NCD003200383_19900301_Koppers Co. Inc._FRBCERCLA SAP QAPP_Final Quality Assurance Project Plan - RI and FS-OCR

I
I
I
·1
·1
·1
I
I
I
I
I
I
I
:1
I
I
I
I
I DCC#Q461
·I
FINAL
QUALI1Y ASSURANCE
PROJECT PLAN (QAPP)
REMEDIAL INVESTIGATION AND
FEASIBILI1Y STUDY AT THE
FORMER KOPPERS COMPANY
SUPERFUND SITE
MORRISVILLE, NC SITE
Prepared for:
BEAZER MATERIALS AND SERVICES, INC.
PITfSBURGH, PA 15219
Prepared by:
KEYSTONE ENVIRONMENTAL RESOURCES, INC.
3000 TECH CENTER DRIVE
MONROEVILLE, PA 15146
PROJECT NO. 179225-04
MARCH 1990
I
I
I
Signature Page
I Quality Assurance Project Plan (QAPP)
I Project Title: Remedial Investigation/Feasibility Study
Beazer Materials & Services, Inc.
I Former Koppers Company Superfund Site
Morrisville, NC Site
I Prepared by: Keystone Environmental Resources, Inc.
I Approved: Date:
EPA Region IV Project Officer
I Approved: Date:
EPA Region IV Quality Assurance Officer
I Approved: Date:
Beazer Materials & Services, Inc.
I Program Manager
Approved: Date:
I Keystone Environmental Resources, Inc.
Project Manager
I Approved: Date:
Keystone Environmental Resources, Inc.
I Quality Assurance Officer
I
I
I
I
I DCC#Q461 i
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
'I
TABLE OF CONTENTS
~
1.0 INTRODUCTION .................................................................................................. 1-1
2.0 PROJECT DESCRIPTION ................................................................................. 2-1
3.0 PROJECT ORGANIZATION AND RESPONSIBILllY ............................. 3-1
4.0 QUALITY ASSURANCE OBJECTIVES ......................................................... 4-1
5.0
4.1
4.2
4.3
4.4
4.5
4.6
Data Quality Levels ................................................................................... 4-1
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
SAMPLING EQUIPMENT AND PROCEDURES ........................................ 5-1
5.1 Sample Container and Equipment Preparation .................................... 5-1
5.2 Surface Water Sampling ........................................................................... 5-3
5.2.1 Sample/Location Selection ........................................................... 5-3
5.2.2 Stream Sampling ............................................................................ 5-3
5.3 Pond Sampling ............................................................................................ 5-4
5.4 Flow Measuring .......................................................................................... 5-6
5.5 Sediment Sampling .................................................................................... 5-9
5.6 Soil Sampling ............................................................................................ 5-10
5.7 Groundwater Sampling ........................................................................... 5-11
5.8 Sample Filtration ...................................................................................... 5-22
5.9 Safety Precautions ................................................. ; .................................. 5-22
5.10 Documentation ......................................................................................... 5-23
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 lnstrurnentation ................................................................................ 8-1
8.2 Laboratory Instrumentation -Conventional Chemistries .................... 8-1
8.3 Laboratory Instrumentation -lnorganics ............................................... 8-2
8.4 Laboratory Instrumentation -Organics .................................................. 8-4
DCC#Q461 Ii
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
:1
I
9.0
TABLE OF CONTENTS (continued)
fm
DATA REDUCTION, VALIDATION,AND REPORTING ........................... 9-1
9.1
9.2
9.3
9.4
9.5
9.6
Laboratory Data Reduction ..................................................................... 9-1
Laboratory Data Validation ..................................................................... 9-2
Laboratory Data Reporting ...................................................................... 9-3
Independent Data Reduction and Evaluation ....................................... 9-3
Independent Data Validation (Non-CLP Samples) ............................. 9-4
Independent Data Validation (CLP Samples) ...................................... 9-4
10.0 QUALI'IY 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 ................................................. 11-1
11.1 Performance Audits ................................................................................. 11-1
11.2 System Audits ........................................................................................... 11-1
12.0 ASSESSMENT PROCEDURES FOR LABORATORY DATA
ACCEPTABILI'IY ................................................................................................ 12-1
12.1 Precision .................................................................................................... 12-1
12.2 Accuracy .................................................................................................... 12-1
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 ............................................................................ 13-1
13.2 Routine Preventive Maintenance
(Field and Laboratory Equipment) ....................................................... 13-2
14.0 CORRECTIVE ACTION ................................................................................... 14-1
14.1 Methods Corrective Action .................................................................... 14-1
14.2 System Corrective Action ....................................................................... 14-1
15.0 QA REPORTS TO MANAGEMENT ............................................................. 15-1
REFERENCES
APPENDICES
Appendix A
AppendixB
DCC#Q461
Export Protocol For Toxics Compliance Monitoring Data
U.S. EPA Functional Guidelines For Evaluating Organics and
Inorganic Analyses
iii
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
LIST OF TABLES
Table Title tm
1-1
2-1
2-2
2-3
2-4
2-5
2-6
4-1
4-2
5-1
5-2
6-1
8-1
8-2
8-3
10-1
10-2
10-3
10-4
10-5
10-6
Quality Assurance Project Plan Criteria ........................................................ 1-2
Su:face Water Sample Analysis Summary ..................................................... 2-2
Sod 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 Blanks ............................................................................... 2-16
Quality Assurance Objectives
(Groundwater/Surface Water Samples) ........................................................ 4-6
Quality Assurance Objectives (Soil/Sediment Samples) ............................. 4-8
Sample Container Oeaning Procedures and Preservation ....................... 5-26
Order of Volatilization .................................................................................... 5-27
Holding Times .................................................................................................... 6-4
Interferent and Analyte Elemental Concentrations Used
for ICP Interference Check Sf.f,!ple ............................................................. 8-10
Method Detection Limits of C12 Labeled PCDD's and PCDF's
In Reagent Water (PPT) and Environmental Samples (PPB) ................. 8-11
~2~i~s f~~Js~~6t•~~~'.~ .. ~.~.~~.~~~.~.~~.~~~············································· 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 with
Corresponding TCL Analytes Assigned for Quanitation ........................ 10-17
Calibration Check Compounds ................................................................... 10-18
Surrogate Spike Compounds and Recovery Ranges ................................ 10-19
LIST OF FIGURES
Figure Title tm
5-1
5-2
5-3
5-4
6-1
6-2
8-1
12-1
14-1
DCC#Q461
Analytical Request Fann ................................................................................ 5-26
FielcfData Sheet for Groundwater Sampling .............................................. 5-27
Purge Volume Configuration ......................................................................... 5-28
Computer Generated Printout ...................................................................... 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
iv
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
1.0 INTRODUCUON
Section No: 1
Revision No: 1
Date: 03/08/90
Page 1 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 (RIJFS) work at the former Koppers Company
Superfund Site (Beazer Materials and Services, Inc.) in Morrisville, North Carolina.
The procedures and criteria that will be used to accomplish the RIJFS work
objectives will be responsive to requirements of the U.S. Environmental Protection
Agency (U.S. EPA). The RIJFS 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 1-1
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I ,.
I
I
Item Number
1
2
3
4
5
6
7
8
9
DCC#Q461
TABLE 1-1
Section No.:1
Revision No.: 1
Date: 03/08/90
Page: 2 of3
QUALI1Y 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Item Number
10
11
12
13
14
15
16
DCC#Q461
TABLE 1-1 (continued)
Section No.:1
Revision No.: 1
Date: 03/08/90
Page: 3 of3
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
o Laboratory Operations
o Field Operations
o Calibration Standards
o Duplicates
o Spikes
o Blanks
o Standard Curves
Performance and System Audits
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
10.0
11.0
12.0
13.0
14.0
15.0
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
2.0 PROJECT DESCRIPTION
Section No: 2
Revision No: 1
Date: 03/08/90
Page 1 of 16
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 (T AL) 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
---- - - - - - - - - - - - - - - -
TABLE 2-1
SURFACE WATER SAMPLE ANALYSIS SUMMARY
No.or Estimated
Sample Samples No.or Analytical Detection Field Rinsate Trip DQO
Location per Location Samples Parameter Method Limit Duplicate Blank Blank Level Comments
SW-I, SW-IO, 2 12 Acid Extractable EPA8040 (2) 0 Ill
. SW-12 Phenols
SW-18,
SW-20, SW-22 (1)
2 12 Pentachlorophenol EPA515 0.010 ug/1 2 0 V
2 12 (sopropyl Ether• EPA8020 1.00 ug/1 2 I/day/cooler V First round only.
N ' N
2 12 pH EPA 150.1 0 0 0 II This analysis will be performed in the
field.
2 12 ~cific EPA 120.1 I umho/cm 0 0 0 II This analysis will be performed in the
onductance field.
2 12 Temperature EPAl70.I 0 0 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 EPA8290 Various I 0 V At each location, one samr.le will be
filtered and one sample wtll remain
unfiltered.
t:j ,cl .,, " .. f. " i;-:s. (IQ •• {ll
f'D -· • .... e~ ~
0j:z:z ""00 ;: 8;.:. ;:.
- - - --

-
---

-
-

-

-
-

-
-

-
-

-
TABLE 2-1
(Continued)
SURFACE WATER SAMPLE ANALYSIS SUMMARY
No.or Estimated
Sample Samples No.of Analytical Detection Field Rinsate Trip DQO
Location per Location Samples Panmeter Method Umit Duplicate Blank Blank Level Comments
See Comments 2 8 Total Organic EPA 415.1 I mg/I 0 0 Ii The locations of these
Carbon samples will be picked
at random from the fire
2 8 Biochemical EPA405.1
Oxygen
Demand
I mg/I 0 0 0 Ii and Medlin Ponds.
