NCD003200383_19900101_Koppers Co. Inc._FRBCERCLA SAP QAPP_Draft Quality Assurance Project Plan RI and FS-OCR

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I DCC#Q461
DRAFT
QUALfIY ASSURANCE PROJECT PLAN (QAPP)
REMEDIAL INVESTIGATION AND
FEASIBILfIY STUDY
AT
MORRISVILLE, NC SITE
Prepared for:
BEAZER MATERIALS AND SERVICES, INC.
PITTSBURGH, PA 15219
Prepared by:
KEYSTONE ENVIRONMENTAL RESOURCES, INC.
3000 TECH CENTER DRIVE
MONROEVILLE, PA 15146
PROJECT NO. 179225-04
JANUARY 1990
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Project Title:
Prepared by:
Approved:
Approved:
Approved:
Approved:
DCC#Q461
Signature Page
Quality Assurance Project Plan (QAPP)
Remedial Investigation/Feasibility Study
Beazer Materials & Services, Inc.
Morrisville, NC Site
Keystone Environmental Resources, Inc.
Section No.:
Revision No.: 0
Date: 1/08/90
Page: i
____________________ Date: ____ _
EPA Region IV Project Officer
=,....,...-=-----,--~,...,,..-----,c---,----~~-----Date: ____ _
EPA Region IV Quality Assurance Officer
____________________ Date: ____ _
Beazer Materials & Services, Inc.
Program Manager
____________________ Date: ____ _
Keystone Environmental Resources, Inc.
Project Manager
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION .................................................................................................. 1-l
2.0 PROJECT DESCRIPTION ................................................................................. 2-1
3.0 PROJECT ORGANIZATION AND RESPONSIBILilY ............................. 3-1
4.0 QUALilY ASSURANCE OBJECTIVES ......................................................... 4-1
4.1
4.2
4.3
4.4
4.5
4.6
Data Quality Levels ................................................................................... 4-l Field Analysis .............................................................................................. 4-1
Non-CLP Laboratory Methods ................................................................ 4-2 CLP RAS Methods ................................................................................... _. 4-3
Non-Standard Methods ............................................................................. 4-3 Quality Control Parameters ...................................................................... 4-3
5.0 SAMPLING EQUIPl\tENT AND PROCEDURES ...................................... 5-1
5.1 Surface Water Sampling ........................................................................... 5-l
5.1.1 Sample/Location Selection ........................................................... 5-1 5.1.2 Stream Sampling ............................................................................ 5-l
5.2 Pond Sampling ............................................................................................ 5-2 5.3 Flow Measuring .......................................................................................... 5-4 5.4 Sediment Sampling .................................................................................... 5-6 5.5 Soil Sampling .............................................................................................. 5-7 5.6 Groundwater Sampling ............................................................................. 5-8
5.6.1 Sample Bottle Preparation ........................................................... 5-9 5.6.2 Equipment Preparation Procedures ......................................... 5-11
5.6.3 Water Level Measurement ........................................................ 5-13 5.6.4 Well Purging ................................................................................. 5-15
5.6.4.1 Purging and Sampling Methods ................................... 5-16
5.7 Sample Filtration ...................................................................................... 5-21 5.8 · Safety Precautions .................................................................................... 5-22 5.9 Documentation ......................................................................................... 5-22
6.0 SAMPLE CUSTODY ............................................................................................ 6-1
6.1 Field Sample Documentation .................................................................. 6-1 6.2 Laboratory Sample Documentation ........................................................ 6-2
7.0 ANALYTICAL PROCEDURES .......................................................................... 7-1
8.0 CALIBRATION CONTROLS AND FREQUENCY ...................................... 8-1
8.1 Field Instrumentation ................................................................................ 8-l 8.2 Laboratory Instrumentation -Conventional Chemistries .................... 8-1 8.3 Laboratory Instrumentation -Inorganics ............................................... 8-2 8.4 Laboratory Instrumentation -Organics .................................................. 8-4
DCC#Q461 ii
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TABLE OF CONTENTS (continued)
9.0 DATA REDUCTION, VALIDATION, AND REPORTING ........................... 9-1
9.1 Laboratory Data Reduction ..................................................................... 9-l
9.2 Laboratory Data Validation ..................................................................... 9-2
9.3 Laboratory Data Reportin~ ......................... : ............................................ 9-3
9.4 . Independent Data Reductmn and Evaluation ....................................... 9-3
9.5 Independent Data Validation (Non-CLP Samples) ............................. 9-4
9.6 Independent Data Validation (CLP Samples) ...................................... 9-4
10.0 QUALITY CONTROL PROCEDURES ......................................................... 10-1
10.1
10.2
10.3
10.4
10.5
10.6
10.7
Laboratory Quality Control Procedures ............................................... 10-1
Organic Analyses -GC/MS ..................................................................... 10-2
Organic Analyses -GC ............................................................................. 10-8
Metals by Inductively Coupled Plasma (ICP) ...................................... 10-9
Metals by Furnace Atomic Absorption ............................................... 10-11
Mercury by Cold Vapor Atomic Absorption ..................................... 10-12
General Chemistry Parameters ............................................................ 10-13
11.0 PERFORMANCE AND SYSTEM AUDITS ................................................. 11-l
11.1 Performance Audits ................................................................................. 11-l
11.2 System Audits ........................................................................................... 11-l
12.0 ASSESSMENT PROCEDURES FOR LABORATORY DATA
ACCEPTABILITY ................................................................................................ 12-l
12.1 Precision .................................................................................................... 12-l
12.2 · Accuracy .................................................................................................... 12-l
12.3 Completeness ............................................................................................ 12-1
12.4 Representativeness .................................................................................. 12-2
12.5 Comparability ........................................................................................... 12-2
12.6 Quality Control Charts ............................................................................ 12-2
13.0 PREVENTIVE MAINTENANCE ..................................................................... 13-1
13.1 Glassware Preparation ............................................................................ 13-l
13.2 Routine Preventive Maintenance
(Field and Laboratory Equipment) ....................................................... 13-2
14.0 CORRECTIVE ACTION ................................................................................... 14-l
14.1 Methods Corrective Action .................................................................... 14-l
14.2 System Corrective Action ....................................................................... 14-l
15.0 QA REPORTS TO MANAGEMENT ............................................................. 15-l
APPENDICES
Appendix A
Appendix B ·
DCC#Q461
Export Protocol For Toxics Compliance Monitoring Data
U.S. EPA Functional Guidelines For Evaluating Organics and
Inorganic Analyses
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1-1
2-1
2-2
2-3
2-4
2-5
4-1
4-2
5-1
6-1
8-1
8-2
8-3
10-1
10-2
10-3
10-4
10-5
10-6
5-1
5-2
5-3
5-4
6-1
6-2
8-1
12-1
14-1
DCC#Q461
LIST OF TABLES
Quality Assurance Project Plan Criteria ........................................................ 1-2
Surface Water Sample Analysis Summary ..................................................... 2-2
Soil Sample Analysis ......................................................................................... 2-5
Sediment Sample Analysis Summary
Fire Pond/Medlin Pond .................................................................................... 2-7
Groundwater Sample Analysis ...................................................................... 2-10
TCL and TAL Parameters and Detection Limits ....................................... 2-11
Quality Assurance Objectives
(Groundwater/Surface Water San:iples ) ......................................................... 4-6
Quahty Assurance Objectives (S011/Sediment Samples) ............................ .4-8
Sample Container Oeaning Procedures and Preservation ....................... 5-25
Holding Times .................................................................................................... 6-4
Interferent and Analyte Elemental Concentrations Used
~::f!i It~t~~~~~ct~~c~/'ff1c;~ Gj;~"i~"ct"rco·o;~··~·~cticor\········· B-rn
In Reagent Water (PPT) and EnV!ronmental Samples (PPB) ................. 8-11
~2gg~s f~~Js7~
0
6~-~~'.~.~.~.~.~~~.~~~.~.~'.~.~~·~············································· 8-12 p-Bromofluorobenzene (BFB) Key Ions and Ion
Abundance Criteria ....................................................................................... 10-14
Decafluorotriphenylphosphine (DFTPP) Key Ions and Ion
Abundance Criteria ....................................................................................... 10-15
Volatile Internal Standards with Corresponding Analytes
Assigned for Quantitation ............................................................................ 10-16
Acid and Base/Neutral Extractable Internal Standards tff
Corresponding TCL Analytes Assigned for Quanitation ................... 10-17
Calibration Check Compounds ................................................................... 10-18
Surrogate Spike Compounds and Recovery Ranges ................................ 10-19
LIST OF FIGURES
Analytical Request Form ................................................................................ 5-26
Field Data Sheet for Groundwater Sampling .............................................. 5-27
Purge Volume Configuration ......................................................................... 5-28
Attachment ....................................................................................................... 5-29
Chain of Custody Record ................................................................................. 6-5
Inorganic Analysis Sample Chronicle ............................................................. 6-6
Calibration Sheet ............................................................................................. 8-13
Accuracy Plot ................................................................................................... 12-4
Invalid Data Notification ................................................................................ 14-3
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1.0 INTRODUCTION
Section No: l
Revision No: 0
Date: 01/08/90
Pagel of3
The purpose of this Quality Assurance Project Plan (QAPP) is to document the
procedures and criteria that will be used to provide accurate, precise, comparable,
representative and complete data during the performance of the Remedial
Investigation/Feasibility Study (RI/FS) work at the Beazer Materials and Services,
Inc. Site in Morrisville, North Carolina.
The procedures and criteria that will be used to accomplish the RI/FS work
objectives will be responsive to requirements of the U.S. Environmental Protection
Agency (U.S. EPA). The RI/FS work objectives are summarized in section 2 of this
document and sections 4 and 5 of the Work Plan for the RI/FS. Requirements of the
U.S. EPA are based on several sources including U.S. EPA guidance documents (e.g.
Interim Guidelines and Specifications For Preparing Quality Assurance Project
Plans, QAMS-005/80, December 29, 1980) and Contract Laboratory Program (CLP)
requirements. Also, the sixteen criteria identified by the U.S. EPA (Region IV) as
document completeness criteria have been incorporated in the preparation of the
QAPP. Table 1-1 lists these sixteen criteria and the section of the QAPP in which the
information is presented.
In general, the QAPP addresses: a) the quality assurance (QA) objectives of the
project; b) specific QA and quality control (QC) procedures that will be
implemented to achieve these objectives; and c) staff organization and responsibility.
These three areas are addressed in the QAPP for primarily the field work, sampling,
and laboratory analysis aspects of the project in accordance with requirements of the
U.S. EPA which focus on the acquisition of environmental data of known and
acceptable quality.
DCC#Q461 1-l
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Item Number
DCC#Q461
1
2
3
4
5
6
7
8
9
TABLE 1-1
Section No.:1
Revision No.: 0
Date: 1/08/90
Page: 2 of3
QUALITY ASSURANCE PROJECT PLAN CRITERIA
Criteria OAPP Section No.
Title Page
o Title
o Organization
o Approval Blocks
Table of Contents
o Introduction
o Listing of 16 QA components
Project Description
o General description
o Flow diagrams, charts, and tables
o Intended use of data
Project Organization and Responsibility
o Project organization and line authority
o Identification of key QA personnel
Quality Assurance Objectives
o Data quality objectives
o Precision and accuracy for each parameter
Sampling Procedures
o Techniques or guidelines used to select sites
o Specific procedures
o Containers, reagents
o Sample equipment and container preparation
o Sample preservation methods
Sample Custody
o Holding times
o Chain-of-Custody
o Field sampling documentation
o Laboratory documentation
Analytical Procedures
Calibration Procedures and Frequency
1-2
Table 1-1
2.0
3.0
4.0
5.0
6.0
7.0
8.0
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Item Number
10
11
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DCC#Q461
TABLE 1-1 (continued)
Section No.:l
Revision No.: 0
Date: 1/08/90
Page: 3 of 3
QUALilY ASSURANCE PROJECT PLAN CRITERIA
Criteria OAPP Section No.
Data Reduction, Validation, and Reporting 9.0
o Data reduction scheme
o Equations to calculate concentration
o Data validation criteria
o Reporting of QC values
o Field measurements
Internal QC Checks 10.0
o Laboratory Operations
o Field Operations
o Calibration Standards
o Duplicates
o Spikes
o Blanks
o Standard Curves
Performance and System Audits 11.0
Assessment Procedures for Data Acceptability
Preventive Maintenance
o Schedule
o Procedures
Corrective Action
o Limits
o Procedures
o Responsible personnel
Quality Assurance Reports to Management
1-3
12.0
13.0
14.0
15.0
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2.0 PROJECT DESCRIPTION
Section No: 2
Revision No: 0
Date: 01/08/90
Page 1 of 15
The primary objective of the Remedial Investigation is to define the nature and
extent of the potential contamination at the site and its effect on human health in
order to perform a public health and environmental assessment, screen alternatives
to determine the most feasible method for the remediation of potential risks to
public health and safety, welfare, and the environment. Specific tasks designed to
accomplish these objectives are given in Section 5 of the Work Plan document. Task
3 involves field sampling and laboratory analysis of groundwater, surface water, soils,
and sediments. A summary of sampling locations and analytical parameters are
given in Tables 2-1 through 2-4. A listing of Target Compound List (TCL) and
Target Analyte List (TAL) parameters are given in Table 2-5. The rationale for site
location and parameter selection are also given in Section 5 of the Work Plan
document.
DCC#Q461 2-1
--1111 -.. --liill - ----------TAIII.E 2-1
SIIIH'ACE WATER SAMPLE ANALYSIS SUMMARY
No.of Estimated
Sample Somples No.of Anol)1ticnl De1ection Field Rinsate Trip l>QO Location per Location Samples Paremeler Method Limit Duplicate lllank Blank Len-I Comments
SW-1,SW-W, 2 12 Acid Extractahle EPA 81140 (2) () 111 SW-12 Phenols
SW-18,
SW-20,SW-22(1)
2 12 Pen1achlorophenol EPA5l5 11.11 IO ug/1 2 () V
2 12 lsopropyl Ether• EPA 81120 1.m ug/1 2 l/day/c<1<1ler V First round only. ':'
2 12 pH EPA 1511. I 0 0 II II This analysis will be performed in the
field.
2 12 ~ecific EPA 1211.I I umho/cm II II II II This analysis will be performed in the onductance field.
2 12 Temperature EPA 170.I 0 II 0 II This analysis will be performed in the
field.
SW-12, 2 TAL/fCL EPA-CLP (4) I/day I/day/cooler IV First round only. SW-18(3) Compounds• (volatiles only)
SW-IO, SW-12(5) 2 4 PCDD/PCDF EPA 82'~l Various II V At each location, one sample will be filtered and one sample will remain
unfihereJ.
----- --------------TAllLE 2-1
(Continued)
SURFACE WATER SAMPLE ANALYSIS SUMMARY
No.or Eslimated
Sample Samples No.or Analytical ()election Field Rinsate Tr-ip IJQO Location per Location Samples Parameter Melhod Limit Duplicate Blank Blank Level Comments
See Comments 2 H Tolal Organic EPA 415.l 1 "'!>~ 0 0 II The locations of these Carhon samples will he picked
at random from the fire 2 H Biochemical EPA 405.1 lmg/1 0 0 () II and Medlin Ponds. Oxygen
Demand
2 8 Chemical EPA 410.4
Oxygen
IOmg/1 0 () 0 II
Demand
N 2 ' 8 Total EPA 160.2 1 mg/I 0 0 w Suspended
(I II
Solids
SW-l6A, SW-16B, 14 Acid Extractable EPA 8040 (2) 0 111 SW-17, SW-23 Phenols
1hru SW-26
SW-28 lhru SW-34
14 Pentachlorophenol EPA 515 0.010 ug/1 0 V
14 lsopropyl E1her' EPA 8020 I.IKl ug/1 I/day/cooler V First round only.
14 pH EPA 150.1 () 0 0 II This analysis will he performed
in the fidd.
14 ~ecific EPA 1211.1 I umho/cm 0 0 0 II TI1is analysis will he performed mJuctancc in the field.
14 Temperature EPA 1711.1 0 () ti II This ananlysis will he perlormcd
in the field.
---~----
N
' ~
-----
TABLE 2-1
(Conlinued)
liiiiil --
SURFACE WATER SAMPLE ANALYSIS SUMMARY
No.or Estimated
Sample Samples No.or
LI.cation per Location Samples
SW-24, SW-26,
SW-34 3
See Comments 7
7
7
7
Notes:
Parameter
TAI./fCL
Compounds•
Total Organic
Carbon
Biochemical
Oxygen
Demand
Chemical
Oxygen
Demand
Total
Suspended
Solids
Analytical
Method
EPA-CLP
EPA 415.1
EPA 405.J
EPA 4 I0.4
EPA 160.2
~ll At each location a sample will be collected from the following depths: 2 EPA Method 8040 Detection Limits henol 0.50 ug/1 2-Chlorophenol 0.50 ug/1 2-Nitrophenol 0.50 ug/1 2,4-Dimethylphenol 0.50 ug/1 2,4-Dichlorophenol 0.50 ug/1 4-Chloro-3-Methylphenol 0.50 ug/1
Delection Field
Limit Duplicate
Rinsale
Blank
(4)
I mg/I 0
I mg/I 0
JO mg/I 0
I mg/I 0
near surface and at 2/3 depth
2, 4,6• Trichlorophenol
2,4-Dinitrophenol
4-Nitrophenol
2,3,5,6. Tetrachlorophenol
4,6-Dinitro-2-Methylphenol
Pen1achlorophenol
0
0
0
(3) At locatio111 SW-12 and SW-18 a sample will be collected from 2/3 depth. (4) Refer to Table SA-I of this Work Phrn for ;1 !isl of detect inn limits.
Tri1>
lllank
DQO
Level
I/day/cooler JV
(volatiles only)
0 II
u
0
0
J .(XJ ug/1
J.IXI ug/1
J.(X) ug/1
I .(XI ug/1
I.IX) ug/1
1.00 ug/1
II
II
II
--
Comments
Firs! round only.
The locations of these
samples will be picked
at random from the
drainageways.
---
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TABLE 2-2
SOIL SAMPLE ANALYSIS
Sample. Ellimalcd
Sample Pc, No. of Aoalytical Detection Picld Rinutc Trip DQO
A,u Location Location Sampica Parameter Mcohod Limit Ouplic■ tc Blank Blank Level Commcnl1
land TreatmCDI X-2 thru X-9 3 ,. Acid E..J:tr1ct1blc Phenolic. EPA 8040 (I) 2 0 UI
3 IIIOpfOpyl Ether EPA 8020 100 ug/kg V • T AUTCL Liau V.riow (2) I (volatile, oo.ly) IV
Lagoon and Celloo X-15 thru X-37; 2 .. Acid E.xtn1c1ablc Phcoolict EPA 8040 (I) • 0 II One Mmplc from locatioo1
Treatment Area X--41 5 laopropyl Ether EPA 8020 100 us:J\i I V X-17. X-26 and X-37 will be
7 TAUTCI. Jiat, Vuiow (2) I (volatile, ooly) IV included in lhe 1n11ly1e1 for
5 PCDDIPCDF EPA 8290 Variow 0 V TALfTCL cooatitucnta and PCDD■
and PCDF1.
Tcc:pec Bwocr x-10, 3 l Acid Extractable Pbc:oolica EPA I040 (I) 0 m 1bc surface 10il N..mplc from
l l Drioting Water Metal■ ()) (3) I 0 m boring X-10 will be 1.D1tyzed
l l PCDOIPCOP EPA 1290 Variow 0 0 0 V for corutituent■ oa the
"' TAUTCL Iida Variom (2) I I (volatile, only) IV T AUTCL Ii 111. I
V,
M-1, SS-2 2 Acid Extractable Pbcoolica EPA 8040 (I) 0 Ill
2 Drinking Water Mcb.11 (3) (3) I I 0 Ill
2 PCDD/PCDP EPA 1290 Varioua 0 0 0 V
Olbcr Areas X-11 to X-14; 2 21 Acid Extnctablc Pbcoolica EPA 8040 (I) 3 0 Ill Ooc aamplc from borioa:• X-14
X-38 '° X-47 l bopropyl fJhcr EPA 8020 100 ug/q I V and X-46 will be analyzed • T AUTCL lill1 VariOUI (2) I (volllilc1 oaly) IV for T Al.ffCL cOllllitucot1.
Background C-3, C-9, 2 • Acid f.nncllblc Phenolic■ EPA 8040 (I) 0 UI
andC-11
X-1 2 2 Acid Enncllblc Phenolic, EPA 8040 (I) 0 m
2 2 T AL/TCL Ji111 V1rioua (2) I I (volltik1 oaly) IV
PCOO/PCDP EPA&290 V1riOU1 0 0 0 V
l.apropyl Ether EPA IK>20 100 uglq V
1!!1!!11
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Note,:
(I) EPA Mclhod 8040 Detection limit,:
Phc~I
2-Cb.loropheool
2-Nitropbeool
2,4-Dimcthylpbcool
2,◄-Dichloropbeool
4-Cbloro--3-Melby lpbcool
(2) Rcfet to Table 5A-I
,0 ... ,..
,0 ... ,..
,0 ... ,..
,0 uglkg
,0 ... ,..
,0 ... ,..
(3) Drinking Water Met.ala Method. aod Detection:
Aneoic EPA 7060 l<XlO "Ilk&
Barium EPA 6010 20000 ... ,..
Cadmium EPA 60JO ,00 ... ,..
Chromium EPA bOIO 1000 ug/lg
Mcrcwy EPA 1'471 100 ug/kg
Lead EPA 7421 ,00 .. ,..
Selenium EPA n.w ,00 uglkg
Silver EPA 6010 IOOOug/k&
---
2,◄,6-T richlorophcnol
2,4-0i.nitropheool
◄-Nitropheool
2, J, 5, 6-T clrac blorophcnol
- -
TABLE 2-2 (conrioucd)
SOIL SAMPLE ANALYSIS
4, 6-Dini I ro-2-Mclhylpheool
Peotachloropheool
100 ugfk.s
100 ug/lg
100 ug/lg
100 ugfk.s
100 1.18/lg
100 ug/lg
-- -- -
- -
Fire Pond &
Medlin Pond
Pmposed
Sediment
Sample
Locations
S-2 S-4 S-5 S-7
S-10,S-'iz,S-IJA
S-14,S-19,S-21
S-4,S-IO,S-I JA
S-4,S-IO,S-I JA
S-4,S-IO,S-IJA
S-IO, S-13A
S-l,S-3,S-6
S-8,S-9,S-11
S-13,S-15,S-18
S-20,S-22
S-l ,S-15,S-18,S-22
S-I ,S-15,S-I 8,S-22
S-l,S-22
S-18
See comments
-l!!!!!!!!!!!I
No.or
Samples
per Location
2
2
2
2
2
2
2
2
2
2
Estimated
No.or
Snmples
20
6
6
6
4
22
8
8
4
4
<IO
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TABLE l-3
SEDIMENT SAMPLE ANALYSIS SUM~IARY
FIRE POND/MEDLIN POND
Parameler
Acid Extractahle
Phenols
PCDD/PCDF
Total Organic
Carbon
Analytical
Method
EPA 8040
EPA 8290
EPA 9060
lsopropyl Ether EPA 8020
TAUfCL Compounds EPA-CLP
Acid Extractahle
Phenols
PCDD/PCDF
Total Organic
Carbon
EPA 8040
EPA 8290
EPA 9060
lsopropyl Ether EPA 8020
TAIJrCLCompounds EPA-CLP
-gra!n size
-moisture
-sieve hydrometer
-A11erherg limits
Deteclion
Um it
Field
Duplicate
(I)
Various
JCXJ mg/kg
100 ugikg
(2)
(I)
Various
JCXJ mg/kg
100 ug/kg
(2)
2
2
()
0
Field
Blank
2
()
()
()
Trip
Hlank
I/day I/day/cooler
(volatiles only)
()
2
()
()
()
0 0
I/day I/day/cooler
(volatiles only)
-
DQO
Level
Ill
V
II
V
IV
Ill
V
II
V
IV
--l!!!!!!I
Ct1mmenls
When field conditions permit,
pond sediment samples will be collected to a depth of
5 feet, with samples collected
at each 2.5-foot interval.
When field conditions permit,
pond sediment samples will be
collected from the surface
and the 2.5 to 5.0-foot
interval.
Several pond sediment
samples will be analyzed
for parameters to determine
the physical characteristics
of Iii.is material. The actual
number of samples allalrz:ed,
and parameters chosen will be
determined in the field hy
the supervising hydrogcologist
and project geophysical
--l!!!!!!!!I
Drainageway
Sample
Locations
S-16A, S-168, S-17,
S-23 thru S-34
S-168, S-23
No.or
Samples
per Loca I ion
Total
No.or
Samples
15
2
2
Ea lliiiil
Parameler
Acid E.xtractahle
Phenols
Total Organic
Carbon
PCDD/PCDF
----TABLE 2-3 (Continued)
SEDIMENT SAMPLE ANALYSIS SUMMARY
ORAINAGEWAYS
Analytical
Method
Detection Field
Limit Duplicate
Field
Blank
EPA 8040 (I)
EPA 9060 I ()(Xl mg/kg
EPA 8290 Various 0 ()
0
0
0
Trip
Blank
S-23,S-25,
S-26,S-3!, S-34 5 TAL/fCL Compounds EPA-CLP (2) I/day I/day/cooler
(volatiles only)
Notes:
(I) EPA Method 8040 Detection Limits
Phenol
2-Chlorophenol
2-Nitrophenol
2,4-Dimethylphenol
2,4-Dichlorophenol
4-Chloro-3-Methylphenol
50 ug/kg
50 ug/kg
50 ug/kg
50 ug/kg
50 ug/kg
50 ug/kg
2,4,6-Trichlorophenol
2,4-Dinitrophenol
4-Nitn)phenol
2,3,5,6-Tetrachlurophenol
4,6-Dinitro-2-Methylphenol
Pentachlorophenol
Fl Refer to Table 5A-1 of this work plan for a list of detection limi1s. One round of sediment sampling will be performed for lhe ahove noted parameters.
lfkl ug/kg
l(Xl ug/kg
](XI ug/kg
IIKI ug/kg
](Kl ug/kg
IOO ug/kg
DQO
Level
111
II
V
JV
--
Comments
At c::ach location a
sample will be
collected from the
surface.
At each location a
sample
will be collected
from the surface.
-
At each location a sample
will be collected from 1he
surface.
At each location a
sample will be coll
from the surface.
----l!!!!!!l!!!!I
Notes:
(I) EPA Method 8040 Detection Limits
Phenol
2-Chlorophenol
2-Nitropfienol .
2,4-Dimethylphenol
2,4-Dichlorophenol
4-Chloro-3-Methylphenol
50 ug/kg
50 ug/kg
50 ug/kg
50 ug/kg
50 ug/kg
50 ugfkg
!!!!!I iiiiil liiiii ----TABLE 2-3 (Continued)
SEDIMENT SAMPLE ANALYSIS SUMMARY
2,4,6-Trichlorophenol
2,4-Dinitrophenol 4-NitroEhenol
2,3,5,6-Tetrachlorophenol
4,6-Dinitro-2-Methylphenol Pc::ntachlorophenol
ICXl ug/kg
100 ug/kg
.l(K) ug!kg
11111 ug/kg
IIXl ug/kg
ICXl ug!kg
,2) Refer to Table SA-I of this Work_ Plan for a list of detection limits.
One round of sediment sampling will be perfonned for lhe above noted parameters.
--- -
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----I!!!!!! ~ liiia liiiil ---
TABLE 2-4
GROUNDWATER SAMPLE ANALYSIS
Sample
Location
C-1 th,u C-32,
M-4, M-9
C-4, C-27A,
C-28A and C-30
C-4, C-25A,
C-26A, C-27A, C-28A
and C-30
Notca:
Samples
Pc,
Location
(I) EPA Method 8040 Detection Limiu:
Phenol
2-Chlorophcnol
2-Nitrophcnol
2,4-Dimcthylphcnol
2,4-Dichlorophenol
4-Chloro-3-Mcthylphenol
(2) Refer to Table 5A-l.
Estimated
No. of
Sampica
. (per round) Parameter
50 Acid Extractable Phcnolica
50 Pcntachlorophcnol
50 lsopropyl Ether(•)
50 pH
50 Specific Conductance
50 T cmpcraturc
4 PCDDIPCDF(')
6 T AL/TCL lio(')
0.50 ug/1
0.50 ugn
0.50 ug/1
0.50 ugn
0.50 ugn
0.50 ugn-
• First round only. Second round parameters and sample locations
dependent upon results of first round.
Analytical Detoction
Method Limit
EPA 8040 (I)
EPA515 O.OIO ugn
EPA 8020 LO ugn
EPA 150.1
EPA 120. I I umho/cm
EPA 170.I
EPA 8290 Various
EPA-CLP (2)
2,4,6-Trichlorophcnol
2,4-Dinitrophenol
4-Nitrophcnol
2 ,3 ,S ,6-T ctrachlorophcnol
4,6~Din_itro-2~Mcthylphcnol
Pcntachlorophcnol
--- -
field Rinsa.tc Trip DQO
Duplicate Blank Blank Level
5 0 Ill
5 0 Ill
5 I V
0 0 0 fl
0 0 0 fl
0 0 0 II
0 V
l(volatilea only) IV
1.00 ug/1
1.00 ug/1
1.00 ugn
1.00 ugn
1.00 ugn
1.00 ug/1
I Section No
TABLE 2-S Revision No
Date: 01)08/
I TCL AND TAL PARAMETERS AND DETECTION LIMITS Pqe 11 or
TAL Parameters
I Water SoiVSediment Parameten .Y&ll mg/kg I aluminum 200 40 antimony 60 12 arsenic IO 2 I barium 200 40 beryllium 5 1 cadmium 5 1 I calcium 5000 1000 chromium IO 2 cobalt 50 IO I copper 25 5 iron 100 20 lead 5 1 magnesium 5000 1000 I manganese 15 3 mercury 0.2 0.04 nickel 40 8 I potassium 5000 1000 selenium 5 1 silver IO 2
I sodium 5000 1000 thallium IO 2 vanadium 50 IO zinc 20 4 ffl cyanide IO 2
TCL Parameters
ID Low Low Level Level Water<2) SoiVSediment<3) Parameters .YILL .!!iL.K: I Volatiles
I Chloromethane IO IO Bromomethane IO IO Vinyl chloride IO IO I Chloroethene IO IO Methylene Chloride 5 5
I Acetone IO IO Carbon Disulfide 5 5 1, 1-Dichloroethane 5 5 1,1-Dichloroethene 5 5 I trans-1,2-Dichloroethene 5 5
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DCC#Q461
I 2-11
Section No: : I Revision No:,
TABLE 2-S (Continued) Date: 01/08/91
PqeUof 1:
I Low Low Level
Level Water(2) Soil/Sediment<3) Parameters !!ILL Y&lK& I Chloroform 5 5 1,2-Dichloroethane 5 5 2-Butanone 10 10 I 1, 1,1-Trichloroethane 5 5 Carbon Tetrachloride 5 5
I Vinyl Acetate 10 10 Bromodichloromethane 5 5 1, 1,2,2-Tetrachloroethane 5 5
I 1,2-Dichloropropane 5 5 trans-1,2-Dichloropropene 5 5
Trichloroethene 5 5 I Dibromochloromethane 5 5 1, 1,2-Trichloroethane 5 5 Benzene 5 5
I cis-1,3-Dichloropropene 5 5
2-Chloroethyl Vinyl Ether 10 10 Bromoform 5 5 I 2-Hexanone 10 10 4-Methyl-2-pentanone 10 10 Tetrachloroethene 5 5 I Toluene 5 5 Chlorobenzene 5 5
D Ethyl Benzene 5 5 Styrene 5 5 Total Xylenes 5 5 e Semi-Volatiles
Phenol 10 330
m bi&Chloroethyl) ether 10 330 2-orophenol 10 330
I 1,3-Dichlorobenzene 10 330 1,4-Dichlorobenzene 10 330 Benzyl Alcohol 10 330 1,2-Dichlorobenzene 10 330 I 2-Methylphenol 10 330
bis(2-chloroisopropyl) ether 10 330 I 4-Methylphenol 10 330 N-Nitroso-Dipropylamine 10 330 Hexachloroethane 10 330
I Nitrobenzene 10 330
Is~horone 10 330
I 2-itrophenol 10 330 · 2,4-Dimethylphenol 10 330
I DCC#Q461
2-12
I Section No:
Revision No:
TABLE 2-S (Continued) Date: 01/08{~
Pqe 13of: I Low Low Level
Level Water<2) Soil/Sediment<3) Parameten .!!ilL Y&lK& I Benzoic Acid 50 1600 bis(2-Chloroethoxy) methane 10 330
I 2,4-Dichlorophenol 10 330 1,2,4-Trichlorobenzene 10 330
N63thalene 10 330 I 4-oroaniline 10 330 Hexachlorobutadiene 10 330
I 4-Chloro-3-methylphenol
(Mra-chloro-meta-cresol) 10 330 2-ethylnaphthalene 10 330
I Hexachlorocyclopentadiene 10 330 2,4,6-Trichlorophenol 10 330 2,4,5-Trichlorophenol 30 1600
I 2-Chloronaphthalene 10 330 2-Nitroaniline 50 1600 Dimethyl Phthalate 10 330
I Acenaphthylene 10 330 3-Nitroanihne 30 1600
I Acenaphthene 10 330 2,4-Dinitrophenol 50 1600 4-Nitrophenol 50 1600 Dibenzofuran 10 330 I 2,4-Dinitrotoluene 10 330
2,6-Dinitrotoluene 10 330
I Diethylphthalate 10 330 4-Chlorophenyl Phenyl
ether 10 330 Fluorane 10 330 D 4-Nitroaniline 50 1600
4,6-Dinitro-2-methylphenol 30 1600
m N-nitrosodiphen~lamine 10 330 4-Bromophenyl henyl ether 10 330 Hexachlorobenzene 10 330 e Pentachlorophenol 30 1600
Phenanthrene 10 330
m
Anthracene 10 330 Di-n-butylphthalate 10 330 Fluoranthene 10 330
I Pyrene 10 330 Butyl Benzyl Phthalate 10 330 3,3 '-Dichlorobenzidine 20 660
I Benzo( a )anthracene 10 330 bis(2-ethylhexyl)phthalate 10 330
I DCC#Q461
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Parameun
Chrysene
Di-n-oc~I Phthalate Benzo b fluoranthene
Benzo~k fluoranthene
Benzo(a pyrene
lndeno( 1,2,3-cd)pyrene
Dibenz( a,h )anthracene
Benzo(g.h,i)perylene
Pesticides
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC (Lindane)
Heptachlor
Aldrin
Heptachlor Epoxide
Endosulfan I
Dieldrin
4,4'-DDE
Endrin
Endosulfan II
4,4'-DDD
Endosulfan Sulfate
4,4'-DDT
Endrin Ketone
Methoxychlor
Chlordane
Toxaphene
AROCLOR-1016
AROCLOR-1221
AROCLOR-1232
AROCLOR-1242
AROCLOR-1248
AROCLOR-1254
AROCLOR-1260
TABLE 2-5 (Continued)
Low
Level Waur<2)
1!ilL
10
10
10
10
10
10
10
10
0.05
0.05
0.05
0.05
0.05
0.05
0.05
0.05
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.5
0.5
1.0
0.5
0.5
0.5
0.5
0.5
1.0
1.0
Low Level
SoiVSediment<3)
l!&LK&
330
330
330
330
330
330
330
330
8.0
8.0
8.0
8.0
8.0
8.0
8.0
8.0
16.0
16.0
16.0
16.0
16.0
16.0
16.0
16.0
80.0
80.0
160.0
80.0
80.0
80.0
80.0
80.0
160.0
160.0
(1) Detection limits listed for soil/sediment are based on wet weight. The
detection limits calculated by the laboratory for soil/sediment, calculated on
dry weight basis, as required by the contract, will be higher. Specific detection
limits are highly matnx dependent. The detection 1imits hsted herein are
provided for guidance and may not always be achievable.
DCC#Q461
2 -14
Section No: ;
Revision No: (
Dau: 01)08/91
Pap 14of If
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(4)
(5)
(6)
(7)
DCC#Q461
Section No:
Rmsion No: TABLE 2-5 (Continued) Due: 01/08/S
Pap1Sor1
Medium Water Contract Required Quantitation Limits (CRQL) for Volatile TCL Compounds are 100 times the individual Low Water CRQL
Medium Soil/Sediment Contract Required Quantitation Limits (CRQL) for Volatile TCL Compounds are 100 tlilles the individual Low Soil/Sediment CRQL
Medium Water Contract Required Quantitation Limits (CRQL) for Semi-Volatile TCL Compounds are 100 times the individual Low Water CRQL
Medium Soil/Sediment Contract Required Quantitation Limits (CRQL) for Semi-Volatile TCL Componds are 60 times the individual Low Soil/Sediment CRQL
Medium Water Contract Required Quantitation Limits (CRQL) for Pesticide TCL Compounds are 100 times the individual Low Water CRQL.
Medium Soil/Sediment Contract Required Ouantitation Limits (CRQL) for Pesticide TCL compounds are 15 times the individual Low Soil/Sediment CRQL
2 -15
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3.0 PROJECT ORGANIZATION AND RESPONSIBILI1Y
Section No. 3
Revision No. 0
Date U08/90
Pagel of4
The following section describes the duties of key personnel assigned to the Remedial
Investigation at the Beazer Materials and Services, Inc. Morrisville, North Carolina
site.
Project Manager
The Project Manager will be the primary point of contact and will have primary
responsibility for technical, financial and scheduling matters. His duties will include:
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Procurement, along with administrative personnel, and supervision of
subcontractor services;
Assignment of duties to the project staff and orientation of the staff to
the needs and requirements of the project;
Review of subcontractor work and approval of subcontract invoices;
Establishment of a project record keeping system;
Review of all major project deliverables for technical accuracy and
completeness; and,
o Project closeout.
Site Hydrogeologist
The Site Hydrogeologist will be responsible for field activities and data evaluation,
including items as follows:
DCC#Q461 3-1
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Section No. 3
Revision No. 0
Date 1/08/90
Pagel of4
Supervising the collection of the samples and providing for their
proper documentation, handling and shipping;
Maintaining a completion log for each monitor well installed;
Monitoring the drilling and sampling operations to verify that the
drilling subcontractor and sampling team members adhere to the
QAPP;
o Coordinating activities with the Project Manager; and,
0 Preparing the field investigation data.
Quality Assurance Manager
The Quality Assurance (QA) Manager is responsible for audits and monitors
adherence to the project QA objectives. The QA Manager acts independently of the
project team. His responsibilities include:
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DCC#Q461
Reviewing and approving of the QAPP;
Conducting field (performance) audits of sampling episodes to provide
that sample identification and chain-of-custody procedures are being
followed;
Conducting systems audits of the project activities and reports; and,
Overseeing for the conduct of the QC auditing activities by the QNQC
staff.
3-2
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Section No. 3
Revision No. 0
Date 1/08/90
Page3 of4
Laboratory Director
Responsibilities of the Laboratory Director include:
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Collaborating with the project management in establishing sampling
and testing programs;
Serving as liaison between the laboratory and other project personnel;
Serving as the "collection point" for reporting of nonconforrnances and
changes in laboratory activities;
Notifying the laboratory and project management of specific
laboratory nonconforrnances and changes;
Maintenance of laboratory data;
Releasing of testing data and results; and,
Responsible for laboratory and data activities by the analytical services
staff.
Site Safety Officer
The Site Safety Officer (SSO) will be responsible for verifying that project personnel
adhere to the site safety requirements. These responsibilities include:
0
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DCC#Q461
Conducting the health and safety training for project personnel and
subcontractors, as appropriate;
Modifying health and safety equipment or procedure requirements
based on data gathered during the site work;
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Section No. 3
Revision No. 0
Date 1/08/90
Page4of4
Determining and posting locations and routes to medical facilities,
including poison control centers; and arranging for emergency
transportation to medical facilities;
Notifying local public emergency officers, i.e., police and fire
departments, of the nature of the field operations and posting their
telephone numbers;
Observing work party members for symptoms of exposure or stress;
Providing first aid if necessary on-site; and
o Performing site audits to verify adherence to the requirements of the
project health and safety plan.
The SSO has the authority to stop any operation that threatens the health or safety of
the team or surrounding populace. The daily health and safety activities may be
conducted by the SSO or his designee.
DCC#Q461 3.4
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4.0 OUALI1Y ASSURANCE OBJECTIVES
Section No. 4
Revision No. O
Date 1/08/90
Page 1 of9
Data Quality Objectives (DQOs) are qualitative and quantitative statements to ensure
that data of known and appropriate quality are obtained during remedial
activities. Data developed during the RI will be used for:
o Risk assessment
o Site characterization
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Screening and evaluation of remedial alternatives
Remedial design
response
Groundwater and surface water are the major pathway for migration of contaminants
from the suspected sources to the receptors. The analysis of groundwater and surface
water for site specific parameters will, therefore, require the most stringent DQO levels.
4.1 Data Quality Levels
There are five analytical levels of data quality available to accomplish the objectives of
the RI.
0 Level I -field screening
0 Level II -field analysis
0 Level III -non-CLP laboratory methods
0 Level IV -CLP RAS methods
0 Level V -non-standard methods
No level I procedures are planned for this project. The following sections describe the
use of the other analytical levels.
4.2 Field Analysis
Level II field analysis will consist of performing pH, specific conductance, and
temperature measurements on groundwater and surface water samples. These
4-1
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Section No. 4
Revision No. O
Date U0S/90
Page 2 of9
parameters can change upon standing if analyses are not performed shortly after
sampling.
4.3 Non-CLP Laboratory Methods
Level III analysis will be performed for those parameters where CLP methods are not
available or in cases where the rigid CLP reporting is not necessary to accomplish the
immediate objective. The following analyses will receive level III analytical treatment.
Groundwater
Acid extractables EPA8040
Arsenic EPA 7060
Barium EPA6010
Calcium EPA6010
Selenium EPA 7740
Surface Water
Acid extractables EPA8040
Total organic carbon EPA 415.1
Biochemical oxygen demand EPA 405.1
Soils
Acid extractables
Arsenic
Barium
Cadmium
Chromium
Sediments
Acid extractables
Total organic carbon
EPA8040
EPA 7060
EPA6010
EPA6010
EPA6010
EPA8040
EPA 9060
4-2
Cadmium
Chromium
Lead
Mercury
Magnesium
Sodium
Potassium
Silver
Chemical oxygen demand
Total suspended solids
Lead
Mercury
Selenium
Silver
EPA6010
EPA6010
EPA 7421
EPA 7470
EPA6010
EPA6010
EPA6010
EPA6010
EPA 410.4
EPA 160.2
EPA 7421
EPA 7471
EPA 7740
EPA6010
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4.4 CLP RAS Methods
Section No. 4
Revision No. 0
Date 1/08/90
Page3 of9
Level IV analysis will be performed on samples receiving TCL and T AL analysis by the
most current CLP statement of work (SOW).
4.5 Non-Standard Methods
The use of non-standard methods are for risk assessment tasks where the standard CLP-
RAS methods do not give the necessary detection limits. The use of level V analysis will
provide quantitative input into the risk assessment;
Contaminant screening process in which each successive step narrows the
field of contaminants that pose a potential threat.
Health and environmental risk estimates.
Set boundaries on the extent of cleanup required to reduce the risk of
adverse effects to an acceptable level.
Groundwater/Surface Water
Pentachlorophenol
Isopropyl ether
Dioxins/furans
EPA 515
EPA8020
EPA8290
Note: If pentachlorophenol is detected at a level exceeding 0.01 ug/liter but not
greater than 30 ug/liter, then a second column confirmation will be performed. This
confirmation will be performed on up to 25% of surface water and groundwater
samples.
4.6 Quality Control Parameters
The following sections define the detection limits and data precision, accuracy, and
completeness that will be maintained throughout the project:
4-3
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Section No. 4
Revision No. 0
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Page4of9
Detection limit -The minimum concentration of a substance that can be
measured and reported with 99% confidence that the analyte
concentration is greater than zero.
