of soil and water samples to the laboratory require thermal preservation in the form of
cubed, block or dry ice. At the time of laboratory receipt, proper thermal preservation is checked by
measuring the temperature of melt water or when provided the temperature blank. The Pace
Analytical acceptable temperature range is 0 to 6°C (or <_-10° for dry ice for biota samples). All
QAPjP and regulatory authority requirements become priority over this requirement.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

O
aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
After receipt, biota samples are stored at 5-10°C until sample preparation. Prepared samples
(digestates) are stored at room temperature until sample analysis.
After analysis, unless otherwise specified in the analytical services contract, samples are retained for
21 days from date of final report and then disposed of in accordance with Federal, State, and Local
regulations.
7.0 EQUIPMENT AND SUPPLIES
7.1 Equipment
Equipment* Manufacturer* Model(s)* Serial Number
Computer Dell Optiplex 755 DJG5L3J
Centrifuge Sorvall (Fisher) Legend XT 4185129
Hot Block Environmental Express SC100, SC154 various
Analytical Balance A&D HR-200 2301449
*Or Equivalent
7.2 Supplies
Supplies* Manufacturer* Vendor* Catalog
number*
50-mL Disposable Digestion Cups Mold Pro Fisher Scientific MP-115PB
Calibrated Pipette 1000 pL Eppendorf Fisher Scientific 21-371-13
Calibrated Pipette 10-50 pL Thermo Thermo 21-377-193
Calibrated Pipette 100-1000 pL Eppendorf Fisher Scientific 05-402-50
Calibrated Pipette 1000-5000 pL Eppendorf Fisher Scientific 05-402-91
Trace Metal Grade Pipette Tips 1 Eppendorf Fisher Scientific 21-372
mL
fi 21-381-198
Tips5 Eppendorf Fisher Scientific Trace Metal Grade Pipette
PPP
mL
N-DEX Nitrile Gloves Best Fisher Scientific 6005 PFM
pH Indicator Sticks Whatman MG Scientific P114-26
Plastic Spatulas (Scrapers) Coopersurgical Inc. Fisher Scientific 11080
*Or equivalent
7.3 All reusable lab ware (glass, quartz, polyethylene, PTEFE, FEP, etc.) should be sufficiently
clean for the task objectives following current revision of SOP ENV-SOP-GBAY-0143, Labware
Cleaning Procedure.
7.4 Digestion tubes — Each lot of digestion tubes has its volumetric increments validated prior to
use.
7.4.1 Each digestion tube is evaluated at the 20 mL, 25 mL, and 50 mL increments.
7.4.2 The digestion tube is first tarred and then filled to the increment to be tested and then
weighed. The weight is documented.
7.4.3 The RPD is calculated between of the average of the 4 digestion tubes for that volume
increment and the expected mass.
7.4.4 The RPD must be <2% to be acceptable for that lot and used as a measurement tool.
7.4.5 This is documented in the Metals Support Supplies Verification Logbook.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
a ,-,f'�11

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
8.0 REAGENTS AND STANDARDS
8.1 The use of any standard or reagent will be terminated if any contamination or problems arise
prior to the expiration date.
8.2 Reagents are tested to determine levels of impurities to be less than the LOD.
8.3 Reagents: Please see Section 8.5 for a list of reagents.
8.3.1 All standards, reagents, and spiking solutions are kept at room temperature. Stock
standards and reagents can be used until they expire. Refer to the most recent version
of ENV-SOP-GBAY-0145 Laboratory Supply Procedures for stock standard and
reagent expiration rules. Intermediate and working standards are given a six-month
expiration date. However, the expiration date may not extend past the earliest
expiration date of any stock standard used to create the solution. The use of any
standard or reagent will be terminated if any contamination or problems arise prior to
the expiration date.
8.4 Log-in of Standards, reagents, and spike solutions are logged as follows:
8.4.1 Stock standards have a copy of their certificate of analysis logged into the LIMS (Epic
Pro).
8.4.2 Reagents are logged in the same manner.
8.5 Reagents
Purchased Catalog Concentration/
Reagent* Alias From* Number* Purity Expiration Storage
Reagent Water Water In House NA >_18 Mega ohm Generated for use -
Hydrochloric Acid ICPMS HCI Fischer A508-P212 Plasma Pure Manufacturer's
Scientific 34-37% recommended
Nitric Acid ICPMS HNO3 Fischer A509-P212 Trace Metal expiration date or 2 Room
Scientific Grade 67-70%, years from Temp
ACS receipt/made date,
Hydrogen H202 Fischer H325-4 Trace Metals whichever is sooner
Peroxide Scientific Grade 30%
*Or Equivalent
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
7, f• n