2 8 Chemical EPA 410.4
Oxygen
Demand
10 mg/I 0 0 0 Ii
2 8 Total EPA 160.2 1 mg/I 0 0 0 Ii
N SusP."nded
' Sohds ~
SW-16A, SW-168, 1 14 Acid Extractable EPA8040 (2) 1 1 0 Ill
SW-17, SW-23 Phenols
thru SW-26
SW-28 thru SW-34
1 14 Pentachlorophenol EPA515 0.010 ug/1 1 0 V
1 14 lsopropyl Ether• EPA8020 1.00 ug/1 1 I/day/cooler V First round only.
1 14 pH EPA 150.1 0 0 0 Ii This analysis will be performed
in the field.
1 14 = EPA 120.1 1 umho/cm 0 0 0 Ii This analysis will be performed
ndu~tance in the field.
1 14 Temperature EPA 170.1 0 0 0 II This ananlysis will be performed i::, ~ ~II>"[ in the field. II> It' .:s. (IQ •• ~
It cC:ro c.ic.i== 0 jzz "" 0 0 .... i·· .. °' .......
- --------- --
TABLE 2-1
(Continued)
SURFACE WATER SAMPLE ANALYSIS SUMMARY
No.or Estimated
Sample Samples No.or Analytical Detection Field Rinsate
Location per Location Samples Parameter Method Limit Duplicate Blank
SW-24, SW-26, TAl/fCL
SW-34 I 3 Compounds• EPA-CLP (4)
See Comments I 7 Total Organic
Carbon
EPA 415.J I mg/I 0
I 7 Biochemical EPA 405.J I mg/I 0
Oxygen
Demand
N ' ,-I 7 Chemical EPA410.4 JO mg/I 0
Oxygen
Demand
I 7 Total EPA 160.2 I mg/I 0
SusP."nded
Solids
Notes:
~
I) At each location a sample will be collected from the following depths: near surface and at 2/3 depth
2) EPA Method 8040 Detection Limits
henol 0.50 ug/1 2,4,6-Trichlorophenol
2-Chlorophenol 0.50 ug/1 2,4-Dinitrophenol
2-Nitroplienol 0.50 ug/1 4-Nitrophenol
2,4-Dimethylphenol 0.50 ug/1 2,3,5,6-Tetrachlorophenol
2,4-Dichlorophenol 0.50 ug/1 4,6-Dmuro-2-Methylphenol
4-Chloro-3-Methylphenol 0.50 ug/1 Pentachlorophenol
i3~ At locations SW-12 and SW-18 a sample will be collected from 2/3 depth.
4 Refer to Table SA-I of this Work Plan for a list of detection limits.
5 Samples will be collected from 2/3 depth.
•one round of surface water sampling will be performed for the above noted parameters.
0
0
0
Trip DQO
Blank Level
I/day/cooler IV
bvolatiles only)
II
0
0
0
1.00 ug/1
1.00 ug/1
1.00 ug/1
J.00 ug/1
1.00 ug/1
J.00 ug/1
II
II
II
- - ---
Comments
First round only.
The locations of these
samples will be picked
at random from the
drainageways.
-------- -- - - ---l!!!!!l!!I
TABLE 2-2
SOIL SAMPLE ANALYSIS
Sample• l!aimated
Sample pe, No. of Analytical Detection Field Rinutc Trip DQO
A,ea Locatioo Location Slmp ... Parameter Method Limit Duplicate Blank Blank Level Comments
Land T rcatmcnt X-2 thru X-9 3 24 Acid Extractable Pbcaolica EPABO<O (I) 2 0 llI
3 bopropyl fJbcr EPA 8020 100 "I,.. V
• TAL/TCLUm Various (2) I (volatile, only) IV
Lagoon and CcUoa X-IS thru X-37; 2 .. Acid Extractable Pbcoolic, EPA 80<0 (I) • 0 n One sample from locatioot
Trcatmc:al Ara X-41 s bopropyl Bbcr EPA 8020 100 "I,.. I V X-17, X-26 and X-37 will be
7 TAlJTCLlilh Varioua (2) l (volatile• only) IV included in the analy1e1 for
s PCDD/PCDP EPA 8290 VariOUI 0 V TAL/TCL conllitucnta and PCDDa
aod PCOPa.
Teepee Burner X-10, 3 3 Acid Extractable Pbcoolic, EPA 80<0 (I) 0 Ill Tbc aurfacc 10il umplc from
3 3 Drink.ltc Water Met.ala (3) (3) 0 Ill boring X-IO will be ao.alyzed
3 3 PCDD/PCDP EPA8290 Variom 0 0 0 V for coostitucnt• oo the
N TAUTCl.Jilh VariOUI (2) I (volatile■ only) IV TAL/TCL lilla.
I
l..n
SS-1. SS-2 2 Acid Extractable Pbcoolic■ l!PA 80<0 (I) I 0 Ill
2 Driak.lDa Water Metal■ (3) (3) I I 0 m
2 PCDD/PCDP EPA 1290 Various 0 0 0 V
Other ArcH X-11 to X-14; 2 21 Acid Extnctablc Pbcoolica l!PA 80<0 (I) 3 0 m Ooc umplc ffl'G1 boring• X-14
X-31 to X-47 3 bopropyl Elbcr EPA 8020 100 "I,.. V and X-46 will be analyzed
• TAUTCLlilll Various (2) 1 (volatile, only) IV for T AUTCL comtitucllla.
lla<qround C·3, C-9, 2 6 Acid Exlnctablc Pbmolie1 l!PA 80<0 (I) 0 Ill
andC-11
X·I 2 2 Acid Extractable Pbmolic1 l!PA 80<0 (I) 0 m
2 2 TAUTCLl.ilb Various (2) I (volatile• oo.ly) IV
PCDD/PCDP EPA l290 VariOUI 0 0 0 V
bopropyl Biber EPA 8020 100 "I,.. I· V
N
I
°'
----
Note1:
(l) EPA Met.bod 8040 Dct.eclioo l.imita:
Phenol
2-Cb.lorophc:nol
2-Nilrophcnol
2,◄-Dimcthylphcnol
2.4-Dichloropbcnol
4-0iloro-3-Metbylpbcool
a) Rdcr to Table SA-I
50"11>&
50"11>&
50 ual>&
50"11>&
50"11>&
50"11>&
(3) Orinling Water Metal• Mcthod:t and DctectioD:
Ancnic EPA 7060 1000 ug/kg
Barium EPA 6010 DX>O ug/kg
Cadmium EPA 6010 500 ug/kg
Ouomium EPA 6010 IOOO ug/kg
Mercury EPA 7-471 100 ug/kg
Lead EPA 7◄21 500 ua/kg
Selenium EPA TI.0 500 IJl/q:
Silver EPA 6010 l(XX) ug/kg
-- - - -
TABLE 2-2 (continued)
SOIL SAMPLE ANALYSIS
2,◄,6-Trichlorophcnol
2,◄-Dinitropbcool
4-Nilropbcool
2, 3 ,S, 6-Tctr■cbloropbeool
4 ,6-Dinitro-2-Methylpbcool
Pcntachloropbcool
100 ug/kg
1()() .. ,..
100"11>&
100 uglq
100"11>&
100"11>&
- - ---- --!111:1
Fire Pond &
Medlin Pond
Pniposed
Sediment
Sample
l,.AlCB(iOQS
S-2,S-4,S-5 S-7
S-JO,S-I 2,S-13A
S-14,S-19,S-21
S-4,S-10,S-13A
S-4,S-10,S-l JA
S-4,S-10,S-l JA
S-10, S-13A
S-!,S-3,S-6 S-8,S-9,S-11 S-13,S-15,S-18
S-20,S-22
S-1,S-15,S-18,S-22
S-1,S-15,S-18,S-22
S-1,S-22
S-18
See comments
--
No.or
Samples per Location
2
2
2
2
2
2
2
2
2
2
Estimated No.or Samoles
20
6
6
6
4
22
8
8
4
4
<JO
- ---- -- -
TABLE2-3
SEDIMENT SAMPLE ANALYSIS SUMMA KY
FIRE PONO/MEDLIN PONO
Parameter
Acid Extractable
Phenols
PCDD/PCDF
Analytical
Melhod
EPA 8040
EPA8290
Total Organic EPA 9060
Carbon
lsopropyl Ether EPA 8020
T Al/fCL Compounds EPA-CLP
Acid Extractable
Phenols
PCDD/PCDF
EPA8040
EPA8290
Total Organic EPA9060
Carbon
lsopropyl Ether EPA8020
T Al/fCL Compounds EPA-CLP
-gr&!n Size . moasture
-sieve hydrometer
-Allerberg limits
Deleclion Field Field Trip
Blank Limit Quplicale Blank
(I)
Various
100 mg/kg
100 ug/kg
(2)
(I)
Various
100 mg/kg
100 ug/kg
(2)
2
2
0
0
I
2
0
0
0
I/day I/day/cooler (volaliles only)
0
0 0
2 0
0 0
I/day I/day/cooler
(volatiles only)
-
DQO
Level
111
V
II
V
IV
Ill
V
II
V
IV
- --
Comments
When field conditions permit,
pond sediment samples will be
collected to a depth of 5 ket, 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 10 5.0-foot
interval.
Several pond sediment
samples will be analyzed .
for parameters to detcrmmc
the physical characteristics
of tliis material. The actual
number of samples ana~. and parameters chosen will be
determined in lhe field by
the supt?rvising hydf~)geologiat
and project geophy51cal i' :ii,
!·· ii ~!ll
-·-- - -
Draioageway No.or Total
Sample Samples No.or
Locations per Location Samoles
S-J6A, S-16B, S-17,
S-23 thru S-34
S-16B, S-23
S-16, S-23
S-23,S-25,
S-26,S-3 I, S-34
Notes:
I
I
I
I
(I) EPA Method 8040 Detection Limits
Phenol
2-Chlorophenol
2-Nitrophenol
2,4-Dimethylphenol
2,4-Dichlorophenol
4-Chloro-3-Methylphenol
15
2
2
5
50 ug/kg
50 ug/kg
50 ug/kg
50 ug/kg
50 ug/kg
50 ug/kg
------ -
TABLE 2-3 (Continued)
SEDIMENT SAMPLE ANALYSIS SUMMARY
DRAINAGEWAYS
- -
Parameter
Analytical
Method
Detection
Limit
Field
Duplicate
Field
Blank
Trip
Blank
Acid Extractable
Phenols
EPA8040 (I)
Total Organic EPA 9060
Carbon
1000 mg/kg
PCDD/PCDF EPA8290 Various 0
T AL/fCL Compounds EPA-CLP (2)
2,4,6-Trichlorophenol
2,4-Dinitrophenol
4-Nitrophenol
I
2,3,5,6-Tetrachlorophenol
4,6-Dinitro-2-Methylphenol
Pentachlorophenol
0
0
0 0
I/day I/day/cooler
(volatiles only)
JOO ug/kg
100 ug/kg
JOO ug/kg
JOO ug/kg
100 ug/kg
JOO ug/kg
~2) Refer to Table SA-I of this work plan for a list of detection limits.