Precision -

A

measure of the mutual agreement among individual
measurements of the same property under prescribed similar conditions.
Precision is determined based on the relative percent difference (RPD) of
duplicates or duplicate spikes as appropriate. (See section 12.1 for
method of calculation).
o Accuracy -The degree of agreement of a measurement with an accepted
reference or true value. Accuracy is determined by calculating the percent
recovery of spiked samples. (See section 12.2 for method of calculation).
0 Completeness -

A

measure of the amount of valid data obtained from a
measurement system compared to the amount expected to be obtained
under normal conditions. (See section 12.3 for method of calculation).
The following rationale was used for developi,ng the completeness
objectives:
Trace organics in groundwater and surface water are the major
concern at the site, so completeness is set at 90% for level V
groundwater and surface water parameters.
The historic completeness of the CLP RAS program is 80-85%, so ·
a minimum level of 80% was selected for level IV parameters.
Level III analyses being used as general indicators that are specific
for the risk assessment will have a minimum completeness of 90%.
A minimum completeness of 75% has been set for level II
parameters.
Tables 4-1 and 4-2 give the target limits for all analyses in terms of precision accuracy
and completeness.
4-4
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Section No. 4
Revision No. 0
Date 1/08/90
Page S of9
For purgeable and extractable compound analyses by GC/GCMS, precision and
accuracy criteria are given only for selected analytes to be used in spiking for method
control purposes.
4-S
I Section No. 4
Revision No. 0 I Date 1/08/90
Page6oC9
I
TABLE 4-1
I QUALITY ASSURANCE OBJECTIVES (GROUNDWATER/SURFACE WATER SAMPLES)
Spiking Preciaion Accuracy Completeness I Parameter Reference Level (RPD) (% RCOOYCry) (%)
pentachlorophenol EPA 515 0.10 ug/1 20 68-122 90 I isopropyl ether EPA8020 5 ug/1 18 75-125 90
total organic carbon EPA 415.1 20 mg/I 9 85-115 90
chemical oxgyen demand EPA 410.1 250 mg/I 9 85-115 90
I biochemical oxgyen demand EPA 405.1 15 90
suspended solids EPA 160.2 15 90
pH EPA ISO.I 0.2 unita 75
specific conductance EPA 120.1 10 75 I Phenols
phenol EPA8040 100 ug/1 42 12-ll9 90
I 2·<:hlorophcnol EPA8040 100 ug/1 40 27-123 90
4-nitrophenol EPA8040 100 ug/1 so 10-80 90
4--chloro-3-methylphenol EPA8040 100 ug/1 42 23-97 90
I pentachlorophenol EPA8040 100 ug/1 so 9-103 90
TCL Volatiles
I, 1-<iichloroethene EPA 8240-CLP 50 ug/1 14 61-145 80 I trichloroethene EPA 8240-CLP 50 ug/1 14 71-120 80
chlorobenzene EPA 8240-CLP 50 ug/1 13 75-130 80
toluene EPA 8240-CLP 50 ug/1 13 76-125 80
I benzene EPA 8240-CLP 50 ug/1 11 76-127 80
TCL Semivola1iles
I 1,2,4-trichlorobenzene EPA 8270-CLP 50 ug/1 28 39-98 80
accnaphthene EPA 8270-CLP 50 ug/1 31 46-118 80
2.4-dinitrotolucne EPA 8270-CLP SO ug/1 38 24-96 80
di-n-butylphth.alate EPA 8270-CLP 50 ug/1 40 11-117 80 I pyrenc EPA 8270-CLP 50 ug/1 31 26-127 80
N -nitrosodi
-n-propylamine EPA 8270-CLP 50 ug/1 28 36-97 80
I 1,4-dichlorobenzene EPA 8270-CLP 50 ug/1 28 36-97 80
pentachlorophenol EPA 8270-CLP 100 Ug/1 so 9-103 80
phenol EPA 8270-CLP 100 ug/1 42 12-ll9 80
I 2-chlorophenol EPA 8270-CLP 100 ug/1 40 27-123 80
4--chloro-3-methylphenol EPA 8270-CLP 100 ug/1 42 23-97 80
4-nitrophenol EPA 8270-CLP 100 ug/1 so 10-80 80
I TCL Pesticides
lindanc EPA8080-CLP 0.2 ug/1 15 56-123 80
heptachlor EPA 8080-CLP 0.2 ug/1 20 40-131 80
I aldrin EPA 8080-CLP 0.2 ug/1 22 40-120 80
I DCC#Q461
4-6
I Section No. 4
Revision No. o I Date 1/08/90
Page7 of9
I
TABLE 4-1 (continued)
I QUALITY ASSURANCE OBJECT1VES (GROUNDWATER/SURFACE WATER SAMPLES)
Spiking Preciaion Accunocy Completeness I Parameter Reference Level (RPD) (% RCCOYCry) (%)
dieldrin EPA 8080-CLP 0.5 ug/1 18 52-126 80
I endrin EPA 8080-CLP 0.5 ug/1 21 56-121 80
4,4'-DDT EPA 8080-CLP 0.5 ug/1 r, JS.lrl 80
T,~L inoaanics I aluminum EPA 6010.CLP 2000 ug/1 20 75-125 80
antimony EPA 6010.CLP 100 ug/1 20 75-125 80 arsenic EPA 7060-CLP 40 ug/1 20 75-125 80 I barium EPA 60JO.CLP 2000 ug/1 20 75-125 80
beryllium EPA 60 JO-CLP 50 ug/1 20 75-125 80
cadmium EPA 60 JO.CLP 50 ug/1 20 75-125 80
I calcium EPA 6010-CLP 50 ug/1 20 75-125 80 chromium EPA 60 IO.CLP 200 ug/1 20 75-125 80
cobalt EPA 60 JO.CLP 500 ug/1 20 75-125 80 copper EPA 6010.CLP 250 ug/1 20 75-125 80 I iron EPA 60 JO-CLP 1000 ug/1 20 75-125 80
lead EPA 742J-CLP 20 ug/1 20 75-125 80 magnesium EPA 6010.CLP 20 ug/1 20 75-125 80
I manganese EPA 60 JO.CLP 20 75:125 80
mercury EPA 7470.CLP 1 ug/1 20 75-125 80
nickel EPA 60 IO.CLP 500 ug/1 20 75-125 80
I poLaS&ium EPA 6010.CLP 20 75-125 80
selenium EPA TI4Q.CLP 10 ug/1 20 75-125 80
silver EPA 6010.CLP 50 ug/1 20 75-125 80
sodium EPA 60JO.CLP 20 75-125 80 I lhallium EPA 7841-CLP 50 ug/1 20 75-125 80
vanadium EPA 60JO-CLP 500 ug/1 20 75-125 80
zinc EPA 6010-CLP 500 ug/1 20 75-125 80
I cyanide EPA 9012-CLP 100 ug/1 20 75-125 80
Dioxins/furans
I 2,3,7,8-TCDD EPA8290 1 ng/1 50 40-140 90
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Revision No. 0 I Date 1/08/90
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TABLE 4-2
I QUALITY ASSURANCE OWEC!lVES (SOIUSEDIMENT SAMPLES)
Spiking Prcciaion Accuracy Completeness I Parameter Reference ~cl (RPD) (%RC<OYCry) (%)
lotal organic carbon EPA 9060 1000 mg/I<& 30 70-130 90
I isopropyl ether EPA8020 500 ug/1<& 20 75-125 90
Phenols
I phenol EPA8040 10000 ug/1<& 35 26-90 90
2-<:hlorophenol EPA8040 10000 ug/1<& 50 25-102 90
4-niirophenol EPA8040 10000 ug/1<& 50 11-114 90
4-chloro-3-methylphenol EPA8040 10000 ug/1<& 33 26-103 90 I pentachlorophenol EPA8040 10000 Ug/1<& 47 17-109 90
TCL volatiles
I 1,1-dichloroethenc EPA 8240-CLP 50 ug/1<& 22 59-172 80
trichloroethenc EPA 8240-CLP 50 ug/1<& 24 62-137 80
benzene EPA 8240-CLP 50 ug/1<& 21 66-142 80
1olucnc EPA 8240-CLP 50 ug/1<& 21 59-139 80 I chlorobenzene EPA 8240-CLP 50 ug/1<& 21 60-133 80
TCL scmivolatiles
I phenol EPA 8270-CLP 3300 ug/1<& 35 26-90 80
2-chlorophenol EPA 8270-CLP 3300 ug/1<& 50 25-102 80
1,4-dichlorobenzenc EPA 8270-CLP 1600 ug/1<& 27 28-104 80
I N-nitroso-di-n-
propylaminc EPA 8270-CLP 1600 ug/1<& 38 41-126 80
1,2. 4-trichlorobenzenc EPA 8270-CLP 1600 ug/1<& 23 38-107 80
4-chloro-3-mcthylphenol EPA 8270-CLP 3300 ug/1<& 33 26-103 80 I accnaphthcnc EPA 8270-CLP 1600 Ug/1<& 19 31-137 80
4-nitrophcnol EPA 8270-CLP 3300 ug/1<& 50 11-114 80
2,4-dinilrotCHuenc EPa 8270-CLP 1600 ug/1<& 47 28-89 80
I pentachlorophenol EPA 8270-CLP 3300 ug/1<& 47 17-109 80
pyrenc EPA 8270-CLP 1600 ug/1<& 36 35-142 80
I T AL inorganics
aluminum EPA 60 IO-CLP 20 75-125 80
antimony EPA 6010-CLP 10 mg/I<& 20 75-125 80 arsenic EPA 7060-CLP 4 mg/I<& 20 75-125 80 I barium EPA 60 l0-CLP 200mg/k& 20 75-125 80
beryllium EPA 6010-CLP 5 mg/I<& 20 75-125 80
cadmium EPA 6010-CLP 5 mg/I<& 20 75-125 80 I calcium EPA 6010-CLP 20 75-125 80 chromium EPA 6010-CLP 20 mg/I<& 20 75-125 80
cobalt EPA 6010-CLP 50 mg/I<& 20 75-125 80
I copper EPA 6010-CLP 25 mg/I<& 20 75-125 80
DCC#Q461
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Revision No. 0
I Date 1/08/90
Page9of9
I
TABLE 4-2
I QUALITY ASSURANCE OBJECTIVES (SOILJSEDIMENT SAMPLES)
Spiting Preciaioo Accuracy Completeness I Parameter Reference 1.-i (RPD) (% RCOOYery) (%)
iron EPA 6010-CLP 20 75-125 80
I lead EPA 7421-CU' 2 mg/1:g 20 75-125 80
magnesium EPA 6010-CLP 20 75-125 80
manganese EPA 6010-CLP 50 mg/1:g 20 75-125 80
mercury EPA 7471-CLP 0.1 mg/kg 20 75-125 80 I nickel EPA 6010-CLP 50 mg/kg 20 75-125 80
potassium EPA 6010-CLP 20 75-125 80
selenium EPA 7740-CLP lmg/kg 20 75-125 80 I sitvcr EPA 6010-CLP 5 mg/kg 20 75-125 80
.scxiium EPA 6010-CLP 20 75-125 80
thallium EPA 7841-CLP 5 mg/kg 20 75-125 80
I vanadium EPA 6010-CLP 50 mg/kg 20 75-125 80
tine EPA 6010-CLP 50 mg/kg 20 75-125 80
cyanide EPA 9012-CLP 10 mg/kg 20 75-125 80
I TCL pesticides
lindane EPA 8080-CLP 32 ug/kg 50 46-127 80
heptachlor EPA 8080-CLP 32 ug/kg 31 35-130 80
I aldrin EPA 8080-CLP 32 ug/kg 43 34-132 80
dieldrin EPA 8080-CLP 80 ug/kg 38 31-134 80
endrin EPA 8080-CLP 80 ug/kg 45 42-139 80
I 4,4'-DDT EPA 8080-CLP 80 ug/kg 50 23-134 80
Dioxins/furans
2.3.7,8-TCDD EPA8290 1 ug/kg 50 40-140 90 I
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5.0 SAMPLING EQUIPMENT AND PROCEDURES
5.1 Surface Water Sampling
5.1.l Sample/Location Selection
Section No: 5
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Two rounds of surface water sampling will be performed with at least a one month
interval between each sampling event. The proposed sampling locations are shown
on Figure 3.1. All surface water samples will be collected prior to the collection of
the sediment samples.
5.1.2 Stream Sampling
The surface water samples collected from: 1) the ditch connecting the fire pond and
Medlin Pond, 2) the effluent stream from Medlin Pond, 3) the eastern drainage
ditch, 4) the western drainage ditch, and 5) the drainage ditch from the wooded area
in the southwestern portion of the site, will be collected using the procedures
outlined below.
2.
3.
DCC#Q461
In shallow streams ( those which can be safely traversed on foot) the
sam pie containers will be filled directly with the flowing water. The
flow in the ditches and streams identified in this investigation is low
enough to enable these samples to be collected in this manner. The
grab surface water samples will be collected at each of the proposed
sampling locations (Figure 3.1) unless insufficient flow precludes the
collection of sample water. Sampling will begin at the most
downstream sampling point and proceed upstream.
Samples will be collected at mid-depth in the mid-section or deepest
flow channel of the sampling location.
It may be necessary to collect the stream and ditch samples by using a
stainless steel sheet metal v-notch weir or similar device to direct the
flow into the sample container. If this situation occurs a decision will
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4.
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be made in the field by the project scientist/geologist. The field notes
and corresponding documentation will reflect such a decision.
After the sample water has been collected, samples requiring
preservation will be preserved (see Tables 6-la and 6-lb for a list of
parameters specific to this investigation and the specific preservation
and holding times). The sample containers will be handled, and
shipped according to the sample handling procedures outlined in
section 6.0.
5.2 Pond Sampling
Six water samples will be collected from both the fire pond and the Medlin Pond.
These samples will include a shallow sample and a depth sample collected at three
locations on each pond ( see Figure 3.1 for the proposed sample locations). All pond
sampling will be performed from a floating platform by a two person crew.
1.
2.
DCC#Q461
The grab samples will be collected just below the surface of the water.
Each individual sampling container will be filled separately from the
same location. Preservatives, if necessary, will be added after the
samples have been collected.
The second sample from each location will be collected from a depth
approximately two-thirds of the distance between the surface and the
bottom of the pond.
The depth of each sampling location will be determined in
advance using a weighted tape measure or similar device.
Depending on the depth of the pond, either a discrete grab
sampling device, a van duren sampler, or a peristaltic pump
with teflon tubing will be used to collect water samples from the
specific location beneath the water surface.
If a peristaltic pump is used, the field decontamination would
be eliminated as new teflon tubing would be used at each
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sample location. Care would be taken to regulate the speed of
the pump to reduce the potential for degassing volatile organic
aromatics if present.
Care will be taken to ensure that the depth samples are
collected from the appropriate depth.
If sampling equipment must be reused, it will be
decontaminated in the field using the following procedures.
1) wash with tap water and non-phosphate detergent.
2) rinse with tap water
3) dry thoroughly
4) rinse twice with pesticide grade hexane
5) rinse several times with distilled deionized water
6) dry thoroughly and if not used immediately, wrap in foil and
plastic until next use.
Wash water and used solvent will stored in designated containers until
sufficient amounts are available for future testing, treatment and/or
disposal.
3. All samples will be handled and shipped following the procedures
outlined in section 6.0. (see Tables 6-la and 6-lb for a list of
preservatives and sample holding times).
4. Field notes will be recorded documenting all field sampling and
measuring activities. Information such as sample collector, date and
time of sampling, location of sampling point, results of field
measurements and weather conditions will be included in the notes. If
sampling decisions must be made in the field due to field conditions,
this information will also be documented in the field notes.
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5.3 Flow Measuring
Section No: 5
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During each of the two rounds of surface water sampling, the flowrate of the ditch
connecting the fire pond and the Medlin Pond, and the effluent stream will be
performed.
The following methods may be used to collect the flowrate from these open channel
flow systems:
1.
2.
3.
4.
DCC#Q461
Time Gravimetric -Two examples include tipping bucket rain gauge,
and bucket and stopwatch.
Practical considerations limit the use of this technique to very low flow
rates, and because of the nature of the measurement, it is not suited
for continuous measurement.
Dilution -Flow is measured by determining the degree of dilution of
an added tracer solution by the flowing water.
Examples of tracer solution include, radioactive, fluorescent dye and
lithium.
o Two general techniques include;
constant rate injection method
total recovery (slug injection)
Velocity Area -Flow is calculated by determining the mean flow
velocity across a cross-section and multiplying this by the flow area at
the point.
Hydraulic Structure -This structure includes the use of primary and
secondary measuring devices to determine flow.
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o Flow in an open channel is measured through the use of a
hydraulic structure inserted into the channel which changes the
level of liquid in or near the structure. With the dimensions of
the hydraulic structure known, the rate of flow through or over
the restriction will be related to the liquid level in a known
manner.
o Weirs and flumes are commonly used primary devices.
Weirs -are a type of dam built across an open channel
which liquid flows over or through some type of notch.
Weirs are classified according to the shape of their notch
( examples include; rectangular, v-notch, and the
trapezoidal). Each type of the weir has an associated
characteristic equation for determining the flow rate
through the weir.
Flumes -are specially shaped open channel flow section
providing a change in the channel area and/or slope
which results in an increased velocity and change in the
level of the liquid flowing through the flume. A typical
flume consists of three sections: 1) a converging section,
2) a throat section, and 3) a diverging section. Examples
of the most commonly used flumes are the Parshall
Flume, and the Palmer-Bowlus Flume.
o A secondary measuring device is used in conjunction with the
primary measuring device to measure the rate of liquid flow in
an open channel. The secondary measuring device has the
following purposes:
to measure the liquid level in the primary measuring
device;
to convert this liquid level into an appropriate flow rate
according to the known liquid level/flow rate
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Documentation
Section No: S
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relationship of the primary measuring device, a totalized
volume can be determine from this flow rate.
Other types of flow measuring devices include;
Float
Dipping Probe
Electrical
Ultrasonic
Bubbler
Submerged Pressure Transducer
All field notes and measurements will be recorded, summarized, and presented at
the completion of the study. Care is taken to ensure the accurate recording and
interpretation of all data gathered.
Field conditions will dictate the device which will be used to measure the flowrate in
the ditch and the effluent stream. Flowrate information may not be obtainable if the
flow in the ditch and/or the stream is minimal. Should this occur the field notes will
document the low flow conditions and the attempts to measure the flow in these
streams.
S.4 Sediment Samplin&
Sediment sampling will be conducted at the fire pond, Medlin Pond, and along
surface water drainage ditches. Proposed locations are shown on Figure 3-1.
Sediment sai:npling of the ponds will be accomplished from a floating platform. Core
samples will be collected in the following manner. A section of 4-inch flush-joint
PVC pipe will be set to the pond bottom sediments. Samples will be secured by
pushing a stainless steel Shelby tube, through the PVC pipe, into the sediments at the
bottom of the pond. Care will be taken so that the sample which is collected has not
contacted the PVC pipe. While withdrawing the sample, the pipe will be pushed or
driven into the sediments to the depth of the previous sample interval. The next
DCC#Q461 S-6
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Section No: S
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sediment sample will then be taken in a fashion similar to the first sample. Surface
sediment samples will be collected using a ponar sampler. Sediment samples will be
mixed thoroughly before being placed in sample containers. The soil will be
contained in new glass containers with screw type lids. The sampling equipment will
be thoroughly washed between each use in soapy water, followed by a clean water
rinse, and rinses with hexane and distilled deionized water. The sediment samples
will be handled, preserved, and shipped in accordance with the U.S. EPA Region IV
SOPQAM (see Tables 6-la and 6-lb).
s.s Soil Sampling
Soil sampling will be conducted using split-spoon sampling techniques and hollow-
stem augers. Samples will be taken continuously in two foot increments to bedrock
or the water table, whichever is first encountered. Weathered bedrock is
encountered at approximately 10 feet in the former lagoon and wood treating areas
and within five feet of the surface in the former landfarm area. Auger or split-spoon
refusal (blow counts greater than 50 over 6-inches) will be used to determine the
bedrock surface and the termination depth of the boring if encountered above the
water table. Depth of groundwater is generally within ten feet of the surface in the
lagoon and treating areas and fifteen feet of the surface in the landfarm area. The
split-spoon will be thoroughly washed between each use in soapy water, followed by a
clean water rinse, and rinses with hexane and organic free water. Downhole drilling
equipment will be decontaminated between boring locations by the following
procedure.
DCC#Q461
1)
2)
3)
4)
5)
6)
Wash equipment with tap water and non-phosphate detergent.
Rinse with tap water.
Dry thoroughly.
Rinse twice with hexane.
Rinse several times with distilled deionized water.
Dry thoroughly and cover equipment unless it will be used immediately
after cleaning.
S-7
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Equipment used for the drilling of borings for monitoring well installation will be
subject to the same decontamination procedure between well locations. All rinse
water and solvent will be stored in designated containers for future testing,
treatment, and/or disposal.
Physical appearance of the soil, including odors or other unusual findings, will be
noted. The soils will be field classified by the supervising hydrogeologist according to
the Burmeister System. A chart of descriptive terms for the Burmeister Soil
Classification System is included as Appendix A of the November, 1989 Final Work
Plan.
If possible, augering will continue to the specified depth of the shallow wells for well
construction: All soil brought to surface will be contained in new glass containers
with screw type lids, labeled, and stored on-site. Sample preservation, shipment,
handling, and chain-of-custody procedures will be conducted in accordance with the
methods described in Section 6.0 and the U.S. EPA Region IV SOPQAM (see
Tables 6-la and 6-1 b ). If the borings are not used for monitoring well construction,
they will be filled from the bottom to the surface with a neat cement grout mixture.
5.6 Groundwater Sampling
Prior to implementing a groundwater monitoring program several tasks must be
performed. Sample bottles and equipment are cleaned and packaged for the
required sampling. The laboratory is notified of incoming samples to prepare for
holding times of specific samples. All of the sampling equipment required to collect,
contain, preserve, filter (if necessary), and ship the samples is packaged and
organized to allow efficient operation in the field. Field decontamination equipment
is also prepared to enable this work to be performed if required. All groundwater
samples will be preserved, handled, and shipped in accordance with the U.S. EPA
Region IV SOPQAM (see Tables 6-la and 6-lb).
DCC#Q461 5-8
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S.6.1 Sample Bottle Preparation
Section No: S
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The preparation of containers for groundwater samples is dependent upon the types
of analyses which will be performed on the samples. Three general types of analyses
are performed on groundwater samples: (i) conventional pollutants, (ii) metallic
pollutants, (iii) volatile organic and semi-volatile organics. The protocols for
preparing the bottles for each type of analysis are discussed below.
Conventional Constituents
2.
3.
Use new bottles with screw-type lids.
Pre label and preserve (where appropriate) all bottles prior to shipment.
Place bottles in suitable shipping packages, for example, ice chests with
adequate packing to reduce bottle breakage (see section 6.0).
Metallic Constituents
2.
New polyethylene containers are used with plastic screw type polyethylene
lined lids.
The cleaning procedures for each new container are as follows:
o Rinse container with 1: 1 nitric acid
0 Rinse container with distilled water two times.
o Rinse container with 1: 1 HCL
0 Rinse container thoroughly with distilled deionized water four times.
o Each container is thoroughly dryed, capped and stored for use.
3. All containers are prelabeled prior to shipment.
4. Once samples are collected, nitric acid is added to preserve the sample at a
pH of 2.0 or less.
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5.
6.
7.
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The preserved samples are then placed m ice chests and cooled to a
temperature of 4 degrees Celsius.
Before the cooler is sealed a chain of custody sheet is completed for each
cooler containing samples.
Each cooler is sealed, with chain-of-custody tape or tag, and shipped
overnight to Keystone's analytical laboratories for analysis.
Semi-Volatiles
1.
2.
3.
4.
5.
6.
New narrow neck amber bottles are used with a teflon lined lid.
The cleaning procedure for each new bottle is as follows:
0
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Rinse with pesticide grade isopropanol.
Air dry in laboratory hood.
Dry with pure nitrogen.
Prelabel Sample Containers.
Pack all bottles securely in ice chests.
Each cooler containing samples must have a completed chain of custody sheet
for the bottles contained inside.
The coolers should then be sealed, with chain-of-custody tape or tag, and
shipped overnight to Keystone's laboratories for analysis.
Volatile Organic Aromatics (VOAs)
1. Wash vials and septa with non-phosphate detergent and hot tap water.
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2.
3.
4.
Rinse three times with pre-filtered tap water.
Rinse again with distilled deionized water.
Section No: 5
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Oven dry containers and closures at 105° Centigrade for one hour.
5. Re-assemble bottles and closures.
The cleanliness of a batch of precleaned bottles is verified by the use of a trip blank.
The trip blank is prepared by filling a batch of precleaned bottles with distilled
deionized water. The bottles are transported to the site and returned to the
laboratory in the same manner used for the samples. The trip blank is subjected to
the same analyses as the samples. Any contaminants found in the trip blank could be
attributed to a) interaction between the sample and the container, b) contaminated
distilled deionized water, or c) a handling procedure which alters the sample. One
trip blank per sampling event is collected. In addition, one trip blank is placed in
each cooler that contains samples for volatile organics.
5.6.2 Eguipment Preparation Procedures
Bailer and Funnel Preparation
DCC#Q461
All stainless steel hailers and porcelain buchner funnels are laboratory
cleaned and prepared after each use by following the procedures outlined
below:
A)
B)
C)
D)
E)
F)
G)
Wash with non phosphate detergent.
Rinse with tap water three times.
Soak for five minutes in a 10% nitric acid solution.
Rinse with distilled deionized water four times.
Rinse with pesticide grade hexane.
Dry using pure nitrogen.
Heat for one hour at 800 degrees Fahrenheit.
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2.
H) Cool to room temperature.
I) · Wrap with aluminum foil (shiny side out).
Section No: 5
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A separate laboratory-cleaned stainless steel bailer is used to purge and
sample each well. All miscellaneous equipment such as shovels, soil trowels,
and stainless steel parts of other pieces of equipment are cleaned using the
procedures A) through F) outlined above, and wrapped with aluminum foil
and plastic.
The equipment cleaning procedures use pesticide grade hexane rinses to ensure the
thorough decontamination of the sampling equipment. After the solvent rinses, the
stainless steel equipment is placed in a heating oven for at least one hour at 800
degrees fahrenheit. This is performed to ensure the removal of residual solvent from
the stainless steel sampling equipment. If equipment can not be placed in the oven it
is blown dry with pure nitrogen to ensure the removal of residual solvent.
To verify that no contaminants are introduced from sampling equipment, a field
(equipment) blank is collected by filling or pumping distilled deionized water through
the sampling device and analyzing the water for the compounds of interest. One
field (equipment) blank is collected each day sampling is performed.
As per EPA Region IV guidance, all work plans, and field sampling plans reference
these cleaning procedures. These cleaning procedures and the procedures used in
the field, will be referenced in the field notes.
Bladder Pump Preparation
2.
DCC#Q461
Each tubing line set is dedicated for use on one well only. The sets of tubing
are packaged securely and marked for future use on the corresponding
dedicated wells.
Each pump should be disassembled according to the manufacturer's manual.
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3.
4.
5.
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The stainless steel parts of each pump are cleaned using the methods outlined
in section 5.6.2 A) through F).
The remaining parts of each pump are washed with non-phosphate detergent,
and rinsed with distilled deionized water.
Each pump is reassembled, wrapped in aluminum foil (shiny side out),
covered with plastic, and stored for future use.
S.6.3 Water Level Measurement
There are several methods used by Keystone when measuring the water levels of
wells. The following methods are listed in order of preference. Preferred methods
will obtain accurate water level and depth measurements, will be easy to
decontaminate, and will eliminate the chance of cross contamination.
Regardless of the method of water level measurement, the upgradient well( s) should
be measured prior to the downgradient. When performed in conjunction with
decontaminating the measuring device between wells, the potential for cross
contamination will be further reduced.
All water level measurements are taken from surveyed points on each well casing
and measured to an accuracy of .01 feet.
Interface Probe
Interface probes are commonly used to detect the presence of any floating or sinking
immiscible layers. However they can also be used to detect the water levels inside
wells.
1.
DCC#Q461
The probe should be lowered slowly inside each well. When water is detected
the probe will make a beeping noise to signify the beginning of the water level.
When the beeping noise is heard observe the calibrated drop line to
determine the water level.
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3.
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If a solid tone is heard, continue lowering the probe ( observing the calibrated
drop line) until the steady tone stops. The measurement on the drop line
between when the steady tone began and when it stopped will determine the
thickness of the light phase immiscible layer.
The procedure as described above can be used to determine the presence
( and thickness) of layers of dense phase ( sinking) immiscible layers.
All measurements should be recorded to the nearest one hundredth of a foot
The probe is decontaminated between each well by wiping it with a cloth
containing distilled deionized water. If visible contamination is present the
probe will be wiped with a cloth containing pesticide grade hexane, followed
by several wipes with a cloth containing distilled deionized water.
Electric Probe Method
1.
2.
3.
DCC#Q461
Lower the weighted probe into the well casing (when the probe contacts
water it will send a pulse to the above ground gauge which will be recorded by
a movement of the gauge stick) and observe the calibrated drop line to
determine the water level.
Mark the point on the cable at the surveyed point on the well, when the probe
is touching the water. Measure the distance from the mark to the last foot
mark and add this measurement to it to determine the water level.
The probe is decontaminated between each well by wiping it with a cloth
containing distilled deionized water. If visible contamination is present the
probe will be wiped with a cloth containing pesticide grade hexane, followed
by several wipes with a cloth containing distilled deionized water.
S-14
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5.6.4 Wen Purgjng
Section No: 5
Revision No: 0
Date: 01/08/90
Page 15 of29
All monitoring wells are purged prior to sample collection. Wells will be purged until
at least three casing volumes of water are removed from each well or until the pH,
conductivity and temperature of the purge water has stabilized prior to sampling.
The pH, conductivity and temperature field measurements will be recorded for each
well included in the sampling program. The final measurement recorded during the
purging process, to verify the stabilization of the water, shall be considered the
record for the well. If a well is purged dry, sufficient time must be allowed for
recovery.
To calculate the amount of water to purge from each well the depth of standing
water must be measured using one of the above noted procedures. In addition the
casing diameter of each well must be known. These measurements, along with the
following appropriate numbers, must be inserted into formula 1.0, to determine the
specific conversion factor to be used on each size well.
Gallons of H2O per Linear Foot of Casing Diameter:
1.5" = 0.1057
2.0" = 0.1623
4.0" = 0.6613
6.0" = 1.5003
Top Filling Stainless Steel Bailer Volume (per ft of bailer)
DCC#Q461
1 1/8" = 300 mis
11/2" = 425 mis
3.0" = 1850 mis
5 -15
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Formula 1.0
Gallons of H2O/linear ft. of casinLJ diameter x 3785 (mls(LJal) X3
volume of bailer
= conversion factor for each well being sampled
Section No: S
Revision No: 0
Date: 0 l/08/90
Page 16 of29
The conversion factor must be multiplied times the depth of standing water in each
well to determine the number of bails which must be purged from each well. The
following conversion factors are listed for the well diameters listed below:
Well Diameter
1.5"
2.0"
4.0"
6.0"
3 Casing Volume Conversion
4.007
4.3363
4.0589
9.2086
5.6.4.1 Purging and Sampling Methods
Wells are purged and sampled by either hand bailing or pumping.
When possible all samples are collected using bailers. Hand bailing for sample
collection is preferred because bailers can be decontaminated much more carefully
than pumps. Also since pumping rates are difficult to control and since most pumps
operate through a pulsating action the potential degassing of volatile organic
concentrations may occur.
Bailing
The following procedures are followed when wells are purged and samples are
extracted using hand bailers.
1. Place plastic sheeting ( or garbage bags) around the well casing to create a
clean surface for the placement of sampling cord and equipment.
DCC#Q461 S -16
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2.
3.
4.
5.
6.
7.
Section No: S
Revision No: 0
Date: 0l/08/90
Page 17 of 29
Use a separate laboratory cleaned stainless steel bailer on each well for the
required purging and sampling.
Use new surgical or nitrile gloves when working on each well.
Use new nylon cord to tie on each bailer.
0 Make sure the knotted cord is securely tied to the bailer.
o After removing the protective foil wrapping from the bailer, lower it
into the well until it touches the bottom.
0 Remove an additional length of cord and tie it securely to the well
head to serve as a safety line for the bailer.
When raising the bailer the cord is collected on the plastic sheeting.
All purged groundwater will be collected and stored for future testing,
treatment and/or disposal.
Separate laboratory-cleaned stainless steel bailer is used to collect samples
from each monitoring well.
0
0
0
0
Samples are collected when the well recharges after purging.
All samples are collected according to their order of volatilization (see
Table 5-1).
All volatile organic samples will be collected with laboratory cleaned
bottom filling stainless steel hailers in conjunction with an emptying
device.
When sampling all hailers should be gently lowered into the well to
prevent degassification of volatile organic constituents which may be
present in the well water.
8. The remaining sample containers will be filled according to their order of
volatilization.
DCC#Q461 S -17
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Section No: 5
Revision No: 0
Date: 01/08/90
Page 18of29
Pumping
As noted above, when possible, pumps are not used to sample wells. However, there
are circumstances when pumps are more effective purging devices than hailers.
Also, in some instances pumps are the only means by which samples can be extracted
from monitoring wells.
There are several pumps which Keystone frequently uses to perform field work.
Peristaltic Pump:
Peristaltic pumps must be operated above ground next to the well being purged and
are limited to purging depths of 20.0 to 30.0 feet below ground surface.
1.
2.
3.
4.
DCC#Q461
New nalgene suction line is used on each well being purged. New silicon
pump head tubing will also be used if the pump is utilized for sampling.
If a peristaltic pump is used to collect a sample, e.g., the well casing is bent
preventing the passage of a bailer, the choice of tubing used to collect the
sample will be contingent on the parameters of interest.
0
0
For example, if conventional parameters are being analyzed then
standard nalgene tubing is sufficient to collect the sample.
If volatile, semi-volatile, or metals parameters are the constituents of
interest, teflon tubing is used to collect the sample.
The suction line should be lowered to a depth in the water column to assure
continued collection should drawdown of the water column occur.
To determine the proper amount of water to be purged, the pumping rate
should be measured in gallons per minute by recording the time required to
fill a selected volume of a calibrated bucket (see Section 5.6.4 on Well
Purging). Flow measurements should be performed three times on each well
to obtain an average rate.
5-18
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5.
6.
7.
Section No: S
Revision No: 0
Date: 01/08/90
Page 19of29
Monitor the pumping to ensure proper pump operation and assure
continuous discharge. If drawdown occurs lower the tubing deeper into the
water column.
When the required amount of water is purged from each well allow for
sufficient recovery before sampling.
Contain all purge water in labelled containers for future testing, treatment,
and/or disposal. All tubing is disposed of after each use.
Bladder Pumps:
The bladder pump is a gas operated positive displacement submersible well pump
that uses inert compressed gas, e.g., nitrogen, to inflate an internal bladder which
pumps water up the discharge line.
These pumps are used when large volumes of water must be purged from monitoring
wells. Usually these pumps are used on wells with diameters greater than 2.0" and
wells with depths up to 150 feet.
The line assembly is dedicated for use on one well only. After use the tubing is
wrapped in a spool, marked, and stored for future use in the specific well to which it
is dedicated.
The bladder pumps are primarily used to remove the required amount of water from
the monitoring well prior to sampling. When this is accomplished the well water is
sampled usirig a laboratory cleaned stainless steel bailer.
1. Connect the line assembly to the pump by first attaching the cable and then
connecting the sample and gas lines. '
DCC#Q46l 5 -19
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2.
3.
4.
5.
6.
7.
8.
9.
Section No: S
Revision No: 0
Date: 01/08/90
Page20of29
Lower the pump down the well by unrolling the line off of the spool until the
pump touches bottom. Raise the pump to the desired position inside the well
allowing sufficient room for drawdown of the water column.
Secure the cable to hold the pump at the desired depth.
Connect the gas line to the control box. The discharge line should be placed
in a container ( e.g. 55 gallon drum) to collect the purged water.
Connect the gas supply to the control box and adjust the pressure according to
the manufacturer's manual.
Tum on the control box and adjust the inflate delay to obtain the best
pumping cycle.
The pumping rate should be calculated to determine the length of time the
pump should run to purge the well. Field measurements of pH and specific
conductance, or the calculation of three casing volumes (see formula 1.0),
may be used to determine when a sufficient amount of water has been purged.
When the sufficient amount of water has been purged the well should be
sampled using a laboratory cleaned stainless steel bailer.
As noted, the tubing is used on one well only and after each sampling it is
packed, sealed, and stored for future use on that well.
Submersible Pumps:
When wells are encountered with depths greater than 150 feet, submersible pumps
are used to purge the required amount of well water. When possible the submersible
pumping apparatus is pulled to allow for sampling with a laboratory cleaned stainless
steel bailer. If this is not feasible the submersible pump will remain intact and will be
used to collect the sam pie.
DCC#Q461 S -20
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Section No: 5
Revision No: 0
Date: 01/08/90
Page 21 of29
When economically feasible the submersible pumps will be dedicated to each well.
However, in some cases this is not economically feasible and the same pump must be
used in several wells. Every effort will be made to ensure that these pumps are used
in wells containing similar concentrations of constituents of concern. A pump will
not knowingly be used in a dirty well prior to use on a clean well.
When the pumps must be reused, they will be steam cleaned between wells. If
possible, the pumps will also be taken apart and cleaned. The stainless steel parts
will be cleaned following procedures A) through F) in section 5.6.2. The remaining
parts will be washed with non-phosphate detergent and rinsed with distilled
deionized water. The pumps will be reassembled and covered until the next use.
2.
3.
4.
5.
6.
The submersible pump should be lowered to a depth in each well between the
middle to bottom screened portion of each monitoring well. The safety line
should be secured to the well casing.
Connect the power cord to the power source (generator) and tum on the
pump.
Continue to monitor the pumping rate and lower the line if drawdown of the
water column occurs.
If the well is pumped to dryness allow ten minutes for the well to recover.
After this period the pump should be re-started and the total discharge
volume should be measured to determine the rate of recharge.
Collect and contain all purged water in labelled containers for future testing,
treatment, and/or disposal.
5.7 Sample Filtration
Filtering will not be performed on samples to be analyzed for organics. Only
inorganics will be filtered as outlined in the approved Work Plan. Specific to this
DCC#Q461 5-21
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Section No: S
Revision No: 0
Date: 01/08/90
Page22oC29
investigation, groundwater samples will be designated in the field for analysis of
dissolved metal concentrations. However, per the request of EPA Region IV, non-
filtered samples will be maintained as the samples of record. The filtering of these
samples will be performed at the project site using .45 micron filter paper.
Filtering is performed using either vacuum pumps with funnels, or peristaltic pumps
with disposable funnels/filters. If using the vacuum pump method a laboratory
cleaned funnel is used for each well. Funnels are cleaned in the laboratory using the
procedures outlined in section 5.6.2. If using the peristaltic pump method, new
silicone tubing is used in the pump head of these pumps with teflon tubing running
from the pump to the disposable filter. Whether using the vacuum pump or
peristaltic pump methods all samples are filtered through .45 micron filter paper.
After filtering, samples requiring preservatives are preserved and all containers are
securely placed in coolers and chilled to a temperature of 4 degrees Celsius. Each
cooler containing samples will contain a completed chain-of-custody form or tag (see
Section 6.0).
S.8 Safety Precautions
When in the field performing sampling work all personnel will comply with the EPA
established level D safety precautions. This includes wearing long sleeve shirts, long
pants, goggles or safety glasses, hardhats, steel toe boots, and safety gloves. In
addition Keystone's Health and Safety officer will determine, in advance, if
additional safety equipment is required, for example tyvek suits, and/or respirators.
S.9 Documentation
A number of documents must be completed before, during, and after each sampling
project. These documents include analytical request forms, chain of custody sheets,
field data sheets and any project notes pertaining to the sampling work. Additional
documents are used as reference information during each phase of a project and they
include holding time sheets, and sample preservation and containment sheets.
DCC#Q461 S -22
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Analytical Request Form:
Section No: S
Revision No: 0
Date: 01/08/90
Page23of29
The analytical request forms (See attachment 1) are completed by the project
engineer/scientist and submitted to the sampling team when requesting sampling
work. These sheets contain the specific parameters of interest for which the
collected samples will be analyzed. The field team coordinator sends the request
forms directly to the sample control department to notify the laboratory of the
incoming samples. If the field team is not used to collect the samples then the
engineer or scientist requesting the work is responsible for providing this information
to the laboratory.
Chain of Custody Sheets:
When the field team sends samples to Keystone's analytical laboratories, each ice
chest containing samples must be accompanied by a chain of custody form (see
attachment 2). These forms contain information pertaining to the samples such as:
the project name, the name of the people collecting the samples, the site of
collection, the date and time of collection, the parameters of interest for each
sample, remarks or observations of samples if appropriate, the signature of the
person relinquishing control of the samples and the name of the carrier shipping the
samples to the laboratory (e.g. Federal Express, Purolator, etc.). The original chain
of custody sheet is sent with the samples, one copy is kept with the client and the
other copy is stored in Keystone's field team files.
Field Data Sheets:
The field data sheets (See attachment 3) serve as a field logbook for information
pertaining to each specific project. The basic project information such as the name
of the project, the date of sampling and the name of the people collecting the
samples is contained on these forms. These forms are specifically designed for the
collection of samples from groundwater monitoring wells. Information pertaining to
the wells being sampled is recorded on these forms. Observations are made on the
integrity of the wells being sampled and the physical characteristics of the water in
the wells. If representatives are on-site to observe sampling activities and or to split
DCC#Q461 S -23
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Section No: 5
Revision No: 0
Date: 01/08/90
Page24of29
samples, the names, positions and departments of these people is noted on the sheet.
The original copy of the field sheets is stored in the project files of Keystone's field
team. One copy is kept with the client and the remaining copies are sent to the
Keystone personnel involved with the project. Data generated from the field
investigations will be reported using the "Export Protocol for Toxics Compliance
Monitoring Data," as requested by EPA Region IV.
Project Notes:
Information specific to each project is written on computer generated printouts (See
attachment 4 ). These sheets are used by the field team members to prepare for and
to perform the work required to successfully complete the sampling project.
Additional Documents:
Tables 6-la and 6-lb contain the holding times, and protocol for proper pr,eservation
and containment of water and soil samples (Reference September 1986, RCRA
TEGD, EPA SW-846 2nd Edition 1982 and U.S. EPA Region IV SOPQAM). All
laboratory procedures and test methods will be consistent with and incorporate all of
the requirements which are set forth in the EPA Region IV support branch Standard
Operating Procedures and Quality Assurance Manual. All sample collection and
handling procedures will be consistent with those outlined in the Field Sampling Plan
(FSP) and the U.S. EPA Region IV SOPQAM.
This information enables the field team to properly preserve samples and it provides
the field team with a time table of when samples must be received by the laboratory
for analysis within the recommended EPA holding times.
DCC#Q461 5 -24
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TABLE 5-1
ORDER OF VOLATILIZATION
Section No: 5
Revision No: 0
Date: 01/08/90
Page 25 of29
Water samples are collected according to the following order of volatilization as
referenced m the September, 1986 RCRA TEGD:
0
0
0
0
0
0
0
0
Volatile Organic Aromatics (VOAs) -No air bubbles
Total Organic Halogens (TOX) -No air bubbles
Total Organic Carbon (TOC) -No air bubbles
Semi-Volatile Organics
Total Metals
Dissolved Metals
Total Phenols
Cyanide
There is not an order of preference for the collection of the remaining conventional
parameters.
0
DCC#Q461
The water samples to be analyzed for radionuclides should be collected last at
each sampling point.