Face Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021Pace Analytical Services,LLC
Stock Standards
Standard/Reagent* Alias Purchased From* Catalog Concentration/Purity Expiration Storage
Number*
As,Ba,Be,Cd,Co,
Basic High Purity HP-7379- 200 mg/L Cr,Cs,Cu, Li,Mn,Ni,
Metals Secondary Source 1 HNO3 Standards 500 Pb,Se,Sr, U,V,Zn
100 mg/L Ag,TI
Custom High Purity HP7376- B,Mo,Pd,Pt,Sb,Sn,
Metals Secondary Source 2 Inorganic 200 mg/L
Standard Standards 500 Ti,Zr
Metals Secondary Source 3 Major High Purity HP7375- 1000 mg/L AI,Ca,K,Mg,Na,S
Cations Standards 500 500 mg/L Fe,P,Si
High Purity HP100033
Mercury Secondary Source Hg-SPK Standards -1100 1,000 pg/mL Hg
Thallium Secondary Source TI-SPK Agilent ICP-081 1,000 mg/L TI Manufacturer's
Iron Secondary Source Fe-SPK Agilent ICP-126 10,000 mg/L Fe
om
Temp Remp
Phosphorus Secondary Source P-SPK Agilent ICP-115 10,000 mg/L P
Potassium Secondary Source K-SPK Agilent ICP-119 10,000 mg/L K
Boron Secondary Source B-SPK Agilent ICP-005 1,000 mg/L B
Zinc Secondary Source Zn-SPK Agilent ICP-030 1,000 mg/L Zn
Sodium Secondary Source Na-SPK Agilent ICP-111 10,000 mg/L Na
Magnesium Secondary Source Mg-SPK Agilent ICP-112 10,000 mg/L Mg
Nitric Acid IHNOS Fisher Scientific P�2 Trace Metal Grade 67-70%,ACS
Reagent Water Water In House NA >_18 Mega ohm Generated for
use
*Or Equivalent
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
4 ..f.1rl

(/ 2Yt
TEST METHOD STANDARD OPERATING PROCEDURE I
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
8.6 Working Standards
Stock or Final Volume Diluent Final Concentration Expiration Storage
Standard Alias Amount Used (W/Diluent)
Intermediate
As, Ba, Be, Cd, Co, Cr,
10 ppm Cs, Cu, Li, Mn, Ni, Pb,
Basic HNO3 Se, Sr, U, V,Zn
5.0mL 5 ppm Ag, TI
Custom B, Mo, Pd, Pt, Sb, Sn, Ti,
Inorganic 10 ppm Zr
Standard Earliest composed
500 ppm AI, Ca, K, Mg, Na, S
Biota Spike* 6000-SPKB Major Cations 50 mL 100mL Water 250 ppm Fe, P, Si of manufacturer's, Room
not to exceed 6 Temp
P-SPK 7.5 mL 750 ppm P months.
K-SPK 15 mL 2,000ppm K
Fe-SPK 2.5 mL 250 ppm Fe
TI-SPK 0.5 mL 5 ppm TI
HG-SPK 0.025 mL 250 ppb Hg
ICPMS HNO3 6.0mL 6% HNO3
B-STK 0.25mL 2.5mg/L B
Zn-STK 0.75mL 7.5mg/L Zn
Earliest composed
Na-STK 3.75mL 375mg/L Na of manufacturer's,
Boita Spike 2 6000-SPKB2 100mL Water
Mg-STK 3.75mL 375mg/L Mg not to exceed 6Room Temp
months.
K-STK 12.75mL 2375mg/L K
ICPMS HNO3 6mL 1% HNO3
*NOTE: In the event of Spike solution instability this list may be more than one solution. (The spike
levels are a summary of volumes and concentrations and due to stability and compatibility of the source
standards will be in multiple bottles)
Anyprinted copyof this SOP and all copies of this SOP outside of Pace are uncontrolled
p copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
0„{on