One round of sediment sampling wt11 be performed for the above noted parameters.
-
DQO
I.eve!
Ill
II
V
IV
- --
Comments
At each loca1ion 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 the
surface.
At each location a
sample will be coll
from the surface.
-------------------
Notes:
(1) EPA Method 8040 Detection Limits
Phenol
2-Chlorophenol
2-Nitroplienol
2,4-Dimethylphenol
2,4-Dichlor9J)henol
4-Chloro-3-Methylphenol
50 ug!.!cg
50 ug/.!cg
50 ug!.!cg
50 ug!.!cg
50 ug!.!cg
50 ug/kg
TABLE 2-3 (Continued)
SEDIMENT SAMPLE ANALYSIS SUMMARY
2,4,6-Trichlorophenol
2,4-Dinitrophenol
4-NitroJ)henol
2,3,t6-Tetrachlorophenol
4,6-uinitro-2-Methylphenol
Pentachlorophenol
(2) Refer to Table 5A-1 of this Work Plan for a list of detection limits.
One round of sediment sampling will be performed for the above noted parameters.
N I "'
100 ug/.!cg
100 ug/.!cg
100 ug!.!cg
100 ug!.!cg
100 ug/.!cg
100 ug/kg
------ - - - ------
TABLE 2-4
GROUNDWATER SAMPLE ANALYSIS
Sample
Location
C-1 thru C-32,
M-4, M-9
C-4, C-27A,
',' C-28A and C-30
C-4, C-2SA,
C-26A, C-27 A, C-28A
and C-30
Notca:
Sampica
Per
I ocedon
(I) EPA Method 8040 Detrctioo 1.;mita:
Pbcaol
2-Chloropba,ol
2-Nitrophcaol
2,4-Dimcthylpha,ol
2,4-Dichloropbcaol
4-Chloro-3-Mc:lhylpha,ol
(2) Refer to Table 5A-I.
Elllimalcd
No. of
Sampica
(per round)
50
50
50
50
50
50
4
6
0.50 ug/1
0.50 ug/1
0.50 ug/1
0.50 ug/1
0.50 ug/1
0.50 ug/1
Parameter
Acid E1tractablc Phenolic,
Pe.ntachlorophcnol
l,opropyl Ether(•)
pH
Specific Conductance
T empcraturc
PCDD/PCDF(•)
T AUTCL Ii.a.(•)
• Finl round only. Second round poramdcn and ,ample locatlorui
dcpa,deal upoo rcoulta of fmt round.
Analytical Detection
Mc:lhod Limit
EPA 8040 (I)
EPA515 0.010 ug/1
EPA 8020 1.0 ug/1
EPA ISO.I
EPA 120.1 1 umho/cm
EPA 170.1
EPA 8290 Variou1
EPA-CLP (2)
2,4,6-Trichlorophcnol
2,4-Dinilrophcnol
4-Nitrophcaol
2,3,5,6-Tetrachlorophcnol
4,6-Dinitro-2-Mc:lhylphcnol
Pcatachloropbc.nol
Field
Duplicate
5
5
5
0
0
0
-
Rimatc
Blank
I
0
0
0
1.00 ug/1
1.00 ug/1
1.00 ug/1
1.00 ug/1
1.00 ug/1
1.00 ug/1
-
Trip
Blank
0
0
I
0
0
0
0
l(volatilca only)
-- -
DQO
Level
w
III
V
II
II
II
V
IV
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
TABLE 2-5
TCL AND TAL PARAMEfERS AND DETECTION LIMITS
(Taken from the CLP Statement of Work for Organics,
2/88 with 9/88 Revisions and In organics, 7 /88 with 9/89 Revisions)
TAL Parameters
Water Soil/Sediment
Parameters !!&Lt mg/kg
aluminum 200 40
antimony 60 12
arsenic 10 2
barium 200 40
beryllium 5 1
cadmium 5 1
calcium 5000 1000
chromium 10 2
cobalt 50 10
copper 25 5
iron 100 20
lead 5 1
magnesium 5000 1000
manganese 15 3
mercury 0.2 0.04
nickel 40 8
potassium 5000 1000
selenium 5 1
silver 10 2
sodium 5000 1000
thallium 10 2
vanadium 50 10
zinc 20 4
cyanide 10 2
TCL Parameters
SectiOIINoc2
RniliollN«l
Date: 03/ea/98
Page 11 of 16
Low
Level Water<2)
Low Level
Soil/Sediment<3)
Parameters Y&lL Y&lK&
Volatiles
Chloromethane 10 10
Bromomethane 10 10
Vinyl chloride 10 10
Chloroethene 10 10
Methylene Chloride 5 5
Acetone 10 10
Carbon Disulfide 5 5
1, 1-Dichloroethane 5 5
1, 1-Dichloroethene 5 5
trans-1,2-Dichloroethene 5 5
DCC#Q461
I Section No: 2
Revision No: 1
I TABLE 2-5 (Continued) Date: 03/08/90
Page 12of 16
Low Low Level
Level Water(2) Soil/Sediment(J >
I Parameters !!ilL Y&lK&
Chloroform 5 5
I 1,2-Dichloroethane 5 5
2-Butanone 10 10
1, 1, 1-Trichloroethane 5 5
I Carbon Tetrachloride 5 5
Vinyl Acetate 10 10
Bromodichloromethane 5 5
I 1, 1,2,2-Tetrachloroethane 5 5
1,2-Dichloropropane 5 5
trans-1,2-Dichloropropene 5 5
I Trichloroethene 5 5
Dibromochloromethane 5 5
I 1, 1,2-Trichloroethane 5 5
Benzene 5 5
cis-1,3-Dichloropropene 5 5
I 2-Chloroethyl Vinyl Ether 10 10
Bromoform 5 5
2-Hexanone 10 10
I 4-Methyl-2-pentanone 10 10
Tetrachloroethene 5 5
I Toluene 5 5
Chlorobenzene 5 5
Ethyl Benzene 5 5
Styrene 5 5
I Total Xylenes 5 5
Semi-Volatiles
I Phenol 10 330
bi~2-Chloroethyl) ether 10 330
2-hlorophenol 10 330
I 1,3-Dichlorobenzene 10 330
1,4-Dichlorobenzene 10 330
I Benzyl Alcohol 10 330
1,2-Dichlorobenzene 10 330
2-Methylphenol 10 330
I bi~2-chloroisopropyl) ether 10 330
4-ethylphenol 10 330
I N-Nitroso-Dipropylamine 10 330
Hexachloroethane 10 330
Nitrobenzene 10 330
I Is~horone 10 330
2-itrophenol 10 330
2,4-Dimethylphenol 10 330
I DCC#Q461 2-12
I Section No: 2
Revision No: 1
TABLE 2-5 (Continued) Date: 03/08/90
I Pase 13of 16
l.nw l.nw Level
Level Water<2) Soil/Sediment<3)
I Parameters ~ .!!llK&
Benzoic Acid 50 1600
I bis(2-Chloroethoxy) methane 10 330
2,4-Dichlorophenol 10 330
1,2,4-Trichlorobenzene 10 330
I Nc!tthalene 10 330
4-hloroaniline 10 330
Hexachlorobutadiene 10 330
I 4-Chloro-3-methylphenol
(Mra-chloro-meta-cresol) 10 330
I 2-ethylnaphthalene 10 330
Hexachlorocyclopentadiene 10 330
2,4,6-Trichlorophenol 10 330
2,4,5-Trichlorophenol 30 1600
I 2-Chloronaphthalene 10 330
2-Nitroaniline 50 1600
I Dimethyl Phthalate 10 330
Acenaphthylene 10 330
3-Nitroaniline 30 1600
I Acenaphthene 10 330
2,4-Dinitrophenol 50 1600
4-Nitrophenol 50 1600
I Dibenzofuran 10 330
2,4-Dinitrotoluene 10 330
I 2,6-Dinitrotoluene 10 330
Diethylphthalate 10 330
4-Chlorophenyl Phenyl
I ether 10 330
Fluorane 10 330
4-Nitroaniline 50 1600
B 4,6-Dinitro-2-methylphenol 30 1600
N-nitrosodiphentamine 10 330
4-Bromophenyl henyl ether 10 330
I Hexachlorobenzene 10 330
Pentachlorophenol 30 1600
, I Phenanthrene 10 330
Anthracene 10 330
Di-n-butylphthalate 10 330
Fluoranthene 10 330
!I Pyrene 10 330
Butyl Benzyl Phthalate 10 330
I 3,3' -Dichlorobenzidine 20 660
Benzo( a )anthracene 10 330
bis(2-ethylhexyl)phthalate 10 330
I DCC#Q461
2-13
I Sec:tl.on No: 2
Revilioa No: l
TABLE 2-5 (Continued) Date: 03/08/90
I Page 14of 16
Low Low Level
Level Water(2) Soil/Sediment(3)
I Parameters Y&lL !!ILK&
I Chrysene 10 330
Di-n-octyl Phthalate 10 330
Benzot ~fluoranthene 10 330
Benzo k fluoranthene 10 330
I Benzo a pyrene 10 330
Indeno~ 1,2,3-cd)pyrene 10 330
I Dibenz a,h )anthracene 10 330
Benzo(g,h,i)perylene 10 330
I Pesticides
alpha-BHC 0.05 8.0
beta-BHC 0.05 8.0
I delta-BHC 0.05 8.0
f:mma-BHC (Lindane) 0.05 8.0
I eptachlor 0.05 8.0
Aldrin 0.05 8.0
Heptachlor Epoxide 0.05 8.0
I Endosulfan I 0.05 8.0
Dieldrin 0.10 16.0
4,4'-DDE 0.10 16.0
I Endrin 0.10 16.0
Endosulfan II 0.10 16.0
I 4,4'-DDD 0.10 16.0
Endosulfan Sulfate 0.10 16.0
4,4'-DDT 0.10 16.0
I Endrin Ketone 0.10 16.0
Methoxychlor 0.5 80.0
Chlordane 0.5 80.0
I Toxaphene 1.0 160.0
AROCLOR-1016 0.5 80.0
AROCLOR-1221 0.5 80.0
I AROCLOR-1232 0.5 80.0
AROCLOR-1242 0.5 80.0
I AROCLOR-1248 0.5 80.0
AROCLOR-1254 1.0 160.0
AROCLOR-1260 1.0 160.0
I (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
I limits are highly matrix dependent. The detection limits listed herein are
provided for guidance and may not always be achievable.