5-25
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ATTACHMENT l Section No: s
Revision No: O
Date: 01/08/90
Page26of 29
ANALYTICAL FIIQU!ST ,oAM
~ t<:luesr '." ax1n Sy: ----------
c:ienr: --------------c: i en t C~nrac:: ?rortct ManaQ1r: ------:-,1ecnon1: ------------Adc:ress: -------
Slart Oate:
No.o, MATRIX ANALYTICAL PARAMITIAS TIJANAROUND SAMPL!S
TIMI, DAYS
APPUCATlON: ONPOU OSCWA 0 ACRA D~ Special lnstruc:tlanl: _____________________
_
5-2G
.,,
I
"' -.J
--- -- - --------l\~~r~§ CHAIN OF CUSTODY RECORD
PLANTCODE I PROJECT NAME
NUMBER
SAMPLERS
OF (Signatu,e/
CONTAINERS
C • • STA. NO. DATE TIME 0 • I STATION LOCATION M • ' • • '
Relinqui.,_ by: (SignMwe) 0... Tlfflll -by: /SJg,ylweJ Rellqulahed by: (SlgnMu,.} Doi•
Rolinquiahed by: (s;gn.ture) o ... Time -by: (SJgtylu,-} Rellqul.,_ by: (SJg,wlure} Del•
Reliqui.,_ by: /5,gnMur•J Dole Time -to, Lal>ofelOfY by: (Signalu,e) o... I Tlfflll Ice Chest Temp
OC • DISTRIBUTION: Orig!,.. ---ohlpment: Copy to C--Fleld Flleo.
-----
t-
' ..,.
;:::
.§' REMARKS OR
f
8 ~ OBSERVATIONS
N
Time -by:{~)
Time -by: (sii,,,.,ute)
h» Oaest Own of Cuotod\l
# Tag# i::, ii
PAGE __ OF WC .... l::'.
51.~
Section No: I A?"i-ACBMDt 3
Revision No:
Date: 01/08/~ p or; age28 I ... .~~ I
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Revised:
Plant Name:
Ch.:irge #:
EXAMPLE
ABCDE
111111-11·11
ATTACHMENT 4
Section No: 5
Revision No: 0
Date: 01/08/90
Page29of 29
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Wells:
Copy Reports To:
R-1, R-7, R-8, R-8B, R-9, R-9C, R-9D, R-10, SF-I, SF-2, SF-3, SF-4 X. Smith, Y. Smith, Z. Smith
Turnaround: Normal
Sampling Dates: Quanerly
The following is a list of parameters for which samples are analyzed:
Field Meas.
pH(4X)
Cond.(4X)
I NaRS04
I TOC(4X)
I NOTES:
EPA83!0
EPA8040
Tox(4X)
TOC, TOX, pH, and Cond. get replicated 4x for all wells. • prepare an additional TOX bottle for all wells being replicated 4x. I DO NOT FILTER ANY p ARAMETERS.
I I THIS IS AN EXAMPLE COPY OF A COMPUTER GENERATED PRINTOUT.
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6.0 SAMPLE CUSTODY
Section No. 6
Revision No. O
Date 1/08/90
Page 1 of6
The primary objective of sample custody is to create an accurate written verified
record, which can be used to trace the possession and handling of the samples from
the moment of collection through data analysis and reporting. A sample is under
custody if:
a. it is in your possession, or
b. it is in your view, after being in your possession, or
c. it was in your possession and you locked it up, or
d. it is in a designated secure area.
6.1 Fjeld Sample Documentation
The field sampler will be personally responsible for the care and custody of the
samples collected until they are properly transferred or dispatched. Samples will be
accompanied by a Chain-of-Custody Record (see Figure 6-1). When transferring the
possession of samples, the individuals relinquishing and receiving will sign, date, and
note the time on the Record, with a separate Chain-of-Custody Record
accompanying each shipping container.
In cases where samples leave the originator's immediate control, such as shipment to
the laboratory by a common carrier ( e.g., Federal Express), a seal is provided on the
shipping container to document the integrity of the samples during transportation.
Any shipping containers that do not arrive at the laboratory with the seal intact will
not be considered to have been in valid custody. Before each container is sealed for
shipment, it is packed with ice or coolant so that the temperature inside the container
is 4°C. The temperature is checked in the field and is recorded on the Chain-of-
Custody Record.
DCC#Q461 6-1
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6.2 Laboratory Sample Documentation
Section No. 6
Revision No. 0
Date 1/08/90
Page2of6
Upon arrival at the laboratory, samples will be checked in by the Sample/Analysis
Coordinator or his designee. The following procedures will be followed:
DCC#Q461
a) The Sample/Analysis coordinator will first examine whether the
shipping container seals are intact or broken. Containers with broken
seals will not be accepted for analysis.
b) He will next open the coolers and determine if proper temperature has
been maintained during shipment. The temperature upon receipt is
recorded on the Chain-of-Custody Record.
c)
d)
e)
If samples have been damaged during shipment, the remaining
samples shall be carefully examined to determine whether they were
affected. Any samples affected shall also be considered damaged. It
will be noted on the Chain-of-Custody record that specific samples
were damaged and that the samples were removed from the sampling
program. Field personnel will be notified as soon as po~sible that
I samples were damaged and that they must be resampled, or the testing
I
program changed. '
He will next compare the samples received against those listed on the
Chain-of-Custody Record and verify that sample holding times have
not been exceeded. Table 6-1 gives the recommended holding times
for analyzing samples. Results from analyses performed after the
given time period should be considered suspect.
The Sample/Analysis Coordinator will then sign and date the Chain-of-
Custody Record and attach any waybill to the Chain-of-Custody
Record.
6-2
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Section No. 6
Revision No. 0
Date 1/08/90
Page3 of6
THe laboratory LIMS (Laboratory Information Management System) computer is
an integral part of the sample custody procedure. Upon verification of sample
receipt at the laboratory, the Sample/Analysis Coordinator will assign a unique eight
character ID number to the sample for entry into the LIMS computer.
The first two characters reference the year, the next two the month, and the last four
tlie actual number of samples received from that plant. For example:
86
year
06
month
0013
sample number
Once samples have been logged-in and transferred to the proper storage areas, the
department manager is responsible for their proper storage and condition.
Each department manager is given a Laboratory Sample Chronicle (see Figure 6-2)
which lists the sample identification, matrix, parameters for analysis, and required
completion date. These forms are used to document sample custody 'while the
samples are in-house. All Chain-of-Custody Records and Sample Chronicles are
kept on file by the Manager of Quality Assurance.
DCC#Q461 6-3
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Parameter
Suspended Solids
Isopropyl Ether, Volatile Organics
Phenols, Pentachlorophenol,
Semivolatiles
8005
TOC, COD, Mercury
Dioxins/Fu rans
Metals
DCC#Q461
Section No. 6
Revision No. 0
Date 1/08/90
Page 4 of 6
TABLE 6-1
HOLDING TIMES
6-4
Holding Time
Within 7 days of collection
Within 14 days of collection
Within 7 days of collection (for extraction)
Within 40 days of extraction (for analysis)
Within 48 hours of collection
Within 28 days of collection
Within 30 days of collection (for extraction)
Within 40 days of extraction (for analysis)
Within 180 days of collection
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Section No. 6
Revision No. 0 I · I Date 1/08/90 ' : f Page S of 6 I . •
I II 'J l't 'J I I I I I ' -a
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, I lz :];' -

-
! I i] : I .J...i,,, ._,, ---~----l ---1 ~j-:I :Ii '•~,., 0 o..,~ , , , : , 1 \ \ ' I I I il 1J ; J 1
-.....;_' ..:,_' ...:..' _1_: _, _1~1 ~' -:-' -1,~'1 ..,..I -tl---r--1 I I· -1,1 I ' ' i I ! I ,!I ,!I
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Wor& Order ____ _
Sample ~umbers ___ _
~7ALS D!GES7::N
!'igure 6-2
Section No. 6
Revision No. 0
Date 1108/90
Page 6 of6
~•trix (~ator.so~~.::~? ~? •el&ht/Vol1Jme :;1es:e~---
'.CP D1cest"on _______________________ _ --------~GA Jicest~on _____ _ i? ::x i&:~10: __ _ ---------------------:::.? ~x-:~1-:: _______________ _
~e:--:·.::-Y : ~i•S~:.. =~·----------------------------
ANA;_ 'fSES Due t Due •• . H· .. m~:::.:::i _________ , ___________________ _ Ant~::iony ___ _ Arsen1: _________________________ _ Barlwn_ _ _________________ _ Bery 11 ~·.1.111 ________ _
C1dmi•.1m__ ------------------------'Cal: l1J.lll~--------------·---------------Chrom1.:m ____ _ Co:alt ______________________ _ Copper _____________________________ _
:r:"----------------:ead _____ _
!'!ac!les l 1Jm __
~•r.can•s•----------------------------!'!er:ury ______________________________ _ ~iekel _______ _
?OtlSSl.lffl _______________ ·-------------Selenium _______ , _____________ ...;.. _____ _ Si:ver ________________________ ...._ ____ _
S<Jd l \l:I ___ _ rhallium _____________________________ _ 7~~---------------------------------r ~ :•n1 •J.m Vanadium ___________________________ _ Zin: ______________ _ -------------
OTHlll A!fAL.YTU 1. _____ _
2. ____ _ 3. ____ _
!Jctraotio11 C.&b M&nacer ____________ Oate ____ _ Inor1u1ca C.&b H&Aacer Oate ___ _ QA Mai1ac•r Oat•-----
Note: rt sup le ■ are re-d11e1ted and re-analyzed because th• initial endeavors ~ailed to meet the required Quality Cont::: Cr~ter~a. t~• da~•• ot r1-di111ti0n ud/or re-analys~s w.~: :e entered 1= Col~:! Addit~onal:y
DCC#Q461 6-6
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7.0 ANALITICAL PROCEDURES
The exact analytical procedures used are given in Table 4-1 and 4-2.
DCC#Q461 7-1
Section No. 7
Revision No. 0
Date 1/08/90
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8.0 CALIBRATION CONTROLS AND FREQUENCY
Section No. 8
Revision No. 0
Date 1/08/90
Page 1 of 13
All field and laboratory equipment is calibrated before use to ensure proper
operating conditions. The following procedures are utilized for this purpose.
8.1 Field Instrumentation
pH Meter
The initial calibration is performed with three standard buffer solutions reading pH
4.0, 7.0, and 9.0. The calibration is checked after every ten samples. In addition, the
meter is checked with an outside calibration reference standard. If the check sample
is out of range, the instrument is recalibrated and the frequency of checks is
increased.
Conductivity Meter
The conductivity meter used does not have a designated calibration knob. The meter
is checked prior to use with an outside calibration standard. If the standard is not
within 10% of the true value, the instrument is not in calibration and a back-up unit
must be employed.
All field instrument calibrations are recorded on a field instrument calibration sheet
(Figure 8-1 ).
8.2 Laboratory Instrumentation. Conventional Chemistries
Colorimetric (Spectrophotometric) Analyses
The instrument must be calibrated before each use using a blank and five calibration
standards. The first standard must be at the method detection limit. In order to
verify the linearity of the curve, the regression coefficient (See Section 9.1) must be
at least 0.9995. If not, the standard curve must be reprepared. Next, to verify
DCC#Q461 8-1
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Section No. 8
Revision No. 0
Date 1/08/90
Page 2 of 13
accuracy of the curve, an outside reference standard is analyzed. Acceptable results
must be obtained on the reference standard before any samples are analyzed. After
every 10 samples and at the end of the run, a reagent blank and the mid-point
standard are analyzed. Any response in the reagent blank is subtracted from the
previous samples and the mid-point standard. If the mid-point standard differs from
the true value by more than 10%, the previous samples are invalidated and must be
reanalyzed. If an undiluted sample gives a response greater than the highest
standard, the sample must be diluted and reanalyzed. If the diluted sample gives a
response less than five times the method detection limit, the sample must be
reanalyzed at a lesser dilution.
Total Organic Carbon (TOC) Analyzer
Prior to each use, the TOC analyzer is calibrated with a standard containing 400 mg/I
of organic carbon. The linearity of the instrument is next verified by analyzing
standards at the 100 mg/I, 40 mg/I, 10 mg/I, and 1 mg/I levels. The acceptable ranges
are + 10%, 10%, 15%, and 50%, respectively. The standardization is next checked
by the analysis of an outside reference standard. Acceptable results must be
obtained on the reference standard before any samples are analyzed. After every 10
samples and at the end of the run, the 40 mg/I standard and a reagent blank are
analyzed. Any response in the reagent blank is subtracted from the previous samples
and the standard. If the 40 mg/I standard is off from the true value by mar~ than
10%, the previous samples are invalidated and must be reanalyzed. If an undiluted
sample reads greater than 400 mg/I, it must be diluted and reanalyzed. If the diluted
sample reads less than 20 mg/I, the sample must be reanalyzed at a lesser dilution.
8.3 Laboratory Instrumentation -Inorganics
Atomic Absorption Spectrophotometer
The instrument is calibrated before each use with a reagent blank and three
calibration standards. The first standard must be at the method detection limit. In
order to verify the linearity of the curve, the regression coefficient must be at least
DCC#Q461 8-2
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Section No. 8
Revision No. 0
Date 1/08/90
Page3 of 13
0.995. The calibration is next checked by the analysis of an outside reference
solution. The results must be within 10% of the true value for the initial calibration
to be verified. After every 10 samples, and at the end of the run, the outside
reference standard and reagent blank are analyzed. If the reagent blank shows a
result greater than the method detection limit, or if the reference standard differs
from the true value by more than 10%, the previous samples are invalidated and
must be reanalyzed. If an undiluted sample gives a response greater than the highest
standard, the sample must be diluted and reanalyzed. If the diluted sample gives a
response less than twice the method detection limit, the sample must be reanalyzed
at a lesser dilution.
Inductively Coupled Plasma Spectrophotometer
The instrument is calibrated before each use with a reagent blank and one other
calibration standard. The initial calibration is checked by the analysis of an 'outside
reference solution. The initial calibration solution is run at each wavelength used for
analysis. The results must be within 10% of the true value for the initial calibration
to be verified. In order to verify linearity near the detection limit, a standard
containing the elements of interest at twice the method detection limit is analyzed at
the beginning and end of each run. This standard is not required for Al, Ba, Ca, Fe,
Mg, Na, and K. After every 10 samples, and at the end of the run, the outside
reference standard and a reagent blank are analyzed. If the reagent blank shows a
response greater than the method detection limit, or if the reference standard differs
from the true value by more than 10%, the previous samples are invalidated and
must be reanalyzed. In order to verify the absence of interelement and background
interferences, an interference check sample is analyzed at the beginning and end of
each run. The results for elements present in the interference check sample must be
within 20% of the true value for the analytes of concern or the instrument must be
recalibrated and all samples since the last good interference check reanalyzed. A list
of the elements present in the interference check sample is given in Table 8-1.
DCC#Q461 8-3
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8.4 Laboratory Instrumentation . Organics
Section No. 8
Revision No. 0
Date 1/08/90
Page4of13
Gas Chromatographs
These instruments are calibrated for the components of interest with a solvent blank
and five calibration standards. The first standard must be at the method detection
limit. In order to verify the linearity of the curve, the regression coefficient must be
at least 0.995. The calibration is next check by the analysis of an outside reference
standard. If a supplied standard (NBS or EPA) is not available, an in-house solution
containing a concentration different than those used to prepare the curve is used.
The results obtained on the check standard must be within 20% of the true value for
the initial calibration to be verified. After every five samples, and at the end of the
run, the mid-point standard and solvent blank are analyzed. Any response found in
the solvent blank is subtracted form the preceding samples and the mid-point
standard.
If the mid-point standard differs from the true value by more than 20%, the previous
samples are invalidated and must be reanalyzed. If an undiluted sample gives a
response greater than the highest standard, the sample must be diluted and
reanalyzed. If the diluted sample gives a response less than twice the method
detection limit, the sample must be reanalyzed at a lesser dilution.
Gas Chromatograph/Mass Spectrometer (Dioxins/Furans)
1.
DCC#Q461
Two types of calibration procedures are required. One type, initial
calibration, is required before any samples are analyzed and is
required intermittently throughout sample analyses as dictated by
results of routine calibration procedures described below. The other
type, routine calibration, consists of analyzing the column performance
check solution and a concentration calibration solution of 500 ng/ml
(Paragraph 2). No samples are to be analyzed until acceptable
calibration as described in paragraphs 3 and 6 is demonstrated and
documented.
8-4
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2. Initial Calibration:
Section No. 8
Revision No. 0
Date 1/08/90
Page 5 of 13 I
I
2.1 Prepared multi-level calibration standards1 keeping one of the
recovery standards and the internal standard at fixed
concentrations (500 ng/ml).
Additional internal standards ( 13c1z-OCDD 1,000 ng/mL) are recommended when
quantification of the hepta-and octa-isomers is required. The use of separate
internal standards for the Pcdfs is also recommended. Each calibration standard
should contain the following compounds:
2,3,7,8-TCDD,
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,4,6, 7,8-HpCDD
2,3, 7,8-TCDF
1,2,3, 7,8,PeCDF
or any available
or any available
or any available
or any available
2,3,7,SX-PeCDD isomer
2,3,7,8,X, Y-HxCDD isomer,
2,3,7,8,X,Y,Z-HpCDD isomer
2,3,7,8,X-PeCDF isomer, ,
1,2,3,4,7,8-HxCDF or any available 2,3,7,8,X,Y,HxCDF isomer,
1,2,3,4,6, 7,8-HpCDD or any available 2,3,7,8,X,Y,Z-HpCDF isom'er,
OCDD,OCDF, 13C12-2,3, 7,8-TCDD, 13C121,2,3,4-TCDD and 13C12-OCDD
Recommended concentration levels for standard analytes are 200, 500, 1,000, 2,000,
and 5,000 ng/ml. These values may be adjusted in order to insure that the analyte
concentration falls within the calibration range. Two ul injections of calibration
standard should be made. However, some GC/MS instruments may require the use
of a 1-ul injection volume; if this injection volume is used then all injections of
1
DCC#Q461
13c12-labeled analytes are available from Cambridge Isotope Laboratory,
Wo15urn, Massachusetts. Proper qualification requires the use of a specific
labeled isomer for each congener to be determined. When labeled PCDDs
and PCDFs of each homolog are available, their use will be required
consistent with the technique of isotopic dilution.
8-5
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7.0 ANALYTICAL PROCEDURES
The exact analytical procedures used are given in Table 4-1 and 4-2.
DCC#Q461 7-1
Section No. 7
Revision No. 0
Date 1/08/90
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8.0 CALIBRATION CONTROLS AND FREQUENCY
Section No. 8
Revision No. 0
Date l/08/90
Page 1 of 13
All field and laboratory equipment is calibrated before use to ensure proper
operating conditions. The following procedures are utilized for this purpose.
8.1 Field Instrumentation
pH Meter
The initial calibration is performed with three standard buffer solutions reading pH
4.0, 7.0, and 9.0. The calibration is checked after every ten samples. In addition, the
meter is checked with an outside calibration reference standard. If the check sample
is out of range, the instrument is recalibrated and the frequency of checks is
increased.
Conductivity Meter
The conductivity meter used does not have a designated calibration knob. The meter
is checked prior to use with an outside calibration standard. If the standard is not
within 10% of the true value, the instrument is not in calibration and a back-up unit
must be employed.
All field instrument calibrations are recorded on a field instrument calibration sheet
(Figure 8-1 ).
8.2 Laboratory Instrumentation -Conventional Chemistries
Colorimetric (Spectrophotometric) Analyses
The instrument must be calibrated before each use using a blank and five calibration
standards. The first standard must be at the method detection limit. In order to
verify the linearity of the curve, the regression coefficient (See Section 9.1) must be
at least 0.9995. If not, the standard curve must be reprepared. Next, to verify
DCC#Q461 8-1
Section No. 8
Revision No. 0
Date 1/08/90
Page2 of13
accuracy of the curve, an outside reference standard is analyzed. Acceptable results
must be obtained on the reference standard before any samples are analyzed. After
every 10 samples and at the end of the run, a reagent blank and the mid-point
standard are analyzed. Any response in the reagent blank is subtracted from the
previous samples and the mid-point standard. If the mid-point standard differs from
the true value by more than 10%, the previous samples are invalidated and must be
reanalyzed. If an undiluted sample gives a response greater than the highest
standard, the sample must be diluted and reanalyzed. If the diluted sample gives a
response less than five times the method detection limit, the sample must be
reanalyzed at a lesser dilution.
Total Organic Carbon (TOC) Analyzer
Prior to each use, the TOC analyzer is calibrated with a standard containing 400 mg/I
of organic carbon. The linearity of the instrument is next verified by analyzing
standards at the 100 mg/I, 40 mg/I, 10 mg/I, and 1 mg/I levels. The acceptable ranges
are + 10%, 10%, 15%, and 50%, respectively. The standardization is next checked
by the analysis of an outside reference standard. Acceptable results must be
obtained on the reference standard before any samples are analyzed. After every 10
samples and at the end of the run, the 40 mg/I standard and a reagent blank are
analyzed. Any response in the reagent blank is subtracted from the previous samples
and the standard. If the 40 mg/I standard is off from the true value by more than
10%, the previous samples are invalidated and must be reanalyzed. If an undiluted
sample reads greater than 400 mg/I, it must be diluted and reanalyzed. If the diluted
sample reads less than 20 mg/I, the sample must be reanalyzed at a lesser dilution.
8.3 Laboratory Instrumentation -Inorganics
Atomic Absorption Spectrophotometer
The instrument is calibrated before each use with a reagent blank and three
calibration standards. The first standard must be at the method detection limit. In
order to verify the linearity of the curve, the regression coefficient must be at least
DCC#Q461 8-2
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Section No. 8
Revision No. 0
Date 1/08/90
Page 3 of 13
0.995. The calibration is next checked by the analysis of an outside reference
solution. The results must be within 10% of the true value for the initial calibration
to be verified. After every 10 samples, and at the end of the run, the outside
reference standard and reagent blank are analyzed. If the reagent blank shows a
result greater than the method detection limit, or if the reference standard differs
from the true value by more than 10%, the previous samples are invalidated and
must be reanalyzed. If an undiluted sample gives a response greater than the highest
standard, the sample must be diluted and reanalyzed. If the diluted sample gives a
response less than twice the method detection limit, the sample must be reanalyzed
at a lesser dilution.
Inductively Coupled Plasma Spectrophotometer
The instrument is calibrated before each use with a reagent blank and one other
calibration standard. The initial calibration is checked by the analysis of an outside
reference solution. The initial calibration solution is run at each wavelength used for
analysis. The results must be within 10% of the true value for the initial calibration
to be verified. In order to verify linearity near the detection limit, a standard
containing the elements of interest at twice the method detection limit is analyzed at
the beginning and end of each run. This standard is not required for Al, Ba, Ca, Fe,
Mg, Na, and K. After every 10 samples, and at the end of the run, the outside
I reference standard and a reagent blank are analyzed. If the reagent blank shows a
response greater than the method detection limit, or if the reference standJ~d differs
from the true value by more than 10%, the previous samples are invalidated and
must be reanalyzed. In order to verify the absence of interelement and background
interferences, an interference check sample is analyzed at the beginning and end of
each run. The results for elements present in the interference check sample must be
within 20% of the true value for the analytes of concern or the instrument must be
recalibrated and all samples since the last good interference check reanalyzed. A list
of the elements present in the interference check sample is given in Table 8-1.
DCC#Q461 8-3
8.4 Laboratory Instrumentation -Organics
Section No. 8
Revision No. 0
Date 1/08/90
Page4ofl3
Gas Chromatographs
These instruments are calibrated for the components of interest with a solvent blank
and five calibration standards. The first standard must be at the method detection
limit. In order to verify the linearity of the curve, the regression coefficient must be
at least 0.995. The calibration is next check by the analysis of an outside reference
standard. If a supplied standard (NBS or EPA) is not available, an in-house solution
containing a concentration different than those used to prepare the curve is used.
The results obtained on the check standard must be within 20% of the true value for
the initial calibration to be verified. After every five samples, and at the end of the
run, the mid-point standard and solvent blank are analyzed. Any response found in
the solvent blank is subtracted form the preceding samples and the mid-point
standard.
If the mid-point standard differs from the true value by more than 20%, the previous
samples are invalidated and must be reanalyzed. If an undiluted sample gives a
response greater than the highest standard, the sample must be diluted and
reanalyzed. If the diluted sample gives a response less than twice the method
detection limit, the sample must be reanalyzed at a lesser dilution.
Gas Chromatograph/Mass Spectrometer (Dioxins/Furans}
DCC#Q461
Two types of calibration procedures are required. One type, initial
calibration, is required before any samples are analyzed and is
required intermittently throughout sample analyses as dictated by
results of routine calibration procedures described below. The other
type, routine calibration, consists of analyzing the column performance
check solution and a concentration calibration solution of 500 ng/ml
(Paragraph 2). No samples are to be analyzed until acceptable
calibration as described in paragraphs 3 and 6 is demonstrated and
documented.
8-4
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Section No. 8
Revision No. 0
Date U0S/90
Page S of 13
2. Initial Calibration:
2.1 Prepared multi-level calibration standards1 keeping one of the
recovery standards and the internal standard at fixed
concentrations (500 ng/ml).
Additional internal standards ( 13c12-OCDD 1,000 ng/mL) are recommended when
quantification of the hepta-and octa-isomers is required. The use of separate
internal standards for the Pcdfs is also recommended. Each calibration standard
should contain the following compounds:
2,3,7,8-TCDD,
1,2,3, 7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,4,6,7,8-HpCDD
2,3, 7,8-TCDF
1,2,3,7,8,PeCDF
or any available
or any available
or any available
or any available
2,3,7,8X-PeCDD isomer
2,3,7,8,X, Y-HxCDD isomer,
2,3,7,8,X,Y,Z-HpCDD isomer
2,3,7,8,X-PeCDF isomer,·
1,2,3,4,7,8-HxCDF or any available 2,3,7,8,X,Y,HxCDF isomer,
1,2,3,4,6,7,8-HpCDD or any available 2,3,7,8,X,Y,Z-HpCDF isomer,
OCDD,OCDF, 13c12-2,3,7,8-TCDD, 13c121,2,3,4-TCDD and 13c12-OCDD
Recommended concentration levels for standard analytes are 200, 500, 1,000, 2,000,
and 5,000 ng/ml. These values may be adjusted in order to insure that the analyte
concentration falls within the calibration range. Two ul injections of calibration
standard should be made. However, some GC/MS instruments may require the use
of a 1-ul injection volume; if this injection volume is used then all injections of
1
DCC#Q461
13c12-labeled analytes are available from Cambridge Isotope Laboratory,
Wo15urn, Massachusetts. Proper qualification requires the use of a specific
labeled isomer for each congener to be determined. When labeled PCDDs
and PCDFs of each homolog are available, their use will be required
consistent with the technique of isotopic dilution.
8-S
Section No. 8
Revision No. 0
Date 1/08/90
Page 6 of13
standards, sample extracts and blank extracts must also be made at this injection
volume. Standards must be analyzed using the same solvent as used in the final
sample extract. A wider cal.Jbration range is useful for higher level samples provided
it can be described within the linear range of the method. All standards must be
stored in an isolated refrigerator at 4°C and protected from light. Calibration
standard solutions must be replaced routinely after six months.
3. Establish operating parameters for the GC/MS system; the instrument
should be tuned to meet the isotopic ratio criteria listed in Table 8-3
for PCDDs and PCDFs. Once tuning and mass calibration procedures
have been completed, a column performance check mixture2
containing the isomers listed below should be injected into the GC/MS
system:
TCDD
PeCDD
Hx:CDD
HpCDD
OCDD
TCDF
PeCDF
Hx:CDF
HpCDF
OCDF
1,3,6,8; 1,2,8,9; 2,3,7,8; 1,2,3,7; 1,2,3,9
.1,2,4,6,8; 1,2,3,8,9
1,2,3,4,6,9; 1,2,3,4,6, 7
1,2,3,4,6, 7,8; 1,2,3,4,6, 7,9
1,2,3,4,6, 7,8,9
1,3,6,8; 1,2,8,9
1,3,4,6,8; 1,2,3,8,9
1,2,3,4,6,8; 1,2,3,4,8,9
1,2,3,4,6,7,8; 1,2,3,4,7,8,9
1,2,3,4,6, 7,8,9
Because of the known overlap between the late-eluting tetra-isomers and the early-
eluting penta-isomers under certain column conditions, it may be necessary to
perform two injections to define the TCDD/TCDF and PeCDD/PeCDF elution
windows, respectively. Use of this performance check mixture will enable the
2 Performance check mixtures are available from Brehm Laboratory, Wright State University, Dayton, Ohio.
DCC#Q461 8 • 6
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Section No. 8
Revision No. 0
Date 1/08/90
Page7 of13
following parameters to be checked: (a) the retention windows for each of the
homologues, (b) the GC resolution of 2,3,7,8-TCDD and 1,2,3,4-TCDD, and (c) the
relative ion abundance criteria listed for PCDDs and PCDFs in Table 8-3. GC
column performance should be checked daily for resolution and peak shape using
this check mixture.
The chromatographic peak separation between 2,3, 7,8-TCDD and 1,2,3,4-TCDD
must be resolved with a valley of 25 percent, where
X
y
Valley Percent= (x/y)(lO0)
=
=
distance between TCDD peaks
the peak height of 2,3, 7,8-TCDD
It is the responsibility of the laboratory to verify the conditions suitable for maximum
resolution of 2,3,7,8-TCDD from all other TCDD isomers. The peak representing
2,3, 7,8-TCDD should be labeled and identified as such on all chromatograms.
4.
5.
6.
DCC#Q461
Acceptable SIM sensitivity is verified by achieving a minimum signal-
to-noise ration of 50:1 for the m/z 320 ion of 2,3,7,8-TCDD obtained
from injection of the 200 ng/ml calibration standard.
From injections of the 5 calibration standards, calculate the relative
response factors (RRFs) of analytes vs. the appropriate internal
standards. Relative response factors for the hepta-and octa-
chlorinated CDDs and CDFs are to be calculated using the
corresponding 13c12-octachlorinated standards.
For each analyte calculate the mean relative response factor (RRF),
the standard deviation, and the percent relative standard deviation
from triplicate determinations of relative response factors for each
calibration standard solution.
8-7
7.
8.
9.
Section No. 8
Revision No. 0
Date U0S/90
Page8of13
The percent relative standard deviations (based on triplicate analysis)
of the relative response factors for each calibration standard solution
should not exceed 15 percent. If this condition is not satisfied,
remedial action should be taken.
The Laboratory must not proceed with analysis of samples before
determining the documenting acceptable cahbration with the criteria
specified in Paragraphs 6.3 and 6. 7.
Routine Calibration:
9.1 Inject a 2-uL aliquot of the column performance check mixture.
Acquire at least five data points of each GC peak and use the
same data acquisition time for each of the ions being
monitored.
NOTE: The same data acquisition parameters previously used to
analyze concentration calibration solutions during initial
calibration must be used for the performance check solution.
The column performance check solution must be run at the
beginning and end of a 12 hour period. If the contractor
laboratory operates during consecutive 12 hour periods (shifts),
analysis of the performance check solution at the beginning of
each 12 hour period and at the end of the final 12 hour period is
sufficient.
Determine and document acceptable column performance as described in
Paragraph 3.
DCC#Q461
9.2 Inject a 2-uL aliquot of the calibration standard solution at 500
ng/ml at the beginning of a 2-hour period. Determine and
document acceptable calibration as specified in Paragraph 3
i.e., SIM sensitivity and relative ion abundance criteria. The
8-8
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Section No. 8
Revision No. 0
Date 1/08/90
Page9 of 13
measured RFFs of all analytes must be within + 30 percent of
the mean values established by initial analyses of the calibration
standard solutions.
Gas Chromatograph/Mass Spectrophotometers (TCL Parameters)
The GC/MS system will be calibrated with a minimum of five concentration levels of
calibration standard for each parameter to be analyzed in the sample. One of the
concentrations of each standard will be slightly above the method detection limit.
The other concentration in the samples or to the linear working range of the GC/MS
system. Within each 12 hour period, calibration check standards will be analyzed to
confirm the validity of the original five-point calibration curve for each constituent
being analyzed. Calibration check compounds, concentrations and procedures will
conform to the applicable provisions of the latest SOW of the CLP.
DCC#Q461 8-9
Analytes
Ag
Ba
Cd
Co
Cr
Cu
Mn
Ni
Pb
V
Zn
DCC#Q461
TABLES-I
INTERFERENT AND ANAL YrE ELEMENTAL
CONCENTRATIONS USED FOR ICP
INTERFERENCE CHECK SAMPLE
!mg/I} Interferents
1.0 Al 0.5 Ca 1.0 Fe 0.5 Mg 0.5
0.5
0.5
1.0
1.0
0.5
1.0
s. 10
Section No. 8
Revision No. 0
Date 1/08/90
Page 10 of 13
(mg/I)
500
500
200
500
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TABLE 8-2
Section No8
Revision No 0
Date 1/08/90
Page 11 of 13
METHOD DETECTION LIMITS OF 13c12 . LABELED PCDDs AND PCDFs
IN REAGENT WATER (PPT) AND ENVIRONMENTAL SAMPLES (PPB)
13c -Labeled Reagent Miuouri Fly-lndualriaJ Still• Fuel Fuel Oil/ 12
Soilb A.lhb Anatyte Wate? Sludge<
2,3,7,8-TCDD 0.44 0.17 0.07 0.82
1,2,3,7,8-PeCDD 1.27 0.70 0.25 1.34
1,2,3,6,7,8-HxCDD 2.21 1.25 0.55 2.30
1,2,3,4,6, 7,8-HpCDD 2.77 1.87 1.41 4.65
OCDD 3.93 2.35 2.27 6.44
2,3,7,8-TCDF 0.63 0.11 0.06 0.46
1,2,3,7,8-PeCDF 1.64 0.33 0.16 0.92
1,2,3,4,6,7,8-HxCDF 2.53 0.83 0.30 2.17
~Sample size 1,000 mL
Sample size 10 g.
~ample size 2g.
Sample size 1 g.
NOTE: The final sample-extract volume was 100 uL for all samples.
Matrix types used in MDL study:
Bottom d Oild Sawdustb
1.81 0.75 0.13
2.46 2.09 0.18
6.21 5.02 0.36
4.59 8.14 0.51
10.1 23.2 1.48
0.26 0.48 0.40
1.61 0.80 0.43
2.27 2.09 2.22
Reagent water: distilled, deionized laboratory water.
Missouri soil: soil blended to form a homogeneous sample.
Fly-ash: alkaline ash recovered from the electrostatic precipitator of a coal-burning power plant.
Industrial sludge: sludge rom cooling tower which received creosotic and pentachlorophenolic
wastewaters. Sample was ca. 70 percent water, mixed with oil and sludge. ·
Still bottom: distillation bottoms (tar) from 2,4-dichlorophenol production.
Fuel oil: wood-preservative solution from the modified Thermal Process tanks. Sample was an oily
liquid ( > 90 percent oil) containing no water.
Fuel oil/Sawdust: sawdust was obtained as a very fine powder from the local lumber yard. Fuel oil
( described above was mixed at the 4 percent (w/w) level.
Procedure used for the Determination of Method Detection Limits was obtained from "Methods for
Organic Chemical Analysis of Municipal and Industrial Wastewater" Appendix A, EPA-600/4-82-057, July
I 982. Using this procedure, the method detectin limit is defined as he minimum concentration of a
substance that can be measured and reported with 99 percent confidence that the value is above zero.
DCC#Q461 8-11
TABLE 8-3
Section No 8
Revision No O
Date 1/08/90
Page 12ofl3
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CRITERIA FOR ISOTOPIC RATIO MEASUREMENTS FOR PCDDs AND PCDFs I
Selected Ions
(m/z) Relative Intensity
I
-----------1
PCDDs
Tetra
Penta
Hexa
Hepta
Octa
PCDFs
Tetra
Penta
Hexa
Hepta
Octa
DCC#Q461
320/322
358/356
392/390
426/424
458/460
304/306
342/340
376/374
410/408
442/444
8-12
0.65 -0.89
0.55 -0.75
0.69-0.93
0.83 -1.12
0.75 -1.01
0.65 -0.89
0.55 -0.75
0.69-0.93
0.83 -1.12
0.75 -1.01
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Figure 8-1
Projec::
Out,
Section No. 8
Revision No. 0
Date 1/08/90
Page 13ofl3 --Mttet1
!u!!., Soiutioru l,lttW
Rucw1 1 '
-Utd ~uor ,.J In, ti&a
I [n1 :i&J C •l i~ ru,on :,.cs~•:.:~:..;u~s.t .. H_,_-t"---+-----;----+----+----
1 ldl\Jt':~
C.ili!lr1 :.:.'"', -: .... ec• \,:.••~ ...... J ~ !~
·•dl'-.,:S~l'd
adiustN
C£Jlbru,.,,, c~ecl<s ,..,ould ~• "'•d• alter evtry lO rea41n11 iailll ,,_ pH 7 iluUw ,otut,on (a.,u,unN ,ud1.s1), lf rudiJlll &rt vitl'wl .l ulllt ot 1'le IOl11tiOft 111 cat~ra1,on 1diust,.,tnt ;1 ·"'•d•. ii &rtattt tl'I.,, .( & complete c:ali.br&tlM la,_._,., (ldjul'H ,aadi"&l, 11 1r11tar t11an ,2 do • co,,,pJatt ~&tlOft 111d illCH&M ,,.,_ frequency ol cal~ratiOt'I c.~adc&.
Operator 5i&nar.,n:
C0NOUCTIV1TY M!T!Jl
Oatei_
___ Ytl ---~o
Ttfflpet&U. AdfYlfflWIUI
2,oe: • It 11'141 tlfflpetatlll't of !lie sample iJ below 2,oc:, 1dd 2" of 1:11 rudilll p,11' HI'"'
2'0C: • I.!. !/It t1mperat11n iJ &Dove 2'0C:, 111btrw. 2,. o! :.~, readu,I ?II
1. J:~
2. J:o
J. J:~
DCC#Q461
011,-
. iartl&N 1! -t• " 1...,,.-allltt '°"'PMaCIIII !&n,p11 Ttfflp uo .. w I.! Y, ldC or Wtract t-p. I !!:st•• ;,oe r, or ~, a · tl'Mllt to "'It• re •· I ·---------!----,---------
8-13
Maire llltt adiuttN rtadilll art renroeo on li1ICI ll'lllt
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9.0 DATA REDUCTION, VALIDATION, AND REPORTING
Section No. 9
Revision No. 0
Date 1/08/90
Page 1 of4
Data transfer and support are essential functions in summarizing information to
support conclusions. It is essential that these processes are performed accurately
and, in the case of data reduction, accepted statistical techniques are used.
9.1 Laboratory Data Reduction
For most analyses, data reduction involves the comparison of samples to a standard
reference curve. Samples ( or extracts) are diluted within the concentration range of
the curve. To verify the linearity of the curve, the linear regression coefficient is
calculated according to the following equation:
The acceptable values for the regression coefficient were given in Sectiop 8. The
sample results are calculated according to the following formula:
y=mx+b
where y is they coordinate, xis the x coordinate, mis the slope, and bis the intercept.
Results from analyses that do not make use of a standard curve are calculated by the
appropriate formula given in the method, taking the number of significant figures
into account.
The digits in a number that are "significant" are comprised of those that are known
with certainty. plus the first digit whose value is in doubt. For example, if three
successive weighings of a sample yield the values 0.656, 0.658, and 0.662, the
calculated average weight would be 0.658666. Obviously the weighings are not
DCC#Q461 9-1
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Section No. 9
Revision No. 0
Date 1/08/90
Page2 of4
I '
reliable in the third decimal place, so that the measurement contains three significant
figures (two certain digits and one about which there is some doubt). The average,
therefore, should contain the same number of significant figures and 'Should be
rounded off to 0.659. This rounding off is done according to the following rule: if the
digit following the last significant figure is greater than 5, the significant figure is
raised by 1; if less than 5, no change is made; if equal to 5, the last significant figure
should be left even. For example, 0.66050 would be 0.660 (three significant figures).
Zeros following a number after the decimal are counted as significant figures ( 4.250
has four significant figures). Zeros preceding a number, or following 'a number
before the decimal, are not counted. Thus, both 0.066 and 66,000 have only two
significant figures, but 1660 and 660.0 have four.
When making calculations involving measured values, results must be expressed so
that they contain only the number of significant figures justified by the certainty of
the original measurement. For example, addition or subtraction results are rounded
off to the position of the number containing the least accurately known value: 13.4 +
1478.224 = 1491.624, rounded off to 1491.6. Multiplication or division results are
expressed with the same number of significant figures as the least certain original
I value used in the calculation: 31 x 350.1 = 10,853.1, rounded off to 11,000. I
9.2 Laboratory Data Validation
The Quality Assurance Department will validate all data prior to reporting. The
following procedures are used:
DCC#Q461
1)
2)
3)
4)
5)
6)
7)
Standard curve is prepared prior to sample analysis
Standard regression coefficient is within the acceptable range
Standard reference materials are analyzed at proper frequency with
acceptable results
Reagent blanks are analyzed at the proper frequency
Precision requirements of this plan are met
Accuracy requirements of this plan are met
Completeness requirements of this plan are met
9-2
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8) Samples are analyzed within the proper holding time
9) All calculations are verified as correct
10) Proper units are reported
11) Proper methodology was used
Section No. 9
Revision No. 0
Date 1/08/90
Page3 of4
All raw data is signed by the Quality Assurance Department to verify that it is valid
before reporting.
9.3 Laboratory Data Reporting
Once data has been validated, it is returned to the laboratory technician who
performed the analyses. The technician enters the result, date analyzed, method
used, and his/her initials into the LIMS system where it is stored prior to reporting.
When all analyses are completed, the laboratory will issue a final report. The QA
Officer will check the final report to ensure that no errors have been made in
transcription from the raw data. He will then issue the report to the Laboratory
Manager for distribution. All applicable QC data is included with the final report.
Laboratory data for transmittal to the U.S. EPA Region JV offices with be in
accordance with "Export Protocol For Toxics Compliance Monitoring Data"
(personal correspondence with U.S. EPA Region IV December 18, 1989). This
protocol is included in Appendix A
9.4 Independent Data Reduction and Evaluation
Data will be compared to project objectives and summarized into a usable format for
data manipulation. Tables will be created to exhibit constituents of concern,
analytical results, frequency of detection, minimum values, maximum values,
geometric and arithmetic means.
Once the data reduction task is complete, the analytical data will be reviewed to
evaluate contaminant distributions and the adequacy of the data base for the risk
assessment.
DCC#Q461 9-3
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9.S Independent Data Validation (Non-CLP Samples)
Section No. 9
Revision No. 0
Date 1/08/90
Page4of4
The following procedure will be used to validate non-CLP samples by an experienced
chemist not directly affiliated with the analyzing laboratory to determine the data's
usability.
1) Review chain-of-custody for completeness
2) Standard curve is prepared prior to sample analysis
3) Standard regression coefficient is within the acceptable range
4) Standard reference materials are analyzed at proper frequency with
acceptable results
5) Blanks are analyzed at the proper frequency and evaluated for
laboratory/field contamination. If contamination is present in any
blank, the criteria outlined in the U.S. EPA functional guidelines
(Appendix B) will be followed.
6) Precision requirements of this plan are met
7) Accuracy requirements of this plan are met
8) Completeness requirements of this plan are met
9) Samples are analyzed within the proper holding time
10) All calculations are verified as correct
11) Proper units are reported
12) Proper methodology was used
9.6 Independent Data Validation (CLP Samples)
CLP samples will be validated by an experienced chemist not directly affiliated with
the analyzing laboratory in accordance with the U.S. EPA Functional Guidelines for
evaluating organic and inorganic analysis.
DCC#Q461 9-4
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10.0 QUALITY CONTROL PROCEDURES
Section No: 10
Revision No: 0
Date: 1/08/90
Page 1 of 19
To check the quality of data from field sampling efforts, blanks and duplicate
samples will be collected for analysis. These samples will be treated as separate
samples for identification, logging, and shipping. Analytical results on blanks and
duplicates will be reported with the appropriate field sample data.
Field and Trip Blanks
Field and trip blanks are used to detect contamination problems from equipment
preparation or sampling and handling procedures. Their use was described in
Section 4.0.