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
9.0 PROCEDURE
9.1 Calibration Procedures:
9.1.1 Analytical Balance Calibration
9.1.1.1 Annual Calibration —The balance must be calibrated at least annually by an
outside agency and checked daily before each use using Class 1 or 2
weights. Refer to Pace SOP ENV-SOP-GBAY-0115 Support Equipment
(most recent revision or replacement).
9.1.1.2 Daily Calibration Check
9.1.1.2.1 Clean the balance and surrounding area prior to starting the daily
calibration check.
9.1.1.2.2 Check the sight level on the balance. If it needs adjusting, level
the balance.
9.1.1.2.3 The weight set ID indicated in the logbook is used as the primary
set. If an alternate weight set ID is used, that ID must be recorded
in the comment section of the balance calibration logbook for that
day.
9.1.1.2.4 Tare the balance before weighing the NIST certified weights.
9.1.1.2.5 Use forceps or other means to lift each weight (Do not touch the
weights with fingertips as the residue may artificially adjust the true
value of the weights). Record the date of the calibration check, the
true value of the weight, and the actual measured weight in the
logbook. Repeat this procedure for the other certified weights. If
calibration weights differ from the certified weights by more than
specified in the balance calibration logbook, corrective action must
be taken.
9.1.1.3 Corrective Action
9.1.1.3.1 Clean the balance and balance pan. Check the sight level on the
balance and adjust if necessary. Re-tare and reweigh all the
certified weights.
9.1.1.3.2 The internal calibration function (if available) of the balance may be
used as a means of corrective action.
9.1.1.3.3 Utilize the internal calibration function and diagnostics. Refer to
instrument manual.
9.1.1.3.4 Contact the QA office for assistance if the balance does not meet
the calibration tolerances.
9.1.1.3.5 If the above action does not correct the problem, the balance
should be taken out of service and appropriately labeled to avoid
improper usage. A service technician should be contacted.
9.1.1.3.6 Record any corrective action. Initial and date all entries in the
logbook.
9.1.2 Thermometer - See the most recent revision of the SOP ENV-SOP-GBAY-0115,
Support Equipment for thermometer calibration and validation.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
9.1.3 Pipette/Bottle Top Dispenser - See the most recent revision of the SOP ENV-SOP-
GBAY-0115, Support Equipment for volumetric dispensing device calibration and
validation.
9.2 Digestion Procedures:
9.2.1 Heat hot block at 95°C ± 5°C (verify temperature with a calibrated thermometer). A
random well is used for each verification. The block has a full temperature evaluation
performed minimally each year. The temperature will be record in the Electronic Prep
Log in accordance with EPIC Pro Training Module 16: Electronic Prep Log Guide
(most recent revision or equivalent).
9.2.2 Batch samples in the LIMS. Identify QC samples at the frequency stated in the Quality
Control Section of this SOP. Additional samples may be added to the batch, so long as 1
the total sample number in the batch does not exceed 20. The digestion of the
additional samples must begin within eight hours of the start of the original digestion.
9.2.3 Log into the Electronic Prep Log. Create a new prep sheet using the
3050B1ICP_ICPMS Soil Template and the LIMS Batch HBN.
9.2.4 Verify sample IDs and LIMs numbers on containers against the prep sheet.
9.2.5 To the extent possible, mix and crush the sample as per SOP ENV-SOP-GBAY-0129,
Sample Homogenization, Compositing, and Sub-sampling (most recent revision or
replacement), in the sample container with a disposable plastic spatula to achieve
homogeneity. Tissue samples with sufficient sample volume are typically blended with
liquid nitrogen to achieve a light fluffy texture. Small volume tissue samples and
vegetative samples may be cut up.
9.2.6 Prepare Method Blank (MB) by leaving the digestion tube empty.
9.2.7 Prepare a Solid Matrix Blank (typically chicken) by weight 0.500-0.504g of blended
chicken into one digestion tube. Record sample weight in digestion log.
9.2.8 Prepare an SRM by weighing exactly 0.500g of the SRM into one digestion tube.
Record sample weight in digestion log.
9.2.9 Prepare Laboratory Control Spike (LCS) by weighing —0.500g of solid matrix material
(typically chicken) in digestion tube. Add 1.0 mL of the Biota Spike and 1.0 mL of the
Biota Spike Ag to the LCS digestion tube. Spikes may be adjusted based on client
requests.
9.2.10 Laboratory Spike Duplicate (LCSD) if there is insufficient volume for an MS/MSD. The
LCSD may be required per client request.
9.2.11 Prepare Matrix Spike / Matrix Spike Duplicate (MS/MSD), by weighing 0.500 to 0.504
grams of parent sample into 3 separate digestion tubes. Record sample weight to
nearest 0.001 gram on digestion log. Parent, MS, and MSD should be approximately
the same weight. Add 1.0 mL of the Biota Spike and 1.0 mL of the Biota Spike Ag to
the MS/MSD digestion tubes. Spikes may be adjusted based on client request.
9.2.12 Weigh 0.500 to 0.575g of homogenized sample into a labeled digestion tube. Record
sample weight to nearest 0.001 g on digestion log. Do this for each sample in the
digestion batch. Record all information in the Electronic Prep Log worksheet. Note: If
a sample contains a significant amount of water a larger mass may be used.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