I DCC#Q461
2-14
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
(2)
(3)
(4)
(5)
(6)
(7)
DCC#Q461
TABLE 2-5 (Continued)
Section No: 2
Revision No: 1
Date: 03/08/90
Page 15 or Hi
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 times 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 Quantitation Limits (CRQL) for
Pesticide TCL compounds are 15 times the individual Low Soil/Sediment
CRQL
2-15
N I -°'
-------------------
TABLE 2-6
QUALI1Y ASSURANCE BLANKS
Blank Number/Frequency Parameter
Trip Blank 1) One per day per cooler 1) Volatile Organic Analysis Only
Field Blank 2) One per day 2) Parameters specific to sample matrix
Preservation Blank 3) One throughout project 3) One complete set of project specific parameters
requiring preservation
Bentonite 4) Three/Beginning-Middle-End of Project 4) PCP
Grout Mixture 4) Three/Beginning-Middle-End of Project 4)PCP
Sand Pack 4) Three/Beginning-Middle-End of Project 4) PCP
1)
2)
3)
4)
See Tables in Section 2.0 of the QAPP and 3.0 of the Field Sampling Plan, for detailed information on sample matrix and
analysis.
See Tables in Section 2.0 of the QAPP and 3.0 of the Field Sampling Plan, for detailed information on sample matrix and
analysis. The field blank will encompass "sprayer solution blanks" as the organic free water used to collect the field blanks will
come from these sources.
One preservation blank will be collected for a complete set of project specific parameters. -
One sample each of Bentonite, Grout Mixture, and Sand Pack material will be collected during the beginning, middle and end
orthe project (assuming this material is from the same manufacturer) and analyzed for PCP. Additional constituents may be
added depending on the outcome of the TAC(l'CL compounds. The sample preparation, holding times, preservation and
analytical procedures used for these samples will be consistent with the procedures used for soil samples.
Note: The preservation, holding times and analytical techniques used for the above QA samples will be consistent with the
procedures required for the specific matrix and parameter of interest.
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
3.0 PROJECT ORGANIZATION AND RESPONSIBILI'IY
Section No. 3
Revision No. 1
Date 03/08/90
Page 1 of4
The following section describes the duties of key personnel assigned to the Remedial
Investigation at the former Koppers Company Superfund Site (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:
o Procurement, along with administrative personnel, and supervision of
subcontractor services;
0
0
0
0
0
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,
Project closeout.
Site Hydrogeologist
The Site Hydrogeologist will be responsible for field activities and data evaluation,
including items as follows:
DCC#Q461 3-1
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
0
0
0
0
0
Section No. 3
Revision No. 1
Date 03/08/90
Page 2 of4
Supervising the collection of the samples and providing for their
proper documentation, handling and shipping;
Maintaining a completion log for each borehole and monitor well
installed;
Monitoring the drilling and sampling operations to verify that the
drilling subcontractor and sampling team members adhere to the
QAPP;
Coordinating activities with the Project Manager; and,
Preparing the field investigation data.
Quality Assurance Officer
The Quality Assurance (QA) Officer is responsible for audits and monitors
adherence to the project QA objectives. The QA Officer acts independently of the
project team. His responsibilities include:
0
0
0
0
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No. 3
Revision No. 1
Date 03/08/90
Page3 of4
Laboratory Director
Responsibilities of the Laboratory Director include:
0
0
0
0
0
0
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 nonconformances and
changes in laboratory activities;
Notifying the laboratory and project management of specific
laboratory nonconformances and changes;
Maintenance of laboratory data;
Releasing of testing data and results; and,
o 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
0
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;
3-3
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
0
0
0
0
0
Section No. 3
Revision No. 1
Date 03/08/90
Page4 of4
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
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
4.0 OUALTIY ASSURANCE OBJECTIVES
Section No. 4
Revision No. 1
Date 03/08/90
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 response
activities. Data developed during the RI will be used for:
0 Risk assessment
o Site characterization
o Screening and evaluation of remedial alternatives
o Remedial design
Groundwater and surface water are the major pathways 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 000 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 descnbe 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No. 4
Revision No. 1
Date 03/08/90
Page 2 of9
measurements 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 EPA6010
Chromium EPA6010
Lead EPA 7421
Mercury EPA 7470
Magnesium EPA6010
Sodium EPA6010
Potassium EPA6010
Silver EPA6010
Chemical oxygen demand EPA410.4
Total suspended solids EPA 160.2
Lead EPA 7421
Mercury EPA 7471
Selenium EPA 7740
Silver EPA6010
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
4.4 CLP RAS Methods
Section No. 4
Revision No. l
Date 03/08/90
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 EPA 515
Isopropyl ether EPA 8020
Dioxins/furans EPA 8290
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
0
0
0
0
0
Section No. 4
Revision No. 1
Date 03/08/90
Page4 of9
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 (RPO) of
duplicates or duplicate spikes as appropriate. (See section 12.1 for
method of calculation).
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).
Representativeness -The sampling program is designed to ensure the
analytical data obtained during the Remedial Investigation represent
conditions found at the site. Sample locations were selected to ensure soil,
groundwater, surface water, and sediment analytical data are suitable for
the intended use and adequately characterize the site. A sufficient
number of samples will be obtained to ensure site conditions are
appropriately assessed.
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 developing 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.
4-4
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
0
Section No. 4
Revision No. 1
Date 03/08/90
Page 5 oC9
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.
Comparability • One of the objectives of the Remedial Investigation is to
ensure analytical data are of comparable quality. The data collection
mechanisms proposed are designed to produce comparable data. To
ensure comparable data, standard recognized analytical methodologies
will be followed.
To ensure comparability between samples over time consideration will be
given to seasonal conditions, flow or other environmental factors that may
influence the analytical results.
Tables 4-1 and 4-2 give the target limits for all analyses in terms of precision accuracy
and completeness.
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.