Duplicate (Split) Sample Collection and Analysis
One of every 10 samples will be collected and analyzed in duplicate to evaluate the
precision of both the collection and analytical procedures. Duplicate samples (splits)
will be collected by field personnel and submitted to the laboratory for analysis. The
relative percent difference will be calculated from the duplicate analysis for the
' particular compounds of interest. Should the relative percent difference be excessive
for the material analyzed and method used, other quality control parameters will be
evaluated to determine whether the duplicates need to be reanalyzed or whether the
entire set needs to be reanalyzed.
10.l Laboratory Quality Control Procedures
The following laboratory QC checks will be performed to ensure that the
measurement systems are under control.
Blind Standard Analysis
A blind standard will be analyzed during the course of the study as a check on
laboratory procedures. The sample will contain selected compounds from, the U.S.
EPA Priority Pollutant List as well as other conventional parameters analyzed in the
DCC#Q461 10-1
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Section No: 10
Revision No: 0
Date: 1/08/90
Page2ofl9
study, and will be unknown to the laboratory performing the analysis. The blind
sample will be prepared by the Quality Assurance Director.
10.2 Organics Analyses -GC/MS
This section outlines the minimum quality control operations necessary to satisfy the
analytical requirements associated with the determination of TCL organics in water.
At all times, the most current revisions of the CLP protocol will be implemented by
the laboratory.
Tuning and GC/MS Mass Calibration
Prior to initiating data collection, it is necessary to establish that a given GC/MS
meets the standard mass spectral abundance criteria. This is accomplished through
the analysis of decafluorotriphenylphosphine (DFTPP) for acid and base/neutral
extractable compounds and p-bromofluorobenzene (BFB) for volatile organics
compounds. The ion abundance criteria for each calibration compound should be
met before any samples, blanks or standards can be analyzed.
p-Bromofluorobenzene {BFB)
Each GC/MS system used for the analysis of TCL volatile organic compoJnds must
I be hardware tuned to meet the ion abundance criteria provided in Table 10-1 as
specified in the most current revisions of the CLP protocol. The criterion must be
demonstrated daily or for each 12 hour time period, whichever is more frequent.
Any samples analyzed when tuning criteria have not have been met may require
reanalysis. Documentation of the calibration must be provided in the form of a bar
graph plot and as a mass listing.
Decafluorotriphenylophosphine (DFfPP)
Each GC/MS system used for the analysis of TCL acid and base/neutral extractables
must be hardware tuned to meet the ion abundance criteria in Table 10-2 as defined
in the current CLP protocol. DFTPP must be analyzed separately or as part of the
DCC#Q461 10-2
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Section No: 10
Revision No: 0
Date: 1/08/90
Page3of19
calibration standard. The criteria must be demonstrated daily or for each 12 hour
time period, whichever is more frequent. Any samples analyzed when criteria have
not been met may require reanalysis. Documentation of the calibration must be
provided in the form of a bar graph plot and as a mass listing.
GC/MS System Calibration
Prior to the analysis of samples and after tuning criteria have been met, the GC/MS
system must be initially calibrated at a minimum of five concentrations to determine
the linearity of response utilizing TCL compound standards. Once the system has
been calibrated, the calibration must be verified each 12 hour time period for each
GC/MS system. The following is a brief summary for the calibration pro~edures as
specified in the current CLP protocol for TCL volatile organic compounds and TCL
acid and base/neutral extractable and pesticide compounds.
TCL Volatile Compounds
For volatile organic compounds, a minimum of five different concentrations plus the
three-designated internal standards at a constant concentration will be used to
develop the calibration curve. The calibration curve will be developed utilizing the
analytical protocol specified in the current CLP. Volatile organic internal standards
with corresponding TCL analytes are listed in Table 10-3.
Once the initial calibration is validated, the average response factor and percent
relative standard deviation for all TCL volatile organic compounds will be calculated
and reported. The laboratory is required to submit this data for each instrument
used to analyze samples.
Acid and Base/Neutral Extractable Compounds
For acid and base/neutral extractable compounds, the curve will be based upon a
minimum of five standard concentrations for the TCL compounds, plus six· internal
standards at constant concentration will be used to develop the calibration curve.
The calibration curve will be developed utilizing the analytical protocol specified in
DCC#Q461 10-3
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Section No: 10
Revision No: 0
Date: 1/08/90
Page4ofl9
the current CLP. Acid and base/neutral extractable internal standards with
corresponding TCL analytes are listed in Table 10-4.
CLP protocol specify both the concentration levels for initial calibration and the
specific internal standard to be used on a compound-by-compound basis for
quantization. Establishment of standard calibration procedures is necessary and
deviations are not allowed.
Once the initial calibration is validated, the average response factor and percent
relative standard deviation for all TCL acid and base/neutral extractable compounds
will be calculated and reported.
System Performance Check Compound Response
A system performance check will be performed on the calibration curve before it is
used. For volatile organics, the five system performance check compounds (SPCC)
are chloromethane, 1, 1-dichloroethane, bromoform, 1, 1,22-tetrachloroethane, and
chlorobenzene. The minimum acceptable average response factor for these
compounds are specified in the current CLP. These compounds are used to check
compound instability and check for degradation caused by contaminated lines or
active sites in the system.
For acid and base/neutral extractables, the SPCC's are N-nitroso-di-n-propylamine,
hexachlorocyclopentadiene, 2,4-dinitrophenol, and 4-nitrophenol. The minimum
acceptable average response factor for these compounds are specified in the current
CLP. These compounds are usually the first to show poor performance and tend to
decrease in response as the chromatographic system begins to deteriorate or the
standard material begins to deteriorate. Therefore, they must meet the minimum
requirement when the system is calibrated.
Continuing Calibration
As specified in the current CLP protocol, calibration standard( s) containing all TCL
volatile organic and acid and base/neutral compounds, including all required
DCC#Q461 10-4
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Section No: 10
Revision No: 0
Date: 1/08/90
Page 5 of 19
surrogates, will be analyzed each 12 hours during sample analysis. The response
factor data from the standards for each 12 hours will be compared with the average
response factor from the initial calibration for a specific instrument. A system
performance check will be made each 12 hours. If the SPCC criteria are met, a
comparison of response factors will be made for all compounds. If the minimum
response factors for individual compounds in the verification standard fall outside
acceptable quality control criteria, appropriate corrective action will be taken (up to
and including re-calibr-tion of the instrument) prior to sample analyses.
Calibration Check Compounds
After the system performance check is met, calibration check compounds listed in
Table 10-5 are to be used to check the validity of the initial calibration. If the
response for any calibration check compound varies from the calibrated response by
more than the criteria limits as specified in the current CLP, corrective action will be
taken, up to and including possible recalibration.
Surrogate Spike Standard Performance Evaluation
Surrogate standards are defined as nonpriority pollutant compounds used to monitor
the percent recovery efficiencies of the analytical procedures on a sample-by-sample
basis. Surrogate standard determinations are performed on all samples anp blanks.
All samples (including matrix spike and matrix spike duplicates) and blanks are
fortified with surrogate spiking compounds before purging or extraction in·order to
monitor preparation and analysis of samples.
Surrogate compounds and recovery levels are given in Table 10-6. \\'.hen the
surrogate recovery level is outside of the control limits, the laboratory must take the
following actions:
DCC#Q461
o Check calculations to assure there are no errors, check internal
standard and surrogate spiking solutions for degradation,
contamination, etc.; also, check instrument performance.
10-5
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0 Recalculate or reinject/repurge the sample or extract.
0 Re-extract and reanalyze the sample.
Section No: 10
Rerision No: 0
Date: 1/08/90
Page6ofl9
If any of these measures listed above fail to correct the problem, the problem, the
analytical system will be considered out of control. The problem will be corrected
before continuing. This may mean recalibrating the instrumentation.
Internal Standard Performance Evaluation
Internal standards are defined as nonpriority pollutant compounds used to monitor
instrumental performance and quantitate target compounds. The intema\ standards
will be used to confirm the integrity of the instrumental analysis should the percent
recovery values for the surrogate standards indicate a problem with the analytical
method.
Volatile Organics Analysis
Standards, method blanks, and samples will be spiked prior to purging with the
following internal standards:
o Bromochloromethane,
o Chlorobenzene-d5, and
o 1,4-difluorobenzene.
Other EPA-suggested internal standards may be added or substituted as necessary.
Acid and Base/Neutral Extractable Analysis
Standards, method blanks, and samples will be spiked prior to analysis ,with the
following internal standards:
DCC#Q461
0
0
0
Acenaphthene-d 10
Chrysene-d 12
1,4-dichlororbenzene-d4
10-6
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Naphthalene-dg
Perylene-d12
Phenanthrene-d 1 o
Section No: 10
Revision No: O
Date: U0S/90
Page 7 ofl9
Other EPA-suggested internal standards may be added or substituted as necessary.
Reagent Blank Analysis
A reagent blank is a volume of deionized distilled water carried through the entire
analytical procedure. A reagent blank analysis will be performed with every 20
samples received or whenever samples are extracted, whichever is more frequent.
An acceptable reagent blarik will meet the criteria established in the current CLP
protocol. If a laboratory reagent blank exceeds criteria, the analysical system will be
considered out of control. The source of the contamination will be investigated and
appropriate corrective measures will be taken before further sample analysis. All
samples processed with a reagent blank that is out of control (i.e., contaminated) will
be reextracted/repurged and reanalyzed.
Matrix Spike and Matrix Spike Duplicate Analysis
In order to evaluate the matrix effect of the sample upon the analytical methodology,
a matrix spike/matrix spike duplicate will be analyzed with every 20 samples. Spike
compounds and acceptable ranges were given in Tables 4-1 -4-2. Using the above
matrix spike/matrix spike duplicate analytical results, the percent recovery and
relative percent error for the respective compounds will be calculated. Should the
percent recovery or relative percent error values fall outside the appropriate quality
control limits, the other quality control parameters will be evaluated to determine
whether an error in spiking occurred or whether the entire set of samples requires
reextraction and analysis.
DCC#Q461 10-7
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10.3 Organic Analyses -GC
Section No: 10
Revision No: 0
Date: 1/08/90
Page 8 of19
This section outlines the minimum quality control operations necessary to satisfy the
analytical requirements associated with the determination of organic parameters
using gas or liquid chromatographic techniques.
Initial Calibration Verification
In order to verify the linearity of the initial five point cahbration curve (section 6.0),
the % RSD between calibration factors must not differ by more than 20%.
Alternatively, the linear regression coefficient must be at least 0.995.
Continuing Calibration Verification
The working calibration curve or calibration factor must be verified after every five
samples by the analysis of a continuing calibration verification solution (CCV). If the
response for any analyte varies from the predicted response by more than + 15%, a
new calibration curve must be prepared and all samples after the last good CCV
reanalyzed. The compounds used as CCV solutions are listed in Table 10-5.
Surrogate Spike Standard Performance Evaluation
Surrogate standards will be used for gas and liquid chromatographic procedures in
' the same manner as for the GC/MS analyses. Surrogate compounds and: recovery
I
levels are given in Table 10-6.
Reagent Blank and Matrix Spike/Matrix Spike Duplicate Analysis
These parameters will be run at the same frequency as stated for the GC/MS
procedures.
DCC#Q461 10-8
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Pesticide and PCB QNQC Requirements
Section No: 10
Revision No: 0
Date: 1/08/90
Page 9ofl9
Samples for pesticides and PCBs will be analyzed according to current CLP
protocols.
Quality control requirements for routine analysis and evaluation of calibration
standards defined in the current CLP protocol will be adhered to; if at any time the
calibration factors exceed control limits for individual analytes, appropriate
corrective action will be taken.
The external standard quantization method will be used to quantitate all
pesticides/PCB's. Before performing any sample analysis, the laboratory will
determine the retention time window for each pesticide/PCB and the surrogate spike
compound dibutylchorendate as defined in the current CLP. These retention time
windows are used to make tentative identification of pesticides/PCB's during sample
analysis.
Prior to establishing retention time windows, the GC operating conditions will be
adjusted so that 4,4'-DDT has a retention time greater than or equal to 12 minutes
on packed GC columns. Conditions listed in the current CLP will be used to achieve
' this criteria.
After the operating conditions are set, the retention time window for each individual
analyte and the surrogate is determined as detailed in the current CLP. The
retention time shift for the surrogate will be evaluated after analysis of each sample;
if the shift exceeds allowable limits, appropriate corrective action will be taken.
10.4 Metals by Inductively Coupled Plasma (ICP)
This section outlines the minimum quality assurance operations necessary to satisfy
' the analytical requirements associated with the determination of metals in water
samples. At all times, the most current revisions of the CLP protocol will be
implemented by the laboratory.
DCC#Q461 10-9
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Initial Calibration and Calibration Verification
Section No: 10
Revision No: 0
Date: 1/08/90
Page 10 of 19
At the start of instrumental operation, the ICP will be calibrated according to the
manufacturers instructions and current CLP protocol. In order to monitor
instrumental accuracy during the run, a mid point standard will be monitored for
each analyte at a frequency of 10% or every two hours during the analysis run,
whichever is more frequent. The check standard will also be analyzed for each
analyte at the beginning and end of each analytical run.
Preparation Blank Analysis
At least one preparation ( or reagent) blank consisting of deionized distilled water
processed through each sample preparation procedure (i.e., water, solids) will be
analyzed with every 20 samples, or with each group of samples digested, whichever is
more frequent. Specific procedures are detailed in the current CLP protocol.
ICP Interference Check Sample Analysis
i
To verify inter-element and background correction factors an ICP Int9rference
Check Sample, Quality Control Sample and Linear Range Verification Sample, will
be analyzed at least twice per eight hours of operation, or once during and again at
the end of analysis. If these monitoring checks fall outside the allowable criteria,
appropriate corrective action will be taken according to current CLP protocol.
ICP Serial Dilution Analysis
Prior to reporting concentration data for the analyte elements, the laboratory will
analyze and report the results of the ICP Serial Dilution Analysis as specifi~d in the
current CLP protocol. The ICP Serial Dilution Analysis will be performed on each
group of samples of a similar matrix type (i.e., water, soil) and concentration (i.e, low,
medium) for each case of samples, or for every 20 samples, whichever is more
frequent. Samples identified as field blanks cannot be used for serial dilution
analysis. If the analyte concentration is high (minimally a factor of 50 above the
DCC#Q461 10-10
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Section No: 10
Revision No: 0
Date: U0S/90
Page 11 of19
instrumental detection limit after dilution), an analysis of a 1:4 dilution must agree
within 10 percent of the original determination as specified in current CLP protocol.
Spiked Sample Analysis
Spiked sample analysis is designed to provide information about the effect of sample
matrix on the digestion and measurement methdology. The spike is added before
the digestion and prior to any distillation steps. At least one spiked sampl_e analysis
will be performed on each group of samples of a similar matrix type (i.e., water, soil)
and concentration (i.e., low, medium) for every 20 samples. Samples identified as
field blanks cannot be used for spikes sample analysis. Spike recovery limits range
from 75-125 percent as defined in the current CLP protocol. If these limits are not
obtained appropriate action will be taken.
Duplicate Sample Analysis
At least one duplicate sample will be analyzed from each group of samples of a
similar matrix type (i.e., water, soil) and concentration (i.e., low, medium) for every
20 samples. Samples identified as field blanks cannot be used for duplicate sample
analysis.
10.S Metals by Furnace Atomic Absorption
Furnace Atomic Absorption (AA) analysis will be performed on me~als not
amenable to analysis by ICAP. These metals include arsenic, lead, selenium and
thallium. The analysis of these metals by Furnace (AA) will be in accordance to
current CLP protocol.
All furnace analyses, except during Full Methods of Standard Addition (MSA), will
require duplicate injections for which the average absorbance or "concentration" will
be reported. All analyses will fall within the calibration range. The raw data package
will contain both absorbance or "concentration" values, the average value and the
relative standard deviation (RSD) or coefficient of variance (CV). For
concentrations greater than CRDL, duplicate injection readings will agree within 20
DCC#Q461 10-11
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Section No: 10
Revision No: 0
Date: 1/08/90
Page 12 of 19
percent RSD or CV, or the sample will be rerun once, as specified in current CLP
protocol.
All furnace analyses for each sample will require at least a single analytical spike to
determine if the MSA will be required for quantization. The spike will be analyzed
and prepared in accordance to current CLP protocol. The quality assuran·ce/quality
control (QNQC) procedures defined by the current CLP will be followed when
performing the specified analysis.
An initial calibration curve will be established using a blank and a minimum of four
standards of different concentrations. The calibration curve will be confirmed wit a
standard and reagent blank before sample analysis.
To assure instrumental stability every 10 samples will be a calibration check. If these
instrumental checks should fall outside allowable criteria, the instrument will be
recalibrated and preceding samples will be reanalyzed.
The analysis will include at least one reagent blank, before the digestion sample spike
and sample duplicate for every 20 samples of similar matrices.
10.6 Mercury by Cold Vapor Atomic Absomtion
Mercury will be analyzed by cold vapor atomic absorption according to the latest
' CLP protocol. An initial calibration curve will be established using a blank and a
minimum of four standards. These standards and blanks will have gone through the
full sample preparation procedure. The calibration curve will be confirmed with a
standard and reagent blank before sample analysis.
To assure instrumental stability every 10 samples will be a calibration check. If these
instrumental checks should fall outside allowable criteria, the instrument will be
recalibrated and preceding samples will be reanalyzed.
The analysis will include at least one reagent blank, before the digestion sample spike
and sample duplicate for every 20 samples of similar matrices.
DCC#Q461 10-12
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10.7 General Chemistry Parameters
Section No: 10
Revision No: 0
Date: 1/08/90
Page 13ofl9
Calibration for general chemistry parameters will be as described in Section 6.0.
Matrix spikes, duplicates and reagent blanks will be run at the same frequency as
described in the CLP inorganic protocol. Cyanide analysis is covered in detail in the
CLP, and analysis will follow all applicable provisions.
DCC#Q461 10-13
I Section No: 10
Revision No: 0
I Date: 1/08/90
Page 14ofl9
I TABLE 10-1
p-BROMOFLUOROBENZENE (BFB)
I KEY IONS AND ION ABUNDANCE CRITERIA
MASS ION ABUNDANCE CRITERIA
I 50 15.0 -40.0 percent of the base peak
75 30.0 -60.0 percent of the base peak
I 95 base peak, 100 percent relative abundance
I 96 5.0 -9.0 percent of the base peak
173 less than 1.00 percent of the base peak
I 174 greater than 50.0 percent of the base peak
175 5.0 -9.0 percent of mass 174
I 176 greater than 95.0 percent but less than 101.0 percent of mass 174
I 177 5.0 -9.0 percent of mass 176
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DCC#Q461 10 -14
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I Section No: 10
Revision No: 0
I Date: 1/08/90
Page 15 of19
I TABLEl0-2
DECAFLUOROTRIPHENYLPHOSPHINE (DFI'PP)
I KEY IONS AND ION ABUNDANCE CRITERIA
51 30.0 -60.0 percent of mass 198 I 68 less than 2.0 percent of mass 69
I 70 less than 2.0 percent of mass 69
127 40.0 -60.0 percent of mass 198
I 197 less than 1.0 percent of mass 198
198 base peak, 100 percent relative abundance
I 199 5.0-9.0 percent of mass 198
I 275 10.0 -30.0 percent of mass 198
365 greater than 1.00 percent of mass 198
I 441 present but less than mass 443
442 greater than 40.0 percent of mass 198
I 443 17.0 -23.0 percent of mass 442
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DCC#Q461 10-15
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TABLE 10-3
Section No: 10
Revision No: 0
Date: 1/08/90
Page 16of 19
VOLATILE INTERNAL STANDARDS WITH CORRESPONDING
ANALYTES ASSIGNED FOR QUANTITATION
Chloromethane 2-butanone 2-hexanone
Bromomethane 1, 1, I-trichloroethane 4,-methyl-2-pentanone
Vinyl chloride Carbon tetrachloride Tetrachloroethene
Chloroethane Vinyl acetate 1,1,2,2-tetrachloroethane
Methylene chloride Bromodichloromethane Toluene
Acetone 1,2-dichloropropane Chlorobenzene
Carbon disulfide trans-1,3-dichloropropene Ethylbenzene
1, 1-dichloroethene Trichloroethene Styrene
1, 1-dichloroethane Dibromochloromethane Total xylenes
trans-1,2-dichloroethene 1, 1,2-trichloroethane Bromofluorobenzene
Chloroform Benzene (surr)
1,2-dichloroethane cis-1,2-dichloropropene Toluene·d8 (s1urr)
1,2-dichloroethane -d 4 2-chloroethyl vinyl ether
(surr) Bromoform
DCC#Q461 10-16
-
-0 -....
-- -- - - ---- - -- --
TABLEI0-4
ACID AND BASE/NEUTRAL EXTRACTABLE INTERNAL STANDARDS WITH CORRESPONDING
TCL ANALYrES ASSIGNED FOR QUANTITATION (I)
I,4-DICHLOROBENZENE-d4 NAPTHALENE-ds
Phenol
Bis(2-<:horethyl)ether
2-chlorophenol
1,3-dichlorobenzene
1,4-dichlorobenzene
Nitrobenzene
Isophorone
2-nitrophenol
2,4-dimethylphenol
Benzoic acid
ACENAPHTIIENE-<110
Hexachlorocyclpentadiene
2,4,6-trichlorophenol
2,4,5-trichlorophenol
2-chloronaphthalene
2-nitroaniline
Benzyl alcohol
1,2-dichlorobenzene
2-methylphenol
Bis(2-chlorosopropyl) ether
4-methylphenol
Bis(2-chloro-ethoxy)methane Dimethyl phthalate
2,4-dichlorophenol
1,2, 4-trichlorobenzene
Naphthalene
4-chloroaniline
N-nitroso-di-n-propylamine Hexachlorobutadiene
Hexachloroethane 4-chloro-3-methylphenol
2-fluorophenol (surr) 2-methylnaphthalene
Phenol-d6 (surr) Nitrobenzene-d5 (surr)
Acenaphthylene
3-nitroaniline
Acenaphthene
2,4-dinitrophenol
4-nitrophenol
Dibenzofuran
2,4-dinitrotoluene
2,6-dinitrotoluene
Diethyl phthalate
4-chlorophenyl phenyl ether
Auofene -
4-nitroaniline
2-fluorobiphenyl (surr)
2,4,6-tribromophenol (surr)
PIIENANTIIRENE-<110
4,6-dinitro-2-methylphenol
N-nitrosodiphenylamine
1,2-diphenylhydrazine
4-bromophenyl phenyl ether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di-n-butyl pthalate
Fluoranthene
CIIRYSENE-<112
Pryene
Butyl benzyl phthalate
3,3 '-dichlorobenzidine
Benzo( a )anthracene
Bis(2-ethylhexyl)phthalate
Chrysene
Terphenyl-014 (surr)
-- -
PERYLENE-<1 12
Di-n-octyl phthalate
Benzo(b) fluoranthene
Benzo(k)fluoranthene
Benzo( a )pyrene
Indeno( 1,2,3-<:d)pyrene
Dibenzo( a,h )anthracene
Benzo(g,h,l)preylene
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Volatiles /GC or GC/MS)
I, 1 dichloroethene
chloroform
1,2-dichloropropane
toluene
ethylbenzene
vinyl chloride
Base Neutrals /GC/MS)
acenaphthene
1,4-dichlorobenzene
hexachlorobutadiene
N-nitrosodi-n-phenylamine
fluoranthene
benzo( a )pyrene
DCC#Q461
TABLE 10-5
CALIBRATION CHECK COMPOUNDS
Section No: 10
Revision No: O
Date: 1/08/90
Page 18 of 19
' I
Acid Extractable Phenols /GC or GC/MS)
4-chloro-3-methylphenol
2,4-dichlorophenol
2-nitrophenol
phenol
pentachlorophenol
2,4,6-trichlorophenol
10-18
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TABLEl0-6
Section No: 10
Revision No: 0
Date: 1/08/90
Page 19 of 19
SURROGATE SPIKE COMPOUNDS AND RECOVERY RANGES
EPA8020 benzotrifluoride 77-124
EPA8040 2-fluorophenol 10-58
2,4,6-tribromophenol 20-95
EPA 8080 ( CLP) dibutylchlorendate 24-154
EPA 8240 (CLP) toluene-d3 88-110
4-bromofluorobenzene 86-115
l,2-dichloroethane-d4 76-114
EPA 8270 (CLP) nitrobenzene-d5 35-114
2-fluorobiphenyl 43-116
p-terphenyl-d 14 33-141
pheno!-d5 10-94
2-fluorophenol 21-100
2,4,6-tribromophenol 10-123
pentachloro-
phenol (EPA 515) 2,4,6-tribromophenol 70-130
DCC#Q461 10 -19
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11.0 PERFORMANCE AND SYSTEM AUDITS
Section No. 11
Revision No. 0
Date 1/08/90
Page 1 ofl
Two types of audit procedures are conducted during this project; performance and
system audits.
11.1 Performance Audits
Performance audits are conducted by the Manager of Quality Assurance on a
monthly basis. Each laboratory analyst is given a performance evaluation sample
containing analytes for the parameters which he/she usually performs. These audit
samples are used to identify problems in technique or methodologies which could
lead to future analytical problems.
11.2 System Audits
System audits are conducted by the Manager of Quality Assurance on a quarterly
basis. These audits are used to ensure that all aspects of this quality control, manual
are operative. This involves a thorough review of all field and laboratory methods
for projects performed and their documentation to confirm that work is performed
according to project specifications.
In some cases, outside certification agencies conduct performance and systen'i audits
to verify contract compliance or the laboratories ability to meet certification
requirements on methods of analysis and documentation.
DCC#Q461 11-1
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Section No. 12
Revision No. 0
Date 1/08/90
Page 1 of 4
12.0 ASSESSMENT PROCEDURES FOR LABORATORY DATA
ACCEPTABILITY
The following discussion describes the procedures that will be employed to evaluate
the precision, accuracy, completeness, representativeness, and comparability of the
generated data.
12.1 Precision
Precision is a measure of agreement among individual measurements of the same
property under prescribed similar conditions. Precision is assessed by calculating the
relative percent difference (RPO) of replicate spike samples or replicate sample
analyses according to the following equation:
RPO = RI -R2
(RI + R2)/2
12.2 Accuracy
X J()() where R 1 = result 1
R2 = result 2
Accuracy is a measure of the closeness of an individual measurement to the true
value. Accuracy is measured by calculating the percent recovery (R) of known levels
of spike compounds as follows:
R = determined value of spiked sample x 100
theoretical value of spiked sample
12.3 Completeness
Completeness is a measure of the amount of valid data obtained, from a
measurement system, expressed as a percentage of the number of valid
measurements that should have been collected. It is calculated as follows:
DCC#Q461 12-1
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Completeness(%)=
Section No. 12
Revision No. 0
Date UOS/90
Page2of4
number of valid samples reported x 100
total number of samples analyzed
12.4 Representativeness
Representativeness is the degree to which data accurately and precisely represent a
characteristic population, a process control, or an environmental condition.
Appropriate sampling procedures will be implemented so that the samples are
representative of the environmental matrices from which they were obtained. The
sampling procedures are described in detail in Section 5.0.
12.S Comparability
Comparability refers to the degree to which one data set can be compared to
another. Appropriate sampling and analytical processes will be implemented so that
the samples of similar matrices may be compared.
12.6 Quality Control Charts
Quality control charts are prepared after every 20 determinations of precision and
accuracy. The charts are prepared by determining the mean value of the
determinations and setting control limits at + 2 standard deviations from that mean.
The following equations are used:
DCC#Q461
~
mean = E yJr,
n=1
12-2
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standard deviation =
Section No.12
Revision No. 0
Date 1/08/90
Page3 of4
I
The control limits should approximate the values given in Table 4-1 and 4-2. If the
limits are found to be outside these values, the measurement system is examined to
determine if possible problems exist. A control chart is shown in Figure 12c1.
DCC#Q461 12-3
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5 u C ..
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!10
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10
70
eo
,.,, ,,
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17 ,.
,s
14
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• • 7 • s
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0
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DCC#Q461
ACCURACY PUJT
Section No. 12 Revision No. 0 Date 1/08/90
Page4of4
I
2 J • 5 I 7 I t 10 II I 2 IJ " II !I 17 II It 3D 0Ullt.lCA1P 'll'WIQ
0 -.. -·-
1 I I 10 11 12 IJ 14 11 II t 7 1.t 'If lO U-4
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13.0 PREVENTIVE MAINTENANCE
Section No. 13
Revision No. 0
Date 1/08/90
Page 1 of3
Periodic preventive maintenance is required for equipment whose performance can
affect results. Instrument manuals are kept on file for reference if equipm~nt needs
repair. Troubleshooting sections of manuals are often useful in assisting personnel in
performing maintenance tasks.
All major instruments are under service contract so that trained professionals are
available on call to minimize instrument downtime.
13.1 Glassware Preparation
Glassware used for conventional chemistries is thoroughly cleaned with hot soapy
water, triple-rinsed with tap water, and triple-rinsed with distilled water immediately
after each use. Other special cleaning procedures are as follows:
Inorganics (metals, cyanide)
a)
b)
c)
d)
e)
f)
Organics
DCC#Q461
a)
b)
c)
d)
e)
f)
Wash with hot soapy water
Rinse three times with tap water
Rinse three times with deionized water
Rinse with 1: 1 nitric acid
Rinse three times with tap water
Rinse three times with deionized water
Rinse with methylene chloride
Wash with hot soapy water
Rinse three times with tap water
Rinse three times with distilled water
Rinse three times with acetone
Rinse three times with tap water
13-1
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g) Rinse three times with distilled water
h) Heat at 500°C for 2 hours
Section No. 13
Revision No. 0
Date 1/08/90
Page2 of3
'
13.2 Routine Preventive Maintenance (Field and Laboratory Equipment)
pH Meters
1)
2)
3)
Store electrodes in pH 7 buffer when not in use
Keep hole for filling solution plugged to prevent evaporation of filling
solution when not in use
Replace filling solution as needed
Conductivity Meters
1) Keep battery fully charged
2) Replatinize cell when response becomes erratic or platinum black has
flaked off the cell
Liquid Chromatographs
1)
2)
3)
Replace pump check valves every 6 months
Replace pump seals as needed
Use 3 to 5 cm pellicular guard columns to protect the analytical
columns
Gas Chromatographs
DCC#Q461
1)
2)
3)
Change septa daily
Periodically clean detectors
Replace columns when instrument response deteriorates
13-2
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Inductively Coupled Plasma Spectrophotometers
Change pump tubing every 4 hours of operation
Oean nebulizer daily
Section No. 13
Revision No. 0
Date 1/08/90
Page3of3
I
1)
2)
3) Periodically clean and replace torch and chimney extension
Atomic Absorption Spectrophotometers
1) Periodically clean sample cells
Auto Analyzers
1)
2)
3)
4)
Oean platen daily
Change tubing and wipe pumprollers weekly
Oean colorimeter monthly
Grease pump and gears every 6 months
Analytical Balance
1) Check daily with class S weights
2) Oean and calibrate once per year
Mass Spectrometers
1) Periodically dismantle and clean the ionizing source
DCC#Q461 13-3
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14.0 CORRECTIVE ACTION
Section No.14
Revision No. 0
Date 1/08/90
Page 1 of3
Corrective action procedures are divided into two subgroups, notably, methods
corrective action and systems corrective action.
14.1 Methods Corrective Action
Methods corrective action is initiated by the Analyst and Department Section
Manager at the time of analysis. Recoveries that fall outside the acceptable window
limits established by the laboratory or the supplier of the control sample is an
example of a reason to initiate methods corrective action. Poor response or poor
sensitivity check response are other causes that require methods corrective action.
The analyst is required to terminate analysis when any of the above is noted, locate
the problem and correct it. This may take the form of recalibration of standards,
reanalyzing a sample or in extreme cases, general maintenance of the instrument
hardware. Documentation of the latter is done in the instruments log book.
Satisfactory methods corrective action will be the proper response that co~ects the
problem for which the action was taken.
14.2 System Corrective Action
The Manager of Quality Assurance initiates the system corrective action. A :memo is
generated which is addressed to the Section Manager responsible. A copy of the
memo is filed in a folder designated for such. The Section Manager then assigns the
responsibility to the appropriate Analyst. Systems corrective action is initi~ted as a
result of any of the following: 1) Poor result in a performance audit (internal or
external) and 2) Poor result in an interlaboratory performance test program.
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When satisfactory progress has been achieved on each requested action, the: Analyst
describes the nature of the problem and the action that was taken to resolve it on the
Quality Assurance Corrective Action Form (See Figure 14-1). Action here may
involve extensive study of extraction solvents, digestion acids, standards froin more
DCC#Q461 14-1
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Section No. 14
Revision No. 0
Date 1/08/90
Page2 of3
'
than one source, etc. The Section Manager reviews the process, signs and dates it.
This form is given to the Manager of Quality Assurance. The Manager of Quality
Assurance evaluates the corrective steps taken, and if satisfied, signs the "Corrective
Action Form" and files it in a folder designated as such. If more corrective steps
should be taken, the Manager of Quality Assurance sends the form back to the
Department Supervisor with comments, suggestions, etc. and the corrective process
starts again.
DCC#Q461 14-2
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Laboratory Group: □
□
□
a
0
a
INVALID CATA NOTIFICATION
GC Date of Notification:
GC,MS
HPLC Parameter:
Metals
Wet Chemistry
Miscellaneous QCBaldlNo.
Section No. 14
Revision No. 0
Date 1/08/90
Page3 of3
Data for the following samples, which have been submitted on _____ _ are not
valid.
TRAVELLER SAMPLE
NUMBER IDENTIFICATION
RIS:S)<. __________________________ _
Submitted by ___________ _
FIGURE 14 -1
DCC#Q461
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15.0 OA REPORTS TO MANAGEMENT
Section No.: 15
Revision No.: 0
Date: 1/08/90
'Page 1 ofl
!
This QA plan provides a documentable mechanism for the assurance of quality work
projects. Audit reports (Section 11.0) will be provided to management as a means of
tracking program performance.
DCC#Q461 15 -1
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APPENDIX A
EXPORT PROTOCOL FOR
I TOXICS COMPLIANCE
MONITORING DATA
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E:.-:p,:,( l F';·.,::.t;,: .. .:,:,l
f ,:::,(
Toxics i:orn~iiance Monitor·ir1g
Dat . .:,
T~iis docunient establis~1es, fer EPA Reqi1~t1 IV RCRA p,..;-r;i"1it1~,:·t:.-·:5 -:::,1·-;d CEPCLA ·:;;1. !;<:" ,:ontra,:t,:,rs, t•1e ;eq1_:.i·r;:•d · fo·r11,at f,:,r 0l~ctr·•Ji'1ic r2pot·tit1g ,Jf toxics n1onitoring data.
3TATI ON. DAT ,::: ,.::,n t 21.i r1 ~ l.Ja·=>i ,: inf,.:,(· ri"1at i ,::,n ab,:,ut
n1,Jt1itoring stati•Jtl l,.:,,:ati1)t·1 ar1d
typ•. D•tail•d d•scriptio,1 of
t•1e structure is c,Jr1t3ir1~d i1··1
app•ndi ,, A.
WELL.DAT
SAMPLE. !:/',T
FARM.DAT
,.:,Jr1tains detailed ir1f,Jimation
ab,:,ut ,: onst ·( uc ti ,::.:in and ',:hara,:-
!; ::.-r i :z !; : ,.: ·:: ,.:.f i;·r,_:,;_lndw-3ter rnoni-
~.,;,::,..-ir1g :::;t.:;·,~~•-11,~. S-c-t: 1..1Pt-J~t1dix B.
,:Gr1t~in= basi,: it1formation ab,Jut
L ht2-c ,:il 112-c ti ,:in ond ,:har1ac t 12-r is-
ti ,: s •~f sampl~s. See appet1dix C.
contains mt:-Qsu-. -;,.•d val ut:·3 ~ind
reportit1g unit3 for sp0~ifi,:
par:--n·1eters. See appE·j"idi:,; D.
These file~ ~re t,J be transmitted it1 ASCII f•Ji·mat usir1q 5.25 in,:h fle:,~ible dis!., nir1e-tY-a,:.k magneti,:. tape-(150b c,r-5250 bpi) or, it1 t•, futur-e, via ,:ommutii,:ations 1:•1ar1r1els yet'to b~ defit1ed. Hardcopy repor-ting Y-equir-ements will c~ntinue as curr·ehtly require~ ur,til further r1:~tic; .. ~.~jiti,Jt1al fil2s may be defir1ed 1 ir1 the f-Lwrc for r,on-gY-oundwater station types should the need aris~.
Several ,~f tJ,ese files will contair, data that iJ usually static in nature. For example, t•,e basic inf,~rmati•~n t•Jntained ir, STATION.DAT will not n•~fij1ally change for ar,y single stati,~n, therefore once the data has been submitted for a particular stati,~n, it will riot be required to resubmit that infor1matior1. If, however, the station record is updat•d or corrected the r••:,:,rd .iould hav• t,:, b• r•subrnitt•d. After th• initial1 report then, STATION.OAT would b• subrnitt•d only .ih•n n•w stations ar• ,:ro;::-ated, ,:,r i.Jhet1 an ,~ld station rt?,:1:ird is n-11:idifie-d, and: ne-1:!'d only contain t:1~ tiew or n·10~ifi~J r·~cords. The 5ame is true 0f filo: WEL:_.DAT. SAMPLE.C-,A\T ..._,,:1uld, of ,:,:iur-se, b~ :5ubmitteQ t:-o.•:h tirne i::in~ or-ruore t1&1,,J sari"1plt"s ,,..,ere t,:, be-rep,Jrti:-d, ,:;< anY sampli:! r~,:ord <equire-d upJating. Agait1, t~1e fil~ ne2d onl/ co~1tait1 t~,~
t1~...., or u~ddt~d t·ecords. PARM.DAT is expected to be submitted at '="a,:h r-=•qLtirt:d re,p;:,rt.ing ir"it,.:;-rv..al, since it will ,..:o.-·,tain th,~ analytical results r·,e~d~J Lo determine compliance. It must contair1 all new results f,Jr the reporting ir1terval, arid mdy
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Datafile STATION.DAT
fie-Id
nc•.
f;. ·l d
t18fl"lt?
1 STATION f:EY l
TYPE
3 LATITUDE :t,
4 LON13 I TUDE t
fic·ld
Dt2-s,: ·r i pt i ,:1t·1
Un·iqt..11:" stati,:,n ide-ntifier. Cc•nsists of a twenty-st"vt"n ,:hara,:ter alphanum~ric field, left ju~tified, ,: ont ai ni ng:
1-12
de-scriptic,n:
Unique site identifier as assigned by EPA. Must be alphanumeric.
13-17 Unique s0:id w~1s~2 mat1agement unit desigr1~t,jr. Must b~ cilp•1anun1eric.
1S
.-,...,. ..;:.,
Media statu3 it1di~ator. Must ~ontain
or,e of t~,e followir1g:
1-· ,:,:,1upliani:1;: rn1:,nit,:.ring stati,:,.n
8 -b3selit12 ~•Jt1it-~rir19 ·:tati 1Jn
Uniqu•::. -;::;tati,:,n -id1:i1tifi•7;t. Mu:;;t !:;:~
al phanurfit"r i ,: •
Type ,Jf m,Jr1itoring stati,Jtl. C,Jnsists of a four--character alphanumeric field, left just:ified, ,:ontainir,g one of t•,e followitig: AIR, S~TR, GWTR, SOIL, SED, and SLDG. The meanings of these
abbreviatiiJns are as follows:
/\!R ·-:''.i.:-.zamplin~ -.::;~a.ti,:,;·;
SWTR Surface wat t"r '~an-,p 1 i ng st at i ;:,1 i GWTR -gr1~wnd ~ater =~mpling ~tatioh
SOIL -soil sa.mpling stc1tion
SED -Stream bed sediment
SLOG-·-pr,Jcess sludge samplit1g
Geographic po~ition of t~1e station 1~, d~gr0es n1Jrth ,~f the equati~r. Mu3t be in t~,e fo~mat DCMMSS.~xxx, where DD rep<es~nts degrees, MM r~preser1ts mir,utes, arid SS.xxxx represe~ts
seconds, wit~, available precision to four
decimal places.
Geographi,: position of the ~tation i~1 Jegrecs ·..:·.::st ,:,~ th-: Py-i;;,.:· M.:.: ~diatl. Must b•.:· in tho:.·
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fi.;ld
1
2
3
5
fi 2-ld
nam~?
AQNAM
TOTDF
DRMTH
DRFLD
f i t=>l d
Dt-s1: rip ti ,:,r1
Unique statiot1 ider,tifier. Cor,sists ,~fa twenty-·st:'~er, chara,:ter alp•1ar1umeri,: field, left justified,
,: ,:,n ta in i n g:
,:i:,lurun:
1 . ◄ .-.
13--1 7
18
1'3 -27
d•2s,: rip 1; i ,:,n:
Uni,:;ui.:-si.-:-:: idi.·t~ti fi•.?-r i:.,·:: ..:i.:;;r::i•~•-:~-,:.~ t:·J
EPA. Must b~ alp•iatlufficri,:.
Ur1ique S•Jlid waste matia~ement ut1it
desigr,ator. Must be alphat1umeric.
M~dia status ir,dicator. ~1ust ,:ont•ait1
,Jr1e ,Jf the foll,Jwing:
C COij1pliar1ce ~loniti)rihg station
8 -baselir1e m,Jr1it,Jrir1g,station
A -ot•1er ambient monitoring station.
Unique stati,Jtl ider,tifier. Must be
alphanume-ric.
USGS Aquifer 1:,Jde for aquifer from whi•;h samples are
obtain.ed. Alphanum,;ric fi.eld with up to ,;ight •:hara,: t e-r s.
Total depth to whi,:h tt,e h,:.ile was Jr"illled, b,:q-·-c:-.j ,.:.:,( dug in f,;.;t bo?l,:,i.; :and sur fa,:.; datur.-•. DECIM,;L NIJMET?IC field wit•, a maximum of twelve cf1aract~rs (ir,cluding
tJ,0 d21:imal p,Jint) at1d may ~,ave up to t·w,~ digit3 ~~t~~
the decimal ~1~ir1t.
Met•1,Jd bJ wf,i,:}1 well was 1:or1~tructed. M~st be
ALPHANUMERIC, consisting of a single charact.;r. chara,:ter must be 1Jr1e of the follcwir,g:
H holl,:.iw stem auger
C -1:abl e t,:,,Jl
V -reverse rotary
J -wat.;r j.;t
S -solid stem auger
R -r,:,tary
D -dug
A air percussi,Jt1
Fl~id used tc, lubri,:ate ,:utting t,:11:,l and/1:,r r1="fl11_•~·•2-
mat~,i~ls from hale. Must be ALPHANUMERIC, cor1si5tir·1g of a single character. T•1e ,:haracter mu~t be or,~ of th.; f,:,l l,:,1,,•ing:
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14 STELVl
15 STEL'-/::::
tG STELV3
17 SBELV1
! 3 SBEL'-.'2
SBEL\/3
::o NOCAS
::::1 TCELV1
23 TC:EL~.'3
decimal p,.:1ir1t), and may ha·✓t.• up to tw,:, digits followir1g t~,e de,:imal p,Jir,t.
TI-H, d 2pt h . -' ~ th::-t ,:,p ,:, f the L ,-:ct b ,:q,. t:' h,:,l s
St"•: ti ,:,n
The d'2pth to th"' t ,:,p .-:if the se,: ,:::,nd bore h,:,l t-so;:-,: ti ,:,n
The dc-p th t ,:, the-top of the-third b 1:•r~ h,:,lt.-.
,3e,: ti ,:,n
Each of the STELV¼ fields is DECIMAL NUMERIC ~itl, a maximum of twelve characters (ir,cluding the de,:imal point) and may have up to two dioits ~fter the decimal poit1t. Tt,ese depths are measurt-d-relat0ive to lar1d
SLIY fa,: e datum ..