ace AnaI ical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
9.2.13 CONTINUE DIGESTION IN HOOD.
9.2.14 Add small amount of water (2mL) to digestion tube (to cover bottom). Swirl to keep
sample from sticking to the tube.
9.2.15 Add 10 mL 1:1 HNO3 using a calibrated repipettor. Cover with watch glass and swirl
gently to mix.
9.2.16 To make 1:1 HNO3, add 1-part HNO3 to 1-part water.
9.2.17 Heat the samples at 95°C ± 5°C for 2 hours. Maintain a covering of solution over the
bottom of the tube at all times. Remove from hot block and cool in hood.
9.2.18 CAUTION: DO NOT BOIL AT ANY TIME DURING DIGESTION.
9.2.19 This may result in metals volatilizing which would require starting the digestion over.
9.2.20 Add 2.5 mL 30% H202 using a calibrated repipettor.
9.2.21 CAUTION: DO NOT ALLOW LOSS OF SAMPLE DUE TO EXCESSIVE
EFFERVESCENCE.
9.2.22 If sample loss occurs the sample must be re-digested.
9.2.23 Reaction may be controlled by the addition of water.
9.2.24 Remove from Hot Block and cool.
9.2.25 Add 2.5 mL 30% H202 using a calibrated repipettor.
9.2.26 Cover with watch glass, swirl gently to mix, and heat in hot block to start peroxide
reaction. Heat the samples at 95°C ± 5°C until effervescence subsides (no more
bubbling). Maintain a covering of solution over the bottom of the tube at all times.
Remove from hot block and cool in hood.
9.2.27 Add 2.5mL of Concentrated HCI and heat until the fuming subsides (minimum of 20
min).
9.2.28 Allow samples to cool to room temperature.
9.2.29 Biota samples tend to completely dissolve in the digestion solution.
9.2.30 Bring samples to final volume of 50 mL with water.
9.2.31 If needed, centrifuge all samples and batch QC for 10 minutes at 750 rpm. Samples
are now ready for analysis.
10.0 DATA ANALYSIS AND CALCULATIONS
10.1 Not applicable to this SOP.
11.0 QUALITY CONTROL AND METHOD PERFORMANCE
11.1 A batch will consist of 20 or fewer samples. Batch Quality Control will include a Method Blank
(MB), Laboratory Control Spike (LCS), Matrix Spike (MS), Matrix Spike Duplicate (MSD), Post
Digestion Spike (PDS), and a Serial Dilution (SD). It may also include a Laboratory Control
Spike Duplicate (LCSD) and/or Standard Reference Material (SRM).
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
11.1.1 The Method Blank is used to verify that interferences caused by contaminants in the
solvents, reagents, glassware, etc. are known and minimized. The method blank is
processed through all clean-ups, etc., which were performed on the samples in the
batch. For a method blank to be acceptable, in the absence of project specific criteria,
the concentration shall not be higher than the highest of the following: The reporting
limit, or ten percent of the regulatory limit of concern for that analyte, or ten percent of
the measured concentration in a particular sample of interest. Each sample in the batch
is assessed against the above criteria to determine if the sample results are
acceptable. Any sample associated with an unacceptable blank is either flagged, re-
prepped for analysis, or if re-prepping is not an alternative, the results are reported with
the appropriate data qualifying codes.
11.1.2 LCS: A laboratory control sample (LCS) consists of a control matrix, which has been
spiked, with the elements(s) of interest. Laboratory Control Samples are analyzed at a
minimum of 1 per batch of 20 or fewer samples or preparation method. Results of the
LCS are expressed in terms of percent recovery and are used to determine batch
acceptance.
11.1.3 An LCS Duplicate may be analyzed to evaluate laboratory precision. The LCSD must
also meet the criteria for the LCS. The Relative Percent Difference (RPD) will be
calculated between the LCS and LCSD.
NOTE: In the event where adequate sample is not supplied by the client to
perform a Matrix Spike/ Matrix Spike Duplicate, the LCS and duplicate can lend
insight on the precision of the analysis.
11.1.4 MS/MSD: Matrix spikes (MS and MSD) are performed to evaluate the effect of the
sample matrix upon analytical methodology. A separate aliquot of sample is spiked with
the element of interest and analyzed with the sample.
11.1.4.1 MS and MSD are performed at a minimum frequency of one pair in 20
samples per matrix type per sample preparation.
11.1.4.2 MS and MSD are done more frequently where regulations and client
requests require.
11.1.4.3 The RPD between the MS and MSD is evaluated.
11.1.4.4 A matrix effect is indicated if the LCS data are within acceptance criteria, but
the matrix spike data exceed the acceptance criteria. Prior to calculating
recovery, the parent sample concentration (results <Reporting MDL = 0) is
subtracted from the spike aliquot concentrations.
11.1.5 DUP — A Laboratory Duplicate is performed by client request; and is performed on a
second aliquot of sample to evaluate consistency in the analytical procedure and in the
sample matrix.
11.1.6 SRM — A Standard Reference Material is typically prepared and analyzed upon client
request. It is a sample of known concentration chosen to resemble the matrix being
analyzed.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
11.2 Method Performance
11.2.1 Detection Limits
11.2.1.1 Detection limits (DL) and limits of quantitation (LOQ) are established at initial
method setup and verified on an on-going basis thereafter. Refer to Pace
ENV corporate SOP ENV-SOP-CORQ-0011 Method Validation and
Instrument Verification and to the laboratory's SOP ENV-SOP-GBAY-0106
Determination of LOD and LOQ (most recent revision or replacement) for
these procedures.
11.2.1.2 The LOD and LOQ are always adjusted to account for actual amounts used
and for dilution.
11.2.1.3 Current LOD and LOQ can be found in the Laboratory Information
Management System (LIMS) - EpicPro.
11.2.1.4 Level of Detection (LOD): The LOD is determined by the 40CFR Part 136B
MDL study. Once the 40CFR Part 136B MDL is determined it may be
elevated if deemed unrealistic as demonstrated using method blank
evaluations.
11.2.2 Periodic performance evaluation (PE) samples are analyzed per ENV-SOP-
GBAY-0107, PE/PT Program (current revision or replacement), to
demonstrate continuing competence. All results are stored in the QA office.
At a minimum, these are performed twice a year for the aqueous and soil
matrices.
11.3 Analyst Qualifications and Training
Employees that perform any step of this procedure must have a completed Read and
Acknowledgment Statement for this version of the SOP in their training record. In addition, prior
to unsupervised (independent) work on any client sample, analysts that prepare or analyze
samples must have successful initial demonstration of capability (IDOL) and must successfully
demonstrate on-going proficiency on an annual basis. Successful means the initial and on-going
DOC met criteria, documentation of the DOC is complete, and the DOC record is in the
employee's training file. Refer to laboratory SOP ENV-SOP-GBAY-0094 Orientation and
Training Procedures (most recent revision or replacement)for more information.
12.0 DATA REVIEW AND CORRECTIVE ACTION
12.1 Data Review
Pace's data review process includes a series of checks performed at different stages of the
analytical process by different people to ensure that SOPs were followed, the analytical record is
complete and properly documented, proper corrective actions were taken for QC failure and
other nonconformance(s), and that test results are reported with proper qualification.
The review steps and checks that occur as employees' complete tasks and review their own
work are called primary review.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
4A ..F 7„

ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
An experienced peer or supervisor also reviews all data and results. Secondary review is
performed to verify SOPs were followed, that calibration, instrument performance, and QC
criteria were met and/or proper corrective actions were taken, qualitative ID and quantitative
measurement is accurate, all manual integrations are justified and documented in accordance
with the Pace ENV's SOP for manual integration, calculations are correct, the analytical record is
complete and traceable, and that results are properly qualified.
Reporting performs a third-level review, called a completeness check, or project management
staff to verify the data report is not missing information and project specifications were met.
Refer to laboratory SOP ENV-SOP-GBAY-0120 Data Review and Final Report Processes (most
recent revision or replacement) for specific instructions and requirements for each step of the
data review process.
Draw a single-line strikethrough for any unacceptable or changed data, then DATE and INITIAL
and provide a written explanation of the reason for the change.
Data are validated and peer reviewed by lab personnel using a batch cover sheet attached to
the raw data and filed.
Any discrepancies and issues occurring with each batch should be included on the cover sheet
to be incorporated into a narrative.
12.2 Corrective Action
Corrective action is expected any time QC or sample results are not within acceptance criteria.
If corrective action is not taken or was not successful, the decision/outcome must be
documented in the analytical record. The primary analyst has primary responsibility for taking
corrective action when QA/QC criteria are not met. Secondary data reviewers must verify that
appropriate action was taken and/or that results reported with QC failure are properly qualified.
12.2.1 Data assessment/Corrective action
Data Assessment Measure If these conditions are not achieved
MB I 1
LCS/LCSD I 2
MS/MSD I 3
DUP I 4
SRM I 5
1. If not<LOQ,verify by second analysis. If second analysis confirms contamination for target analyte at or greater than
the LOQ, re-digest sample batch and batch QC provided sufficient sample volume remains. If insufficient sample
volume remains,consult with project manager and client on how to proceed. For MB detections greater than or equal
to the LOD, but less than the LOQ;qualify applicable sample results.For negative measurements more negative than
the LOD,applicable data is given the following data qualifier: "Analyte was measured in the associated method blank
at a concentration of-#.#units."
*For positive MB failures,samples that are non-detection need not be qualified. In addition,samples that are greater
than 10 times the MB detection need not be qualified.
*For negative MB failures samples that are greater than 10 times the MB detection need not be qualified.
2. Verify failure by second analysis. If second analysis confirms LCS(LCSD)failure,re-digest sample batch and batch
QC provided sufficient sample volume remains. If insufficient sample volume remains,consult with project manager
and client on how to proceed.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

U
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
3. If the parent,MS,or MSD is greater than the reportable linear dynamic range,dilute and reanalyze the parent,MS,and
MSD. If the concentration of the spike is less than 25%of the concentration of the parent,the MS and MSD recoveries
are not evaluated. Any failures resulting from this are qualified appropriately. If the concentration of the spike is
greater than 25%of the concentration of the parent,appropriately qualify the parent sample if either the MS and/or
MSD fail accuracy. If the MS and MSD fail precision control limits flag the parent with the appropriate precision data
qualifier.
4. If the DUP fails precision control limits flag the parent with the appropriate precision data qualifier
5. Outside of client specific criteria,the SRM is digested and analyzed only to demonstrate analyte recovery in a standard
reference material. When the recovery is outside the lab generated statistical limits,the element that failed recovery
will be flagged in the samples for the element that failed.Client specific action may also exist. A specific SRM may also
be requested by the client and with the lack of statistical evaluation of an SRM the default calculations of the existing
SRM will be used due to software limitations.
1 13.0 POLLUTION PREVENTION AND WASTE MANAGEMENT
Pace proactively seeks ways to minimize waste generated during our work processes. Some
examples of pollution prevention include but are not limited to: reduced solvent extraction, solvent
capture, use of reusable cycletainers for solvent management, and real-time purchasing.
The EPA requires that laboratory waste management practice to be conducted consistent with all
applicable federal and state laws and regulations. Excess reagents, samples and method process
wastes must be characterized and disposed of in an acceptable manner in accordance with Pace's
Chemical Hygiene Plan/Safety Manual.
For further information on waste management, consult ENV-SOP-GBAY-0125 Waste Handling and
Management(most recent revision or replacement).
14.0 MODIFICATIONS
A modification is a change to a reference test method made by the laboratory. For example, changes
in stoichiometry, technology, quantitation ions, reagent or solvent volumes, reducing digestion or
extraction times, instrument runtimes, etc. are all examples of modifications. Refer to Pace ENV
corporate SOP ENV-SOP-CORQ-0011 Method Validation and Instrument Verification for the
conditions under which the procedures in test method SOPs may be modified and for the procedure
and document requirements.
14.1 The elements listed in the scope as reportable from analysis of this digest is more extensive
that those listed in SW846 3050B Rev.2 1996. All elements reported from this digestion
procedure have passed the necessary method performance criteria. This includes MDL, IDOC,
CDOC, and double-blind performance samples.
14.2 SW846 3050B Rev.2 1996 section 4.8 describes the Heating source as Adjustable and able to
maintain a temperature of 90-95°C. The lab follows the temperature criteria in the Procedure
section 7.2 of 95°C±5°C.
14.3 Digestion occurs in 50 mL digestion tubes. These offer more refluxing action than a beaker
even when uncovered. Digestion occurs with a ribbed watch glass. This allows for added
refluxing while still allowing volume reduction. This is why the procedure uses the time limits
instead of the volume reductions.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
"Ibot"LU