4-5
I
Section No: 4
I Revision No: 1
Date: 03/08/90
Page6 of9
I
I TABLE 4-1
QUALITY ASSURANCE OBJECTIVES (GROUNDWATER/SURFACE WATER SAMPLES)
I Spiting Precision Accuncy Completeness
Parameter Reference Level (RPD) (% RCCOl'CI)') (%)
I pentachlorophenol EPA515 0.10 ug/1 20 68-122 90
isopropyl ether EPA8020 5 ug/1 18 75-125 90
I total organic carbon EPA415.l 20 mg/I .9 85-115 90
chemical oxgyen demand EPA410.I 250 mg/I 9 85-115 90
biochemical oxgycn demand EPA405.I 15 90
suspended solids EPA 160.2 15 90
I pH EPA 150.1 0.2 units 75
specific conductance EPA 120.1 10 15
I Phenols
phenol EPA8040 100 ug/1 42 12-39 90
2<hlorophcnol EPA8040 100 ug/1 40 27-123 90
I 4-nitrophenol EPA8040 JOO ug/1 50 10-80 90
4-chloro-3-methylphenol EPA8040 100 ug/1 42 23-97 90
pentachlorophenol EPA8040 JOO ug/1 50 9-103 90
I TCL Volatiles
1, 1-dichloroethene EPA 8240-CLP 50 ug/1 14 61-145 80
trichloroethenc EPA 8240-CLP 50 ug/1 14 71-120 80
I chlorobcnzcne EPA 8240-CLP 50 ug/1 13 75-130 80
toluene EPA 8240-CLP 50 ug/1 13 76-125 80
benzene EPA 8240-CLP 50 ug/1 II 76-127 80
I ICb ScmrYOlatiles
1.2.4-trichlorobcnzene EPA 8270-CLP 50 ug/1 28 :l'J.98 80
acenaphthene EPA 8270-CLP 50 ug/1 31 46-118 80
I 2,4-dinitrotolucne EPA 8270-CLP 50 ug/1 38 24-96 80
di-n-butylphthalatc EPA 8270-CLP 50 ug/1 40 11-117 80
pyrcne EPA 8270-CLP 50 ug/1 31 26-127 80
I N-nitrosodi
-n-propylamine EPA 8270-CLP 50 ug/1 28 36-97 80
1,4-dichlorobcnzeoe EPA 8270-CLP 50 ug/1 28 36-97 80
I pcntachlorophcnol EPA 8270-CLP 100 ug/1 50 9-103 80
phenol EPA 8270-CLP JOO ug/1 42 12-39 80
2-chlorophenol EPA 8270-CLP 100 ug/1 40 27.123 80
4<hloro-3-methylphenol EPA 8270-CLP 100 ug/1 42 23-97 80
I 4-nitrophenol EPA 8270-CLP 100 ug/1 50 10-80 80
TCL Pesticides
I lindanc EPA8080-CLP 0.2 ug/1 15 56-123 80
heptachlor EPA 8080-CLP 0.2 ug/1 20 40-131 80
aldrin EPA 8080-CLP 0.2 ug/1 22 40-120 80
I DCC#Q461
4-6
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
II
Parameter
dieldrin
endrin
4,4'-DDT
TAL inorganics
aluminum
antimony
arsenic
barium
beryllium
cadmium
calcium
chromium
cobalt
copper
iron
lead
magnesium
manganese
mercury
nickel
potassium
selenium
silver
sodium
thallium
vanadium
zinc
cyanide
Dioxins/furans
2,3,7,8-TCDD
DCC#Q461
TABLE 4-1 (continued)
Section No: 4
Revision No: 1
Date: 03/08/90
Page 7 of9
QUALITY ASSURANCE OBJECTIVES (GROUNDWATER/SURFACE WATER SAMPLES)
Spiking Precision Accunlcy
Reference Lc,,el (RPD) (% RecoYCt)')
EPA8080-CLP 0.5 ug/1 18 52-126
EPA 8080-CLP 0.5 ug/1 21 56-121
EPA 8080-CLP 0.5 ug/1 Tl 38-ITI
EPA 6010-CLP 2000 ug/1 20 15-125
EPA 6010-CLP 100 ug/1 20 15-125
EPA 7060-CLP 40 ug/1 20 15-125
EPA 6010-CLP 2000 ug/1 20 15-125
EPA 6010-CLP 50 ug/1 20 15-125
EPA6010-CLP 50 ug/1 20 15-125
EPA6010-CLP 50 ug/1 20 15-125
EPA 6010-CLP 200 ug/1 20 15-125
EPA 6010-CLP 500 ug/1 20 15-125
EPA 6010-CLP 250 ug/1 20 75-125
EPA 6010-CLP 1000 ug/1 20 15-125
EPA 7421-CLP 20 ug/1 20 15-125
EPA 6010-CLP 20 ug/1 20 75-125
EPA 6010-CLP 20 75-125
EPA 7470-CLP I ug/1 20 75-125
EPA6010-CLP 500 ug/1 20 15-125
EPA 6010-CLP 20 75-125
EPA 7740-CLP 10 ug/1 20 75-125
EPA 6010-CLP SO ug/1 20 15-125
EPA 6010-CLP 20 15-125
EPA 7841-CLP SO ug/1 20 75-125
EPA 6010-CLP 500 ug/1 20 75-125
EPA 6010-CLP 500 ug/1 20 75-125
EPA 9012-CLP 100 ug/1 20 75-125
EPA8290 I ng/1 50 40-140
4-7
Completeness
(%)
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
90
I
I Section No: 4
Revision No: 1
Date: 03/08/90
Page 8of9
I
I TABLE 4-2
QUALITY ASSURANCE OBJECTIVES (SOITJSEDIMENT SAMPLES)
I Spiking Precision Accuracy Completenes.\
Parameter Reference LcYel (RPD) (% Rcoovcry) (%)
I total organic cartx>n EPA9060 1000 mg/kg 30 70-130 90
isopropyl ether EPA8020 500 ug/tg 20 75-125 90
I Phenol!
phenol EPA8040 10000 ug/tg 35 26-90 90
2-<:hlorophenol EPA8040 10000 ug/tg 50 25-102 90 I 4-nitrophcnol EPA8040 10000 ug/tg 50 11-114 90
4-chloro-3-methylphcnol EPA8040 10000 ug/tg 33 26-103 90
pcntachlorophcnol EPA8040 10000 ug/tg 47 17-109 90
I TCL volatiles
1, 1.dichlorocthene EPA 8240-CLP 50 ug/tg 22 59-172 80
I trichloroethcnc EPA 8240-CLP 50 ug/kg 24 62-137 80
benzene EPA 8240-CLP 50 ug/kg 21 66-142 80
toluene EPA 8240-CLP 50 ug/kg 21 59-139 80
chlorobcnzenc EPA 8240-CLP 50 ug/kg 21 60-133 80
I TCL scmivolatilcs
phenol EPA 8270-CLP 3300 ug/tg 35 26-90 80
I 2-chlorophenol EPA 8270-CLP 3300 ug/kg 50 25-102 80
1,4-dichlorobenzenc EPA 8270-CLP 1600 ug/kg Tl 28-104 80
N-nitroso-Oi-n-
I propylaminc EPA 8270-CLP 1600 ug/kg 38 41-126 80
1,2,4-trichlorobcnzcnc EPA 8270-CLP 1600 ug/tg 23 38-107 80
4-<hloro-l-mcthytpbcnol EPA 8270-CLP 3300 ug/kg 33 26-103 80
accnaphthene EPA 8270-CLP 1600 ug/kg 19 31-137 80
I 4-nitrophcnol EPA 8270-CLP 3300 ug/kg 50 11-114 80
2,4-dinitrotolucne EPa8270-CLP 1600 ug/kg 47 ~ 80
pcntachlorophenol EPA 8270-CLP 3300 ug/kg 47 17-109 80
I pyrenc EPA 8270-CLP 1600 ug/tg 36 35-142 80
TAL inorganics
I aluminum EPA 6010-CLP 20 75-125 80
antimony EPA 6010-CLP 10 mg/kg 20 75-125 80
arsenic EPA 7060-CLP 4 mg/tg 20 75-125 80
barium EPA 6010-CLP 200 mg/kg 20 75-125 80
I beryllium EPA6010-CLP 5 mg/tg 20 75-125 80
cadmium EPA 6010-CLP 5 mg/tg 20 75-125 80
calcium EPA 6010-CLP 20 75-125 80
I chromium EPA6010-CLP 20 mg/tg 20 75-125 80
cobaU EPA6010-CLP 50 mg/tg 20 75-125 80
copper EPA 6010-CLP 25 mg/tg 20 75-125 80
I DCC#Q461 4-8
I
I Section No: 4
Revision No: 1
Date: 03/08/90
I Page 9 of9
I TABLE 4-2
QUALITY ASSURANCE OBJECTIVES (SOILJSEDIMENT SAMPLES)
I Spiking Preci!ion Attul'll<:)' ComplelCncss
Parame1er Reference Level (RPD) (% Rccow:,y) (%) I iron EPA 6010-CLP 20 75-125 80
lead EPA 7421-CLP 2 mg/kg 20 75-125 80
I magnesium EPA 6010-CLP 20 75-125 80
manganese EPA 6010-CLP 50 mg/kg 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 TI40-CLP 1 mg/kg 20 75-125 80
silver EPA 6010-CLP 5 mg/kg 20 75-125 80 I sodium EPA 6010-CLP 20 75-125 80
thallium EPA 7841-CLP 5 mg/kg 20 75-125 80
vanadium EPA 6010-CLP 50 mg/kg 20 75-125 80
I zinc 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
aldrin EPA SOSO-CLP 32 ug/kg 43 34-132 80
I dieldrin EPA 8080-CLP 80 ug/kg 38 31-134 80
endrin EPA 8080-CLP 80 ug/kg 45 42-139 80
4,4'-DDT EPA 8080-CLP 80 ug/kg 50 23-134 80
I Dioxins/furans
2,3,7,8-TCDD EPA8290 I ug/kg 50 40-140 90
I
I
I
I
I
I DCC#Q461 4-9
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 5
Revision No: 1
Date: 03/08/90
Page 1 of31
5.0 SAMPLING EQUIPMENT AND PROCEDURES
In order to achieve the objectives of the Remedial Investigation and confirm and/or
obtain site specific information as outlined in Section 2.0 of the Field Sampling Plan,
the following areas will be investigated at the Morrisville, NC site:
0
0
0
surface water (ponds, ditches, streams), including flow measurements
sediment sampling (ponds, ditches, streams)
soil sampling
o groundwater monitoring
The number and location of the samples from each matrix are outlined in Section 3.0
of the Field Sampling Plan. This section outlines the procedures to be used in the
laboratory and in the field.
5.1 Sample Container and Equipment Preparation
The following procedures for the sample container and equipment preparation (and
decontamination) will be complied with during all phases of the RI investigation. To
ensure the cleanliness of the containers and equipment, quality assurance measures
will be employed.
Sample Container Preparation
All jars and bottles used to contain samples to be analyzed for project specific
parameters, will be cleaned and prepared in Keystone's Monroeville, PA laboratory,
according to the procedures outlined in Table 5-1. The containers used to collect the
surface water and groundwater samples require specific cleaning procedures
depending on the parameters of interest. The containers used to collect soil samples
do not require cleaning procedures. All sample containers required for this project
will be new, and will not be reused. Lids for all sample containers will be lined with
teflon.
DCC#Q-461 5-1
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: S
Revision No: 1
Date: 03/08/90
Page 2 of31
The cleanliness of a batch of precleaned 40 ml vials used to collect samples analyzed
for Volatile Organic Aromatics, is verified by the use of a trip blank. The trip blank
is prepared by filling a batch of precleaned 40 ml vials with organic free water. The
vials are transported to the site and returned to the laboratory in the same manner
used for the samples. Any contaminants found in the trip blank could be attributed
to a) interaction between the sample and the container, b) contaminated organic free
water, or c) a handling procedure which alters the sample. One trip blank is placed
in each cooler that contains samples for volatile organics.
Equipment Cleaning Procedures
Equipment prepared in Keystone's laboratory will be cleaned following the
procedures outlined below. Oeaning and/or decontamination performed in the field
will comply with EPA Region IV protocol. The field decontamination procedures
will be outlined in the specific sub-sections of this section.
Bailer and Funnel Preparation
1. 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)
H)
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 isopropanol.
Dry using pure nitrogen.
Heat for one hour at 800 degrees Fahrenheit.
Wrap in aluminum foil.
2. 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 polyethylene.
DCC #Q-461 S -2
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
;I
Section No: S
Revision No: l
Date: 03/08/90
Page3of31
To verify that no contaminants are introduced from sampling equipment, a field
(equipment) blank is collected by filling or pumping distilled organic free 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.