The deptt, to the bott1Jm of the first bore t,ole
st"ctiori.
Tt1e depth to the b0ttoro ,Jf tt,~ 5ecor1d bore •1ole
se,: ti ,:,n.
The d~pt~, to the b,)tt,Jm ,Jf
~t"•.: t; ion.
J_,_ -',,,j'j-:_•
Each of the SBEL\•'x fit?lds is DEC:!MAL r.tUMCR.r::: 'Nith a maximum •~f twelve ,:haracters ~ir1 1:ludit1g the d~cir~~l
poit1t) and may t1ave up to two digits after the de,:imal poit1t. T•iese dept~,s ar& ij1easured rela~ive t,J lar1d Sl.lY' fa•:e datum.
Nurnbe-Y' of 1:asing secti,:,r1s. A ca.sing section is
defir1ed as a ler1gth of casing of constlnt dia~~et2r and ur1iforij1 material.Casing ~~,:ti0t1s ~;1: d~s~g~~t~d
numeric3lly f~om top tc b,Jttom of ~~11. !~JTEGER NUMERIC field ,:ontait1in~ a value ,)f 1Jr1J ,)r tw~.
The depth t,J the top ,~f the fir~t secti•on ,~f ,:a~ing(in feet).
The depth t,::, tht: top of tht' ·:5f•c.:,nd S(:cti,:,n ,:..,f casingCitl fee-t).
The depth to the top of the thiY"d section ,Jf •:asir1g(ir1 feet).
The-TCEL'h; fi;,lds ar€> DECIMAL NUMEF:IC, c-ao:h with ,a ~aximum wf twelve ch3r~ctcrs (in,:lwJir1g t~~2 d~,:imal ~0int) ~nd may have up ti~ two digits after t~,~ deciffial poir1t. These dept•,s aY'~ measured relative t,~ lat1d
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App •nd i ,,, 8
35 CMATR3
~-']~•";'('."=' ._, ,:,
37 TOELV
38 BOEL'.'
3'3 OMATR
40 OWIDT
41 OLEN13
Description or r,ame of casing material fr,Jm wl1ic~, the t•iird se,:ti,Jt1 of .,:asir1g is made.
Th• CMATRx fi•lds ar• ALPHANUMERIC, each with a ,·r1~xii~~un1 •~f ~ig~,t c•1aracters.
OPEN INTERVAL any
ir,t~ri,:,r of the ~211
surroundit1g soil 3nd
p,:1·l"ti,:,n ,:,f t~it.• •,,Jtl: i,··1 •..,;hi,::,
i 3 1-, ,:.:, t i :; .:, l .J. ": -:-d f ':'" ,: ~:: th•=
rc,ck by unbY'E-C:\1.:::-,ed ,:.:asi1·-1g.
Ind_: .. ·.:.:tti:,y of th-.:: typ-:• ,:,f ,.:,p;:;nirig in ':~"1~ ,:,p•2-n interval. Th• field is ALPHANUMERIC, cor1sisting of~ '5in;;le ,:hara,.:tl::"·r". The• 1:hara,:ter r11u·:it b~ on·,;: ,:,f th.:-f,:,111:it...Ji ng:
0 -,Jpen end P -perforated or slotted
S -s,:r~o?-ned
W walled
Z -other
T -sat1d point
X -,:,pen ~,c,l e
The d•pth to the top of th• open interval.
Tha TOELV fi•ld is DECIMAL NUMERIC with a
d~,:im~l poir,t) and may ~,ave up to ~~ter th, decimal poit1t. Measui-ed land s1_u,. fa,: e.
t (,,JO d i g i I~ s
' I..,_,
The dept•, to the bottom of the open int~y•.·al.
The 80ELV fit.?ld i=, DECIMAL NUMERIC · .. :::.t:·~ ;.:, ma::;irnurn •~f twelve c•iaracters (including the ~2cimal p,~int) and may have up t,:i tt..Jo digits after tht:." 1de,:iji"121l p,:,ir,~. Measur2d relative to land surface.
Description or name of material used to ~•=r~~t, th~ open int~rval. The OMATR field is ALP~~A~~Ut1ER!C ~i~}1 ~ maximum of 0ight ,:•iaracter=.
' Widtl1 or short dimension •~f slot •~r mesh' ,Jf screen material for tl1e ,:iper1 intt"rval, in incl1eS. The OWIDT fi•ld is DECIMAL NUMERIC with up to twel~e characters (ir1cluding the decimal), and may l1ave u~ to 3 digits following the decimal point.
Lt?ngth or 1,:,ng dimet1sion c•f slot ,:,r r,H.•sh ,of s,:reen material for the open int•rval, in inches. Th• OLENl3 field is DECIMAL NUMERIC with up to tw•lv• charact•rs (including the d~cimal), and may have uR to 3 digit5 f,Jllo(,,Jing the decimal point.
FILTER PACK -material pla•:ed in the 6,1t1u.c.·~ ,~[ ~:.,s t..Jell b~t1w~~•·1 tho2 beir·o::•h,.:,lfr 1,,,1all and ~:1•2-(,,Jell :;i:·re-1:n lo;;,.~.
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TSLELV
SO ~?SLEL'v'
51 SF:FSL
52 DN13F:AD
53
54 L THU::i
55 WLUSE
1 t required field
:t.
B b+:t1t,:,ni tE-
13 -· ,:€.·m~nt
'1•-•1 I --
C ·-,:,t t1 •?r
Z otheY
T~,e d2pt~1 to th2 t~~ .~f t~,e ~~~~~~lar
T~1e TSLELV fielJ is DECI~1AL 7~Ll~ER!1:
maximum ,Jf twelve chara,:t~rs (including th~
decimal p,Jint) and m~y t1av+: up to tw,~ digit3
aft~r the decim~l poit1t. Measured r~lati·.,~
to l . .;1nd :;ur fa;:::.•.
The dept~1 t,~ th2 bottom of the at1nular· seal.
Th., BSI_EL 1; f i ,, 1 d is DEC I MAL NUMEF: IC with a rc,a:d rc,ur,,
of twelve ,:haract~rs (including the detimal poit1t)
dr1d may ha·;2 up t,:, tw•J digits after the decimal
p,.:,int. Measu1--ed ·ro2-lative t,:1 1-::s,G ~wrf.3.,:i:::.•.
Surf . .3.ce-se2.: !ndic.:i.tor. In.::!i,: ... 1.t·:,:-~ 1..Jh,.:tt11;.•r ,.::,r ,·1ot th~-
upper p,~rtion •~f the boreh,Jle is 5eal~d to prevent
inflow of surface water. Sitigle 1:haracter
ALF·HANUMEF:IC, ,:ontaining "Y" if well is sealed.
□t•1er~Jise ,:,Jntains 1'N''.
Downgradient it1di 1:at1:1r. Indicates wht"thel" 1.:ir· n,:it,
the well has been installed hydrauli,:ally d0w11gradient
of ihe source of pott"t1tial groundwater pollution,
and is 1:apable of detecting the migrati6t1 of
,:ontaminants. Single ,:hara,:ter ALPHANUM~RIC,
containing 11 Y" if well is di:iwngradient fr,:.rn wast.::
disposal site. Othe-Ywise ,:ontains "N" ..
Drillt:Y·~ l,:,g inJi,.:ator. Indicates a·-.,,,all~bil~~:,·
dri::ers log. Single ,:hara,:ter ALPHANUMERIC,
contait1ing "Y 11 if log is d'i-3.i lable. Other 1..Jis,:;--
1: ,:,n t a i n s "N" .
-C U1
Lithologic log indicator. Litt,,Jlogic l1~~ 3•1•Jws
distributicn of litholc1gJ: • ... 1ith depth i:··, :the bol"'.;;· h,:,1,:-.
Single ,:hara,:te,· ALPHANUMEPIC, ,:ontaining "Y" if l,:,,;
is available. Otht?-rwise ,:,:,ntains "N".
Well use indi,:ator. Must be ALPHANUMERIC,
of a single character.
tt1Q-f,:11 l 1::iwi ng:
The character mJst
D dc.r:1i.•s~::.,.: '-r-'' l·.,.:ite) we1.t~r suj,::iply
I industrial uater supply
M monitci·it1g ~~1:
P -µubli,: waL~r· su~ply
0 ·-•~ther·
1:,:,ns i ,;ting
be one 1:1 f
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Datafile SAMPLE.DAT
field field
1
DELH:
3 DATE
:t
:1:
f i .:,1 d
D•?S•:ripti,:,n
Unique sample identifier. C,Jnsists of a f,~rtj-tw,J ,:t1.3.ra.,:tt.•r field, le-ft justi fi,?d, ,:,:,ntaining!
1-12
18
1 ":/ -27
28 -42
c!C::·:5C!ipti,:,n:
Utiiqu~ 3ite 1der1t1f1er 35 ass:~:~:~ ~1 EPA. Must be alphat1umeric.
Ut1ique solid waste mat1agemer1t unit
designator. Must be alp~1~numeric.
Media status it1di,:at,Jr. Must contair,
or1e of the f 1Jll0wing:
r con,pliance m,Jt1itorir1~ station
8 baseline rnonitorir1g statiot1
A -,Jtt,er ambient monitoiir,g stati 1Jr1.
Ut1iqLte station i·denti fier,. MLtst bl?
alphanumeric.
Unique sample identifier., Must be
alphanumeric.
'.'.:.-i·ti•.:al dl.5pla.cernt;""nt ,:;f ~aif1pl"2-ft,:irn tht:, (~ftrt.-r.,:s;;-0levati-~~, Cir, f~;t) of the samp!ir1g stati 1Jt1. F,Jr
su\,.-face w<:\ter, ~,:,ils, and gr-c,undwater-st1ati:;ns this •.Jould be-the depth ,:,f tho: sample and f,:,r: -3.lr ii11:,nitoring
stations, the height above ground. Must ~e DECIMAL NUMERIC ,.:,:1n·~i-~ting ,:,fa rn.J.:-~imum ,:if ·si:-,; 1:hara,:ter:5
(includit1g the dc,:im~l) arid may have up t,~ two di~its after the de1:imal p•)ir,t.
Date of sample c•~llection.
field consisting ,)f:
Eight character integer
1: ,:1 I ur.-,n s
1--4
5--E,
7-8
,: ont ent
year including cer~tury, e.g.
1 •:;3•:;
num-=ri,: n11:inth
numeri,: day of mohth
Column numbers are relative t•~ the beginr1ir1g oft~)~ DATE Field. Each subfiald described above must be right justifi~d, and may ,:ontaitl leadit1g ~eri)s.
I I I App,rndi :,; D Datafil~ PARM.DAT I field fidd ; 11:..a 0 n,3.ri"1•? I 1 C• ... C•.A.M vr.v ''" ,,· .. ,_, ........ ' I I I I I I I I I I I I .-. :JU/\L!'" i, I ,, Vt,LUE ~ ! I :t: rt:quir•?d fi,:·ld :t: :t field Oo;:-s,: rip ti ,:,r-; Ur·1iqw2 data r~•=-~r~ i~2ntifier. C:on=i3t= of a fifty· f,Jur ,:~1ara,:ter fio2-ld, left justifio2-d, cot1tair1ir1g: ,:1:11 ur11n ~ 1-12 13-17 18 Vii -27 ·-•·".:' -~ ,a~.::: 43 -54 55 -58 dt:-scripti,:1n: Ur1iqui2 :5it~ id-2-nti fit"t· as assigno2-d EPA. Must be alphanumeri~. Utiique solid wast~ mar1ag~mer1t ur1it designator. Must be alp~1ar·1umeri~. by Media status ir1di,:dt1Jr. Must ,:ontain one of the followit1g: C -compliance monitoring station B -baselir,e monitorit1g ~tation A -1Jtt1o2-r ambient mor1itorir1g station. Unique station identifier. Must be alp~1ar1umeric. Utiique ~ampl~ ~!~~13nu~~2rt,:. idt2i·1Li fie,~. ' I Must , .. ~~ Parameter identifier. F,~~ ch~mi,:al c0n~titu~r1ts for whi•:•1 CAS r,umbers ~~ist, the CAS numb~r will be t~~2 identifier. For 1Jt•1er constituents, the identifier ~il! to d0t~rmir1ed on at, as-rl~~ded b3sis. Repli,:ate t1umber. I dent i fies th,e value as one •~f tw,J or-more ar1alyiti~al results for the same parameter on the same sample. INTEGER NUMERIC, up to f6ur ,:har-act er s. Not used unI:ess repli,:ate results are rep)Jrted. Qualif::..2-r· fi'2-ld. ,\LPHt\i~UMERIC:, may c.:,nta1in up t,:i four STORET qu~l!fi~r ,:odes. · The reported analytical result for the chemical. Mu3t b~ DECIMAL NUMERIC, consisting of up to twelve ,:h.3'r'".:i,:t::-r !:i:·1i:ludi:··,.;; the de,:iri",Ql), .:i.nd ri"i;Z..y l1ave up to
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I APPENDIX B
I U.S. EPA FUNCTIONAL
GUIDELINES FOR EVALUATING
ORGANICS AND INORGNIC
I ANALYSES
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LAl!ORATORY DATA VALIDATION
FUNCTION Al. GUID~ FOR EVALUATING ORGANICS ANAL YS:ES
.. -
Prepared for the
HAZARDOUS SITE EVALUATION Dl'VlSION
U.S. ENVIRONMENTAL PROTECTION AGENCY
Olmpiled by
Ruth Bleykr
Samplr Management Office
Prepared by
The USEPA Data Review Work Group
Scon Siders -EPA HQ -0,-Chairperson
Jeanne H2nk.ins -EPA Region m -Ol-Chairperson
Deborah Szaro -EPA Region I
Leon Lazarus -EPA Region Il
Charles Sands -EPA Region m
Charles Hooper -EPA Region IV
Patrick Churilla -EPA Region V
Debra Morey -EPA Region vn
Raleigh Farlow -EPA Region X
hbrary l. 1988
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TABLE OF CQ!YU1''IS
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11''TRODUCTION ······-------------····-------·-··· I
PRELIM11'ARY RLVZE1r ---·----··---··-·········---"--
-..... 3
VOLATILES AND SE.MTVOLATll.ES .l'llOO:t>Ull ____ _ -······4
Holding Times. ____________________
_ -·5
L
n. GC/MS Tuning-----·------------·---
·-····6
._ ... 9
m. eaumtio,ll-----------------------
IV. Bla.nlcs-'-----------------------_12
V. Surrogate Recovery_. ____________ , ________ _ .. 14
VI. Mattix Spike/Mattix Spike Duplicate _______________ _ .... 16
VD. Field Duplicates--------------------•---,---
•. 17
VIIL ln°tenw Standard$ Performance--------------,.--
.I&
IX. TCL Compound Identification---------------------
.19
X. Compound Quantiution and Reponed Detection Limits-·------.. -20
XJ. Tentatively Identified Compounds-·----·------
__ 21
XIl. System Performance---------·
_23
XIII. Overall Assessment of Data for a Case _____________ _ -24
J'ESTICID.ES l'ROCEDur<.-"-----------------'--
_25
L Holding Times. _________________________
_ --26
n. J'esticides Instrument Performance, __________ . ___ ....., __ -26
m Calibntio-----------------------
_ 30
IV. Blanlcs _______________________
_ 33
V. Surrogate Recovery ____________________
_ 34
VL Matrix Spike/Matrix Spike Duplicate ____________ .,.... __ 35
Vll. Field Duplicates _____________________
_ 36
VllL C.Ompound Identification __________________ ...,. _ 37
IX. C.Ompound Quantitation and Reported Detection Limits·---·--------.38
X. Overall Aaenmenl of Data for a Case---------------39
GL~AR Y k Data Qualifier DefJ.Ditious -----------------··40 I
-·!
GLOSSARY B: Other Terms ____________________
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LABORATORY DATA VALIDATION
FUNCTIONAL Cl/ID!LINES FOR [VALUATING ORGANICS ANALYSES
JNTRODUCJlON
This ~-nt is designed to offer .sui,daDce in laboratory data e~uation a.nd
validation.. ln some 11:St)effl, it ii equinleJJI t.o a Sa:ndaro Operating Prccedur'e (SOP). ln
other, more subjectiw aras, a)y ~neral pidancr ~ offrnd due to the complexities a.nd
uniqueness or data relative III specific: sam-ples. These Guidelin~ have been updated to
include all reqwremcnts in lM tO/J6 Slatemen1 of Wort. (SOW) for Orgwc:s 1.11d 10/86 SOW
for Volatiles.
Those arus where ~ic SOP.l are possible are primarily areas in which deffuitive
-performa.n~ yequinaents vc emblished.. These mus also correspond I to specific
requirements in Agenc:, co11trac:u. "Ibese requirements are concerned with specifications that
are not sample dependent; they specify performance requirements on matten that should be
fully under a laboratory's control These specific areas include blanks, calibration standards,
-performance nal12J1tion stand&rd materials, and tuning. 1D particular, mistakes such as
calcul.atiO'n and transcription emm must be rectified by resubmission or corrected data sheets.
This document is intended for technical rniew. Some areas of ove'rlap between
technical review and ContrKt Compliance Scrffa.ing (CCS) exist; however, contn.ct
compliance is not intended to be a goal or these guidelines. JI is assumed that the CCS is
available and can be utilized to assist in the data review procedure.
'
Some requirements are not identical for every Case or batch of Amples.
Requirements for frequency or Quality Control (QC) actions are dependent on the number of
samples, sample preparation techn.ique, time or analysis, etc. Specific Case requirements 1.11d
the impact of nonconformance must be addressed on a case by case basis; no specific
guidance is provided.. For example, there is a contn.ct requirement that a blank analysis be
performed a minimum of once every twelve houn of analysis time. This requirement must be
translated into the number or blanks required for a specific set or samples; the data reviewer
may have to consider the impact on data quality for a sample analyzed thirteen, houn after a
blank. in terms of the acceptability of that particular sample.
At times, there may be u. 11rgent Deed to use data which do not meet all contract
requirements and technical eriteria; Use or these data does ~ coDStitute 'either a new
requirement standard or full acceptance or the data. Any decision to 11tiliu data for which
performance eriteria havt 9IOt bee.a met is strictly to facilitate the progress of projects
requiring the ava.ilability or die data. A contract labora\Dcy submitting data which are out of
specification may be ftQ'llired 10 rerun or resubmit data even iC the previously submitted data
have been atilized due to IIJ'gent program ae,eds; data which do not 111eet specified
requirements are never fully acceptable. The only exception to this requirement is in the
area of requirements for individlll.J sample analysis; if the nature of the sample itself limits
the attainment or specifications, appropriate allowances must be made. The overriding
concern or the Agency is to obtain data w~h are technically valid ud legally defensible.
All data reviews must have, as a cover sheet, the Organic Regional Data Assesiment
form. 1f 1D&ndat0Ty actions are required, they should be specifically noted on ,this form. ln
addition, this form is to be 1ISCd to summariu overall deficiencies requiring attention; as well
as general laboratory performuce and any diicel'llible trends in the quality of the data. ('Ibis
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form is aot a replacement for the d.au revie.,..,) Sufficient 1upplemenury doc:umentatioo
must accompany the form to clearly identify the problems a.ssoc:iated ,.·ith a Ca.se. Tbe form
and any attach.menu must be 1ubmined to the Contract Laboratory Program Quality
Assurance Office1' (CLP QAO), the Regional Deputy Project Officer (DPO), and the
£nvironmencaJ Monitori.Dg S)'1tems Laboratory iD Las Vegas (EM.SL/LY). ·
It u tht ,espon,;bllity of the data n:vie-wtt tD notify the Regional DPO concerning
problems and shonc-ominp with regard In laboratory data. If there ir u 11rgent requirement,
the DPO may be co11-.:f by lekphoae ID npe,d.iu ciom,ctive acticD. It is recommended
that all items for DPO 1cti011 be preail.ed at -time. In all) cue, the Orguic Regional
Data As.sessment form mmr lie compJeu,d IIDd 111bmitted. '
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:I I I PRELIMINARY REVIEW In order to use this dcx:umcDI effectively, the reviewer should have I gcDcral overview of tM Case ar h.and. The euct number of amples, their assigDed 11umbers, their matrix, an:! ~ .mumber of laboratories involved in their anal~i.!. &re esseDtial ioformatioD. Background inf or-mat.ion on lM silt is belpful but often this information is ftf)' difficult to locate. Tlte site pro_i= officoeI ii the best 'IO\l1CC for n:,,,,en or further direction. CCS a a ,ov:rce of a brge qlllUJtity ol snm-rl"Zd information. Jt Cllll be used to alert the revie~ of ,:,n>blnns in tM Case or wut may be sample-specific problems. This information m.ay be utilu.ed ill dan "rllidation. 1£ CCS is unavl.ilable, those criteria affecting data validity must be addressed by the data reviewer. -1 • Cases routiDely have unique samples which require special anention by'thc reviewer. Field blanks, field duplicates, ed performance audit samples Deed to be identified. The sampling records should provide: · ,· . J. 2. Project Officer for site Complete list of samples with notlltions on a) sample matrix b) blanlcs• c) field duplicates• d) field spikes• e) QC audit sample• n shippiDg dates g) labs io volved • If applicable The chain-of-custody record includes sample descriptions ed date I of sampling. Although sampling date is not addressed by contract requiremeDts, the reviewer must take into account lag times between sampling and shipping while assessing sample ho\diDg times. The Case Namitive is another source or geaenl information. Notable problems with matrices, insufficient sample volume for analysis 01 reanalysis, and unusual events should be found in the Narrative. 1 3 -·----~·:.. :r.. , 2/SS
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VOLA TILr.5 Al'\D StMIVOLA TIL'ES
PROCtDURt
The requirements ID be checked in va!idatiou are listed below: recs-i~diates that
the contnctual requirements for these items will also M checked by CCS; CCS requirements
are 1101 alw.ys the s:ame as the data review CTiteria.)
I. Holding T-.es (CCS -Lal) hoJdillg times only)
II. GC/MS Tuo.i11g
m. Calibration
0 IDaf (CX:S) -
0 Co11tillui11g (CCS)
IV. :Blanlcs (CCS)
V. Surrogate Recovery {CCS) .. '
VI. Mattix Spike/Mattix Spike Duplicate (CCS)
VIL F.ield Duplicates
vm . Internal Standards Performance (CC:S)
-IX. TCL Compound lde11tificatio11
X. Compound Quaotitatio11 and Reported Detection Limits
XI. Tentatively Identified Compounds
XII. System Performance {CCS)
XIII. OYerall Assessment or Data for • case
.... . . .... .... I .
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I. HOLDISG u,1rs
A. Objecth•
B.
C.
D.
The objecli~e is to asceruiD tlle \'lllidity of results based on the holding, time of the
sample from tjme of cpl)ectipn II) time or analysis or sample Pffp:antion, as
appropr~a.
Crlurl.a
T~hll.ical re-quin:mena for sample holding times have only been established for water
matrices. The holdi.a.g times for aoils are nnc.ndy uder investigation, l\'hen the
results are available they will be incorporated into the data evaluation process. On
October 26, 1984 in Volume 49, Number 209 of the Federal Register, page 43260, the
following holding time requirements ftre established under 40 CFR 136 (Clean Water
Act):
..
Purgeab!es; Ir unpreserved, aromatic volatiles must be analyud within 7 days
and non-aromatic volatiles must be analyud wilhiD 14 days. lf preserved with
hydrochloric acid and stored at ... C, then both aromatic and non-aromatic
"olatiles must be analyzed within 14 days.
Extnmb)e) Clncllldes Boe/Neutrals and Acids): Both samples and extncts
must be preserved at 4'C. Samples must be extncted within 7 days and the
extract must be analyzed within 40 days.
EuluUlon Procedure
. Ac:tual holding times are established by comparing sampling date on the EPA Sample
Traffic Report with dates of analysis and/or extnction on Form I. Examine the
&ample records to determine if samples were properly preserved. (If' there is no
indication of preservation, it must be assumed that the samples are unpreserved.)
Actloa
I
If -10 CFR J 36 holding times are exceeded, flag all positive results as estimated (J)
and sample quantitation limits as atimated (UJ) and document that holding times
were exceeded.
The following table illastrata when the qaalif".ien are to be used for volatiles:
I.
Matrix
'Water
Preza ttd
No
Yes
?7J>ays
All 1TOJ111tics An compounds
None All compounds
If holding times are grossly exceeded, either on the fint analysis' or upon re-
analysis, the reviewer must use professional judgment to 41etermine the
nliability of the data and the effects of additional storage on the sample
.-esults. The reviewer 1111y determine that non-detect data are 1musable (R).
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-2. Due 10 limited informatioc coccenucg boldicg times for soil samples, it is lert
to the discretion or th.e data reviewer to apply ,nter bolding time criteria to
soil samples.
D. ct £MS JUNlliG
A. Objecthc
Tuning and performance criteria are established to ensure mass reJOlution,
. -

-
identification and: to some degree, sensitivity. These criteria are not sample specific;
conforma.cce is determined using ltl.Ddard materials. Therefore, these criteria should
be met in all circu.msta.nces. · ' ~
B. Criteria
1. Decafluan>tripbalylphosphlne (DFTPP)
,· mL1 JON ABUNDANCE CR,TIERIA
51 30.0 -60.0 % of m/z 198
61 less than 2.0% of m/z 69
70 less than 2.0 11b of m/z 69
127 -40.0 -60.0% of m/z 198
197 less than 1.0 11b of m/z 191
198 base peak, JOO% rebtive abundance
199 5.0 -9.0% or m/% 198
275 10.0 -30.0% of m/z 198
36S greater than 1.00% of m/z 191
MI present, but less than m/z -443
-442 greater than 40.0% of m/z 198
443 17.0 -23.0% or m/z -442
2. Bromonuorobeazeftf' (BFB)
ml.I.. JON ABUNDANCE CRITERIA
15.0 -40.~ or the base peak so
15
95
~
3o.o -60.0'lli or t1ii: ~ peak 1 ·
baz peak. IOO'lli nbtive abandance
173
174
175
176
177
5.0 -9.0% of tbe l>ue peak
Jess than 2.0% or m/z 174
greater than 50.0'l(, or the base peaJc
5.0 -9.0% or m/z 17-4
greater than 95.0'l(,, but less than 101.0% or m/z 174
5.0 -9.0% or m/z 176 .• . -~ .~
~ M contracts are 111od.if'Jed, new criteria would then apply. ~·
C. Enluatloa P,oc:eclurc
I. Verify from the nw data that the mass calibration is correct.
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D.
2.
3.
. -' 4.
Action
1.
2.
Compare the data presented on each GC/MS Tuning Llld Mass C.libration
(Form Y) wit.h each nws listing submitted.
:Ensure the following:
a. Verify that Form V is present for each 12-hour period A111ples are
analyzed.
b. The \aboratoT)' bu -IUde ay truJaiptioo ffTOn.
c.
d.
The appropri.a.u amnber or rignifica.at figures .bas been reported
(number of 1igtilricut figuns given for each ion in the ion abundance
criteria column).
Tbe \aborUory Jw DOI made uy calculation erron. For e.umple.--the %
m.a.ss o(' m/r. "'43 relative to the DUW o(' m/-z. '42 is calc:ulated using the
foUowing equation:
'lo abanda.ace • relati~ abu.ada.ace or m/-z. 443
relative abu.ada.ace of m/-z. 442
X 100
If l)OSSible, verify that 1r.,ec:ba were generated ming appropriate backgrou.ad
subtraction techniques. Since the DFTPP and BFB spectra are obtained from
chronutographic peaks tut should be free from coelution problems,
background subtrartion lhonld be straightforward a.ad designed only to
eliminate col= bleed or instrument background ions. · Background
subtraction actions resulting in spectral distortions· for the sole purpose of
meeting the contract specifications are contrary to the Quality assurance
objectives LDd are therefore a.aacx:eptable.
I
If mass calibration is in error, classify all associated data as un~ble (R).
lf ion abund&Dce criteria are not met a.ad the data in Question .L nee4ed on •
priority basis, professional judgment may be applied to determi.ae to what
extent the data may be utili-z.ed. Guideti.aes to aid in the application of
professioaal judgment to this topic are discussed as follows: '
L DFTPP -The most critical facton in the DFTPP criteria are the
1100-imtnzme.at specific RQUirements thal are also not unduly affected
by cbe location ol the spectrum on the chromatographic profile. The
m/1. 191/199 LDd 442/443 ntios are critical. These ntios are based on
die natural abundances or Carbon 12 and Carbon 13 a.ad: should always
be meL Similarly, cbe m/-z. 61, 70, 197, a.ad 441 relative abundances
indicate the condition or the instrument a.ad the suitability of the
resolution adjustment a.ad are very importanL Note that all of the
foregoing abundances relate to adjacent ions -they, are JJlatively
i.asensitive to differenoes in instrument design and position of the
spectrum OD the chromatographic profile. For the ions at m/-z. SI, 127,
a.ad 275, the actual relative abunda.nce is not as critical.: For insta.ace,
if m/r. 275 1w 40'lb relati~ abundance (criteria-10-30%) a.ad other
criteria are met, the deficiency is minor. The relative' abunda.ace or
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3.
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b.
m/z 36S is a.n indkator of suitable instrument zero adjustment. If m/z
36S relative abUDdance is zero, minimum detection limits may be
affected. On the other wd, if 111/1. 36S is present, but less than the
I% minimum abundance criteria, the deficiency is not as serious.
. I
l!l]! -As with DFrPP, the most important facton to consider are the
empirical res11la that are relatively insensitive to loc:ation on the
chrom.aiognpllic prorili ad the l)1)e of instNmentation., Therefore,
the critical iOtl a)mDdaa<:e -:rin:Tia (ar BFB are the m/z 9S/96 ratio, the
174/li'S ~. ~ 176/171 ntio, ud the 17.C/176 ntio. The relative
abundances of m/z 50 and 1S are of lower imponance.
In tine with the above discussion, an expansion of minus 25% of the low limit
and pl11S 259'. ol the high limit Cot ael~ iom may be appropriate. For
cu.mple, .ID DFTPP the m/7. 51 ion abUDdaDce c:riteria might be expanded
from~ of m/z 198 to 22-7S,. of m/z 198.
a. The complete expanded criteria for DFI'J'P and BFB are as 1follows:
I
1) Decafluorotripbeoylpbosphine (DFil'P) (Expanded Criteria)•
2)
mll ION ABUNQANCT CRITERIA
SI no -75.0% of m/z 198
61 less than 2.0% of m/z 69
70 less than 2.0% of 111/z 69
127 30.0 -75.0% or m/z 198
197 less than 1.0% of m/z 198
198 base peak, 100% relative abundance
199 S.0 -9.0% of m/z 198
275 7.0 -37.0% or m/z 198
· 36S greater than 0.75% of m/z 198
44 l present, but less than m/z 443
442 greater than 30.0% of m/z 198
443 17.0 -23.0% of m/1 442
BromoOuorobenune (BFB) (upanded Criteriat
ma ION ABUNDANCE CRrrERJA
50 11.0 -50.0% of the base peak
75 22.0 -7S.~ or the base peak
95 ba!e pealc, 100% n:lame abundance
96 S.0 -9.0'l of the base peak
J73 less thaD 2' of the base peak
174 ,-1.er lhaD SO% of the base peak
175 S.O -9.0% of m/z 17.C
176 greater than 95%, but less than 101% of m/z 17.C
177 S.0 -9.0% of m/z 176 '
•~ Does NOT change contract l'e(luirements. .,
. . .·~-I
b. If results fall •within th-expanded c:riteria, data may lie acceptable.
c. If results fall outside these expanded criteria, all data are unusable (R).
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A.
B.
d.
e.
f.
r •
ObJectl•e
Tuse c:riteria do NOT establish new contract requirements. Contnct
labontories meeting expanded criteria but not meeting contract
requirements are NOT in compliance.
Decision.s to we analyili::al daa assoc:ia•~ ,..jth DFTPP and BFB tunes
not meeting contract RQuirements should be clearly aoted on the
Orgacic Regional Data Assessment Form. '
If the ttViewer has reason to believe that tuning criteria were achieved
■isma tedmjqaes that distDtlltd or skewed the lpec:IJ"a, full
doc:11we»UWJD OIi 1ht tmuni qmlity COlltTOl should be obtained. If the
re:hluques ~Jared are foand to be at Yariance with accepted
· .,.actices, the quality aswmce program or the laboratory may merit
evaluation.
Jr ii vp to the reviewer's discretion, based on professional judgment, 10
flag data associated 'With ta!leS meeting expanded criteria, but not basic
criteria. JI only one element Calls within the expanded criteria, no
qualificati011 may be needed. On the other band, if several data
elements are in the expanded windows, all associated data may merit an
estimated flag (J). P\ease note lhat the data reviewer is not: required to
we expanded criteria. The reviewer may still Ch00$e to flag all data
associated ,..ith a tune not meeting contract criteria as unusable (R) if
it is deemed appropriate.
m. CALTBRATIQN
Compliance requirements for satisfactory imtrument calibration are established to
ensure that the instrument is capable of producing acceptable quantitative data.
Initial c:alibnation demonstrates that the instrument is capable of, acceptable
performance in the beginning, and continuing calibration checb document
satisfactory mailllrnance and adjustment of the instrument on a day-to-day basis.
Crlterl.a
l. Initial Calibration
L Volatile and Sem.ivolatile Fractions
I)
2)
All average llelative Response Facton (RRF) for TCL
compounds !Dast be ~ o.os.
All Percent Relative Standard Deviations ~RSI>) must be
s 30'll,. ._.,..,. I
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2. Continuing Calibration
a. Volatile and Semivnlatile Fractions
J) All Relative Response Facton (RRFJ for Ta. compounds must
M t,0.0~.
l) AD Pacu.t Dif'Tes-eace ('Jl,D) must be 5 25'1b.
C. Enluatlon Procedure
1. J.nj tial Cali bntioll
..
L Evaluate the RAF for all TCL compounds and verify the following:
1) Check and recalculate the RRF and RRF for one or more
volatile and semivolatile TCL compounds; verify that the
recalculated value(,) agrees with the laboratory reported
value{s).
2) Verify that aD volatile and semivolatile TCL compo11Dds have
avera,e Relative Response Facron of at Jeast O.OS.
b. Evaluate the Percent Relative Standard Deviation (%1lSD) ,for all TCL
compounds and verify the following:
(J
IN, RSD • ~ x 100
lt
-cJ • Swidard deviation of S response facton
'"i: • Mean or 5 response facton
I
J) Qeck ud nc:aJClllate 1be ~ for one or' 111ore TCL
compollDds; ~J that Ole recaku\ated value agrees with the
laboratory repor1ed niue. '
2) Verify that alt TCL compounds (volatile and semivolatile) have
a «N,RSD or :s. ~-·
c. If erron are detected in the calculations of either the ill or the
411,RSD, perform a 111ore comprehensive rec:a.lculatio11. ·; 1
·--.~-.. -r.·:
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D.
2. Continuing Calibration
a.
b.
,·
C.
Action
Evaluate the RRF for all TCL compounds:
I) Verify that all volatile and ,emivolatile TCL compounds have
Relative Response Fa=n of at leas\ 0.05. '
Eftlmre dl.e l'en:ent Diffi:reuee and verify the following: ,
1) Cbec:\c aJnlaiion el 'Ii> Diffen:nce (lli>D) between initial
c:alibratimi ~e Jlelative Respome Facton and continuing
Alibn.tion Relative RespoQSj! Facton for one or more
c..,mpo;u1ds, ming the following equation:
2)
where,
RRF1-RRFc
---------i 100
'
-·
.R.RF1 • average relative response factor from
initial calibration.
RRFc • relative resi,oase factor from
continuing calibration standard.
Verify that the '!bD is s 25% for all volatile and .semivolatile
TCL compounds.
If erron are detected in the calculations of either the RRF or the IM>D,
-perform a more comprehensive recalculation.
1. Initial c.alibration
2.
L If any wlatile or aemivolatile TCL compound rault has an average
Relative Response Factor of Jess than 0.05:
1)
2)
Flag pasjtive ruults for that compound as estimated: (J).
I
Fag noa-detects for that compoud as unusable (R).
I
b. U any volatile or Rmn"Olatile TCL componod has a lib RSD of greater
than 30%:
I) Flag positive results for that compound as estimated (1).
2) Non-detects may be qualified using professional JudgmenL
. I
Continuing Calibration
.. -_ ... ._
L
.:.:-;-.:
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If any volatile or semivolatile TCL compound has a Relative Response
Factor of less than 0.05: '.
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B.
c.
D.
b.
1)
2)
Flag positive results for that ~mpouod as estimated (J).
Flag non-detects for that c:ompouDd as uniuable (R).
U any vobtile or aemivolatile TCL compound has a 'II, 1 Difference
i,ec,o·~.a wtial a.ad Continuing Cal.ibntion of greater tha.D 25%:
'
Flq a?I positi+c results for th.al comi,o'1nd as estimated (J).
Noa· ti ts _., be qmftfled ming professional judgment.
IV. JILANJS
ObJecdTe
The assessment or blanlc &nalysa results is to determine the existence and magnitude
of cootwrniuati® probkms. The criteria for evaluation of blanks apply to any blank
~dated with the amples. If problems with w blank exist, all data associated with
the Case must be c::amully evaluated to determine whether or oot there is an inherent
variability in the datw for the Case, or if the problem is an isolated occurrence not
affecting other data.
'
Criteria
No co11tarnioaots should be pRSeDt in the blank(s).
·Euluatloa Proceclme
1.
2.
Actloa
•
Review the l'C$ults or all associated blank(s), Form I(s) I.lid raw data
(chromatograms, =nstructed ion chromatograms, quaotit2tion reports or data
system printouts).
. ,
Verify that Method J!laok analysis has been reported per , lll3trix, per
cooceotration level., for each GC/MS system used to analyze V,OA samples,
and for each extractio.a batch for semivolatiles. The reviewer can v.se the
Method J!lank Summary (Form JV) to mist in identifying samples associated
with ea.ch Method Blank. .
Action in tJae ease a 11DSUita~ bwllc results depend! oo the circumst2oces and origin
of the blank. No positive Ample results should be reported unless the concentration
or the compound m lhe sample exe<ech 10 time, the amount in any blank for the
common ~ntaminann listed below, or 5 times the amount for other co~pounm. In
instances where more than one blank is associated with a given ample; qualification
should be based upon a comparison with the associated blank having the highest
eonceotratioo of a coot.amin•nt. The results must ~ be corrected by 1ubtr1cting any
blank value. Specific actions are as follo'IVS: '!_' •
. '!.:; . ' '
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2.
.-.
3.
lf a compound is found in a blank but ~ found in the sample,' no action is
a.ken.
'
Any compound (other than the five listed belo.,.·) detected illi the sample,
,.-tuch was &!so d~tec1ed in any 1-!.SOCiated bla.nk, mwt be qualified when the
a.mplr co~tration is less tiwl five times the blank concentration. For the
fotloWUII f" m: coa,pounds, the results an qualified by elevating the limit of
cterection wi,,nr ~ Ampi,: eoocorntion ii. less than 10 times the blank
co ocenrnition.
Common bb C('"laminan~
a. Methylene chloride -· -
b. A~tone
c. Tol~ne
d. l-\:nrtaMDe
e. Common pbihalatc esien
ne rniewer shoa\d note that the blank analyses may not involve the aame
..,eiglals,, volumes. or dilution facum as the associated samples. ,These facton
mast be taken into considuation when applying the Sx and lOx, criteria. aucb
dial a c:om,paris'1n of the iotal amount of contamination is actually made.
Additionally, there may be instances where little or no contamination was
i)resent in the associated blanks, but qualification of the sample was deemed
necessary. Contamination introduced through dilution water is' one eumple.
Although it is not always possible to determine, instances of thh I occurring can
be detected when contarnin•nts are found in the diluted sample result. but are
absent in the undiluted sample result. Since both results are 1 not routinely
Teported, it may be impossible to verify this source of contamination.
However, if the reviewer determines that the contamination is from a source
other than the sample, he/she should qualify the data. In this case, Che Sx or
lOx rule d<>e$ not apply; the sample value should be reported as ·a non-detect.
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The following are eumples of applying the blank qualification guidelines.
Certain cimunstaaccs m&y wvrut deviations from these guidelliles .
Ott J: Sample result is greater than the Contract Required Quantitation
Limit (CRQL), but is less than the required amount (Sx or lOx)
from the blank resulL
Blank Result
CRQL
Sample Result
Qualified Sample Result
Rll1i
lli. :a
7
5
60
60U
,7
,5
30
.JOU
' ·•·
ID the example ror the JOx rule, sample results less'than 70 (or JO
s 7) would be qualified as non-detects. In the case: of the Sx rule,
ample res11lts less tha.a 35 (or S s. 7) would be qualified as non-·
decect3.
.
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CPC 3:
Sample result is less thaa CRQL, aad is also less thaa the required
.amouat (51. or 101.) from the bla.Dk result.
Blank Result
CJtQL
SamJ)l,cbwr
Qmlified Sample JltSllit
R.llk I
lli a
6
5
4J
sti
Nott that data are not reported as 4\J, as th.is would be reported as
a de~tioa limit below the CJlQL. -··-··-
Sample result is greaw than the required amount (Sx or I0x)Jrom
tbe blaDk resulL '
Blank Result
CRQL
Sample Result
Qualified Sample Result
~
lli a
10 10 s s
120 60
120 60
For both the 10x and Sx rules, sample results exceeded the
adjusted blank resula of 100 (or 10x10) and SO (or Sxl0),
respectively. ·
4. If gross contamination exists ("i.e.. saturated peaks by GC/MS), all compouads
affected should be flagged as unusable (R), due to iaterfereace, in all samples
affected.
S. ·· 1£ inordinate amounts of other TCL compounds are found at lowl levels in the
blank(s), it may be indicative of a problem at the laboratory and should be
noted in the data review comments which are forwarded to the DPO.
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6. S"mubr consideration should be gr,en to TIC compounds which are found in
both the sample and associated blank(s). (See Section XI for TIC guidance.)
V. SJZREQGATE RECQYEEY
ObJecthe
Laboratory performa.nce on individual samples is established by means of spiking
activities. All samples are spiked with surrogate compounds prior to sample
preparation. ne evaluation of the nsulu of these surrogate spikes is not necessarily
straightforward. The sample itself may produce effec:ts due ID such faclon as
interferences and high concentrations or ualytes. Since the effeets or the sample
matrix are frequently outside the control or the laboratory and may present relatively
11J1ique problems, the review and validation of data based on specific aauiple results is
2/1&
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D.
freciuently subjective and demands analytical experience and 11rofessional judgment.
Accordingly, this section con.sisl3 primarily of auidelines, in some ca.ses,with several
optional approaches suggested.
Criteria
Sample nnd bluJ: nn-o,ate ncoveries for volatiles and aemivolatiles must be within
limits as per appl.icable SO,.. (Form D).
1. Cbeck nw data (u .• eh.romatosrams, qant list. etc.) to wrify the recoveries
,on the Sllrrogate :Recovery (Form ll).
2. The following should be determined from the Surrogate Recovery'form(s):
r •
3.
L
b.
If any t!:'.J2 surrogateS with.in a base/neut:nll or acid fl"ICtion (or one
surrogate for the VOA fl"ICtion) are out of specification, or if any one
ba.se/neutnl, acid or VOA surrogate has a recovery of less than I 0%,
Chen there should be a reamlysis with surrogate results still outside the
criteria. ~ Wben there are 11mcc:ept1ble surrogate recoveries
followed by su=ful re-analyses, the labs are required to report only
the succe.ssful run.)
The lab has failed to perform satisfactorily if' surrogate recoveries are
out of specification with no evidence of repurging, reinjection, or re-
extraction. ,
c. Verify that no blanks have surrogates outside the criteria.
Any time there are two or more analyses for a particular fraction the reviewer
must determine which are the best data to report.
Considerations should include:
L
b.
C.
Surrogate rocovery (marginal -.s. J1"0SS deviation).
Holding times.
Comparison of dae fflues of the TCL compounds reported in each
fraction.
For surrogate spike recoveries out of specif'ication, the following approaches are
suggested based on a review of all data from the case, especially con.sidering the
apparent complexity of the sample matrix:
J.