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
14.4 The sample is not dried, ground, and sieved prior to digestion. The sample aliquot has been
adjusted to use 0.500 — 0.575 g in place of 1.0 g. All standards and reagents have been
reduced to ensure that the ratios are still consistent with the procedure.
14.5 If a client fails to provide sufficient volume for the method required Matrix Spike/Matrix Spike
Duplicate (MS/MSD), the laboratory will analyze a Laboratory Control Spike Duplicate to
demonstrate precision. The analytical batch will be qualified with the "M5"data qualifier.
14.6 SW846 3050B Rev.2 1996 section 6.3 describes storage as: Non-aqueous samples should be
refrigerated upon receipt and analyzed as soon as possible. No target temperature or range is
specified. The lab practice is to have thermal preservation at 5.6°C. This is based on 40CFR
Part 136, page 29808, footnote 18. Chapter Three Rev. 4 2007 TABLE 3-2 while not providing
a temperature for most metals, does provide a storage temperature for Hg and Hexavalent Cr
in solids of .6°C.
14.7 SW846 3050B Rev.2 1996 was written targeting a wet sample amount of 2.0 g. The lab targets
0.50 g of sample. The acid and peroxide reagent volumes used have been adjusted to the
maximum amount used in the method resulting in a final acid matrix of 10% HNO3 and 5% HCI.
This is a very high acid matrix but provides an aggressive digestion while maintaining
consistent acid matrix that is required for analysis. This also keeps the acid matrix consistent
with batch QC and method QC such as LOD studies.
14.8 SW846 3050B Rev.2 1996 Section 7.2 describes the HNO3 addition being done in multiple
steps. First a 1:1 addition followed by subsequent additions of concentrated HNO3. The lab
SOP is to add all of the HNO3 in a single step but maintain the amount of acid digesting the
sample during the 2-hour digest in this section. Samples that are visibly high organic material or
continue to give off brown fumes at the end of the Section 7.2 2-hour heating period will be re-
set with a lower sample volume that is more applicable to the acid amounts being used.
14.9 SW846 3050B Rev.2 1996 section 7.5 and 7.5.2 both have the final step in the digestion
process as filtering. The lab will centrifuge the samples to eliminate/minimize and undissolved
solids present after digestion. This reduces the possibility of increasing the background for
target elements. There are only a few instances where there is any solid or sediment remaining
after the digestion is complete.
15.0 RESPONSIBILITIES
Pace ENV employees that perform any part this procedure in their work activities must have a signed
Read and Acknowledgement Statement in their training file for this version of the SOP. The
employee is responsible for following the procedures in this SOP and handling temporary departures
from this SOP in accordance with Pace's policy for temporary departure.
Pace supervisors/managers are responsible for training employees on the procedures in this SOP
and monitoring the implementation of this SOP in their work area.
16.0 ATTACHMENTS
Attachment I: Flowchart
Attachment II: Biota Batch QC on Instrument Concentrations
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

(5ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services, LLC
17.0 REFERENCES
17.1 Pace Analytical Services, LLC—Green Bay, WI Quality Assurance Manual - current version.
17.2 TNI Standard, Management and Technical Requirements for Laboratories Performing
Environmental Analyses, EL-VI-2016-Rev.2.1.
17.3 USEPA, SW-846, Method 3050B, "Acid Digestion of Sediments, Sludges, and Soils",
December 1996.
18.0 REVISION HISTORY
This Version: ENV-SOP-GBAY-0018-Rev.02
Section Description of Change
9.2.5 and Add second addition of H202 to flowchart.
Attachment
II
This document supersedes the following document(s):
Document Number Title Version
ENV-SOP-GBAY-0018 Acid Digestion of Biological Tissue by EPA 3050B 00
Modified
ENV-SOP-GBAY-0018 Acid Digestion of Biological Tissue by EPA 3050B 01
Modified
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050B Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021Pace Analytical Services, LLC
Attachment I: Flow chart for Biota Digestion Method
CStar) Add 2.5mL of Concentrated
Remove from block and allow HCl to each digestion tube.
1 I to cool.
Turn on Hot blocks
that will be used. 1
1 Heat batch on block until
Add 2.5mL of 30% H202 — fuming subsides.
Create new page in Make sure samples do not
Electronic Prep Log using effervesce excessively
the solids prep template and Remove from block and allow
batch HBN. Document the to cool.
prep procedure here. J Again, place the batch on the
1 Hot Block and heat until
peroxide reaction is complete.
Weigh out solid matrix for i
Solid Matrix Blank and LCS. Bring samples to a final volume of
1 Remove from block and allow to cool. 50mL with Nano Pure Water.
Samples are ready for analysis.
Weigh out two additional
sample aliquots for MS/MSD
prep. Add 2.5mL of 30% H202 —
1 Make sure samples do not
effervesce excessively
Finish documenting procedure
Weigh out representative 1 in the Electronic Prep Log and
sample amounts. (0.5-.575g) save.
Again, place the batch on the
it' Hot Block and heat until
peroxide reaction is complete. 1
Add —2mL Nano-Pure Water
and 10mL 1:1 HNO3. /Post digestion information from\
Electronic Prep Log to the
if LIMS, get peer review, and
clone for analytical batch.
Remove from block and allow J
Heat samples and QC for two i to cool.
hours covered w/ a ribbed
watchglass.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
la ,-f•In

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Acid Digestion of Biological Tissue by EPA 3050B Modified
TEST METHOD SW-846 3050E Modified
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2020-2021 Pace Analytical Services,LLC
Attachment II: Biota Batch QC on Instrument Concentrations
Element LCS/ LCS/LCSD MS/MSD MS/MSD
LCSD Limits(%) Amount Limits (%)
(PPb) (PPb)
Aluminum 10,000 80-120 10,000 75-125
Antimony 200 80-120 200 75-125
Arsenic 200 80-120 200 75-125
Barium 200 80-120 200 75-125
Beryllium 200 80-120 200 75-125
Boron 200 80-120 200 75-125
Cadmium 200 80-120 200 75-125
Calcium 10,000 80-120 10,000 75-125
Chromium 200 80-120 200 75-125
Cobalt 200 80-120 200 75-125
Copper 200 80-120 200 75-125
Iron 10,000 80-120 10,000 75-125
Lithium 200 80-120 200 75-125
Lead 200 80-120 200 75-125
Magnesium 10,000 80-120 10,000 75-125
Manganese 200 80-120 200 75-125
Mercury 5 80-120 5 75-125
Molybdenum 200 80-120 200 75-125
Nickel 200 80-120 200 75-125
Phosphorus 20,000 80-120 20,000 75-125
Potassium 40,000 80-120 40,000 75-125
Selenium 200 80-120 200 75-125
Silver 100 80-120 100 75-125
Sodium 10,000 80-120 10,000 75-125
Strontium 200 80-120 200 75-125
Thallium 200 80-120 200 75-125
Tin 200 80-120 200 75-125
Titanium 200 80-120 200 75-125
Uranium 200 80-120 200 75-125
Vanadium 200 80-120 200 75-125
i
NOTE: In the event of Spike solution instability this list may be more than one solution. Elements
may be added due to requests by clients for additional tests. The typical IDL, LOD, LOQ, LDR,
DOCs, and any applicable PE tests will be performed before reporting the elemental additions.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
'A,f%1 1