S.2 Surface Water Sampling
S.2.1 Sample/Location Selection
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 of the Field Sampling Plan. All surface water samples will be collected
prior to the collection of the sediment samples. The surface water sampling will
begin at the most downstream location and proceed upstream. This is intended to
avoid agitation of sediments upstream prior to collecting surface water samples at
downstream locations.
S.2.2 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.
1.
DCC#Q-461
In shallow streams (those which can be safely traversed on foot) the
sample 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 of the Field Sampling Plan) unless
insufficient flow precludes the collection of sample water. Sampling
S-3
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
2.
3.
Section No: S
Revision No: 1
Date: 03/08/90
Page4 of31
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
be made in the field by the project scientist/geologist. The field notes
and corresponding documentation will reflect such a decision_. If a weir
device is used it will be cleaned following procedures A) through F) of
Section 5. 7 of this document.
4. After the sample water has been collected, samples requmng
preservation will be preserved (see Tables 6-la and 6-lb of the Field
Sampling Plan 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 of the Field Sampling Plan.
S.3 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 of the Field Sampling Plan for the proposed
sample locations). All pond sampling will be performed from a floating platform by
a two person crew.
1.
DCC#Q-461
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.
S-4
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
2.
Section No: S
Revision No: 1
Date: 03/08/90
Page S of31
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.
1)
2)
3)
4)
5)
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
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.
wash with tap water and non-phosphate detergent.
rinse with tap water
rinse twice with pesticide grade isopropanol
rinse several times with organic free water
dry thoroughly and if not used immediately, wrap in foil and
plastic until next use.
Wash water and used solvent will be stored in designated containers
until sufficient amounts are available for future testing, treatment
and/or disposal.
DCC #Q-461 S -S
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
3.
4.
5.4
Section No: 5
Revision No: 1
Date: 03/08/90
Page6of31
All samples will be handled, preserved and shipped following the
procedures outlined in Section 6.0 of the Field Sampling Plan.
Field notes will be recorded (using indelible ink) to document 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.
Also, notes and documentation of field decisions will be submitted to
the EPA RPM and designated personnel on a regular basis and if
significant changes are required these personnel will be notified in a
timely manner.
Flow Measuring
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 effiuent stream will be
performed.
The following methods may be used to collect the flowrate from these open channel
flow systems:
1.
DCC#Q-461
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.
5-6
I
I
I
2.
I
I
I
I
I 3.
I
I 4.
I
I
I
I
I
I
I
I
I DCC#Q-461
Section No: S
Revision No: 1
Date: 03/08/90
Page 7 of31
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.
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 co=only 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.
5-7
I
I
I
I
1:
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I DCC#Q-461
Section No: S
Revision No: 1
Date: 03/08/90
Page 8or31
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
relationship of the primary measuring device, a totalized
volume can be determine from this flow rate.
o Other types of flow measuring devices include;
Float
Dipping Probe
Electrical
Ultrasonic
Bubbler
Submerged Pressure Transducer
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: S
Revision No: 1
Date: 03/08/90
Page 9 of31
Documentation
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. If flow measuring devices are used in a stream, the equipment will be
cleaned using procedures A) through F) in Section 5.7 of this document.
5.5 Sediment Sampling
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 of the
Field Sampling Plan. Sediment samples collected from surface water drainage
ditches will be collected from the O to 6-inch depth interval. The depths of sediment
samples collected from the Fire Pond and Medlin pond will be as follows:
0
0
0
at each pond sampling location, samples will be collected from the 2.5
to 5-foot interval,
at half the sampling locations in each pond, samples will be collected
from the Oto 2.5-foot interval, and
at the location where no sample is collected from the O to 2.5-foot
interval, a surface sediment sample will be collected using a ponar
dredge sampler.
Sediment sampling 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
DCC#Q-461 5-9
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: S
Revision No: 1
Date: 03/08/90
Page 10of31
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
sediment sample will then be taken in a fashion similar to the first sample. Surface
sediment samples will be collected using a ponar dredge sampler. Sediment samples
will be contained in new glass containers with teflon lined screw type lids. The
sampling equipment will be thoroughly washed between each use in non-phosphate
detergent, followed by a clean water rinse, two rinses with pesticide grade
isopropanol and organic free water rinses. 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 of the Field Sampling Plan).
5.6 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.
Downhole drilling equipment (i.e. augers, bits, spoons, samplers) will be
decontaminated between boring locations by the following procedure.
DCC#Q-461
1)
2)
3)
4)
5)
Wash equipment with tap water and non-phosphate detergent.
Rinse with tap water.
Rinse twice with pesticide grade isopropanol.
Rinse several times with organic free water or air dry for as long as
possible.
Dry thoroughly and cover equipment unless it will be used immediately
after cleaning.
5-10
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: S
Revision No: l
Date: 03/08/90
Page ll of3l
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. Soil samples will be contained in new glass containers with teflon lined
screw type lids, labeled, and stored on-site. As mentioned in Section 3.0 of the Field
Sampling Plan, the drill cuttings will be stored in labelled containers for future
storage, testing, treatment and/or disposal. 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-lb of the Field Sampling Plan). 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.
S.7 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 according to the procedures outlined above in Section 5.1. 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,
DCC#Q-461 S -11
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 5
Revision No: 1
Date: 03/08/90
Page 12 of31
handled, and shipped in accordance with the U.S. EPA Region IV SOPQAM (see
Tables 6-la and 6-lb of the Field Sampling Plan).
Equipment Preparation
Prior to performing a groundwater sampling project, the equipment used to collect
groundwater samples will be prepared in Keystone's Monroeville, PA laboratory, in
accordance with those procedures outlined above in Section 5.1. As outlined, the
stainless steel hailers and porcelain buchner funnels will be laboratory cleaned using
the following procedures:
A) Wash with non phosphate detergent.
B) Rinse with tap water.
C) Soak for five minutes in a 10% nitric acid solution.
D) Rinse with organic free water.
E) Rinse with pesticide grade isopropanol.
F) Dry using pure nitrogen.
G) Heat for one hour at 800 degrees Fahrenheit.
H) Cool to room temperature.
I) Wrap with aluminum foil (shiny side out).
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.
Bladder Pump Preparation
1. 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.
2. Each pump should be disassembled according to the manufacturer's manual.
DCC#Q-461 5-12
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
3.
4.
5.
Section No: S
Revision No: 1
Date: 03/08/90
Page 13 of31
The stainless steel parts of each pump are cleaned using the methods A)
through F) outlined above.
The remaining parts of each pump are washed with non-phosphate detergent,
and rinsed with organic free water.
Each pump is reassembled, wrapped in aluminum foil (shiny side out),
covered with plastic, and stored for future use.
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 co=only used to detect the presence of any floating or sinking
i=iscible layers. However they can also be used to detect the water levels inside
wells.
1. 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.
DCC #Q-461 S · 13
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
2.
3.
Section No: 5
Revision No: l
Date: 03/08/90
Page 14 of31
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
(.01).
The probe is decontaminated between each well by washing with a non-
phosphate detergent and tap water, rinse with tap water, rinse with organic
free water and wrap in polyethylene bag or foil until next use.
Electric Probe Method
1. 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.
2. 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.
3. The probe is decontaminated between each well by washing with a non-
phosphate detergent and tap water, rinse with organic free water and wrap in
polyethylene bag or foil until next use.
DCC #Q-461 5 • 14
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
. I
I
Well Purging
Section No: S
Revision No: 1
Date: 03/08/90
Page 1S of31
All monitoring wells are purged prior to sample collection. Purging of each well will
be performed from the top of the water column, using pumps or top filling stainless
steel hailers. 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 HzO 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#Q-461
1 1/8'' = 300 m1s
11/2" = 425 m1s
3.0" = 1850 mis
S-15
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Formula 1.0
Section No: 5
Revision No: l
Date: 03/08/90
Page 16 of31
Gallons of H20Dinear ft. of casini: diameter x 3785 (mls/1:al) x 3
volume of bailer
= conversion factor for each well being sampled
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 Casini: Volume Conversion
4.007
4.3363
4.0589
9.2086
After the purge volume is calculated, an amount equal to an additional five full bails
of water will be removed to ensure that, at a minimum, the required amount is
removed from each well.
Purginc and Samplinc Methods
Wells are purged and sampled by either hand bailing or pumping. The
determination to purge a well using pumps or ballers is influenced by the amount of
water to be removed from each well.
When possible all samples are collected using ballers. Hand bailing for sample
collection is preferred because ballers 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. Normally, pumps are used as sampling devices when
hailers can not be used as a result of well obstruction or the installation of
submersible pumps.
DCC#Q-461 5 -16
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Bailing
Section No: 5
Revision No: 1
Date: 03/08/90
Page 17 of31
The following procedures are followed when wells are purged and samples are
extracted using hand hailers.
1.
2.
3.
4.
5.
6.
7.
Place plastic sheeting ( or garbage bags) around the well casing to create a
clean working surface.
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
0
0
Make sure the knotted cord is securely tied to the bailer.
After removing the protective foil wrapping from the bailer, lower it
into the well until it touches the bottom.
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 by hand, over the plastic
sheeting.
Purged groundwater will be collected and stored for future testing, treatment
and/or disposa~ with the exception of purged water from designated off-site
wells.
As indicated, a separate laboratory-cleaned stainless steel bailer is used to
collect samples from each monitoring well.
o Samples are collected when the well recharges after purging.
DCC#Q-461 5-17
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
0
0
0
Section No: S
Revision No: 1
Date: 03/08/90
Page 18ot31
All samples are collected according to their order of volatilization (see
Table 5-2).
All volatile organic samples will be collected with laboratory cleaned
bottom filling stainless steel bailers in conjunction with an emptying
device.
When sampling all bailers 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.
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 bailers.
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. New nalgene suction line is used on each well being purged.
2. H a peristaltic pump is used to collect a sample, e.g., the well casing is bent
preventing the passage of a bailer, new silicon pump head tubing and teflon
tubing is used to collect the sample.
DCC #Q-461 S -18
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
3.