•
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If at least t!:'.J2 surrogates in a base/neutral or acid fraction or one surrogate in
the volatile fraction are out of specif"',cation, but have recoveries 1reater than
BO%:
a. Positive results for that fraction are flagged as estimated (1) • .
15 2/18
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B.
C.
2.
3.
4.
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b. Negative resulu for that fnctioo are flagged ,.,ith the
quantitatioo limit as estimated (UJ).
If any surrogate in I fraction shows less than 10% recovery:
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b.
Pcwtive resw for du.I fnctio& arc C\aued as estimated (J).
NC&lltive nsults for that fraction are l'lag1ed as uusable (R).
No Qual;rica1io0 with resP«"'( ao nrroga.t~ ~ry is placed on clita unless at
least two 1UrT011tes are out of specification in the base/neutral or acid
fnaction, or one in the vobtile fraction, or unless any surrogate has I less than
10% recovery.
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ID the specw case or a blank aoalysiJ wil.h SUJTOptes out of spec:ificati011, the
rniewer must give spec:ial con.sidenU011 to the validity of associated sample
data. The basit ~ is whether the blank problems repre3ent an isolated
problem with the bbAlt alone, or whether there is a fundamental problem with
the analytical process. For e.umple, if one or more samples in the batch show
acceptable IU1TOgate recoveries., the reviewer may choose to consider the blank
problem to be an isolated occurrence. However, even if this judgment allows
some we or the affected data, analytical problems remain that must be
corrected by the labontory.
VI. MATRIX SPIKIIMATJUX SPIKE DUPLICATE
ObJecthe
These data are genented to determine long-term prec1S1on and accuracy or the
analytical method on various matrices. These data alg.tt cannot be used to evaluate
the precision and accuracy or individual samples.
Criteria
I. Spike recoveries must be within the advisory limits established in the
appropriate 1FB and OIi Form m.
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2.. Relative Pertmt Diffemices (RPD) betw&:.1 -tri.x spike and, matrix spike·
duplicate reai1"erics must be within the advisory limits established in the
&pp,opaiate IFB and OD Form m
EnlutJoa Procedure
I. Inspect results for the ~trix Spike/Matrix Spike Duplicate. Recovery {Form
lli).
_ I ·-. -::,. I
2.. Verify tnnscriptions from raw data and verify c:alculatiom. :;i
16 2/1&
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A.
B.
C.
D.
Action
No a.c:tioc is takec oc Marro: Spike/Matrix Spike D\lplicate (MS/MSD) chta a.!.2.tt to
qualify ac entire C&se. However, using Wormed professional judgmtct the chta
revie,.-er =r ~ lbe imrri.1 spike and matriJ. spike duplicatt n:sulis ill c:onjunction
with other QC c:rnrria and determine tbe need for some qualificatiou or the cht:2.
T~ du& reviewer should £int try ID determine to what e.11e.11t 1he rbults of the
MS.IMSD affect rJN! 1noci:11ed cbt:1... ~ dnennimtion should be made with regard
to the MS/MSD sample i.uelf ~ w-eU 115 specific analytes for all u.mpies associated
with lhe MS/MSD.
In those instances where it ClUJ be det..1 wined that b results of the MS/MSO affect
only the sample spiked, then qualification sbould be tim.iied ID th.is umple alone.
However, it may be detenDined tbrougb Uie MS,'MSO n,su\ts that a lab is hrting a
systematic problem in the amlysis oC one or 111ore amlytes, which af'fects all
associated samples.
. -• VII. rn:LD DUPLICATES
Objecthe
Field duplicate samples may be taken and analyud as an indication of overall
precision. These analyses measure both field and lab precision; therefore, the results
may have more variability than lab duplicates wb.ich measure only lab performance.
It is also expecied thlt soil duplicate ruults will have a greater variance than water
matrices due to difficulties associated with collectiug identical field samples.
Criteria
There are no specific review criteria for field duplicate analyses comparability.
EYaluatloa ProcNures
Samples whieh are field duplicates should be identified using EPA Sample Traffic
Reports or sample field sheets. The reviewer should compare the resutis reported for
each sample and calculate the Relative Percent Difference (RPD).
Action
Any evaluation or the field daplicates Jhould be provided with the reviewer's
commenu.
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17 2/&8
I :I I I : I A. B. C. D. VIII. It,TIR!"Al STANDARDS PEBEPBMANCE ObJecthe ln1er11~ St:anchrds (IS) penonzant:4! criteria C!ISllTe that GC/MS sensitivity &Dd respoc.se is su.ble during ~ I\ID. Criteria • 1. 111\nlW stsndard area counts must not .-ary by more than I factor of two l-50'li. 10 +JOO%} fniin the as.soaated calibration 1t111dard. 2. The retention time or the internal standard must not vary more than ±30 seconds Crom the associated calibration IWldard. -ETaluatloa P,ocedllft I. ,· 2. 3. Action 1. :2.. Cbec:k raw data (i.e., chromatograms, quantitation lists, etc.) : to verify the recoveries reported on the lntenial Standard Area Summary (Form VlllA, VIIIB). . -Verify that all retention times &0d JS areas are acceptable. Any time then are two am\yses for a partjcuhr fraction., the ,reviewer must determine which are the best data to report. Considerations should include: I L b. c. Magnitude of the 1hifL Holding times. Comparison or the values of the TCL compounds reported in each fnction. Jf an JS area count is outside -509& or +IOCl'l& of the associated standard: L Positive raults for compounds quantitated asing that IS are flagged as fflimated (J) for that sample fraction. i b. Noa-det«ts for compounds quantitated ming that 1S are flagged "'ith the sample quantitation limit classified as estimated i (UJ) for that ample fraction. c. IC extremely low area counts are reported, or if performance exhibits a major abrupt drop-off, then a severe loss of sensitivity is indicated. Noa-detects should then be flagged as 1111usable (R). ,-. -.• . 1: .., I . .. tr an 1S retention time nries by more than 30 seconds, the ·chromatographic profile for that sample must be eumiaed to determine iC any false positives or 11 2/18
·I ,_I I A. B. C. negatives exist. For shifts of -a large a,,agnitude, the reviewer may consider partial or total rejection of the data for that sample fraction. IX. Tn CQMfOVND IDtNTlflCAJJQN Ob)ectin ne ob~ of the cri1er.ia for GC/MS qualiw.ive analysis is to minimize the number of erTDneous identif,catiom of c,ompounds. All em:,neous identification can either be a false positive (reporting a compound pres eel 111•),ea it, is not) or a false negative (not reporting a compound that is present). ~ The identification criteria can be applied m'IICh more easily in detecting false positives than false negatives. More information is available due to the requirement for aubminal of data SIIPl)Orting positive identifications. Negatives, or 1non-detected compounds, ou the other hand represent u ~nee of data llld are, therefore, much more di(ficult to assess. 'Criteria 1. 2. Compound must be withiJI ;t0.06 relative retention time (RRT) units or the standard RRT. Mass spectra or the sample compound and a current laboratory-generated standard must match according to the following criteria: a. b. C. All ions present in the sta.11dard mass spectrUm at a relative intemity greater than 10% lllllll be present in the sample s~m: i I The relative intensities or ions specified above must agree within ±20% between the sta.Ddard and sample spectra. (Example: For an ion with an abundance or 50% in the standard spectrum, the 'corresponding ample ion abudance must be between 30% and 70%.) I I Ions greater than 10% in the sample spectrum but not present in the 1t1.ndard spednlm must be considered and accounted for. ' Euludoa Plw:mre 1. Oect that the RRT of reported compounds is within 0.06 RRT units of the ffltra>Ce Sta.Ddard. / 2. Oleck the laboratory lta!ldard spectr. vs. the sample compound ipectra. 3. I The reviewer should be aware of situations (e.g., high concentration samples preceding low concentration samples) when 11mple carry-over is a possibility and should use judgment to determine if instrument cross-conllUllination bu affected any positive compound identification. ·...:.. ' 19 2/18
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D.
A.
B.
C.
D.
Actloa
1.
2.
The application of qualitative criteria for GC/MS a.aalysis of TCL compounds
requires pt"ofessional judgment. lf it is determined that incorrect
idcotifiations were made, all such data should be flagged as .DDl cietec:ted (U)
m -.nasable (R).
Profesriom.J judame-at must be used \0 q,zatifJ the data if it is determined that
• • -A I
C1'0S!-ccm1:arnm11>011 W OCC:U••~·
X. COMJ'OUNJ) OUA"ffiTATION AND R£PORTID nrnmoN Llh{ITS
I
Ohjecthe
The objecti,-e js to e.asure that the reported quantitation results and· CRQLs are
accurate.
,9fte.na
1. Coml)OU!ld quantitation, as well as the adjustment of the CRQL, must be
calculated according to the appropriate SOW.
2.
1.
2.
Compound RRF must be calculated based on the IS specified in the SOW for
that compound. Quantitation must be based on the quanticition ion (m/z)
specified in the SOW. The compound quantitation must be based,on the RRF
from the appropriate daily standard.
I
For all fractions, raw data should be examined to verify the correct calculation
or all sample results reported by the labontory. Quanticition lists,
chromatograms, and sampk preparation log sheets should be compared to the
reported positive sample results and quantitation limits. i
I •
Verify that the correct internal standard, QlWltitation ion, and RRF were med
to quantitate the compound.
3. Verify 1hat 1M CRQLs ba-.e bee.II adjusted to reflect all ample dilutions,
conceatrationi,, splits, clean-up ac:tivities, and dry weight Cacton' that are not
accounted for bJ the ~ '
ActJoa
IC there are any discrepancies found, the laboratory msy be ,contacted by the
designated representative to obtain additional information that could . resoJve any
differences. IC a discrepancy remains unresolved, the reviewer must decide which
value is the best value. Under these c:ircumswices, the reviewer_ IDBY determine
qualification of data is warranted. · '
20 2/18
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XI. ll"iIATIVtL)' IDPffiOtP COMPQl1t:iPS
Object!••
ChromarogMlphic pew in volatile and eemivolatile fn.c:tion an.al~' that are not
target compound list (TCI..) analytes, IWTI)JW:S. or imterual 1widards are potential
tent:atr<ely ~ie.d c:ompound! {TIC). nes mlllt be (lualitatively I identified by
(GC/MS) libnl)· xvd ud t)Je identifications aseswf by the data re-newer.
Criteria
.. •
2.
For each ~le. the labontory must conduct a mass spectral NCPel! er &loe
NBS h"brary IIDd repon 11>.e possible identity for the JO largest :VOA fraction
pcab 11.Dd the 20 lariest BNA fn.c:tion peaks whkh are not surrogate, interual
standard,, or TCL compovn.ch. but whia have area/height greater than 10
percent of the am o{ the -.rest internal nandard. TIC results are reported
for each sample on the Orpnic Analyses D&ta Sheet (Form l, TIC).
~ SOW nvision October 1986 does not &llow the laboratory to report as
tentatively identified campoullds (TICs) any TCL compound which is properly
repo.rud in anolhu fraction. (For example, late eluting 1volatile TCL
compounds must not be reported as BNA llCs.)
Guidelines for tentative identification are IS follows:
L Major ions (gTUter than J()'II, relative intensity) in the reference
1pectnm1 lh2.ILll1 be present in the sample specuum.
b.
C.
d.
e.
r.
Tbe relative intensities of the major ions s'bould agree I within :t:2()'11,
between the sample and the reference ,pec;ba.
Molecular ions present in the reference spectrum should be present in
the sample spectrum.
Ions present in the sample ,pec:trum but not in the reference spectrum
should be reviewed £or possible background contamination,
interference, or coelution of additional TIC or TCL compounds •
• I
When the above criteria are not met, but in the technical judgment of
the data ae+i.ewer or mass spectral interpretation spec:ialist the
identification is eouect, the data reviewer may : report the
identif'JC:lltioD. '
I
If in the data revie-r's judgment the identification is, uncertain or
there are extenuating facton affecting compound identifications, t.'le
TIC result may be reported IS "wllcDown•.
£,..h,atlo ■ Procedare
.. I
l. Cbec:lc the nw data to verify that the laboratory Jw genented a library tearch
for all required peab in the chromatogram1 (Amples and blanks).
21 2/U
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2.
3.
4.
Blank chromatogruns should be cum.iced to verify that TIC peaks present in
samples are not found in blanks. When a low-level non•TCL compound that
is a common artifact or labontory coota.minant is detected in a sample, a
thoroagh check or blank chromatogruns may require looking for peaks which
are less than JO percent or the internal standard height, but present in the
blank chromat01ram at 1imHar relative retention time.
All mas. """"'b• ia every 11mple ud blalllc. must be examined. · •
Sm~ TIC h"bnr/ llQJ'Qles often yield 11nual candidate comi>duods having a
dose matc'hina IQlff, all -ra,onable d>oiees most be consldered. ·
__ ...._ __ The reviewer Jhould be aware of common laboratory artifacts/contaminants
a.nd their sources (aldol prodocu, IOlvent preservatives/reagent contaminants,
etc.). These may be pn:scnt in blanb a.nd 1101 repon.ed as ample TICs. ,
D.
,·
Examples:
L
b.
c.
I
Common 1ab eo11taJnjnanis: CO2 (m/e 44), 1ilounes (m/e 73), diethyl
ether, hexane, certain frCOIU (l,1,2-trichloro-1,2,2-trinuoroethane or
nuoro-trichloromethane), phthalates at levels less than 100 ug/1 or
-1000 Ilg/kg.
Solvent prc$erv&tive.s:: cyclohexene is a 111ethylene chloride preser-
vative. Related by-products include cycloheunone, 'cyclohexenooe,
cyclohexanol, cyclohexeool, chlorocyclohexeoe, chlorocyclohexanol.
I
Aldo! reaction products of acetone include: 4-hydroxy-4-methyl-2-
peotanooe, 4-methyl-2-peoteo-2-ooe, 5,S-dimethyl-2(5H)-furanone.
6. Occasioually, a TCL compound may be identified in the p.loper a.nalytical
fraction by non-target library search procedures, even though it was not found
on the quaotitatioo list. If the total area quaotitatioo method was used, the
reviewer should request that the laboratory recalculate the result using the
proper quantitatioo ion. lo addition, the reviewer should i evaluate other
sample chromatograms a.nd check library reference retention times on
quantitatiou lists to determine whether the false negative result is an isolated
.occm-renc:e or whether data from the entire Case may be affected.
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7. TCL compouuds may be identified in more than one fnctioil.. Verify that
q111Dti11tio1 is made Crom the proper fraction. j
Action
1. An TIC ftSDhs 1boald be (lagged IS tentatively identified with estimated
concentrations {IN).
2. General actions related to the review of TIC results are IS follows:
L
•. • I
If it is determined that a tentative identification -or a JIOn-TCL
compound is not acceptable, the tentative identification .should be
clwlged to "unlcnown• or a.n appropriate identification.: ·1
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4.
5.
6.
8.
b. If all contractually required pew were oot libnu-y surched, the
designated represenative could request these data from the laboratory.
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TIC results which are oot sufficiently above the level in the blank should not
~ reported. (Dilutions and sample aiie 111us1 be talcen into account when
comp&ring the amounts prc:seot in blanks ai,d samples.) ·
1''H11 • C10111po11DC! is 90\ {olllld ill any blanks, bot is a suspected artifal:\ of
CDll1Dl()G bbora1or] coenmivnt. tile n:su.lr. may be flagged as uusable (R).
la decidmg whether a library ~ result for a TIC repr~nts a realistic
idesbf'iat:ia:, profem011111 judgznent must be exercised. If there is IDOre thao
ooe ~h, ~ ffSlllt may be reported as "either compound X or
compound Y." 1f there is a w:k of iso111er specificit-j, the TIC result 111ay be
changed to a oon-apeciiJC DCl!ller result (1,3,S-trimethyl be.ozene to trimethyl
beoune isomer) or to • compound c:las:s (2-inethyJ.. 3➔thyl beoune to
substituted aromatic compound).
The reviewer may elect to report all similar isomen as a total. (AU allwies
may be summarized and reported as total hydrocarbons.)
Olber Case factors may inlhieoce TIC Judgments. If a sample TIC match is
poor but other aami,lu .ban a TIC with a good libnry match, similar relative
retention time and the same ions, identification information may be inferred
fro111 the other sample TIC results.
Physical constants, 111ch as boiling point, may be factored into professional
judgment or TIC results.
XII. S)'STEM PERFORMANCE
During the period following Instrument Performance QC checks (e.g. blanks, tuning,
calibration), changes may occur in the system that degrade the quality of the1data. While this
degradation would not be directly shoWD by QC checks ntil the next required series of
analytical QC ram, n thorough review oC the ongoing data acquisition can yield indicaton of
instn1111e11t perfonzw1ce.
'
Some rnmpli=s of .imtniment perfonzw1ce indicators for YariouS facton are a:s
follows:
I. Abrwi>l. ditcrete shifts ill .-tiuc:ted .011 chnnnatogram (RIC) baseline may
indicate pin or threshold dlaqes.
2.. Poor chromatographic perfol'Jlllllce affects both qualitative ud qoantitative
results. Indications of substandard perfonxwice include: --•;
L
.'.:: I
High RIC baekgn,und leveb or shifts in absolute retention ti111es or intenw
1tanda.rds.
• ' _-....i,~ •
b. Excessive baseline sue at elevated temperature.
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c. utraneow pe2ks.
d. Loss of relOlutioo a.s auggestcd by facton auch a.s non-resolution of 2,4-and
2,S-dinitrotolueoe.
c. fea.k tailuig or peak 1plittin, may result in iaaccurate QIWltitation.
Continued a.n~ytical acti\·ity "W\tb 6,gracled p,tnOl'tDU~ sa~ts laclc 1of attention or
professional experieoce. llaJrd on !he instnmxat perionn.uice indicaton, the data reviewer
must decide if tM 1)'1te1a bas degraded IQ 1lu poinl cf affecting data quality' or validity. lf
data Qualicy cmy bf'!: bee-A afTecled, data JhOQld be qmfiiaed ming the ,n:viewer's best
professional judgment.
XIII. OVIRALL ASStsSMfNT QF DATA FOR A CASE
It is appropriate for the data reviewer to make professional judgments and express
concerns and com.menu on the nlidity of the overall data package for a Case. This is
particul~dy appropriate for Cases in which there are several QC criteria out 'or specification.
The additive nature of QC facton out or specification is difficult to assess; in an objective
manner, but the n:viewe1 bas a n:sponsibility to inform usen con~raing data Quality and
data limiutions in order to assist that user in avoiding iaappropriate use of, the data, while
not precluding any considention or the data at all. The data n:viewer would be greatly
assisted in this eode1.vor if the data quality objectives were provided. i
~1 -::C. ··"'--._ ,-,
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PESTICIDES PROCI:DURE
The requirements to be checked in ~idation are listed below. recs-indicates that
the contra~! requirements for these items will also be checked by CCS; CCS ~uirements are
not always the same as the dats nv.iew criteria.)
L Holding Times (CCS -Lab holding times only)
n. ,....,icidr< rz.so -nt h.fozrm (CCS}
m. Calibration
o hi tial ( CCS)
o Analytical Sequence (CCS)
o Continuing (CCS)
JV. Jlbmks (CCS}
'V. Surrogate ~very
VI. Matrix Spilce/M&trix Spilce Duplicate (CCS)
VII. Field Duplicates
vm. Compound Identification
IX. Compound Quantitation and Reported Detection Lim.its
X. Overall .MSessment of Data for a Case
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B.
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A.
I. HOLDING TI~trs
ObjKthe
The ob~i:tiv~ is t.o '5CUtlin the .-alidity of results wed OD the holding time of the
samp~ from J>rnt of ro!le:;:ticn ., WM or analysis or sample preparation, as
approrr.i:I te.
Criteria
Technical requirements for sample lloldiDg times bave only been estllblisbed for ,...ter
matrices. The holding times for aoils are currently 11.Dder ia¥CStii-12tle11, When the
results are available they will be inc:¢rpora~ into the datll r,ah:ation process. On
October 26, 1984 in Vollll:M '49, Namber 209 of tM Federal Register, page '43266, the
holding time requiremeJUs for pesticides WeR esiablished ll!lder 40 CFR 1)6 (Clean
Water Act). Samtm:S mw:st be extracted within 7 days and the extract must be
analyzed within 40 days. Both samples and extracts must be stored at 4• C.
ETah,alloo Procedare
,il.~al holding times are established b:, comparing sampling date on the EPA Sample
Traffic Report with date.s of analysis and ennction on Form I. Eumille the sample
rec:¢rds to detennine if samples were properly preserved. (I{ there is no indication of
prese~tion, it mwt be assumed that the samples are unpreserved.)
Action
If 40 CFR 136 holding times are exceeded, flag all positive results IS estimated (J)
and sample quantillltion limits IS estimated (UJ) and document to. the effect that
holding times were exceeded.
J.· If holding times are grossly exceeded, either on the fint analysis or upon re-
analysis, the reviewer must use professional judgment to' determine the
reliability of the datll and the effect of additional storage on the sample
nsults. The reviewer may determine non-detect datll are unusable (R).
'
.2. Due to limited information concerning holding times for aoil samples, it is left
to the d.iscreti011 of tu data reviewer to apply water holding time criteria to
soil JamPles.
U. PESTICIDES INSTRUMENT PERFORMANCE
ObJec:tl..e I
These criteria are esublished to ensure that adequate cbromatographic resolution and
instrument sensitivity are achieved by the chromatographic system. nese criteria are
1101 umple specific; conformance is determined asing standard materials. Therefore,
these criteria should be met in all cln;umstances.
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B. Criteria
1.
2.
3.
,· -
DDT Retention Time
DDT must have retention time OD packed columns (except OV-1 llDd OV-10 I)
gn:.a tu ttw, or eqaal ID 12 miD u tes.
Retention Time Windows
The labonitory must ~ retention time window data on tbe Pesticide/PCB
Sta.11dards Siimmary (Form IX) for each GC column used to analyze samples.
DDT ,'Elldrin Degradation Check
The total percent breakdown for neither DDT nor endrin may exceed' 20%.
TM percent brea.kdoWII is tht amoant or decomposition that eni:irin and 4,4'-
DDT l!Ddergo •hen analyzed by the c:hromau>gl'IJ)hic system.
a.
b.
c.
d.
For endriD, the percent breakdown is determined by the presence of
endrin aldehyde and/or endrin ketone in the GC chromatogram.
For 4,4'-DDT, the percent breakdown is determined from the presence
of 4,4'-DDD and/or 4,4'-DDE. in the GC chromatognm. •
A combined percent breakdown must be calculated if th~re is evidence
oC a peak at the retention time of eodrin aldehyde/4,4'-DDD, which
co-elute on the OV-1 packed column (er an equivalent column).
Percent bre.alcdown is calculated using the following equa1tions:
'Mi Breakdown •
for 4,4'-DDT
Total DDT degradation peak area (ODE. + ODD) OO
-----------------·-xi
Total DDT peak area (DDT + ODE + DOD) 1
'
'Mi Breakdown • Degradation halt Areas (endrin aldehyde + ecdria ketone) x 100
for endrin Peak Area (endrin + endrin aldehyde + endric ketone)
Combined •
'lb Breakdown
Nt;,te J;
Note 2:
i
Peale area of endrin aldehyde mast be uieasured during
1he degradation check to verify ayitem performance .
.Eadrin aldehyde is DOI reported OD Formi I because it is
ranoYed by alumica cleanup. I
The tenn 9peak height" may be 111bstitut~ for the term
'"peak area". I
Total degradation peak areas · 1 1
,(DOE + DDD + eadrin aldehyde + eadrin btone)
Total DDT and endrin peak areas·· 1
(DDT+ DDE + DOD + endrin + eadrin aldehyde + eadrin ketone)
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4. DBC Retention Time Check
The retention time or DBC io each a.nalysis must be compared (o the retention
time of DBC in EV11uatioo St1.0dvd Mix A. Tbe Percent Difference (%D)
must 1101 exceed 2.0% for packed col11mlll', 0.3~ for unow~bore capillary
ccl11auu, a.nd LS% if wide-bore c:apilhry colWll!d an IIISed. i
-ll 100
'
• Absolute retention time of dibutylchlortndate in the, initial staodard
(Evaluation SWldard Mix A).
• Absolote retention time of dJcotyk:hlorendate ill the subsequent
analysel.
:ETaluatio11 Pl...:elb.rc
L-Check raw dllta tn verify that DDT relelltioD time is greater than 12 minutes
on the standard d!romatognm and that there is adequate resolution between
peaks.
.
2-Check raw data to verify that retention time windows are reported on Form
IX. and that all pesticide standards are within the establishe'd retention time
willdows.
3.
Acdo■
I
Check raw data to verify that the percent brealcdoWII for/ eDdrin and 4,4'
-DDT, or the combined percent breakdoWII, does not exceed 20'!& in all
Evaluation Standard Mix B analyses oo Form vm D. I
i
Check nw data to verify that the percent difference ill retention time for
dibutylchlorendate in all standards and samples is s. 2.0% fcir packed column
azwysis, s. 0.3'!ii for capillary column analysis, and s. 1.5% for wide-bore
capillary colum11 analysis OD Form VlIJ E.
I. DDT Reteruioa Tmie
'
Jr the 1'CU'lltion time of DDT is less than 12 miDotes (except on OV-1 and
OV-101). a close examination of the chromatography is 11ecessary to ensure
dat adequate sepantion of illdividual components is achieved. If adequate
sepantion is Dot achieved, flag all affected compouod data ~ unusable (R).
Retention T1111e Windows ·• I
R.ete11ti011 time windows are used in qualitative identif"1e1tio£ If the 1tai1dards
do 1101 fall within the retention time windows, the IJSOCiated sample results
should be carefully evaluated. All samples injected after the last jn-cqntroJ
studard are potentially affected.
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3.
a.
b.
For the affected samples, check to see if chromatograms contain any
peaks within a.n expanded window surrounding the expected retention
time window of the pesticide of interest. lf no peaks are! present either
with.in or close to the retention time window of the deviant target
pestie~ compound., there is usually no effect on the: data. {Non-
detected values c:u be considered valid.)
'
If the affe<:ted sample chr01mrogranu contain peaks which may be of
conceni (i.e., abo~ tae CRQL a.nd either close to or within the
e:xpecied re~ntiou time window of the pesticide of interest), then two
options are available ID ~ reviewer to determine the: extent of the
effect on the data.
1) If uo additional effort is wan-anted by the reviewer, flag all
positive resulu and quantitation limits as unusable (R).~ The
JWT11tive should empba.siu the pouibiliry of either false
uegatives or f~ positives, as appropriate.
2) 111 IOIDe cases, additional effort is wan-anted by the reviewer
(e.g., i{ the data an needed on a priority basis and if the
peak(s) pr-esenl might represeut a level or concern for that
particular pesticide). In these sit\llltions, the1 reviewer may
undertalce the following additional efforts to determine a usable
retention time window for affected samples:
(1)
(b)
(c)
(d)
The reviewer should examine the data package for the
presence of three or more ,standards · containing the
pesticide of interest that were run within a 72-hour
period during which the sample was analyud.
If three or more such standards are present, the mean
and standard deviation of the retention time window can
be re-evaluated. I
If all standards and matrix spikes fall within the revised
window, the valid J>O$itive or uegative sample results can
be determined using this window. I
The narrative should identify the addition.al efforts
1aRll by the rev~wa-and the resultant impact on data
IISlbility. In acSdition, the support documentation should
-taia all calcvlatioas and comparisons generated by
the reviewer.
DDT /Endrin Degradation Check
L If DDT breakdown is greater than 20%, begiwng with the samples
following the last jp-controJ standard: ' , . ·•
I) Flag all quantitative results for DDT as estimated (J). If DDT
was not detected, but DOD and DOE are positive, then flag the
quantitation limit for DDT as unusable (R).
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B.
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b.
2) Flag results for DDD and/or DDE a.s presumptively present at
an estim2ted quantity (NJ). :
11' endrin breakdown is greater than 20%:
J)
2)
Fhg all qm.ntitative resula for endrill as estiimted (J). If
eadrin was aot detected, llu1 endrin aldehyde and endrin ketone
are positive, then flag 1lie qwmtitation limit {or endrin as
1miuat,le (R). '
Flar, results {or endrin ketone as presumptively present at an
. estimated quantity (NJ). ·
Retention 'fime Check
L
b.
If the n1entim-time shift (or dibutyk:hlorendate (DBC} is greater than
2.0% for packed col11t1111, greater than 0.3% for narrow-bore capillary
column, or greater than 1.5% for wide-bore capillary column, the
analysis uiay be flagged unusable for that wnple{s) (R), but
qualification of the data is left up to the professional judgment of the
reviewer. 1
The retention time shift cannot be evaluated in the •~nee of DBC.
m. CALJ»RATION
Objecthe
Compliance nquiremena for satisfactory instrument calibration are established to
ensure that the instrument is capable of producing acceptable quantitative data.
Initial calibration demonstrates that the instrument is capable· of acceptable
performance in the beginning, and continuing calibration c:heclcs document
satisfactory mainteDADce and adjustment of die instrument over specific time periods.
I
Criteria
I. lnitw Calibration Linearity Chec:k
'The Perc:ent Relative Standard Deviation (111,RSD) of c:alibrntion factors for
aldrin, endrin, DDT, and dibutylchlorendate must not e:i:ceed I 0%. 11'
10:uphene is identified and quantified, a three-point calibration is required.
If the calibr2tion factor for DDT or 10uphene is outside the 10% RSD
window, calibration auve, must be used for quantitation. of DDT, DOE,
DDD, cw 10upheue. :
Calibration Factor • Tota! Area of Peak
Mass lnjec:ted (ng)
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lli>RSD • 1 JOO
CF
where,
O • $taTM1ard Deviatio11
CT • Mean Callbratio11 Fac:tllr
~ The IO'lii RSI> lillearity checJc is required only for columns whic:h are
used (o, quantitative clet.cnninations. Qua!ltitatio11 of the surrogate
requires the 11st o{ a column lbuto'JI ao a,cet the J()qi, linearity criterion.
Co\umm aed oafy 10 pr,ividc Qmlitative c:oarumation · are not required
to meet this criterion.
2. Analytic:aJ Sequence
...
3.
a. Primary AnalY$is
At die begillning or each 72-hour period all standards must be
'
analyzed.
b. Confirmation Allalysis
1) Evaluation Stalldard Mix A, B, and C are ;required for the
'
curve.
2) Only the atandards containing the compound(s) to be confirmed
are required. These standards must be repeated after every five
samples. ,
3) E.valuatioa Mu B is required after every tea lptes.
Continuing Calibration I
I
Tbe calibnti011 factor for each studard must be within ISC!b'of the standard at
the begillning of die analytic:aJ seque11c:c on quantitation columns (2~ on
confirmation c:olalllJlS).
C. E•alaa6oa Procedure
I. lllitial Calibration
a.
b.
I
lmpect the Patic:ide Evaluatio11 Stand&rds Summary (Form VIII) and
¥erify agreement with the nw GC data (chromatograms and data
system printouu). !-. .-.-
' . I
Cbeck die nw data and rec:alculate some of the calibration facton and
the percent relative ltalldard deviations (%RSD) for aldrin, endrin,
.wr <. I>ec.
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3.
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Actloa
1.
2.
3.
c. Verify that the 'loRSD for the calibration factor of each spe:ifi;
pesticide is less than or equal to 10% for each 72-hour peri,od.
d. Jf errors are detected, more comprehensive recalculation should be
perfonned.
e. lf 10:upbene or tbt DDT serjes -.-as identified and quantitat£d, verify
thi\ r. t'ar«-point ~libr21iou was establi~hed. 1
Verify that all s=dards were &nalyud fa the 72~hour sequence.
Continuing C1libntion
a. Review the pesticide sample data to verify whether the standard was
wed as a Quantita tion standard or as a confirmation standa_rd. ~
I>. For the 11aanti1ation standards, check the nw data to verify the percent
difference ('lbD), using the following formula, for approximately ten
percent of the reponed values by recalculation.
X 100
where,
R1 • Calibration Factor from first analysis
R2 • Calibration Factor from subsequent analysis
•
Initial Calibration
If criteria for linearity are not met, flag all associated quantitative results as
estimated (1). ·
Analytical Sequence
I
If the i,roper standards have not been analyzed, data may be af'fected. The
data ttviewer must use professional judgment to determine severity of the
effect and qualify the data accordingly. I
O:mtinuing Calibration
L If tbe l!bD between cah'"bntion factors is greater thani IS% for the
compound(s) being quantitaled (20% for compounds being confirmed),
flag all associated positive quntirative resutu as estimated (1).
,
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IV. IILASKS
Objecti••
n~ P.<stttl"l''lt or hank anaJysis results is to determine u,e nis1e!ICC: and 1112gnitude
or con1>mimtloci prob!=.. The crileria for •nluation or l>l:allks apply to any blank
associated with the Rm?~-l! proble= wjt}i &Ill. bank uist, all data associated ... ·ith
the Case uiust bt card"IIY evamated u, determii.e w~eT or not tl,ere is a.n inherent
va.ria!n1ity in the data for the Case, or the problem is llll isolated: 0C:':11rrence not
affu:tm1 other data.
Criteria-----
No coutamill3.llts should be present in the bla.nlc(s).
Euluatlo11 Proc:-edarc
1. Review the RDlts of all IS$0Ciated blllllk(s), Form l(s)' ud nw data
(chromato,nms. quutitation reports or data system printouts).
•i Verify tha.t. the method blank analysis(es) contains less thin the Contract
Required Qua.ntitation Liutlts (CRQL) of uy Pesticide/PCB or interfering
peak. '
3. · Verify that method blank analysis has been reponed ~r matrix, per
concentration level, for each GC system med to analyze samples, and for each
extraction batch.
Action in the case of unsuitable blllllk results depends on the circumstances ud the
origin of the blank. No positive sample results should be reponed unless the
concentration of the compound in the sample exceeds S times the amount in the
blanlc.. In instances where more than one blank is associated with 1a given sample,
qualification should be based upon a comparison with the associated blank having the
highest concentration or a c:ontamillllllL The results must J2l2l be corrected by
subtracting the bwik value. Specific actions are as follows: I
1. If a Pesticide/PCB is found in the blank but J2l2l found in the sample(s), no.
action is taken.
1
I
2. Any P~ide/PCB detected ill the lll!llple ud also detected in any associated
lilaok, must be qualii,ed when the llllllple concentration is less than S ti.mes
t.be Wank concentratiou.
The reviewer should note that the blank analyses may not involve the same
weights, volumes or dilution facton as the associated samples. These facton
must be taken into consideration when applying the Sx criteria. such that a
comparison of the total amount of contamination is actually made. .
'
Additionally, there may be instances where little or 110 contamination was
11resent in the associated blllllks, but qualification of the san\ple ..as deemed
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necessary. Contamination introduced through dilution water is I one example.
Although it is not always l)O$Sible to determine, i.Dsta.Dces of this'OCturring can
be detected wben contam.i!WllS are found in the diluted sample result, but
absent in the undiluted sample result. Sin~ both results are I not routinely
reported, it 111J1Y be impossible to verify UW source of contamination.
Howe;'<u, if tbe reviewer deteT11l.ines that tbe c:onamwtioa is Crom a source
other lban the aamp\e, k/lbt $bculd qwwfy the data. la this case, the .Sx rule
does 110t applr; the .sample nlue should be reported as a noa-detecL
The folluwi.D.1 are eu.mples of applying the bluk qualifieatioa guidelines.
CemiA cirrumst11res 'IIIIY wwrut deviations Crom these auidelines.
1,,[.ii,n,~e.~l·----""'-•mwple nsult is greater tha.a the CRQL, but is less tha.a the
Ose 2:
required amount (.Sx) from the blank resulL
Blank Result
CRQL
Sample Result
Qualified Sample Result
a
1.0
.5
4.0
4.0U
In this case, sample results less tha.a .S.0 (or .S :a: 1.0) would be
qualified as DOD-detects.
Sample result is ,1reater than the required amount (Sx) Crom the
blank teSIIIL !
B\aak Result
CRQL
Sample Result
Qualified Sample Result
V. SURROGATE RECQYEBY
., a
1.0
.5
6.0
6.0
Objecd.e ,.
1.aboratOT}' perf'onnance on individual samples is established by means of spiking
activities. All samples are apibd wida a sun-ogate compound prior to sample
prepanti011. Tbe ~uatioa ol die .resalts of these surrogate spikes is not necessarily
straightforward. 'J1oe sample itself 111&y produce effects due to 1uc:h Cac:ton as
interferenc:a ud hi&b conc:entntions of rnalytes. Since the effects of the sample
matrix are frequently outside the control of the labontory and may present relatively
unique problems, the review and validation of data based on specific: ample mults is
frequently subjective and demands analytic:al experience and professional jlidgmeoL
Accordingly, this IOttion consists primarily of 1uidelilles, lo some .c:nses with several
optional approac:bes 111uested. · · · . ' :.!
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B. Crlttrla
Sample aod blaok recoveries or dibutylchloreodate must be withio I limits as per
applicable SOW (Form II).
C. Euludo. P,uudun
D.
A.
B.
1.
2.
Action
Checl<. nw datt (i.e~ chromatograms, qua.nt list, etc.) to verify; the recoveries
oo ~ SDTTO&:ltr 1lec:oven (Form U).
lf ncoverlC:$ tn not "Within limits, check raw data for possible interferences
which may hive affected surrogate recoveries. '
If pesticide surrogate recoveries are ou~ of advisory windows, the following
guidance is saggested:
1. If lo~ recoveries are obtained, flag associated positive results and quantitation
limits as estimated (J).
3.
If high recoveries are obtained, professional judgment
determine appropriate action. A high bias may be
interferences.
should be used to
due to co-eluting
I
U zen, pesticide nrrogate recovery is reported, the reviewer should enmine
the sample chromatogram to determine if the surrogate may be present, but
alightly outside its retention time window. If this is the c:asei in addition to
assessing surrogate recovery for quantitttive bias, the overriding consideration
is to investigate the qualitative validity of the analysis. If the surrogate is DOI
present, flag all negative results as unusable (R).
VI. MAJJUX SPITT/MATRIX SPIKE DUPLICATE
ObJecd•e
These dala are pnen~ to determine long-term precision and ~ccuracy of the
analytical method on various matrices. These data &J.gnt c:anuot be used to evaluate
the pre · ••• ud accuracy of individual ~-I
Criteria
J.
2..
Advisory limits are established for spike recovery limits in i the appropriate
sow and OD Form m. ,i· 1
Advisory limits are established for relative percent differen~ betwee~ matrix
spike and matrix spike dupl.icate recoveries in the appropriate SOW and on
Form Ill. , '
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D.
A.
B.
C.
D.
E.aluatioa Procedure
lmpect results fer the Ma.trix Spike/Matrix Spike Duplicate Recovery (Ferm
III).
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2. Verify~ (roe n,. dat& IUld veri(y c:alclllatiom.
Ne act.ion is talcen on Matrix Spike/Matrix Spike Duplicate (MS/MSD), data wn: to
qu~ify an entire Case. However, IISUII informed professional judgment, the data
reviewer may me the matrb. spike and matrix 11)\kc duplicate results in conjunction
with other QC criteria and determine the n~acaticn ofithe data.
The data reviewer should first try to determine ID what extent the results of the
MS/MSD affect the wociatM data. This de!Uminaticn should be made with regard
to the MS/MSD ample itself as wen as specific a.nalytes for all aamples asscciated
with the MS/MSD.
In these instaD0CI wberr it can be determined that the results of the MS/MSD affect
on_ty the sample spiked., then qmlification should be limited ID this , sample alone.
However, i:t may be determined through the MS/MSD results that a lab is having a
systematic problem in the analysis or one or more analytes, which affects all
associated sampk:L. '
VD. DttP DUPttCATIS
ObJectlYe '
Field duplicate samples may be taken and analyud as an indicabcn of overall
precision. These analyses measure both field and lab precision; there(cre, the results
may have mere variability than lab duplicates which measure only lab performance.
It is also expected that soil duplicate results will have a greater variance th.an water
uatrices due to difficulties associated with collecting identical field a.mples.
Criteria
There are ao apeci{°Mo 1eoiew cri1eria for field dvpl.icate analyses comparability.
I
l:Yaluatl• Proce4ffa
Samples which are field duplicates should be identified asing EPA 1Sample Traffic
Reports or sample field sheets. The reviewer should compare the results reported for
each sample and calculate the Relative Percent Difference (RPO). -
Actloa
.. ~ . ,.e:.
I -·~
. Any evaluation of the field duplicates ahoald be provided with; the reviewer'•
comments.
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B.
YIU. CQ"f POUND IDEZ:.TiflCATIO"i
ObJrc:tl.e
Qualiatin c:rill'ria for comz,ound ideutuJC&tiOD have been established 10 min.imize the
number of en-oaeous ide.otificatiolls of compounds. An erroneous ideilti(ication can
eitlle-r be a fee posjtive (repcw1iJig • compoUDO pnsent ""beu it is ~ot) or • false
11eptive (IJOf reportmg ■ CDtDpom,4 tli&t .is present).
Criteria
1. Retention times of reported compomids mmt f■ll ""ithin
retention time "".iudoWJ for the two chromatDgnpbk colWllllS.
the c:alc•..,,t,.atsc.e ... d--
2. GC/MS conrumatiou is required if the concentration of a compound exceeds
10 ng/uL in the imal sample extract.
C. Enluatloa Procedare
2.
3.
D. A.ctloa
1.
2.
~ Form I, the ■ssocia~ n"" data (chromatograms and data syitem
l)rintoats) ■Dd the Pesticide/PCB Identification Summary (Form :X). Con.firm
n,paned positive de~. ming •ppropriate retention times and retention time
windows, and verify that the compounds listed IS "aot detected" mre correct.
I
Verify that positive identifications have dissimilar column analysis. (The 3%
OV-1 column caDllot be used for confirmation if both dieldr.iu 11111d DDE are
identified.)
For multipcak pesticides (chlordane and toupbene) and PCBs,' the retention
times and relative peak height ntios of major component pealcs should be
compared against the appropriate standard chromatograms.
I
Verify that GC/MS confirmation was performed for pesticides/PCB
CODCeDtntions in the final sample extract which exceeded 10 11g/¥L.
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If the qu■litative criteria for two-colu11111 coniirmation were I not met, a.II
reported positive de1ects should be considered non-detects. The reviewer
should use professional jud&,me.Dt ta assign aa appropriate quantitation limit
ming the followin& 111icbace: '
L Jf the misidentified peak -safTJciently outside the target pesticide
retntioe time window, then the CRQL can be reported. ;
II. If the misidentified peak poses aa interference with potential detection
or a target peak, then the reported value should be considered aad
flagged IS the estimated quantitation limit (UJ). ,_ · ~---~.
If PCBs or multipealt pesticides exhibit marginal pattern-matching quality,
professional judgment should be v.sed to establish whether the differences are
attributable to environmental "weathering". If the presence or •
37 2/18
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3.
PCB/multipeak pesticide is strongly suggested, results should be reported LS
presumptively present (N).
Jf a.a ~rved pattern ckuly matches more \he one Aroclor, professional
_j,ocigma:.t shoo!d be med to ~ whc\bet the 11eishboring Ar~lor is a better
mau:h., 0t i! .->llti;>k Au:,c:loa an preseziL · ·
If GC/MS confiruufion 1"'&! ,equine but not performed, the reviewer should
notify the DPO.
IX. COMPOUND QUANTJTATIQN AND Bt?PBUP J>IDOJQN LIMIT$
ObJecttre
The objcane .is to earme that the reported qmntitation results and CRQLs are
ac:c:unite.
Compound qu&ntitation, as well LS the adjustment of the CRQL, must be calculated
ac:cordiag to the appropriate SOW. ',
EnJ11atlo11 Proc:ed11re
I. Raw data should be eumined to verify the correct 'calculation of all sample
results reported by the laboratory. Quantiution reports, chromatograms, and
sample preparation log sheets should be compared to the reported positive
sample results and quantitation limits.
i Verify that the CRQLs have been adjusted to reflect all sample dilutions,
conc:entntions, spins, clean-up activities, and dry weight factors that are not
accounted for by the melhod.