aceAnaIyticaI ®
ENVIRONMENTAL SCIENCES
Document Information
Document Number: ENV-SOP-GBAY-0129 Revision: 03
Document Title: Sample Homogenization, Compositing and Sub-Sampling
Department(s): Other
Date Information
Effective Date: 09 Feb 2021
Notes
Document Notes:
All Dates and Times are listed in: Central Time Zone

Signature Manifest
Document Number: ENV-SOP-GBAY-0129 Revision: 03
Title: Sample Homogenization, Compositing and Sub-Sampling
All dates and times are in Central Time Zone.
ENV-SOP-GBAY-0129-Rev.03 Sample Homogenization, Compositing and Sub-Sampling
QM Approval
Name/Signature Title Date € Meaning/Reason
Kate Verbeten (007119) Manager-Quality 08 Feb 2021, 07:26:11 PM Approved
Management Approval
Name/Signature Title Date Meaning/Reason
Nils Melberg(007142) General Manager 2 09 Feb 2021, 08:41:28 AM Approved
Christopher Haase(007121) Manager 09 Feb 2021,01:28:41 PM Approved
of 10

1
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Sample Homogenization, Compositing and Sub-Sampling
TEST METHOD NA
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2002-2021 Pace Analytical Services, LLC
1.0 SCOPE AND APPLICATION
This standard operating procedure (SOP) describes the laboratory procedure for homogenizing soil,
liquid, and biota samples to obtain a representative sample aliquot used for analysis or composite.
This procedure is restricted to use by, or under the supervision of, technicians experienced in the
preparation of samples.
2.0 SUMMARY OF METHOD
Solid, liquid, or biological samples are thoroughly mixed or blended to ensure that any aliquots taken
are representative of the sample as a whole. The samples are mixed in either their original containers
or, in the event that original container does not allow for adequate mixing, transferred to an inert
container for thorough homogenization.
Necropsy and/or filleting of whole-body animals may be performed to isolate the individual organs or
portions of the specimen to be homogenized and utilized for analysis.
This SOP involves instruction to chop, grind, and blend plant materials, biological tissue, sediment and
synthetic materials into a homogenized sample compatible with preparation of semi volatile organic
extracts and metals digestates.
Analysts must make reasonable judgments when sub-sampling materials in order to obtain a
homogenous, representative aliquot of the material. Because of the nature of environmental samples,
the analyst may have to treat samples on a case-by-case basis ensuring that all aspects of the
analytical method are performed. In the event that the analyst cannot reasonably determine what
constitutes a representative sample, the project manager or supervisor must be involved so that the
client can help ensure an appropriate representative aliquot is utilized.
3.0 INTERFERENCES
Metallic Devices—Samples to be analyzed for metal constituents must not be homogenized using any
metallic mixing devices or containers as it may result in contamination of the sample with a variety of
metals. Use only glass, plastic or ceramic materials when working with these sample types. This may
not be applicable for tissue samples since metallic devices (blenders, etc.) may be necessary for
grinding and chopping prior to sample homogenization.
Plastic Devices — Samples to be analyzed for organic constituents must not be homogenized using
any plastic mixing devices or containers as it may result in both positive and negative interferences.
Use only glass and ceramic devices when working with these sample types. Metal instruments may
also be used if analysis for metals is not required from the same sample
Solvents, reagents, glassware, and other sample processing hardware may yield discrete artifacts
and/or elevated baselines causing misinterpretation of the analytical results. All these materials must
be free from interferences under the conditions of the analysis, demonstrated by performing method
blanks.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
'1.,f10

ace Analytical®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Sample Homogenization, Compositing and Sub-Sampling
TEST METHOD NA
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2002-2021 Pace Analytical Services, LLC
4.0 DEFINITIONS
Refer to the Laboratory Quality Manual for a glossary of common lab terms and definitions.
Biota-the flora or fauna of a region.
Composite-combining the typical or essential characteristics of individuals, making up a group.
Fillet- to cut an edible portion of fish. This may or may not contain the ribcage and belly flap and is
dependent upon the regulatory, scientific, and data quality objectives for the project.
Head-the upper or anterior division of the animal body that contains the brain, the chief sense organs,
and the mouth.
5.0 HEALTH AND SAFETY
The toxicity or carcinogenicity of each chemical material used in the laboratory has not been fully
established. Each chemical should be regarded as a potential health hazard and exposure to these
compounds should be as low as reasonably achievable.
The laboratory maintains documentation of hazard assessments and OSHA regulations regarding the
safe handling of the chemicals specified in each method. Safety data sheets for all hazardous
chemicals are available to all personnel. Employees must abide by the health, safety and
environmental (HSE) policies and procedures specified in this SOP and in the Pace Chemical Hygiene
/ Safety Manual.
Personal protective equipment (PPE) such as safety glasses, gloves, and a laboratory coat must be
worn in designated areas and while handling samples and chemical materials to protect against
physical contact with samples that contain potentially hazardous chemicals and exposure to chemical
materials used in the procedure. Hearing protection should be worn when a blender is in operation, or
during sediment processing when applicable.
Liquid Nitrogen presents additional hazards and may cause cryogenic burns or displace oxygen and
cause rapid suffocation. Use in a well-ventilated area with additional PPE designed for handing these
materials.
Contact your supervisor or local HSE coordinator with questions or concerns regarding safety protocol
or safe handling procedures for this procedure.
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
d of 1Q

aceAnalytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Sample Homogenization, Compositing and Sub-Sampling
TEST METHOD NA
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2002-2021 Pace Analytical Services, LLC
6.0 SAMPLE COLLECTION, PRESERVATION, HOLDING TIME, AND STORAGE
The laboratory does not perform sample collection for this procedure. Samples should be collected in
accordance with a sampling plan and procedures appropriate to achieve the regulatory, scientific, and
data quality objectives for the project. The laboratory will record any nonconformance to these
requirements in the laboratory's sample receipt record.
Details concerning sample shipping, preservation and storage can be found in the applicable extraction
and/or analytical SOPs, or as specifically discussed below. Samples must be stored separately from
all standards and reagents. Where possible, samples for trace analysis should be segregated from
highly contaminated samples to avoid cross contamination. Food or drink products must always be
kept away from samples and never stored in the same area with samples.
Biota samples must be kept frozen at .-10°C in their original sample containers until the
homogenization process occurs.
Small rodents must undergo a special procedure to destroy any Hantavirus which may be present.
Refer to the Pace SOP: ENV-SOP-GBAY-0130 Small Rodent Handling and Homogenization (most
recent revision or replacement)for details.
After homogenization, biota samples are kept frozen at 5..-10°C in glass jars sized closest to the
prepared homogenate sample volume. Individual jars of samples are grouped together as appropriate
and stored in a labeled cardboard box within the freezer.
Sediment samples which will be air-dried are received at <_6°C. After the dry and grind procedure is
completed the samples are retained at room temperature.
Synthetic materials may be kept at room temperature.
7.0 EQUIPMENT AND SUPPLIES
7.1 Equipment
Table 7.1: General Laboratory Homogenization Equipment and Supplies
Supply Vendor* Model /ID* Catalog#* Description
Spatula Fisher Stainless Steel S50822 -
Spatula Fisher Cooper Surgical Inc 11080 Plastic scrapers
Analytical Balance Varied Capable of weighing NA Analytical or top
nearest sensitivity loading
Sample Mixing Varied Metal, plastic, glass or NA Dependent upon
Containers ceramic sample composition
*Or equivalent
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.

('
ace Analytical
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Sample Homogenization, Compositing and Sub-Sampling
TEST METHOD NA
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2002-2021 Pace Analytical Services,LLC
Table 7.2: Biota Homogenization Equipment and Supplies
Supply Vendor* Model/ID* Catalog# Description
Spatula Fisher Stainless Steel S50822 -
Spoons Fisher Spoonulet 14-375-2 Lab spoon
Cutting Board Cooking Supply HDPE Stainless Steel NA Inert
Knives Sharp Hi Carbon Stainless Steel or NA Inert
Titanium
Meat Cleaver Sharp Hi Carbon Lamson NA Stainless Steel
Mallet Stanley 21b Mallet NA Plastic Face, 2-3Ib
Robot Coupe Robot Coupe R2UB NA Serial#2471016003J-11
Meat Grinder Hobart E-222/Cast Iron NA Serial#9243-0011-02990
Bell Housing Berkle Cast Iron NA For Meat Grinder
Stainless steel blade and
blender cup (may use
Blender Waring Industrial Grade NA glass)
Scaler NA NA NA Stainless Steel
Aluminum Foil NA Heavy Duty NA NA
Pliers NA Stainless Steel NA NA
Analytical Balance Mettler Toledo PE-16 NA Capable 15000±0.1 g
Analytical Balance Sargent Welch 400DR NA Capable of 150±0.001g
Analytical Balance A&D GH200 NA Capable of 50±0.0001 g
Vial C&G 40mL NA Amber Glass
2oz CG
Wide-mouth 4oz AG Clear or Amber Glass with
Container C&G or QEC 9oz AG Various Teflon lined cap
Foam ear plugs or
noise reducing
Ear plugs or Earmuffs Howard Leight earmuffs NA Moldex
Paper Towels NA 11x8.8inch NA Georgia Pacific
*Or equivalent
Any printed copy of this SOP and all copies of this SOP outside of Pace are uncontrolled copies.
Uncontrolled copies are not tracked or replaced when new versions are released, or the SOP is made obsolete.
Users of the SOP should verify the copy in possession is the current version of the SOP before use.
!. -L A!1

7eAnaIyticaI®
TEST METHOD STANDARD OPERATING PROCEDURE
TITLE: Sample Homogenization, Compositing and Sub-Sampling
TEST METHOD NA
ISSUER: Pace ENV—Green Bay Quality—GBAY
COPYRIGHT©2002-2021 Pace Analytical Services, LLC
Table 7.3: Sediment Homogenization Equipment and Supplies
Supply Vendor* Model/ID Catalog# Description
Spatula Fisher Stainless Steel S50822 -
Cutting Board