4.
5.
6.
7.
Section No: 5
Revision No: 1
Date: 03/08/90
Page 19of31
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 will
be measured in gallons per minute by recording the time required to fill a
selected volume of a calibrated bucket (see Section 5.7 on Well Purging).
Flow measurements should be performed three times on each well to obtain
an average rate.
The pumping is monitored to ensure proper pump operation and assure
continuous discharge. If drawdown occurs the tubing will be lowered 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, as appropriate, 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.
DCC#Q-461 5 -19
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: S
Revision No: 1
Date: 03/08/90
Page20 or31
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 using a laboratory cleaned stainless steel bailer.
1.
2.
3.
4.
5.
6.
7.
Connect the line assembly to the pump by first attaching the cable and then
connecting the sample and gas lines.
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.
Turn 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.
8. When the required amount of water has been purged, the well should be
sampled using a laboratory cleaned stainless steel bailer.
9. 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.
DCC #Q-461 S · 20
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 5
Revision No: 1
Date: 03/08/90
Page 21 of31
Submersible Pumps:
When wells are encountered with depths greater than 150 feet, stainless steel
submersibl_e 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 sample.
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 5.7. 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.
1.
2.
3.
4.
DCC #Q-461
The submersible pump and teflon discharge line should be lowered to a depth
in each well between the middle to bottom screened portion of each
monitoring well. The nylon 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 sufficient time for the well to recover.
This time will vary depending on the characteristics of each well and the time
required for recharging the well.
5-21
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
5.
6.
Section No: 5
Revision No: 1
Date: 03/08/90
Page 22 or31
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, as appropriate, in labelled containers for
future testing, treatment, and/or disposal.
5.8 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
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. 7. 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 of the
Field Sampling Plan).
5.9 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.
DCC#Q-461 5-22
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
5.10 Documentation
Section No: 5
Revision No: 1
Date: 03/08/90
Page 23 of31
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.
Analytical Request Form:
The analytical request forms (See Figure 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
Figure 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.
DCC#Q-461 5-23
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Field Data Sheets:
Section No: S
Revision No: 1
Date: 03/08/90
Page 24of31
The field data sheets (See Figure 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
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
Figure 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 of the Field Sampling Plan contain the holding times, and
protocol for proper preservation 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.
DCC#Q-461 5-24
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 5
Revision No: 1
Date: 03/08/90
Page25 of31
This infmmation 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#Q-461 5 -25
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
TABLE 5-1
Section No: S
Revision No: 1
Date: 03/08/90
Page26of31
SAM:PLE CONTAINER CLEANING PROCEDURES AND PRESERVATION
Parameter Matrix Preservative Sample Container
Extractable Organics water cool to 4°C I liter glass (amber)
Pentachlorophenol(515) water cool to 4°C 1 liter glass (amber)
Metals water HNO3 to pH <2 1 liter plastic
Isopropyl Ether,
Volatile Organics water cool to 4°C 40 ml glass with teflon septum
Total Organic Carbon water HOtopH<2 250 ml glass with teflon septum
BOD5,Suspended
cool to 4°C Solids water 1 liter glass
COD water NaHSO4• to pH <2 500 ml glass
All Parameters soil/sediment cool to 4°C 1 liter glass
1.
2.
Use new b()ttle; rinse with (pesticide grade) isopropanol, dry with pure nitrogen.
Use new b()ttle; rinse with 1:1 nitric acid and drain; rinse with D.I. water; rinse with
1:1 hydrochloric acid and drain; rinse with D.I. water and drain thoroughly.
3.
4.
•
•
Wash con11ainers and closnre with pre-filtered hot tap water using non-phosphate
detergent. Rinse three times with pre-filtered tap water. Rinse again with ASTM
Type 1 dei,()nized water. Over dry containers and closures at 105°C for one hour.
No cleanillig reqnired. Use new oottle.
NaHSO 4 is the salt form or H2so4 which is formed upon the addition or water to
act as the 1~reservative.
Lids for all containers will be lined with tenon .
DCC#Q-461 5-26
Cleaning
Procedure
1
1
2
3
3
4
4
4
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
TABLE S-2
ORDER OF VOI.ATILIZATION
Section No: S
Revision No: 1
Date: 03/08/90
Page27 of31
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 miscellaneous
parameters.
DCC#Q461 S -27
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I II
I
FIGURE 5-1
ANAi, Y'T'lCAL ,.,0u1n "0111M
:::int: ------------
-lec:r1u: -------------
Section No: 5
Revision No: 1
Date: 03/08/90
Page28of31
SIM 0111: -------
~•c. 0, MATJIUX AHAL YTIC,U, JII AIIAllfflM TUIIINAIIOUNO SA,IIIILII
TIMI. DAYS
• • a NrCa a SOWA a -.C:IIA a,..__ a 0a'ltr
Sc,1~111 lftll'IICllllfll; -----------------------
5 -28
I I I I I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
! I i i ,_, -I ~ ' ~ -\.i,,.,, .,., ;.:;,, i 0-"CQ ' '
:----------
:-----------:._______
,t::::
~
~
~
/ ac I
/ l11iJ Li ~
i Cl a: I !
8 §
I ...
5 ,.
8 ~ -• ... en :, u •··-...
0 ....
I .....
5 J I --<.)
~! ~ .. a
>-I I~ , ... i ~-1~1 ~ ~-~ ,i •
l I ! •
FIGURE 5-2 I ! I I I I I ' I I I
i ! i i I ' i
I I I I ! I
I i I I I I
I I I ! ! I
I I I I i '
I I I I !
I I I
!
I
I l ' I i i I I J J i I I ! I I I
I I I I I I I I I --i I I
I I J J
I
I '
I I , i
J J
I I • •
J )
! !
J J
I I • ,
I I
.. ;,;; ,.._
Section No: 5 Re .. N I VISIOD o: Date: 03/08/9CJ Page 29 of31 ~ 0 ' '1 ! ! ; ' I .. &
J
.. I
f ~ ..
!
J
!
1--
J
I
i
I i
J ' )
J
J I
!
J I
I I I
I a I ..
i -!
I I I I ' 1t:-1'~ I I
I
I
-! i -I I ii f! ! I · 'tr 1. I
' Iii, I : !i;; -1 , .. I ., I •• I~ I , 'l , I i1 I ii I .If-I ' I ,,. I ' ,
/_: 'llj
I j
! I
i
I ~ I ·;
I I C
a f
I I ;
I i i I C ...
I 5 i C ; ...
1JJ i 1•
i . ,J!] :I ~
i I 11,: I I a a rlii r= r= • a a
II '= 1:, z•
I
I ilfl
I Ill
I
I • !
•
I • • Ji
FIGURE 5-3 I ' I I I I I I I ' ! I ! I I I I ! I I I
I I
I i I I I '
I I I I
I I I I I I I
' I I I I I I .
I I I I I I I
' I I I '
I I I
I
I
I I
I I
I
. C 'lln
I I I I I
"
I
C • I
i
i
Section No: 5 Revision No: 1 Date: 03/08/90 3 (31 Page Oo ' ' ' ' I ' ' I ' i I ' I I I I :
i ' ',
:
' ! I ' I :
I
I
I I
!
!
' i ' I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Revised:
Plant :'-lame:
Ch:irge #:
FIGURE 5-4
COMPUTER GENERATED PRINTOUT
-EXAMPLE
ABCDE
111111-11-11
Section No: S
Revision No: 1
Date: 03/08/90
Page31 ot31
Wells:
Copy Reporu To:
R-1. R• 7, R-8, R-8B, R-9, R-9C, R-9O, R-10, SF· 1, SF-2, SF-3, SF-4 X. Smith, Y. Smith, Z. Smith
Turnaround: Normal
Sampling Dates: Quanerly
The folJ()wing is a list of parameten for which samples are analyzed:
field Meai.
pH(4X)
Cond.(4X)
'llaRSQ4
TOC(4X)
~OTES:
EPA8310
EPA8040
Tox(4X)
TOC, TOX. pH. and Cond. pt replicated 4x for all wells. • prepare an additional TOX bottle for all wells beinl replicated 4x.
DO NOT FU.TER ANY PARAMETERS.
THIS IS AN EXAMPLE COPY OF A COMPUTER GENERATED PRINTOUT.
I
I
I
I
I
I
I
I
I
I
I
n
I
I
I
I
I
I
I
6.0 SAMPLE CUSTODY
Section No. 6
Revision No. 1
Date 03/08/90
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.
b.
C.
d.
6.1
it is in your possession, or
it is in your view, after being in your possession, or
it was in your possession and you locked it up, or
it is in a designated secure area.
Field Sample Documentation
The field sampler will be personally responsible for the care and custody of the
samples colle,:ted until they are properly transferred or dispatched. Samples will be
accompanied by a Chain-of-~ustody 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 when: 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
I
I
I
I
I
I
I
I
I
I
I
i I
I
I
I
I
I
I
I
6.2 Laboratory Sample Documentation
Section No. 6
Revision No. 1
Date 03/08/90
Page 2 of6
Upon arrival at the laboratory, samples will be checked in by the Sample/Analysis
Coordinator or his designee. The following procedures will be followed:
a)
b)
c)
d)
e)
DCC#Q461
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.
He will next open the coolers and determine if proper temperature has
b,!en maintained during shipment. The temperature upon receipt is
recorded on the Chain-of-Custody Record.
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 possible that
samples were damaged and that they must be resampled, or the testing
program changed.
He ,vill 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-
Custocly Record and attach any waybill to the Chain-of-Custody
Record.