Actloa
Quantitation limits affected by Jarse, orr-scale peaks should be flagged as unusable
(R). If the interference is on-scale, the reviewer ca!l provide an ·, estimated
quantltatlon limit (UJ) for each affected compound. :
~ ~peaJ, pesric:ide results c:u be dlec:lc.ed for ~ugh agreemen~ between
quanti~ulu obcaiaed 011 die rwo GC columns. The reviewer should use
professional judgment to decide whether a much Jarser concentration obtained on one
column versus the other indicates the presence or an interfering compoun~. If an
interfering compound is indicated, the lower of the two values should be reported and
qualified as presumptively present at an estimated quantity (NJ). Tlais necessitates a
determination or an estimated concentration on the comumation column. The
urrative should indicate that the presence of interferences has obscured the attempt
at a aecond colu..mn comumatlon. ·
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X. QYtRALL ASStSSMtfil Of DATA £QB A CAS!
It is a;,;>ro;,riate (ar tbe data rev.iewer to make professional judgments a.nd express
concerns and COIDJMnt:. OD u,~ nli,djry of die ovuall data package for a ,Ca.se. This is
particularly a.ppropri:l!e (CT Casa s ~'\id, U>eR an 11ewn! QC criteria out of specification.
The additi'le nature of QC faeton out of ~~ ~ diffi::ult to 1-SSelS i.n a.n objective
manner, but tht reviewer w • responsibility to inform 'GSelS concerning dau quality a.nd
data limitatiom in order to asus1 th.at wer in avoiding inappropriate we of the data, while
not precludin& any com:wen.tioa ol tM clall at all lbe data reviewer would be greatly
assisted in th.is endeavor if the mta quality objec:tives weze provided.
.-.
. '
2/18
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GLOSSARY A
Data Qlaallfler DeO■ltloa,
For the pu~es of tha doaunea! tm folliowiD& cock ldten ad associated. definitions are
provided.
U -The materw was ana.l:,=d for, but was DOI detected. The associated
numerical value is the sample quantitation limit.
J -Tbe associated n'U!!lerical YPl11e i, an estimated quantity.
'
R -Tbe data are unusable (compoUDd may or may not be present). Resampling
N
NJ
.-.
and nanalysi.s is ftecesnry fen: ~ac:ation.
-Presu:mptiyt evidence of presence of material.
-Presumptive ~videnc:e or the presence of the material 11t an estimated
quantity. ·
UJ -The material 'W1IS analyzed for, b11t was not detected. The sample
quantitation limit is an estimated quantity.
The reviewer may detennine that qualifien other than those used in this doc11ment are
necessary to de.scribe or qualify the data. In these instances, it is the respo11Sibility of each
Region to thoroughly document/explain the qualifien med. '
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BFB
BNA
Case
GLOSSARY B
Other Tcr1111
llromoOIIMObe!!ZeDt -~ tamllg ~
Base/Neutral/ Ac)d CQmpouads -comJ)Olm(b ualyi.ed by semivolatile technique
A finite, usually predetermined number of wnples collected over a given time
period for a particular site. A c::ase consisu of one or more Sample Delivery
Grou;,(s).
'
CCC Calibration Cbeck CQml)OllJld
cc:::s
CF
CRQL'
DTTPP
DPO
EICP
GC/EC
GC/MS
GPC
IS
MS/MSD
'fJI/%
<:oatract Compliance Scnening -process in which SMO inspects 'analytical data
for contnctllal complianc:,e and provides RSults to the Regions, laboratories and
EMSL/LV.
,
Calibration Factor
Contract Required Qaantitstion Limit
Decafluorotrjphenylphosphine -semivolatile tuning com'pound ,
Deputy Project Officer
E.xtncted Ion Current Profile
Gas Chromatography/Electton Capture Deteetor
Gas Chromatograph/M&Ss Spectrometer
Gel Permeation Chromatography -A ~pie clean-up techniqub that separates
compounds by size and molecular weighL Generally used to remove oily
materials from sample extncts. I
I
Jnta11al Standards -Compo11nds added to every VOA and BNA standard, blank,
~.ix spike dupl.ic:ale, ud aample extract at a known concentration, prior to
inst, moe..ial amlym. la8!rml ltlDdards are used as the basis for quantitation
or the target compoimck. !
Matru Spike/Matrix Spike Duplicate
The ratio or= (m) to charge (:r.) or ions measured by GC/MS 1
OADS Organic Analysis Data Sheet (Form I) -. ' I
. ·~ -~ .. )
PCB Polychlorimted bii,henyl
,;.< I
PE Sample Performance Evaluation Sample
2/SS
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Primary
Analysu
QA
QC
RJC
.RPD
R.RF
100=
RRT
RSD
RT
SDG·
SMO
SOP
. -•
One or two types or pesticide/PCB analysu by GC/EC techniques, the other
t,eiog confirmation analysis. If the two analysei; are run at se~te times, the
primary analysis is the {int analysu chronologically, and is used to ~tabluh the
tentative identificatioD o( any P=ticid~/PCBs deteeted. The identification is
then confirmed in lhe ccminnalioD aaa1ysis.. If the two analyses are done
titllulcuieoasly, eitloer may be CIICrideted tJit primary analysis. Either may be
used for quantitation if contract c:riteria are meL '
Quuiry ~W"Lllce • Total prosnm for assuring the rdi&bility of d.ata.
'
Quality Control -Routine application of procedures £or c::ontrol!ing the
monitoring proce.ss.
.Reconstructed Ion Chromatognm
JularM ~m Diffuence (betwee11 matrix spike and matrix spike duplicate)
Relative RespollSC Factor
Average Relative Respo11SC Factor
Relative Retention T11De (with relation to internal standard)
Relative Standard Deviation
Retention Time
I
Sample Delivery Gronp -Defined by 011e or the fotiowing, whichever =rs
'
first I
o Case or field samples
o Each 20 field samples :within • Case
o Each 14-day calendar period during which field samples 'in • Cue are
received, beginning with receipt or the first sample in the SDG. (For VOA
contracts, the calendar period is 7-day.) ·
Sample Management Office
Standard Operating Procedure
SOW Statement or Work
SPCC
sv
TCL
TIC
VOA
System hrformance Check Compound
Semivolatile analysis -Metaod based on aaalysis by OC/MS fo~ BNA organic
eompoun~ I
I
Target Compound List .
•• •• I
Tentatively Identified Compound -A compound not on the TCL:
Volatile Organic Analysis -Method based on the purge and tni, technique for
organic compound analysis.
42 2/18
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VTSR
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Validated Time of Sample Receipt -rune of sample receipt at the laboratory as
recorded on the shipper'• delivery rec:eipt u.d Sample Traffic Report.
~d Deviatioa Estimate (of I AJDple)
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LA~URATURY DATA VALIOATIUN
t'UNC:TlUNAL GUIDELINES FOR t:VALUATlUN INURGANICis ANALYSt::S
Uniteo States ~nvironmental Protection A~ency·
Ottice of ~rnergency ano Remedial Response
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Table of Contents
section
Title Page
Table of Contents
Introduction
Responsibilities of Key Individuals/Offices
Communication System
Preliminary Review
Procedure
I. Sample Holding Times
II. Calibration
A. Initial Calibration, Calibration
verification
B. Continuing Calibration Verification
III. Blanks
IV. ICP Interterence Check Sample Analysis
v. Laboratory Control Sample Results
VI. Specific Sample Results
A. Duplicate Sample Analysis
~. Spiked sample Analysis
C. t'urnace AA OC Analysis
D. ICP OC Analysis
E. Sample Result Verification
VII. Field and Other OC
VIII. Quarterly Verificat{on of Instrument Parameters
Report
IX. overall Assessment of Data for a Case
Appendix I
Appendix II
Apenndix III
Appendix IV
Appendix V
Appendix VI
Glossary
Contract Required Deliverables
Contract Required Detection Limits
Spiking Levels for Spiked Sample Analysis
Furnace Atomic Absorption Analysis Scheme
CLP Telephone Record Log/DPO C0111rnunication'
summary
Regional DPU List/Report Distribution
Addresses
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13
16
16
19
22
25
30
33
33
37
40
45
46
51
53
54
55
64
66
67
68
70
72
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LABORATORY DATA VALIDATION
FUNCTIONAL GUIDELINES FOR EVALUATIN~ INORGANICS ANALYSES
'
Introduction
This document is designed to offer guicance in laboratory
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data evaluation and validation, In aome aspects, it is equivalent
to a Standard Operatin~ Procedure (SOP) in other, ■ore subjective
areas, only general ~uidance is offered due to the complexities
'
and uniqueness of data relative to specific samples,
Those areas where specific SOPs are possible are pri~arily
areas in which definitive performance reQuirements are e~tablished,
These requirements are concerned with specifications that are not
sam~le dependent; they specify performance requirements ~n matters
that should be fully under a laboratory's control. These specific
areas include laboratory preparation blanks, calibration standarcs,
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calibration verification standards, laboratory control standards
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and interference check stancards, Failure to meet the contract
performance requirements warrants that corrective action·be taken
by the laboratory,
At times, there may be an urgent need to use data which do not
meet all contract requirements. Any decision to utilize; data for
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which non-sample specific criteria have not been met is strictly
to facilitate the progress of projects requiring the av~ilability
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of the data and such decisions should be clearly noted o,n the
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summary review form, Use of this data does .nEl constitute
acceptance (contractually) of the data nor does ~t release the
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contractor from the obli~ation to perform as per the terms of
the contract. A contract laboratory submitting data which is out
of specification may .be required to -re-run or resubmit d'ata. The
only exception to this is in the area of requirements for indivi-
dual sample analysis1 if the nature of the sample itsel~ limits
the attainment of specifications, appropriate allowances, must be
made. An overriding concern of the Agency is to preven~ non-sample
'
specific data validation requirements from adversely affecting
overall data valiOation activities. There is ultimatel~ no
justification for noncompliance on requirements for performance
relative to such areas as blanks, calibration and performance
verification standards: data validation activities shoul.O only be
concerned with subJects requiring professional juO~ment ,on
indivioual sample results.
I
With these concepts in mind, this Guideline is des~gned to
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permit structured data review, and to include automateo:data
,. I
checkout procedures when such capabilities are available. '
ObJective, unambiguous requirements are easily and efficiently
I
rele~ated to personnel other than experienced professionals and
to automated procedures for verification of compliance with
requirements. To this end, the guideline is arranged in order,
with the most objective, atrai~httorward validation elements
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given first.
Responsibilities of Key Individuals/Offices
The data reviewer is a critical link in the chain of people
and events involved in the collection, analysis, and interpreta-
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tion of Superfund environmental measurement. The ■uccess, useful-
ness, and validity of the data review depends on the technical
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expertise ot the data reviewer and communication with othe.r key
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individuals. Although each Region is ■et up somewhat ditferently
from an organizational point of view, the following individuals/
offices should be known to the reviewer:
(ll National Program Office (NPO)
(21 National Program Manager (NPMI
(3) CLP QA Officer (QAO)
(41 ProJect Otficer (POI
(51 Sample Management Office (SHO)
(61 Deputy Project Officer (DPOI
(71 Regional Sample Control Center (RSCC)
(8) on-Scene Coordinator (OSCI
Each of the above is responsible for a particular set of
functions related to sampling, analysis and/or management of
I
the CLP. The data reviewer should be aware of the respo~sibilities
of each in order to ensure effective col'l1lllunication. The' following
hiyhlights the responsibilities and authorities of each of the
above and includes the type: of information likel~ to be ,communicated
to and from the data reviewer.
( l I National ProQram Office (NPOI I
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The CLP is directed by the National Proyram Office l(NPO), in
EPA Headquarter'& Analytical Support Branch (ASB), Hazardous
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Response Support Division (HRSD), Office of Emergency arid Remedial
Response (OERR), in Washington, D.C. The NPO is comprised of the
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National Program Manager, Organic and Inorganic Technical Officers,
and a oualitt Assurance Officer, who also provides OA support to
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the OERR.
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NPO responsibilities include: overall aanagement of the
CLP in terms of vroyram objectives, expansion ana interface
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with clients and other groups; policy and bud~et fol"lllation-and
implementation; administration of analytical and aupport,
I
contracts; development and technical review of analytical,
protocols; review of analytical special services aubcontracts and
CLP generatea laboratory data; development of CLP analytical
and support services contracts; monitoring and formal evaiuation
of analytical and support contractors; and in direction of CLP
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quality assurance (QA) in coordination with overall OERR bA
activities.
(2) The National Program Manager (NPMl, in addition to
directing pro\dram staff, is responsible tor the formulation of
program policies and direction; communicates with the Re11:ional
and Ayenc:r communities on a continuing basis, keeping all
parties apprised of program ,.activities and receiving input on
program effectiveness; administers several program suppott ' I
contracts; and handles financial and contractual aspects !of the
pro1,1ram.
The National Program Manager is responsible for the'
I
overall success of CLP operations, identifying ~uperfund
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analytical requirements, and establishing Program object~ves to
meet the analytical requirements. POs and DPOs assist the
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Program Manager in achieving Pro11ram objectives and aanaging
the CLP on a day-to-day basis. Program issues which cannot be
resolved by the POs, or which arise between the Pos and DPOs
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will be referred to the NPM for resolution.
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( 3)
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The OU ■lity Asaurance (OA) Offi~?" coordinates all ,aspects
of pro~ram application of QA procedure&._ The QA Officer: work&
closely with EPA Headquarter' s Off ice of Reaearch and De:v~lopment
(ORD) and the ORD's Environmental Monitoring Systems Laboratory
in Las Vegas (EMSL/LV) which provides QA ■upport to the CLP.
The QA Officer also coordinate& with the POs and EMSL/LV in
refininy and updating analytical method QA procedures.
(4) The Organics and Inorganics Technical Officers serve as
Project Officers (POs) on laboratory analttical contracts. The
POs are responsible for technical program decisions, contract
administration, and contractor performance evaluation. The POs
work closely with the Regional Deputy Project Officers (DPOs)
and laboratories on a daily basis in re&olviny technical
issues,
I
The POs direct the ongoing effort to improve contract
languaye and analytical methodologies, and conduct technical
caucuses for purposes of CLP data and protocol review. :
The Pos have primary responsibility for all administrative
,
I
aspects of contract formation and procurement, and will
administer all CLP contracts on a Program level,
The PO is responsible for the followin~ activities,
1)
2)
:?>
4)
S)
6)
Definin~ the Government's requirements and initiating
the procurement process by developing appropriate
procurement packages. !
Technical and programmatic evaluation of laboratories
for possible contract award. I
Award of contract. ·
Implementation of contract modifications and ~hange
orders.
Resolution of Program level issues between Regions.
Resolution of issues between DPOs and contract labora-
tories.
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7) Certification of invoice vouchers for 85\ prC>Qresa payment,
8) Evaluation of collective laboratort performance,
9) Recommending to the Contracting Officer that sanctions be
imposed for laboratory non-compliance or non-performance,
10) Other tasks normally performed by ProJect Officvs.
(5) Sample Management Office (SMO)
The contractor-operated Sample Management Office functions
in direct support of the NPO, providing management, operations,
and administrative support to the CLP, The primary objective
of the SMO operation is to facilitate optimal use of program
'
analytical resources. SMO activities fall into the following
areas: (1) sample scheduling and tracking; (2) Special analy-
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tical services (SAS) subcontracting: (3) laboratory invo~ce pro-
cessing: (4) maintenance of CLP recoras and management reportiny:
and(~) NPO management and administrative support.
SMO routinely receives analytical requests from the' Regions,
coorainates and schedules sample analyses, tracks sample; shipment
and analyses, receives and checks data for completeness,; and
maintains a repository ot s'ampling records and program data. In
response to client requests for non-routine types of ana~yses,
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SMO subcontracts for SAS, performing scheduling and tracking for
SAS efforts as outlined above. SMU maintains a comprehe,nsive
data base of CLP services, performance and utilization, ~nd
yenerates a variety of management and user reports.
(6) Contract Deputy Project Officers
In January 1984, Regional Administrators appointed a CLP
technical Deputy ProJect Ofticer (DPO) for each Regional: office.
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Under direction ~f the NPO, the Regional DPO assumes a I portion of
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the responsibility for monitoring the laboratory contractors
physically located in the Region.
DPOs will have overall responsibility for ■onitoring'the
cay-to-cay technical performance of assigned laboratories, for
'
improving that performance where necessary, and for resolving
issues between clients and laboratories, If contract requirements
are unclear, or if the issue involves Program policy or CLP
'
laboratories as a whole, then a coordinated response will,need to
'
be developed through NPO and DPO consultations. In general, DPU
responsibilities are specific to contracts, protocols, and
laboratories and.are related to ensurin11 the successful performance
of the laboratories under his/her jurisdiction. More specifically,
DPOs have responsibility for:
1)
3)
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Participation in audits of laboratories within his/her
Region.
i
Recommending contract changes. Recommendations ot t.echn ical
contract modifications~·
Monitoring contractual terms and conditions.
Resolution of issues between CLP clients and the laboratories
within his/her Re11ion.
Evaluation of inaividual laboratory performance within
his/her Re11ion.
1
Recommending to POs that sanctions be imposed on laboratories
tor non-compliance or non-performance. 1
POs' and DPOs' roles will overlap in areas requiring inter-
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pretation of contract language or resolution of conflicting
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contractual reyuirements, and in the imposition of laboratory
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sanctions such as recommendations of non-payment for
non-performance. There will be a cooperative eftort between the
POs and DPOs when the settling of individual issues will'
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reflect cnanges that will benefit the entire CLP.
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It will be the data reviewer's prero<;1ative and resp6nsibility
to notify the Regional Deputy Project Officer (DPO) conc~rning
problems and shortcomings vi th regard to laboratory data. -If
manaatory actions are required, they should be specifically
noted on the DPO Action Report. This form should also~ used to
note overall deficiencies reQuiring attention as well as1 c0111111ents
on general lab performance and any discernible trends in the
quality of data. It is recommended that the DPO be noti'fied of
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all problems and requirements for a case at one time. If there
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is an ur.ient requirement, the DPO may be contacted by phone to
expedite corrective action. However, it is appropriate Ito submit
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a Data Review Summary in any event to provide documentat;ion of
the Data Review,
(7) Regional Sample Control Centers (RSCC)
In January 191!4,
&ample Control Center
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each Region established a Regional
to centralize ordering of CLP samJle
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analyses within the Reyion. The RSCC is comprised of t~ree or
more indiviauals designated as CLP Authorized Requestors, with
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one individual named as the Primary Authorized Requestot (AR)
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directin~ the RSCC, The RSCC is responsible for coordinating
the level of Regional sampling activities to correspond,with
monthly allocations of CLP analyses. The Primary AR makes final
determinations reyarding Regional analysis priorities when
con~licts occur. RS~C ARs routinely place all Reyional,
requests for CLP analyses, coordinate with SMO during sam~ling
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and sample shipment, and resolve any problems which aria~
concerning the samples •. The RSCC serves as the central point
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of contact for questions concerning Regional sampling efforts.
(8) Un-Scene Coordinator
This individual may have various titles (e.g., On-Site Team
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Leader) but, whatever the title, the person is primarily,
responsible for the sampling effort.
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This person is a good
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source of information related to the sample collection ( i.e.,
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identity of blanks, duplicates, etc.).
Communication System
~everal communication networks and links have been,
established to assist in the transfer of information to ,the
appropriate individual. Data reviewers should be aware :of
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these links and utilize the procedures as is appropriat~ to the
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issue at hand.
(1) Regional/Laboratory Communciation System
In Janua'ry 1983, the NPO established a S/Stem of ailrect
communication between the Re11ions and contract laboratori1es as
a routine methoa for Regional data review staff to obtain
answers to technical questions concerning program data Jn the
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timeliest and most direct manner possible. In this ·•ysiem,
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desi11nated Re11ional communication contacts call designated
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laboratory communication contacts as needed to resolve technical
data question~. This communication link also benefits the
laboratory by providing direct feedback on its data product.
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Issues warrantin~ further investigation by the reviewer correspond
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to areas where the contract reQuirements were not met, une~plained
discrepancies between report forms and raw data exist or·..tiere
analytical problems and/or concerns were discovered in a case.
Reviewers are reminded of the ground rules for this system:
o Regional contact of laboratories is permissible ~nly after
laboratory data submission.
o Regions may contact laboratories with technical or format
questions on the final data packa~e only.
o All logistical Questions involving data delivery, contrac-
tual requirements, procedural recoffll1\endations, and other
general matters continue to be referred to SHU or Proyram
management (i.e., DPO), as a~propriate.
o only authorized Regional personnel may contact laboratories,
and they may contact only the specified laborato'ry
personnel. '
o All conversations between the Regions and the laboratories
·are recorded by both laboratory and Regional contacts on
. the CLP Telephone Record Log (Appendix V).
o one copy of each Telephone Recore Log is forwarded by the
Region and the laboratory to SMO on a weekly basis, and
becomes part of tne Case Fi le Record. !
o similarly, a copy of the Telephone Record Log is. forwarded
by the Region to the laboratory for their information,
and the laboratory forwards an intormation copy
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1to the
Region.
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(2) DPO Communication System
similar to the above, DPO communications with POs, 'labs,
SHO, and data reviewers are documented utilizing the form shown
in Appendix v. The DPO receives numerous reports from SMO and
EMSL-LV. Those which relate directly and specifically to data
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review will be torwarded to reviewers as appropriate (i.e.,
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Quarterly Verification of Instrument Parameters Report)~ The
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DPOs will also provide updates to protocols as they are received.
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Inter-Regional questions or problems with laboratory
performances are referred to DPOs for resolution. For instance,
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it Region V data reviewers uncovered a possible contamination
problem in a laboratory assigned to Re~ion II, the problem is
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first referred to the Region V DPO w.ho then contacts the. DPO in
Region II.
(3) Report distribution (See Appendix VI for addresses)
A copy of each data review should be sent to:
Duane Geuder, QAO
kOSS Robeson, EM~L-LV
DPO for the laboratory
Preliminary Review
In order to use this document eftectively, the reviewer 1should
have a general overview of the case at hand. The exact number
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of samples, their assigned traffic report and laboratory numbers,
their matrix, and concentration level, the identity of any tield
QC samples (blanks, duplicates, spikes, s1,>l its, performance
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auoit samples), sampling dates and the number ot labs involved
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for their analysis are essential information. Background informa-
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tion on the site is helpful but oftentimes it is very ditficult
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to locate. The site project officer is the best source\for
answers or further direction.
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The sample tracking record which
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ia initiated in the field provides:
a) Project Officer for site
b) Complete list of samples with notations on:
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1) 11ample matrix
2) field blanks
3) field duplicates
4) field spikes
S) OC audit
6) &hipping dates
7) labs involved
The chain-of-custody record provides sample descriptions
and the date of sampling. AlthOU<Jh the sampling date is ·not
addressed by contract requirements, the reviewer should be
aware of any lag time between sampling ano shipping, The case
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narrative which is submitted by the laboratort is anothe~
source of general information. Notable ~roblems with matrices,
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insufticient sample for analysis or reanalysis, and unusual events
should be found here.
The requirements to be checked in validation, in order, are as
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follows:
l. sample Holding Times
11. Calibration
III.
a.
b.
c.
Initial Calibration and Calibration
Continuing Calibration Verification
Calibration Blank
Blanks
a. Laboratory preparation blank
b. t'ield blank
IV. Interference Check Sample Analysis
v.
VI.
Laboratory Control Sample Analysis
S~cific Sample Results
a. Duplicate Sample Analysis
b. bpiked sample Analysis
c. G~'AA OC Analysis
Verifi~ation
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VII.
VIII •
IX.
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l. Duplicate Injections
2. Analytical Spikes
d. ICP OC Analysis
e. Sample Result Verification
Field and Other 0C
Quarterly Submissions
overall Case (Batch) Assessment
Procedure
I. bample Holding Times
A. ObJective
The objective is to ascertain the validity of ,results
based on the holding time of the sample from time of
collection to time of analysis or sample prep~ration, as
appropriate. From the standpoint of contract9r
performance, the time from Verified Time of S~mple
Receipt (VTSR) until analysis or sample preparation is
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needed to determine compliance with contract reQuirements.
~. Requirements
The followin~ holding time reQuirements were established
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under 40 ct·R 136 ( Clean Water Act l and are found in
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Volume 49, Number 20!1 of the Federal Re~ister1, page 28,
issued on October 26, 1984.
M~TALS: 6 months
MERCURY: 28 days
CYANIDE: 14 deys
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The 40 c~·R 136 requirements are recommended fo,r use in
determining datl! usabi 11 ty. With the exceptio'n of aercury,
the contract follows these 40 CFR 136 requirements, The ' .
contractual holding time for ■ercury is 30 days, Technical
re~uirements for sample holding times have only been
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established for water matrices, however, they are also
suggested for use as guidelines in evaluating lseoiment data.
c. Evaluation Procedure
Actual holding times are established by comparing the
sampling date on the SMO Sample Traffic Report with the
dates of analysis found in the laboratory data,
'contractual holding times are established by comparing
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verifieo Time of Sample Receipt (VTSR) with dates of
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analysis. I
Exceeding the holdi~g time for a sample I gener~lly
affects a loss ot the analyte(s), This occurs through
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any number of mechanisms such as deposition on the
sample container walls or precipitation, Therefore, I .
from a usability standpoint, when holding tim~ violations
occur, the results which are most severely callee into
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question are those which fall below or close ~o the detection
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limit. Relatively speaking, analytical resul:t& which tall
significantly above the detection limit could, be minimally
affected by a holding tiiie violation. Deteraiinati,-,n of
the effects of holdin~ time violations on the usability
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of analytical results is extremely aubJective. The
degree and nature of the eftect is dependent on ~ultiple
factors, such as the nature -of the analyte and aat.cix,
the degree of the violation (days), and the concentration
of the analyte in the sample. Ultimately, the decision
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whether to accept the data is best left to the d'ata
reviewer's/user's professional Judgment.
D. Action
If 40 Cr'R 136 holding times are exceeded, flag all positive
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results (Jl and minimum detection limits (UJ) as estimated
and annotate data to the effect that holding times were
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·exceeded. In the review narrative, state that the
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possibility of false negatives may exist and indicate that
the aetection limit for that sample may be elev~tea over
what is reportea. Reanalysis of samples which occurs
after holdin~ times are exceeded must also be evaluated
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for the ramifications of sample age in the interpretation
of the re-analysis results.
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In that analytical holding times tor soils or sediments
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have not been statiatically determined, do not ,reJect
data that have exceeded the contract holdin~ t1mes. If
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contract holdin~ times are exceeded, &u111111arize the defi-
ciency on the DPO Action Report and forward tolthe appro-
priate DPO tor that laboratory upon completion of the
review.
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Calibration
A.
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Initial Calibration and Calibration Verification
l. ObJective
The obJective in establishing compliance re~uirements
for satistactory instrument calibration is to insure
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that the instrument is capable of produciny acceptable
~uantitative data. Initial calibration dem~nstrates
that the instrument is capable ot acceptabl,e yertormance
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at the be~inniny ot the samyle analysis runs.
2. Reyuirements
t'or each ot the categories listed below the followin~
criteria apply:
o Instruments must be calibrated daily and eacn
time the instrument is set up. I
o Calibration veritication shall be made by the
analysis ot ~PA Quality Control Solutions.
Where an EPA ~C sample is not available/the
accuracy ot the calibration shall be conducted
on an indep~ndent standard at a concent~ation
otner than that used tor calibration, but
within the calibration range.
a) ICP Analysis
o Calibration blank and at least one
standard must be useo in establishing
the analytical curve.
o Calibration veritication results must tall
within the control limits ot 907110\ ot
the true value.
bl Atomic Absorption Analysis
o Calibration blank and at least three
stanoaros must be used in establishiny
the analytical curve. r
o Calibration veritication r~sult~ must
tall within the control limits ~t 90-110\
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C)
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for all AA analytes with the
of tin and mercury for which
of eo-120, apply,
Cyanide Analysii
I exception
the limits
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o Calibration blank and at least three
standards must be used in establishing
the analytical curve,
o Calibration verification results must
fall within the control limits of,90-1101
of the true value.
3. Evaluation Procedure
4.
a) Verity that the instrument was calibrated
at the proper trequency using the correct
number of standards and a calibration blank.
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bl Verity that the calibration verification
source used met contract requirements.
c) Review Form II for failure to meet acceptance
criteria. Spot check calibration verif~cation
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checks for each case/batch by recalcula~ion of
the percent recovery from the
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raw data ii verify
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that the recalculated value agrees wit~ the
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laboratory reported values, To allow possible
rounding discrepancies allow results t~ fall
with 11 of the contract windows (i.e., ,8!1-1111),
Action
The inability of a laboratory to perfonn acceptably I .
on the calibration criteria indicates aevere problems
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exist in the analytical system which must be resolved.
Any data generated under such conditions s~ould be
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considered suspect. If contractual windows are
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exceeded or if improper calibration procedure& were used,
all data associatea with that calibration ehould be. re-
. analyzed, Summarize any deficiencies on the DPO 'Act.ion
Report. If the data in question are needed on a :priority
basis, professional judgment may be applied to d~termine
to what extent the data may be utilized, Guidel~nes to
aia in the application of professional judgment to this
topic are as follows.
Q If the initial calibration verification falls outsiae
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the contract windows but within the ranges of .S0-89\
or 111-1501 the flag the positive bit data as:estimated
(J), .In the review narrative, give an indicaiion to
the data user as to the percent bias of the r~&ults
(i.e., if the initial calibration verificatiori for an
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analyte is 150\, then it coula be stated that 1the
reported results for that analyte could be biased
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approximately SOI high).
• If an analyte is not detected in a sample and,the
initial calibration verification result i&
110\ then the usability of that analytical
determination is acceptable,
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' I sample '
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than
9 If analyte is not aetected in a sample and the initial
calibration verification result is less than 90\,
then the aetection limit may be biased low, If the
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IDL and CRDL fall close to each other the possibility
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exists that the CRDL was not met. In the revi:ew
narrative, report that the ·detection limit tot, t-hat
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sam~le may be elevated and ~ive an estimate of the
bias. t'lag the data tor these samples as est1111ated
( UJ).
If initial calibration verification results fall less
than 50\ or greater than 150\ ~his is indicative of
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severe analytical deticiencies and the data s~ould be
reJected as unusable (R).
~. Continuiny Calibration Verification
l • UOJective
Continuin~ calibration verification documents satisfactory
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instrument pertormance (calibration accuracy) over
specitic time periods.
t<eyuirements
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ror each of the catewories listeo below, the tollowin~ I .
criteria apply: I
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A Continuinw calibration checks and calibration I
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blank analysis must be pertormed at a minimum
freyuency of 10\ or every 2 hours durin~ an
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analysis run, whichever is more treQuent, ~no
atter the last analytical sample.
Continuin.., calibration checks must be pertormed
with one of the tollowin',I solutions:
~AA 1643a, or a contractor prepareo •tnoependent
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standard• (i.e., from a ditterent source than that
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used for the initial calibration atandards).
o Continuinw calibration verification must occur at
or near the aid-range level of the calibration
curve.
o The calibration blank result must be less than the
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CRDL.
a) ICP analyses
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o Continuing calibration results must fall within the
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control limits ot 90-1101 of the true value,
b) Atomic Absor~tion analyses
o Continuiny calibration results must tall within the
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control limits of 90-110\ for all M analytes with
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the exce~tion ot tin and mercury tor Which the limits
ot so-1~0, apply.
c) Cyanide analysis
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o Continuin~ calibration results must tall within the
' I • control limits of 90-110\ ot the true value,
3. ~valuation Procedure
a) ~eview the supporting raw data to verify 1 that
continuing calibration verification and calibration
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blank analysis were performed at the proper
tre~uency.
bl ~erity that the standard used tor pertorminw
the continuing calibration met contract
criteria.
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c) Review t·orm II for any results outside control
limits. ,
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di Verity approximately 10\ of the re~rte,o
value& by recalculation from the raw da.ta;
4. Action
follow yuioelines as presented under lniti~l Calibra-
tion ano Initial Calibration Veritication,
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III. l:llanks
A. UbJeCtive
The assessment ot results .on blank analyses is tt>r the
purpose ot determinin,. the existence and magnitude of
contamination problems. The criteria for evaluation
ot Blanks applies to all blanks, including rea,.ent
blanks, method blanks, field blanks, etc. The
responsibility for action in t~e case ot unsuitable
blank results aepenos on the circumstances an6 the
ori~in of the blank. If problems with any blank
exist, all data associated with the Case must'be
caretully evaluateo to determine whether or not there
!
ia an inherent variability in the aata tor the Case,
or the problem is an isolated occurrence not
other data.
affecting
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1:1. Rec.uirements
\
1. The laboratory preparation blank (rea~ent:blankl
is the only in-house blank the laboratory 1 is
responsible tor reportin~ and:
al
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At least one preparation blank must be
prepared ano analyzed for every 20 samples
received, or for each batch ot samples
di,-esteo, whichever is more trequent.i
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It the concentration ot the blank is less than
the CRUL (see Appendix Ill, no correc~ive action
is required to be taken by the laboratory.
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It the concentration ot the
contract re~uireo detection
,.ro~p of samples associated
blank, the concentration of
blank is above the
level I for any
with a particular
the sam.l:'le with the
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least concentrated analyte must be 1ox 1
the
blank concentration, or all aamples associated
witn the blank and less than lo times the blank
concentration must be redigested and reanalyzed,
with the exception ot an identitied 8Queous
soil field blank, . The sample value is 1 not
to be corrected tor the blank value.
I
d) Results must be reported to the instrU111ent
detection limit.
2, No contractual criteria apply to the levels ot
contaminant in tield blanks.
c. ~valuation Procedures
l. Review the results reported on the Preparation
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~lank Summary (~·orm 111) as well as the Pr,eyaration
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blank(&) raw data (lCP ~rintouts, strip charts,
printer tapes, bench sheets, etc.) and verity that
results were accurately reported.
i. lt any blank contaminants were identitied ~t levels
greater than the CRUL, determine it redi1,1e1stion/
reanalysis was necessary by comparinw Dla~k levels
with the reported sample results.
D. Action
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lt contaminant analytes are detected in aamples
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at a concentration of less tnan ~ times the concentration
tound in the hi~hest associated Dlank (pre~ar~tion,
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field), these result• ahoulo be consioereo •u•vect.
Cooe the revorted results as estimated (J.).
I ln this
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instance, a statement should be included in tne nar-
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rative tnat indicates tnat it is not possible :to
verify wnether tne level of analyte aetected ~n tne
aam~le was due to contamination.
To minimize error in interpretin~ blank level~ in tne
range of the IDL, whicn is subJect to noise tluctuations,
I tne 5 times criteria is a~plied only wnen the level of
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the contaminant in tne blank is greater than i times I
tne IUL or wreater than the CRDL for the analy~e,
wnicnever value is lower.
I If contract criteria were not met, summarize the deficiency
on tne DPU Action Report for tnat case and submit to
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I tne appropriate DPU upon completion of the review.
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It contaminants were identitied in the field blank
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whicn were aosent trom tne laooratory preparation blank,
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this could be indicative of a potential field oc problem,
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a deficiency· in the bottle preparation procedure or tnat I
tne laboratory neylected to prepare the laboratory
blank in a manner similar to tne field blank. I
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IV. lCP Interterence Check tiample Analysis
A. UbJective
The ICP Interference Check i,;"ample Analysis i& pertormeo
to verity the contract laboratories interelement ana
back~rouno correction tactors.
1:1. Requirements
1. ICP Check sample must be run at the be~inning
and eno of each sam1,1le analysis run (or a minimum ot
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twice per 8 hour workin~ shitt, whichever is
more tre._uent).
~-If available, the check sample must be obtained
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3.
4.
from EPA. Otherwise, it must be ~repareo at the
contract specitiea levels.
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Results for the check sample analysis must,fall
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within the control limits ot + ~u, of the establisheo
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mean value.
The check sample results as well as the mean values
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ano stanoara deviations must be recoroed on t·orm IV.
Corrective measures are specitieo in the contract
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when check sample results fall outside the1
control
limits (i.e., termination of analysis, recalibration,
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reanalysis).
Evalu~tion Procedure
1.
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Review Form IV and verity that results meet the
contract criteria.
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2. Spot check raw data (lC}' printout) to verity the
accuracy ot the recoveries reported on t'Orlll 1~.
~. Spot check aample raw data for negative results.
4. If results do not meet the specified criter:ia,
verity that all atfected samples were reana,lyzed.
D. Action
It the ICP interterence check sample analysis results
tall outside the contract windows, summarize the: deti-
ciencies on the DPU Action Report for that case ano sub-
mit to the appropriate DPO upon com~letion ot the review.
}'rofessional JUd\lement may be applied to oetermi'ne to
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what extent tne data may be utilized in the eve~t that
the ICl' interterence check sample results exceed the
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contract windows. ~uidelines to aid in the apptication
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ot protessional JUdyement to this tOJriiC are as f,ollows:
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o for samples witn concentrations ot Al, Ca, t-·e, and
My which are compara0le to or ~reater than their
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resi,>ective levels in tne Interference Check ~ample:
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a) If the I~b recovery for an element is> 1201
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and tne re~orted sample result• are< lDL then
tnis data is acceptable for use.
b) It the l~S recovery for an element is> 1201
and the reported sample results are> IDL then
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tla~ the attect~d data as estimated (Jl ,nd
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indicate in the review narrative the potential
bias in the results.
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c) If the Ici:; recovery for an element ta:lls
oetveen 30 and 7111 ano reportable qua'nti-
,
ties of the analyte vere detected the.n rta11
the data as esti■ated (J). Jn the re,viev
narrative, give an indication as to the
potential bias of the results,
a) It an analyte is not detected in the 111am.,ile
and the ICS recover, for that analyt~ falls
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within the ranye of 3U-7lll then the l,)OSsi-,
bilitt of false neyatives aay exist. : Io the
review narrative, report that the detection
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limit for that sample may be elevated and
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give an estimate of the bias.
tor these samples as estimateo
t·1a11 the data
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e) It ICS recovery results tor an element fal!
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<3UI, this is indicative ot severe arialytical
oef icienc'ies and the data should be reported
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as unuseaDle (R).
o If u~on review ot the ICS rav data positiv~ results
are observed tor elements vhich are not present in
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tne EPA provided ICs solution then the possibility ot
talse positives exists.
. I .
An evaluation ot the assoc1ateo
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sample data tor the affected elements should be made.
r·or samples with com~araDle or hi1,1her levels of inter-
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terents, positive samples results, which approximate
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those levels tound in the ICI> (talse 1,>0sitives), shoulo
be tlayyed as estimated (J).
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o It upon review of the IC~ raw oata, newative resulta
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which are > than CkDL or -

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• IDL, whichever; is less
neyative are observed for •l-•nta which are n~
present in the EPA ICt; solutions, tben tbe ~••ibility
ot talse newativea ■ay exist. An evaluation ,ot tne
associateo sample data should be made. ror a'amples
with comparable or hiyher levels ot interterents, all
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results for the attecteo analytes which are reported
as< IDL ahoulo be flagged as estimateo (UJ), In the
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review narrative, state that the detection limit for
these sample& may be elevated,
o In yeneral, the sample data can be accepted without
turther evaluation it the concentrations of ~l, ca,
re and M11 in the sample are found to be signifi-
cantly less than tneir respective concentrations
' in the Interterence Check ~ample (i,e,, ~Oil, How-
ever, if other elements are present in the sample
' at ~reater than 10 ppm the reviewer should inves-
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tiyate tne possibility ot other interterence,eftects
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by using the table given on paye D-41 ot thel~Ow
or one ot the reterences listed below.
concentration equivalents presented in these1
reterences shoula be consiaerea only•• estimated
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values since the exact value ot any analytic'.al &)'stem
will del,)8nd upon a variety of factors such a,s the
viewiny position, shape ot the plasma ,nd back-
ground compensation techniques employee, Theretore,
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a.
b.
c.
d.
e.
t.
29 -I
in the instance where interteriny elements produce
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an •Quivalent analyte concentration greater than·
i ti■es the CRDL and greater than lU\ of the analyte
concentration identitied in the sample, flay t~e
aftected results as estimated (JI.
Additional References
Ml~ wavelenyth Tables, 1969, Massachusetts Institute'of
1·echnolo1,1y.
I
Table of Spectral Lines, iaioel et.al., !fl/Plenum, New York,
l!:l7U. I
Inductively Coupled Plasma -Atomic Emission Spectroscopy·:
Prominent Lines, u.s. ~PA, Environmental Research La~s, Athens,
~eoryia, EPA 6UU/4-7!:l-Ol7, l!:179.
Tables ot spectral Line Intensities, Part II -Arranyed by
Wavelenyths, inc ~a., W.F. MeQyess, et.al., National, bureau ot
stancaras, May l!:17~.
A TaDle of Emission Lines in the Vacuum Ultraviolet for All
~lements, UCRL ~4612, R.L. Kelly, University ot California,
Lawrence kaci at ion Laboratory, Livermore, California·, 19 !">!:I.
I
Line coinciaence TaDles 'tor lnauctively Cou~led Plas~a Atomic
~111ission spectrometry, Vols. I, II, J,M. boumans, Peryamon
Press, New York, 198U.
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-30 -
v. Laboratory Control ~ample Analysis
A. ObJeC'tiVe
The laboratory control sample. analysis is cses iwne'~ to
serve as a monitor of the etticiency of the oige~tion
proceaure.
a. Re~uirements
l. one a~ueous LCs must be analyzea tor every 20
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4.
:, .
sam~les receivea or tor each batch ot samples digestea,
• I
whichever is more frequent. Results for eacri analyte
should be reported on t·orm VI I.
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The aqueous LCS must be an tPA OC solution or a
standard which satisfies criteria tor use as Ian
jnitial calibration standard.
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t·or c:i,·anide, at least one mi a-range stanaard must be
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Oistillea ana com~ared to the calibration curve to
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insure that tne aistillation technique is reliable.
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The aistillea s~andara must a~ree within+ 10, of the
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unaistillea stanoaras.
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An aqueous LCS tor mercury is not required in that all
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tne calibration standaros as well as OC stanoards I
must be diwestea prior to analysis.
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one soliO LCS must be preparea ano analyzea each
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month tor each analyte and results must be reportea ' .
on t·orm VII.
The solid LCS must be obtained from tPA.
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-31 -
7. All aqueous LCS results must tall within the control
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limits of 80-1201 otherwise analyses should ha·ve been
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terminatec, problem correctec and all batch associatec
samples reanalyzec.
ij. All soliC LCS results must tall within the control
limits establ ishec b:i-t;PA, samvle analysis must be
terminated until satisfactory Les results are, obtainec,
C. Evaluation Procedure
1. Review form VII enc verity results fall within contract
control J.imits. I
2. ::;pot check raw data ( ICP pr in tout, strip charts, 'bench
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sneets) to verity the reverted recoveries on form VII.
3. If results co not meet criteria, verity corrective
action was taken.
D. Action I
Tne inability of tne laboratory to successfully analyze
a known I.IC cneck saml,)le .. (LCS) is indicative ot an anl1y-
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tical problem relatec to the di~estion/samvle prevaration
/ i i Ad I.
procecures anc or nstrument operat ons. ny ata associated
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witn tnat LCS should De considerec suspect. It the control
windows are exceeced, all data associatec with the LCS
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should be reanalyzed. A summary of the deficiency should
be included in the DPU Action Report for the case an'.d tor"".
' .
warcec to tne avprol,)riate DPU upon completion ot tn~ review.
It the data in question are needeC on a priority baiis,
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protessional JUd~ement may be ap1,>lied to de~ermine ~o what
extent the data may be ~tilized.
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o If the LCS recovery for any analyte tall• within the
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range ot 3U -791 or > 1201 then flag the positive :hit
aata as estimated (J). In the ·review narrative 1,1ive
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an indication to the data user as to the potential:bias
of the results and the oetection limits.
o It an analyte is not detected in a aample and the LCS
recovery is 1,1reater than 12UI then the usability of
that analytical sample determination is acceptable;
'
o It an analyte is not oetectea in a sample ano the LCS
recovery falls within the range of 30 -7~1, then the
report.ea oetection limit may be biased low. It the
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IDL ano CRDL tall close to each other then the pos~
sibility exists that the CRDL was not met. In the
review narrative, report that the detection limit for
that sam~le may be elevatea ana give an estimate dt
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the bias. t'la..i the data tor these samp.Les as esti.matea
( UJ) •
o It LCS recovery results tall less than 301 this is
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inaicative of severe laboratory or method oeficteAcies
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ano the data should be ret,,0rted as unusable (R).
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VI.
-33 -
tipecific tiample Results.
A. Duplicate Samp~e Analysis
l. UbJective -The percent ditterence data vill be
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usea by EPA to evaluate the lon~ term precision of
the methoas for each parameter. The data reviewer
can use the results ot the duplicate analys~s as an
inaicator of the precision of the sample results.
2. ke-.uirements
a) At least one duplicate sample must be analyzed
trom each ~roup of samples of a similar,matrix
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type (i.e., water, soil) ana concentration (i.e.,
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low, meaium) tor each case ot samples or for
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eacn 2U samples receivea, whichever is ~ore
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tre.,.uent.
b) t;amples identitiea as tield blanks cannot be
used tor duplicate sample analysis.
c)
d)
el
t)
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IJui.,l icate results must be reportea on t·orm VI.
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A control limit ot + 201 tor kPD shall be usea
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tor sample values>~ times the CRIJL. I
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A Control limit ot ! the CRDL Shall be usea
tor sample values less than S times the,CRDL.
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t-·or samples less than the CRDL the RPO is
not calculatea.
w> All results which tall outside the acceitance
'
criteria must be fla~gea with an••• on'
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t-·orms I and VI •
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-34 -
J. Evaluation Proceaure
al keview J'orm VI and verify results fall w\thin
the control limits.
bl 1:ipot check the raw data to verify that results
have been correctly reported on t'orm VI.:
cl ror duplicate results which fall outsid• the
control limits verity the correct usage of tlay
on both t·orms VI and I.
4. Action/Discussion
I
Act ions taken as a result of duplicate sampl,e
analysis must be weiyhed carefully since it may be
aitticult to aetermine if poor precision is a result
· ot sam1,1le non-homogeneity, methoa aetects or-laboratory
technique. The non-nomogeneous nature ot soil samples
often makes it more aitficult to achieve yooa au1,1licate
results compare .. a to al.lueous sam1,1les. uoweve_r, aqueous
sam~les containiny hifilh levels ot solias cari proauce
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erratic du1,1licate results as well. In 'ilene~al, the
results ot du1,1lic1te sample analysis Should lbe usea
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to support conclusions arawn about the quali,ty ot
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tne a11t11 rather than as I basis tor tnese conclusions.
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i:;ince only one du~licate is generally i,erformed per
matrix type (i.e., w AO, MLD AO, w £UL, MLU ~UL)
the 1,1recision results snould be applied to all other
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samples ot the same matrix type. An exce.,ti:on to
this can be maae when it appears evident that the
duplicated sam~le was ot II difterent chemical and,
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physical nature than other aamplea yiven tne aame
matrix classification. Unfortunately, aescriptive
intormation re~arding ceTtain aspect• of th~ iample
nature (i.e., appearance) is currently limited and
not readily availaole to the reviewer.
The fol!owinw guidelines are offered to enable the
reviewer to make a usability determination1,
o It the proper number ot duplicates for each matrix
'
type nave not been analyzed, ,reject the data and
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notity the DPU immediately to initiate reanalysis.
. i
o If aqueous duplicate analysis results tor a
particular analyte fall outside the control
winoows of+ 201 or+ CRDL, whichever is,ap~ropriate, --'
the results for that analyte in al! othe~ aamples
!
ot the same matrix type should be flay~eo as
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estimated(~). (Limits of! 3SI or! CkpL apply
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tor aoil/sediment duplicate resulta.)
o ~hen aqueous ouplicate analysis results for a
particular analyte exceed ~O RPD and the1 sample
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concentration level in the auplicate is>~ x the I
CRDL, the results should be considered QUanti-
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tatively questionable (J l. However, the' nar-
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rative should state that the qualitative1 pre-
sence ot the analyte was confirmed.
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-36-
0 When soil/sediment duvlicate analy ■i ■ for a
particular analyte exceed 100 RPD and the sample
concentration level in the duplicate ii> S"x the
.,
CRDL the results 1hould be considered quantita-
'
tively questionable (J). bowever, the narrative
should state that tne qualitative presence ot
the analyte was confirmed.
o Althouyh there is no contractual basis for
requiring laboratory reanalysis based UJ,)On submit-
ted duvlicate analysis results, reanalysis requests
can be made if the reviewer/user deems the informa-
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tion is critical. Reanalysis occurs at EPA's
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ex~ense and theretore all requests must be processed
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throuyh the DPU not by direct contact with the
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laboratory.
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-37 -
~. Spiked sample Analyais
1. UbJective -The ~piked sample analyais i• aeaigned
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to provide infor111ation about the eftect ot thl
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sample matrix on the 0111estion ana ■eaaurement
methodo.1011y.
2. Requirements
a) At least one spiked sample analysis must be
performed on each 11roup_ot samples of a
similar matrix type (i.e,, water, soil) 1and
concentration (i.e., low, hi11h) tor each
case of samples or for each 20 samples
received, whichever is more fre~uent.
bl
cl
0)
e)
samples identitied as field blanks cannot be
used tor spiked sample analysis,
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The analyte spike must be added prior t?
'
oi~estion ano in the amounts Sl,IE!Cifieo in
• the contract (Appendix 111).
If the spike recovery is not within the1
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limits of 75-1251, the aata of all the 1
samples associated with that spiked
must be tla11~ed with the .letter •R•
I sample
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(by/ the
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contract laboratory). An exception is ~ranteo
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when sample concentration exceeds the spike
concentration by a factor ot 4 or ■ore. :
When sample concentration is less than :the
CIU>L, SR•U is to be useo for the pur1,>0se
of calculatin11 recovery.
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-38 -
t) bpiked •am~le results must be reported on
l:'orm v.
J. Evaluation Procedure
a) keview l:'orm V and verify results fall vi,thin
tne s.,ecitiea limits.
bl t;pot check raw data to verify results were
correctly reported on t·orm V.
c) t·or &pikea sample results which fall outside
' the control limits verity the correct u~a~e
ot t la~s on t·orms I ana V.
4. Action/Discussion
ln oroer to properly assess spike sample analysis
results, it is necessary tor the reviewer to consiaer
a variety ot factors which could impact tneir outcome,
I
such as:
0 Matrix suppr,ession eftects
0 Matrix enhancement etfects
0 Duplicate presicion results
0 Diyestion eft:iciency
0 Contamination
o Relative levels ot analyte in the spike ~nd sample
t·or examJr>le, it the endogenous SalllJr>le level is
yreater than 4 times the spike
recovery results should not be
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level the'percent
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considered accurate
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or used to JUd~e the accuracy of the ■ample results.
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-39 -
As with the duplicate analysiu results,,the accuracy
statement implied by the s~ike recovery should be
,
appliea·to all other samples of the same matrix
. -
t)pe. An exception to this can be ■ade;when it
ap..,.ears evident that the spiked sample was a dif-,
terent chemical and physical nature than other
sam~les given the same matrix classification.
o If the proper number of •ample spikes have not
been processeo, reJect the data and notify the
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DPU immediately to initiate reanalysis.:
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Tne followiny guidelines are recommended fpr use in
evaluatiny aata usability when the spike recoveries
I
do not fall witnin contract limits:
o If the spike recovery is >1251 and the ~eported
0
,
sample results are less than tne IDL then this data
is acce~table for use.
It the spike recovery is >1251 and the
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reporteo
sample levels are ijreater than the IDL then £lay
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the data as estimated (J) and give an inaication
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in the review narrative as to the potential bias
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in the results,
I
o It the spike recovery falls between 30 ~nd 741
and reportable Quantities of analyte were detected,
fl•~ the data as estimated (J). In the: review
narrative, wive an indication as to the: percent
bias ot the results,
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c.
-40 -
o It an analyte i• not detected in a aample and
the apike recovery fall• within the ran~e ot
30-741 then the detection limit aay be biaaed
low. In the review narrative, report th~t the
aetection limit tor that sample aay be elevated
I
ana give an estimate of the bias.
tor these samples as estimate (UJ).
flag the data
o ror sample results reported as< IOL, iflspike
recovery results fall <301, the data should
be reportea as unuseable (Rl. This is indica-
tive ot severe analytical deticiencies and the
reviewer shoula state in the narrative that the
possibility ot a false neyative exists and that
' ' ' the aetection limits are elevatea over what is
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reported.
o l-'or positive hit data, if the spike recoyery
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results tall <JOI, the data should be reportea
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as ~uantitatively questionable (J). The'
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reviewer shoula state in the narrative that
the results could be biased siynificantly low
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and that the reported concentration is the
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' minimum concentration at which the analyte is
present.
~·urnace Atomic Absorp-tion OC Analysis
1. ObJective
Duplicate inJections and analytical spikes were
incorporatea into the vc scheme in order to establish
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-41 -
I a mechanism whereby the reviewer could better esti-
1
aate the precision and accuracy ot the indiv·iaual
I -analytical determination relative to the overall
method precision and accuracy,
ReQuirements
In addition to the previously described OC'
requirements, the followin11 adoitional criteria
apply to t·urnace AA determi-nations:
a) Du~licate inJections are required for all
furnace analyses except durin~ rull Me~h6ds
ot standaro Addition. Averawe result is
to be reported, raw data must contain all
readin11s,
b) ror concentrations> C~DL, duplicate
inJections must ayree within+ 2UI RSD,
I
or the sam~le must be rerun at least once
(third inJection),
c) All analyses must tall within the calibration
I
d)
ranye.
i:;ach sample (includin.,; the method duplicate,
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LCS ano blank) reQuires at least a sinc,i;le
I analytical spike to determine if MSA is,
necessary tor Quantitation.
el 'l'he spike is reQuired to be at a concentration
twice the CRUL,
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-42 -
f I The percent recovery of the 11pike determines
!
how the aample must be quantitated (also see
Al,lV9ndix IV I I
o If the spike recovery is less than ~01,
the sample must be diluted by a factor of
' S to 10 and rerun with another spik~.
This step must be performea only once.
'
If, after the Oilution, the spike recovery
is still <40\, fl•~ aata with an•~~ to
inaicate interterence problems.
o It the s~ike recovery is yreater than
40\ ana the sample absorbance or
concentration is less than SUI of the
spike, report the sample as less tn~n the
i
CkUL or less than the CRUL times anr
dilution factor.
o If the,sample absorbance or concentration
I is >SUI ot the spike ana the spike
1
recovery is between 8)\ ana 11S1, the
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sample shoula be ~uantitated directly
from the calibration curve,
o It the sample absorbance or concentration is
> sol ot the spike and the spike recovery is
I less than 851 or yreater than 11S1,1 the
sample must be quantitated by MSA, :
1) MSA aata must be within th~
linear ran~e establishea by the
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-43 -
3)
4)
5)
6)
initial calibration curve.\
The aam~le and three •pike~
must be analyzeo consecutive~y
for MSA QUantitation. (Th.e
I
initial sample and spike data
cannot be used,) Only ainyle
I
inJections are re14uired fo,r MSA
QUantitation.
Tne spikes should be prepa:red
at approximately 50, luu ano
I
150\ of the sample absorbance.
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It the correlation coetticient
is less than O.Y95, the MSA
analyses must be repeated pnce,
Tne data for MSA i.uantitat:ion
' shoulo be recorded in the 'raw
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oata with the slope, inter:cept
ano correlation coefficient tor
the line ano the results should
also be recoroeo tor t·orm ,VIII,
' keporteo values obtained by MSA
I
should be tla\'l11e0 with a •1s•.
I If the MSA has been rerun ,a
second time and the correlation
I
coefficient still is less 1than
'
U.YY5, the results on t·orm I
should be fla11yed with a•~•.
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-44
3. ~valuation Procedure
a) Review t'urnace AA raw data and ton VII'I to
..
verity that all analysis re~uirements have
been met (i.e., ouplicate inJections, MSA,
etc.).
bl verity re.,orted results by recalculati'1..i at
least 10\ ot the oata tor eacn varamet~r.
4. Action
a) If auplicate inJections have not been
performea, reJect the oata, notity the l>PU
and reyuest reanalysis.
bl . If au.,licate inJections are outsiae th~ !2U\
ktil> iimits and a thiro inJection has not
been mace as requirea, tlag the data as
C)
0)
e)
I
estimatea •J•, ana summarize the aeticiency on
the OPU ACfiOn Revort.
If the thiro inJection aoes not a~ree witn
either of the tirst two inJections l! 20\
RSO), tlay the data as estimateo (J).
'
If the analytical spike recovery is less than
I
40\ ana a dilution has not been analyzed,
tla~ the data as estimatea (J), ana summarize
the deficiency on the OPO Action Revort tor
tnat case.
1~ the analytical spike recovery is le~s than
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lU\ the oata ahoula be re.,ortea as unuseao!e (kl.
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f I ' If KSA is reQuired but has not been aone,
'
flay the data as estimatea (Jl, and summarize
the aeticiency on the DPu Action Report for
that case.
g) If the correlation coetficient is <0.995 ana
a duplicate KSA has not been performea, flay
I
the data as estimated (JI and su11D11arize the
aeticiency on the DPU Action Report for that
case.
h) If auplicate MSAs have been performed ana
'
Doth correlation coetficients are <0.99~,
the data should be reported as estimated (J).
ii It auplicate KSAs have been pertormed and
I
bOth correlation coetticients are <0.995,
tlay the data as unuseable (~).
I<.:P O<.: Analysis
1. ObJective
' ~erial dilution analysis is reyuirea so that the
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reviewer can ascertain whether siyniticant physical
'
or chemical interferences exist due to sample matrix.
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i. keguirements
al one sample from each ~roup of samples of a similar
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matrix type and concentration (i.e., low, meaiwnl,
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for each case of samfles, or for each 20 samples
. I
received, whichever is mc,re treyuent, must underyo
at least one serial ailution.
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b)
-46 -
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Results ot the OiluteO ■ample analyaia ano t.,he
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ori~inal analyses must a~ree within 101. It_t.he
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oilution analyees is not within 101, a chemical
or pnysical interference effect ahould be auspected,
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and the Oata ■uat be flawwed with an•~• by ,the
laboratory. The 101 criteria apply only it the
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analyte concentration i• minimally factor of 10 above
the IOL after dilution.
3. ~valuation Procedures
al Review raw data to insure that serial Oilution
I
analysis was ~rformed at the 1,>ro~r fre~uency I
tor each matrix type.
· bl ~~ot check the raw oata ano verity, by recalculation,
I
that the dilution analysis results com1,>are within
I
10\. Verify that the correct fl•~ was aoded to
t'Ol"lll I, if required.
4. Action
a) It the lUI criteria is not met, flaw the associated
oata as estimated (J).
b)
I
If ~erial Dilution Analysis was not performed
I
summarize the deticiency on the DP0 Action Report.
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E. ~am~le Result Verification
l. ObJective -The Sample Result Verification proc~ss
checks the correctness ot the data com1,>utat ion 1and I
transcri1,>tion, the validity ot the calibration and
M~A curve construction, and the correct use of ;the
codes oescribed on t.he cover page of the data report.
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Re~uirements -It is implicit within the so~ that all
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re~uired data reduction, reportin~ and documentation
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must be performed and presented in such a aanner as
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to insure the data package is both complete•• well
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as free of computational and/or transcription e~rors.
3, ~valuation Proceaure
It is optimal to perform a 100\ valiaation of the
data package. lt is recoynized however, that instances
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exist wnere this level ot effort mat not be practical
cue to resource constraints, The tollowiny yuiaelines
stioula be ap,:,lied in determinin1,1 the minimum level ot
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oata valioation requirea to assure ttle acceptability
ot the oata packaye:
a. t·urnace AA Parameters
Ctioose at least two furnace AA parameters for
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com~lete valiaation. lf any errors are ideritified
I i be in the review o! these parameters it will
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necessary to evaluate all case associated turnace
data.
b. ICY Parameters
Choose at least two ICP parameters for complete
validation, If any errors are identified in this
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review then evaluate an additional two para~eters. '
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It errors are still encountered then all remaininy
lCP parameters must be evaluated.
c. t'lame AA Parameter11
At a minimum, 10\ ot the flame AA parameters must
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be verified. _.,.lf error• an iaentifie4 re<view
additional p&r ... ter• are required unoer the
previous •eet. ton.'
d. Mercury ana Cyanide
uata for theae ~raJHters should be validated lOU\.
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e. Percent solids
Due to the impact an error could have on the,
results for an entire sample the data tor the
percent solids determination should be validated 100\,
In aaoition to the evaluation ~rocedures previously
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outlined within this document, the specific elements
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ot the data valiaation process shoula include the
tollowin<J:
a, A review ot all the deliverables tor completeness
as aescribed in Appendix I -Contract Re'1,juired
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b,
Deliverables.
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An evaluation of the calibration/MSA curre in
reyards to linearity, ran~e, outliers and coetti-
cient of correlation. Ascertain that the CRUL
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nas been 111et.
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c. veritication that results tall within the linear
ran\Je ot the ICP (reter to Quarterly form ~II and
within the calibrated range for the non~ICP para-
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meters. I
d, An examination ot the raw data tor any anomalies
(i.e., baseline shifts, neyative absorbance,
omissions, etc.) ,
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•• Verification that all the codes used on! the Form
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I's submitted for the case are approprfat,.
f. A comparison of furnace and ICP results: for the
4. · Action
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same element. When a furnace analyte fa also in
the ICP analytical scheme, and is ident1ified at 11
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concentration greater than the ICP dete,ction
limit, compare the results with the ICP. (This
frequently occurs for Pb and Cd.) This' is a
useful method for verifying these value.s or
determining if a problem exists in the 'analysis
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of the parameter. Professional judgment will be
required for both evaluation and action.
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a. If differences are identified between the reported
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result and the reviewer calculated result ~nd the
reported result is:
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within 101 of the reviewer calculated result
and the difference could be attributed to
rounding, then no action is required.
21 greater than 101 different from the rev,iewer
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calculated result, or leas than 101 but not
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attributable to rounding, ·contact the iabora-
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tory for verification. If an error is 1con-
firmed, request resubmission of corrected
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data sheets. summarize all contacts with the
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labordtory using the CLP Telephone Log Record,
Attach copies of all phone logs to the ,final
Quality Assurance Data Review Report.
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b. When the improper use ot flaws is identifiea or when
~roblems ar~ noticed with the calibration/MsA·curves,
contact the laboratort tor resubmission ot the correcteo
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aata.
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VII. Field and Uther 0C
This Bection is pr.oviaea for guidance only and as auch
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no tormal evaluation procedures or actions are aet. torth.
UbJective, Detinitions ana Assessment:
' t•iela vc consists ot field blanks and tiela duplicates.
.Uther types of OC samples incluae split samples, blind
blanks and blind spikes.
These types ot OC are not a part of the sow, but are a
usetul tool that the Reyional aata reviewer can take
advanta~e ot to monitor the performance of a laboratory.
The extent to which these types of oc are used is lett up
to the Re~ional field and laboratory personnel.
A tield blank is Dl water that has been •run throuwh•
all the samplinw eyuipment. The intent of a tield,
blank is to monitor tot contamination introduced by
samplin~ .,ersonnel, althou1,1h any laboratory introauced
contamination will also be present.
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A blind blank is bottled and .,reserved in the Re1,1io,nal
lab and shippea •as is• to the contract lab, The
purpose ot a blind blank is to monitor tor contamin'ation
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introduced by the contract lab. A blina Si,>ike is i,ire;,>ared
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by the 1<ewional lab. Usually the spike is inorganic stanar-
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daras spiked into Dl water. This prociaes an inter~erence
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tree matrix with which to monitor the lab's abilitY'. to reach
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the CRDL or the lab'■ ability to quantitatively recover an
analyte, i.vecitic ■pikes can be prepared to ■onitor. •~citic
areas (e,w,, oryanic mercury, lCP interferant ■, etb~
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A split sample is one that is divided between the
contract lab and Regional lab. When analyziny a split
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sample it is important that the same methodology i~
used by both labs so that there is a basis for the
comparisons ot the results.
~lanks, spikes and splits are usetul as supportin~·
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evidence in the overall assessment of a case. blarks
and spikes are samples ot a known composition and
matrix. As such, they are usetul in assessing a
laboratory's performance independent ot sample or method
problems which ma~ arise in a real sample,
t:xcept in the case of gross errors, blanks, spikes! and
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splits should not be the basis of accepting or reJ~ct1ng
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data, but rather as additional evidence in supportl ot
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tnese conclusions arrived at bt a review of the total
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packaye, blank, spike and split sample results of~en
will point out areas that the reviewer needs to look at
more caretully,
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VIII. Quarterly Verification of Instrument Parameter& ~eport
The contract laboratory must pertorm ana report ,
.veritication ot the followin11 parameters,
o Instrument Detection Limit& (AA and lCP)
The contract requires that before ant fiela samples
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are analtzed under the contract, the instrumen~al
detection limits (in u11/Ll must be documented 'and
must meet the specified levels (CRDL). The
instrumental detection limits are determined by
multiplyiny by 3, the standard Oeviation obtai~ed
for the analysis ot a &tanoard solution (each
analyte in reayent water) at a concentration 3~~ times
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the lDL on three (3) non-consecutive days with,7
consecutive measurements per day.
o Linear ~anye (ICP)
The linear ranye veritication check standard m~st
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De analyzed and reported tor each element on form
XI. The standaro must be analyzed durinw a routine
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analytical run pertormed under this contract. : The
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analytically determineo concentration of the standaro
must be within~~\ ot the true value. This
concentration is the upper limit of the ICP linear
ran11e beyond which results cannot be reportea under
this contract.
o Interelement Correction ~actors (ICP)
o Wavelen11ths Used (ICP)
o Inte11ration Times (ICP)
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IX. overall Assessment of Data tor a case
It is appropriate for the aata reviewer to make
protessional JUd1Jnients ana express concerns and coaimtnts
on the validity of the overall aata packa~e for a
Case. Tnis is particularly appropriate tor Cases in
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whicn there are several QC criteria out of specification.
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The aoditive nature of oc tactors out of specification
is ditficult to assess in an obJective manner, but ~he
reviewer has a responsibility to intorm users of th~
data of all concerns in order to assist that user in
avoidiny inap~ropriate use ot the data, while not
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.precluoiny any consideration of the aata at all. The
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aata reviewer would be ~reatly assisted in this endeavor
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if the s~ecitic expected use of the data was provided.
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ror instance, if the reviewer was aware that the pr~mary
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element of concern at a ~upertund ~ite was tor exam~le
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lead, then less eftort and resources would have to be ex-'.
pended than be necessary to do a com~rehensive
the entire aata case. It is important for the
have all ~ertinent information available.
review of
.1 reviewer to
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Apvendix 1
Contract ReQuired Deliverables
Contents
A. Inoryanic Cover Paye
II. Data Report iny -t'orm I
c. Qualitt Control summary
1. Initial and Continuiny Calibration Veritication -' t'orm II
:l. l!lank Reportin\,I -t'orm III
3. ICP Interference Check -t'orm IV
4. S~ike Sam~le Recovery -form V
S. Dui,;l icates -t·orm VI
6. IDL and Laboratory Control standard -form VII
7. stanoard Addition Results -t·orm VIII
D. Raw Data
1. IC~ Sequential Measurement keadout Record
2. t·lame AA Sequential, Measurement Readout Record
3. 1.a·AA sequential Measurement keadout Record
4. t.:olo va.,or Mercury t;equential Measurement Reaoout Recore
s. CN sequential Measurement Reaoout Recore
6. Diyestion loys tor AA, ICP and Hy digestions
7. Percent solids raw data
~-sample Trattic ke~orts
Data Completeness
A. Inoryanic Cover Paye
1. submitted ~ith Case
2. Properly com~leted
a. Laboratory name
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b, Case number
c, Date
d, t;OW NO,
e, OC Report No.
t. t:PA/Laboratory sample ID numbers
~-Indication of use or non-use of ICP interelement
and backyround correction
b. Data Reportiny -t'onn I
1, Ensure that form I has been submitted
l, Properly comfleted with the tollowiny:
a, Laboratory name
b, Case number
c. EPA sam~le No.
d, Lab IU samyle No.
e, SUW NO,
f, OC Neport No.
g. Date
h. Correct units
i. Instrument used (P-ICP/t'lame or F-~·urnace
J, sample results tor each parameter corrected for percent
solids on soils
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k, Values reported to IDL's and bracketea between
IDL's and CIU>L's.
1, Correct use ot footnotes for MSA, spike recovery
outside windows, du~licate RPU outside windows and
r < 0,995,
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c.
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Oual i ty <.;ontrol ~ummary t·orms
1. Initial and Continuiny Calibration verification -
t·orm II
a) t:nsure tnat t·orm II has been submitted with a
minimum ot one continuing calibration veriti'cation
per every 10 samples.
bl t:nsure tne torm is l,)roperly com~letea by evaluatin1,1
tne following:
o Laboratory name
o Case number
o Units
o :;cope of work
' o Acce~table initial calibration source (EPA
0
stanaard or otner inael,)endent standard)
<.:ontinuiny calibration source (!::PA stanaa~a or
otner inaepenaent stanaard)
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o Instrument used
i. !!lank !teporting -t'orm III
a) t;nsure that the laboratory has submitted'1 Form
Ill with l,)reparation blanks tor each matrix
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and cont1nuin1,1 blank checks tor every 10,
samples.
b) Check that t·orm III contains the tollowin1,1
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information recordea l,)ro1,>9rly1
o Laboratory name
o <.:ase number
o Date
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o Units
o Matrix
o Values reportea to IDL's
3. IC!' Interterence Check -t·orm IV
a) ~nsure that torm IV has been submittea by the
laboratory it ICP analysis is usea on tne
case. Tne form must contain analysis at: tne
beyinniny ano ena of each sample analysi~ run
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{or a minimum ot twice per ij-hour workin~
snitt, whichever is more trequent).
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bl Check that t'orm IV is properly completea by
evaluatiny the tollowiny:
o Laboratory name
o case number
o Date
o Check sample ID
• o Check sample source
o Mean and stanaaro aeviation or true v~lues
for all rei.uirea elements
o Means baseo on~ or more measurements ,(it
UNLV ICP check solution is not usea).
c. kequirea elements are definea as all elements
analyzea by ICP, exc1uain~ the interteren'ce
elements of Al, t·e, Ca, ana My.
o. The ICP check solution should be usea it it
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is available to the laboratory. It the IfP
check solution is not available, the laboratory
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ahoula prepare their own ana determine the'
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true concentrations by analyziny the solution
a minimlJlll ot five times.
4. spike sample Recovery -form V
a) Ensure that the spike sample recovery form(s)
has been submitted.
bl At least one pre-di~estion spike analysis
must be performed on each ~roup ot samples ot
a similar matrix type and concentration tor
each case or tor each 20 samples, whichever is
more treQuent.
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c) Check that the form V(s) are properly c~m.,leted
by evaluatin~ the tollowiny:
o Laboratory name
o case number
o Date
o EPA sample number
\
o Units
o Matrix
o spikes at the contract specitiea levels
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a. The levels to spike both water and soil
samJ,Jles betore ai~estion is specitiea in',
t:xhibit E, 'l'able 31 see Appenaix 2.
e) spikes are not rel.luirea tor Al, ca, t'e, ':'Y•
K, or Na on soil/sediment samples.
5. L>upl icates -t·orm VI
a) Ensure that form VI(s) have been submitted
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with at least one auplicate analysis for each
l,lroup ot aamples ot" a similar matrix and' ·
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concentration or for.each group ot •am~les
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receiveo, Whichever is more frequent.
b) Check that the Form VI(s) have been properly
completed with the tol.Lowiny information:
o Laboratory name
o Case number
o Uate
o EPA sam~le number
o Units
o Matrix
o Correct tootnotes
c. Duplicate results shou.Lo be tlayyeo with~
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••• on ~orm VI if the results are outsioe1 the
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control limits. A control limit ot 20\ RPO
on sam~les ~reater than Sx CORL or+ CRDL'on
sam~les less than ~x CRDL.
4. IOL ano Laboratory contro.L ~tanoaro -Yorm vlII
al t;nsure that t·orm \II I has been submit tea with
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instrument detection limits for each element
usiny tne instrumentation used in this case,
and laboratory control sam.-,le results tor 1a
.Li"uio sam.-,.Le.
bl Check that t'orm VII is pro~rly completed ',bY
evaluatiny the tollowinl,l:
o Laboratory name
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o Case number
o IDL's below CkDL for each parameter
o Units on the LCs
cl It an element is analyzed by both ICP/AA ana
turnace AA, instrument detection limits 'must
be supy!iea tor both methods.
5. stanaara Aaaition Results -t·orm '11111
al l::nsure that t·orm VIII has been submitted.
bl Check that ~·orm VIII is properly com~letea by
evaluatiny the tollowiny:
o Laboratory name
o Case number
o oate
o Units
o t"ootnotes torr values less than 0.9':I!>.
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cl All turnace analyses that are done Dy the '
method of standara adaition must be rec~rded
on t·orm VIII.
al Correlation coefticients below 0.995 should
be tlayyea with an••••
o. Raw Uata
1, A leyible ~hotocopy ot raw data (sequential
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measurement reaaout recoral clearly labeled
with sufficient information to une~uivo~ally
identity the followin<,1 intormation aust .be
suomittea with each case.
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-62 -
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2. ~nsure that the followiny raw Gata elements
are present1
o Digestion lo~ for ICP preparations
o Digestion log tor·AA preparations
o Di~estion log for Hw preparations
o Distillation lo~ tor CN preparations
o Measurement readout recora for ICP an~lyses,
if ICP is usea.
o Continuiny calibration recora in ICP raw
aata, if ICP is usea.
o Initial and final l~P interference check,
it ICl' is used.
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o Dilutions tor sample outsiae ICP linear
ranye (checked ayainst laboratory's
~uarterly linear ranye values).
o Measurement reaaout record tor furnace AA
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ana flame AA (it flame AA is used).
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o kecora of tour point calibration on all
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' non-ICP analyses (3 atandaras ana blanks).
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o Recora of parameter, Gate, atanaaro prepa-
ration aate, ana analyst tor AA, H,.., a_na CN-.
o correlation coetticients, ~rep. blanks,
spikes, continuiny calibrations, dupl(cates,
MSA, and dilutions clearly inOicatea in
the raw data.
o Percent solids raw data.
o Dual burns on t'urnace AA, not required·. on MSA,
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-63-
3. All sample results must be recorded in
sequential order.
4. Check that raw data intensities and/or AA
absorbances are contained in the raw data
unless the instrument is in concentration mooe.
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' 5. Check that all metals were analyzed within
holdiny time (6 months).
6. Check that My was analyzed within holdiriy
time (2tl days),
7. Check that cN-was analyzed within hold{ny
time (14 days).
sample Trattic keports
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t::nsure that copies of comi,:,leted SHU Sam.he
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Re;.;orts speci tic to the Case are include:d.
Tratfic
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Plasma
t:le1Dll!nt
Alu11inum
Antimony
Anenic
llarium
lleryllium
Cadroium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Seleniul!I
Silver
Sodium
Thallium
Vanadium
Zinc
APPENDIX II
EletMnt ■ l>eterained by lnducthaly Coupled
Eminion or Atomic Ab•orption Spectro ■copy : -·---------'
~ontr ■ct llequired
Detection Levell,2
(ug/L) ;
200
60
10
2llU
5
5
5uuo
10
5U
25
lU\J
5
5000
15
0.2
40
5000
5
lU
5UUU
10
50
2U -------------------------------,.------
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Element
Cyanide
-65-
Cyanide Deterainatioa
Contract Required
Detection Lavell, 2
(ll&/1.)
10
.!.:,_ Any analytical method apecified in SOW Exhibit Duy be,lltili&ed a•
long as the documented instrument or ■ethod detection limit& aeet
the Contract Required Detection 1.evel (CllDL) requirement,, Higher
detection levels uy only be used in the following circumstance:
If the aample concentration exteeda tvo ti ■ea the detection limit
of the instruaent or ■ethod in u1e, the value uy be reported even
though the instrument or aethod detection limit uy not'equal the
contract required detection level, Thi• i1 illustrated' in the
example below:
for lead:
Method in use• lCP
Instrument Detection 1.imit (lDL) • 40
Sample concentration• 8~
~ontract Required Detection 1.evel (CllDL) • S
The value of 8~ may be reported even though inatruaent detection
limit is greater than required detection level, The instrument or
method detection lilD4t auat be documented•• described ,in Exhibit t,
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2: These CRllL are the instrument detection limit• obtained in pure
water that muat be met using the procedure in Exhibit E. The
detection limit, for sample• uy be considerably higher depending
on the aample utrix, · '
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APPENDIX Ill
SPlKlNG LEVELS I FOR SPIKED SAMPLE ANALYSIS:
For lCP/AA For· Furnace AA ' Other
Element (uj!/L) ( u1:1/L) (ug/L)
Water Sediment1 Water Sediment I
Aluminum 2,000 *
Antimony 500 500 100 100
Araenic 20 40
larium 2,000 2,000
Beryllium so so
Cad11iU1D so so s
Calcium * *
Chromium 200 200
Cobalt 500 500
Copper 250 250
Iron 1,000 *
Lead 500 500 20 so
Magnesium * *
H&ngane11e 200 500
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Mercury
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Hickel 400 500
Potassium * *
Selenium
10 10
Silver so so
Sodium * *
Thallium
so so
Vanadium 500 500
Zinc 200 sou
Cyanide
I 100 --------------------.-·----
NOTE: Elements without spike levels and not de11ignsted with an asterisk, should
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be spiked at appropriate levels.
lThe levels shown indicate concentratlons in the final dlgestate of the splked
sample (lUU ■L FY)
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APPENDIX IV
FllRHACE ATOHIC AISOUTlON ANALYSIS SattKE
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PR£PAU AND ANALYZE SAMPLE ◄ AND ONt SPIKE (2 l c.a.D.L.) f (double injection• required)
♦ II DILUTE SMPl.E l
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ANALYSIS WITHIN CAJ.IBRATION RANGE ' .
♦ YES
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1f NO, repeat only once .
llCOVERY OF SPIKE 1.40X
'-----------L_!:1fL!•N~ot!.1
1
!
1 1LJ►•I Fl.AG DATA WITH ,.,. ·r I
i n;s --
SAMPLE .USORBANCE >50i of SPlKJ:: .USORBANCt•l--
11-0----~:~
j SPIKE tt.t:~uYERY <851 OR )1151
QUANTITATE iY KSA WlTK 3 SPIKES
AT 50, 100 AND 150Z OF SAMPLE
AB!:llRJIANCE
(only single injection• required)
CORRELATION COEFFICIENT )0.995
NO
r
◄
repeat only once
I 1.EPORT SAMPLE AS
<C.R(D.L. l ANY
DILUTION FAC.."TOK
' QUANTlTATE FKUM
CALIBRATION
CURV,E AND llf PORT
I fl.Al,; DATA WlTK -.-, I .. ------------•►! FL.AG ukrA w1t11 A ·+·
if ltill NU
*•pike ebsorbance defl,;ed as (ab1orbance of 1pike •ample) ainu1 (1bsorbanco, of the
,ample)
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UPENDIX V
Contract Laboratory Program
llGIONAL/LA&ORATORY COMMUNICATION SYSTEM
Telepto.e lleaird Log
Date of Call:
L&bontory Name:
Lab Contact:
Region:
Regional Contact:
Call Initiated By: _ Laboratory _Region
In reference to data for the following 5ample i.irnber{s):
Summary of Questions/ls.sues Discussed:
Summary of Resolution:
Signature
Distribution: (I) Lab Copy, (2) Region Copy, (l) SMO Copy
Date ,
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CONTRACT LA80RATORY PROCRAM
Deputy Project Officer Commwucation Summary
Date DPO Notified of Issue: ____ _ DPO Notified By: ________ _
Subject Laboratory: ____________ _ Cue/Sas No:
Conact for Rnolution: (Laboratory or Po)
Date of Contact:
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Call or Visit (Circle One)
Summary of Issues & Resolutions:
Document the issue(s), resolution(s), and action deadlines, if any._
Signature
Date
Region
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(I) DPO Copy (2) Project Officer Copy 0) SMO Copy (i.) Lab Copy
5/84
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APPtNDll V1
lt.ECilONA.1. DEPUTY PROJECT OFFICERS
FOR.
Q.P TECHNICAL ADMINISTRATION
USEPA R.egion I
Edward Taylor
Chief, Chemistry Section
USEPA Region I
Environmental Services Division
60 'l'estvlew Street
Lexington, MA 0217]
617/161-6700
USEPA Region U
"l'illiam Coakley
Superfund QA Coordinator
USEPA Region n
Environmental Services Division
Woodbridge Avenue
Edison, New Jeney 01137
201/)21-6702
USEPA Region m
Patrkia Krantz
QA Officer
USEPA Region m
AMapolis Field Office
Central Regional Office
139 Sestgate Rd.
Annapolis, MD 21110 l
30 l /2211-271t0
USEPA Region IV
. Tom S. Sennett, Jr.
Chief, Chemistry Section
USEPA Region IV
Environmental Services Division
College Station Road
Athens, Georgia )061]
,011/,116-3112
USEPA Region V
Chuck Elly
SMO Coordinator
USEPA Region V ,>& S, Clark St.
Tenth Floor, CRL
Chicago, Illinois 6060,
)12/),3-9017
•'
USEPA Region VI
'l'illiam Langley
USEPA Region Vt _
Monterey Park Plaza, Bid&, C
6601 Hornwood Drive :
Houston, Teus 77071t
7 U/954-1766
USEPA Region VD
Dr, Robert Kleopfer
Chief Chemist
USEPA Region VU
Environmental Services Division
2, Funston Rd,
Kansas City, Kansas u11, '
· 913/23'-)Ul
USEPA Region vnt
John Tilstra
Chief, Laboratory Services Section
USEPA Region Vlll • Laboratory
Denver Federal Center ·
Building '3, Entrance '1'-1, ~nd Floor·
Denver, CO 10225
303/it,11-3263
USEPA Region IX
Harold Takenalca :
Chief of Laboratory Support Section for OES
USEPA Region IX
21' Fremont Street
San Francisco, Califomla 91f10'
It 1'/97,._71tllf .
USEP A Region X
Arnold Ciahler
Chief, Laboratory Brandl
USEP A Region X
P.O. Sox k9
Manchester, Ti A 9&.l,]
206/ltlt2-0370
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Data Review Uistribution Addresses
l) Duane Geuder
Analytical Support branch (WH-!'>48A)
Hazaraous Response Support Division
4Ul •M• St,, S,W,
Washinyton, D.C. 2U460
2) Ross Robeson
t:M::,L-LV
P,O, box l!'>U27
Las Veyas, NV ij9ll4
3) Cognizant DPO
Laboratory/DPU Assiynments (by Reyion):
Reyion I:
keyion II:
Cambridge Analyticl Associates
Chemtech Consultiny Group, Ltd,
u.s. Testin~ company
Reyion III: Centec Analytical Services
ttittman-~basco Associates, Inc.
Reyion IV:
ke;iion VI:
JTC t:nvironmental Consultants, Inc.
Mack Laboratories
Versar Laboratories, Inc.
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CompuChem Laboratories, Inc,
Anacon
Radian
spectrix Corporation
l'oxicon Laboratories, Inc,
Re~ion VII: Wilson Laboratory
Reyion ~III: Accu-Labs Research
Rocky Mountain Analytical Laboratory, Inc,
keyion IX:
Reyion X:
Calitornia Analytical Laboratories, Inc.
Weyerhaeuser Company
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Glossary
Data Qualifier Definitions
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t·or tne vurposes ot this document the ·tollowin<,1 coae letters and
associated definitions are provided, Use of these apecitic code
letters is not manaatory1 use ot ditferent coaes with the aame
qualifier definitions is optional,
u -Tne material was analyzed tor, but was not cetectea. Tne
associated numerical value is the estimated sample QUantitation
limit.
J -The associateo numerical value is an estimated quantity
because quality control criteria were not met,
I( -Quality control indicates tnat tne data are unusable, (com,-,ound
may or may not be present), l(esamplin1,1 and/or reanalysis is
necessary tor verification.
2 -No analytical result
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Other Terms
AA -Atomic Absorption
CLP -Contract Laboratory PrO',jram
CRUL -t:ontract Re~uired Detection Limit
DPO -Oe1,1uty ProJect Utficer
I GfAA -t.raphite •·urnace Atomic Absorption
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I<.:P -Inductively <.:ou1,1lea Plasma
IUL -Instrument Detection Limit
LC::; -Laboratory Control l:iample
M!::iA -Method ot l:;tandard ACdition
IIIPU -lliational Proyram Ott.ice
O!::iC -Un scene coorcinator
PU -ProJect Ufticer
OA -Ouality Assurance
UC -Quality Control
R!::iCC -Reyional sam~le Control Center
SMu -sample Manayement Uttice
Vl'SR -Validated Time of t:.ample Receipt
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U.S.E.P.A. Region
INORGANIC QUALITY ASSURANC:"":E~o==--A~T~A,-R""'·EvlEW REPORT
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Case No. __________ _ Project Nar,~------
Laboratory _________ _ DPO for Lab _____ _
I Applicable Sample Nos.
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Date Sampled: _________ _
Date Data Received: _______ _
Review Date:-----------
Contact of laboratory required (yes, attach CLP logs) ' (no) ----,---
Res u b missions requested Received ---
Data Oualifers:
U -The material was analyzed for but was not detected. The 1associated
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numerical value is the sample quantitation limit. NOT DETECTED.
J -The associated numerical value is an estimated quantity b~cause one
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or more quality control criteria were not met. ESTIMATED,VALUE.
R -Quality control indicates that the data are unusable (analyte may or
may not be present). Resampling and/ or reanalysis is necessary for
verification. UNUSABLE.
Z -No analytical result.
DPO Action FYI ------
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Quality Assurance Data Review Report (Cont.)
Case No. __________ _
Laboratory _________ _
Comments
DPO Action Items
Reviewed by: ---------
Attachments
CC:
Regional DPO (for laboratory)
Contract Laboratory Program, QAO
John Fowler. EMSL-LV
Phone No. Date: ---
,
----
Caw No.-----------
laboratory
EPA TR I
Labl.0.
Aluminum
Antimony
An.nit
Barium
B•ryllium
Cadmium
Calcium
Chromium
Cobalt
Copp•r
Iron
lud
MagnHium
Manaan.w
M•rcury
Nick•I
Pota1Sium
~~•~nium
Silv~r
Sodium
Thallium
Tin
Vanadium
Zinc
Cyanid•
~ Solidi
-----DATAS --.1MARY ---Matrli ________ _ Unit•----------
-
---
-----
COMMENTS
(~•..< ;..o.
l•bora1cry -
Oat@ --------
\AMPU FIHDOC IIEGIONALOC OTH(~/
OVEIIAll CASE 0C MATRIX SPECIFIC OC Sl'(CIIICQC COMM(NT\ :-·: ._ ,.... ---'~(,? ....... .... 'Po'• ~ ,J!. Ml ... Ml"" ... """ 61M -le\,. ...... ...... -.. . -...
. '• .... .... u .. . •o ''" ... -· ... -•-~ ..., ... ....
1'."tp:~ •r -,I,, Ml .. "" ... Ml ""-
·;." -· ... _ <el• : :, ~ ....
Aluminum
AnltfflOll'ly ,.,_ ... ,_
I .. ,yfhuffi
le°"""""' I •
r .. <"""
,lo .. -..... . .
/ j Cobell
ij(-.......
' : 't_•.cl
.
'IMl...-,.iUffl
I I ... _
. ....,.(UfJ ,1.
\ ;N,(_ ....
I PolMIIUffl
'
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\odi"'91
1f\ellium ,.
· · l1n
v~""'
l•n< ,,_
..
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