6-2
I
I
I
I
I
I
I
I
D
I
I
I
I
I
I
I
I
I
Section No. 6
Revision No. 1
Date 03/08/90
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 th1! 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
the 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
I
I
I
I
I
I
I
I
I
I
D
I
I
I
I
I
I
I
I
Parameter
Suspended Solids
Isopropyl Ether, Volatile Organics
Phenols, Pentachlorophenol,
Semivolatiles
BOD5 Within 48 hours of collection
TOC, COD, Mercury
Dioxins/Furans
Metals Within 180 daiys of collection
TABLE6-l
HOLDING TIMES
Holding Time•
Within 7 days of collection
Within 14 days of collection
Section No. 6
Revision No. 1
Date 03/08/90
Page4 or 6
Within 7 days of collection (for extraction)
Within 40 days of extraction ( for analysis)
Within 28 days of collection
Within 30 days of collection (for extraction)
Within 40 days of extraction (for analysis)
• (Federal Regi:iter, Vol. 49, No. 29, 1984, p43260)
6-4
-------------------
----Pl.ANTCOOE
-SAMPtfRS
(S.,,,,.,.,,•I
STA NO.
CHAIN OF CUSTODY RECORD
----PAOJECTNAME . -
DATE T-i Q : • .. • • STATION LOCATION • • •
NUMBER
OF
CONTAINERS
l
REMAAo<SOfl
0881:RVATIOINa
F===+=+=t=t=1~t======±===t=Jc{=J_c ·~-------
0.. p ¥ I I ted bw: /Sip I,,..,
flalN r I hdby: l~J 0.. T-,._ I adll.,:.-S. -.J
0..
looa-t
II JI I 71'11.... I I, CGpf IO Coor4iftllkW Raid f'-..
PAOE __ O
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Figure 6-2
Wors Order ____ _ s~1ple M~berJ ______ _
AN~1~ '!SIS t
Section No. 6
Revision No. l
Date 03/08,'90
Page6 of6
•• . H ~-:11~::-.-:1 _________ ::·_:::::-·----------------An: ~~ony _____ _ Arsen1: __________________________ _
9arl..m __ _
Beryl!~ -.. m ____________________ -_-_-_-_: _____ -_-_:_-_-_-___ ,. ______________________________ _ Cad.11·.-m __________ _
"Cal: ~· .. 111=--------------·---------------
Chr,:1111~--------------------------C:b,1l t ---------------------------C:;i~•r --------·----------------------: r: iii _______________ _ :.eaci_, ____ _
~ar.1111 .. 111 __ _ ~ar.4rane1e ___________________________ _ ~•r~:ury ______________________________ _
"' L, l . 1:,.1 --------:'~i:1111 i .. 111 ______________ _
S l -------------
• t,n1.·..m _______ , ___________________ _
Si.:ver
s~a1ia _____________________________ _
.. ,. '1 · ·"·• .~-----------·------------------... . ~~-----------,--------------------r~:a,u·..m Vanad1~----------------------------
Zinc _______________ ·-------------
OTHl:ll AJIAZ.YTU 1._, ____ _
z._, ___ _ 3. ____ _
btr11d1oa C.ab K&aqer ___________ Date ___ __,;,,,_ I:or1ru1c1 C.ab K&a•c•r Dat•----QA !'!1lAacer Dat•-----
~ote: !t 1aaple1 are re•di1e1ted and re•ualvzed bee•~•• the in1tl,al e:1deavor1 ta1!ed to meet the required Q"alitY Con:::: Cr:.:•1ri.a. :~e aa:11 ot re·di1e1:toll acd/or re·analv•~• w.:.~ :, 1nte1·ed l.e C~l:.i:r. :: Addit.:.=nal:y
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
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. 1
Date 03/08/90
Page 1 ofl
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
8.0 CALIBRATION CONTROLS AND FREQUENCY
Section No. 8
Revision No. 1
Date 03/08/90
Page 1 ofl3
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, and a post
calibration is performed at the end of each day. 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 cahbrations are recorded on a field instrument cahbration sheet
(Figure 8-1 ).
8.2 Laboratory Instrumentation • Miscellaneous 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No. 8
Revision No. 1
Date 03/08/90
Pagel ofl3
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. H 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No. 8
Revision No. 1
Date 03/08/90
Page3ofl3
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
8.4 Laboratory Instrumentation -Organics
Section No. 8
Revision No. 1
Date 03/08/90
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 descnbed 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
I
I
I
I
I
I
I
I
I
I
I
I
I
D
I
I
I
I
2. Initial Calibration:
Section No. 8
Revision No.1
Date 03/08/90
Pages of13
2.1 Prepared multi-level calibration standards 1 keeping one of the
recovery standards and the internal standard at fixed
concentrations (500 ng/ml).
Additional internal standards ( 13c12-0CDD 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-H pCDD
2,3, 7,8-TCDF
1,2,3, 7,8,PeCD F
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 isomer,
OCDD,OCDF, 13c1z-2,3,7,8-TCDD, 13C121,2,3,4-TCDD and 13c1z-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 caltbration
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 13c12-Jabeled analytes are available from Cambridge Isotope Laboratory,
Woourn, 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.
DCC#Q461 8-5
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No. 8
Revision No. 1
Date 03/08/90
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 calibration 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
HxCDD
HpCDD
OCDD
TCDF
PeCDF
HxCDF
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
l,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
l,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/fCDF 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.
CC#Q461 8-6
I
I
I
I
I
I
I
I
I
I
I
I
I
n
u
I
I
I
I
Section No. 8
Revision No. 1
Date 03/08/90
Page 7 ofl3
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)(lOO)
=
=
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.
DCC#Q461
4. 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.
5.
6.
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 13C1z-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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
7.
8.
9.
Section No. 8
Revision No. 1
Date 03/08/90
Page8 ofl3
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 calibration 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.
9.2
DCC#Q461
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No. 8
Revision No. 1
Date 03/08/90
Page9 of13
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
:I
I
I
I
I
Analytes
Ag
Ba
Cd
Co
Cr
Cu
Mn
Ni
Pb
V
Zn
TABLE8-l
INTERFERENT AND ANALYTE ELEMENTAL
CONCENTRATIONS USED FOR ICP
INTERFERENCE CHECK SAMPLE
(mg/I} Interferents
LO Al
0.5 Ca
LO Fe
0.5 Mg
0.5
0.5
0.5
LO
LO
0.5
LO
8-10
Section No. 8
Revision No. l
Date 03/08/90
Page 10 ofl3
/mg/I}
500
500
200
500
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
TABLE 8-2
Section No 8
Revision No 1
Date 03/08/90
Page 11 of13
METHOD DETECTION LIMITS OF 13C12 · LABELED PCDDs AND PCDFs
IN REAGENT WATER (PPT) AND ENVIRONMENTAL SAMPLES (PPB)
13c -Labeled 12 Reagent Mi.s.souri Fly-Industrial Slill-Fuel Fuel OiV
Analytc Water3 Soub Ashb Sludgec Bottomd Oild Sawdustb
2,3,7,8-TCDD 0.44 0.17 0.07 0.82 1.81 0.75 0.13
1,2,3,7,8-PeCDD 1.27 0.70 0.25 1.34 2.46 2.09 0.18
1,2,3,6,7,8-HxCDD 2.21 1.25 0.55 2.30 6.21 5.02 0.36
l,2,3,4,6,7,8-HpCDD 2.77 1.87 1.41 4.65 4.59 8.14 0.51
OCDD 3.93 2.35 2.27 6.44 10.1 23.2 1.48
2,3,7,8-TCDF 0.63 0.11 0.06 0.46 0.26 0.48 0.40
1,2,3,7,8-PeCDF 1.64 0.33 0.16 0.92 1.61 0.80 0.43
1,2,3,4,6, 7,8-HxCD F 2.53 0.83 0.30 2.17 2.27 2.09 2.22
~Sample size 1,000 mL
Sample size 10g.
~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:
-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 from cooling tower which received creosotic and pentachlorophenolic
wastewaters. Sample was~-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
1982. Using this procedure, the method detection limit is defined as the 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
TABLE 8-3
Section No 8
Revision No 1
Date 03/08/90
Page 12 ofl3
CRITERIA FOR ISOTOPIC RATIO MEASUREMENTS FOR PCDDs AND PCDFs
PCDDs
Tetra
Penta
Hexa
Hepta
Octa
PCDFs
Tetra
Penta
Hexa
Hepta
Octa
DCC#Q461
Selected ions
(m/z)
320/322
358/356
392/390
426/424
458/460
304/306
342/340
376/374
410/408
442/444
8-12
Relative Intensity
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
F'igure 8-l
~H MIT'IJI.
Section No. I
Revision No. 1
Date 03/08t'9G P,o;ec:: Oater Page 13 oll3 --Mt!ltl
1 ' I lr1i :,aJ C1li~,11,or1 ·::.cs,_1:.,:.,'u..,1_,_N.._-t----+-----4----i----,._ ___ 1
ICI l',,jl°t I'd
~ill.a 1iOl'I c~eclcs 111ould ~• ""•* attar ... .,,, l O r1M11111 IIIUII IN '" 7 ..Uw 101 .. 1,0fl (· •. •U1unN ,ua,.•.,). It rHGll'II .,. WltNl'I .I 0Uli1 at Ille NA11iM "9 cauAr11ior1 1Giun:,,er1r .1 ,,.,., •• 1I 1ru11t fflM .l a coffl,lete ~UM ll -■-,y (Uiu•~" ,eadir11), 11 '""" !,'la,, .2 40 I C01"1PJ•1• ~--.,_ iw-11M N lrequa,,cy ol e&l~tl llOl'I C.'lecil&.
Ooen1or 5i&fla!\U'&i
CQN0Uc:TMT"\' MITU
!1 -l■t 1e111,a,1Nt _ • 1111 hAfN. (U 1111, -tl!'!'!P. a.lilll1ffletlt)
Teffl,-,&U. Aa,.,_,..111
___ Ytt
z,ec: • II N '9111,-i'lfllf■ ., 'Cl\t .. ,,.,, • .a lleJow 2,~ ••• 2" o, \.'II , ... ill.
Swiw11
( H"'"es1 smJ
l. ,:, z. ,:o
j, i:~
,..., ..
• 11. ll'le ttffl,.INr■ i, ..... z,ec, Mtt&r. 211 ol ':.'II rt&Cilll par d .. , ..
,...,., .,,.,,
•
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
9.0 DATA REDUCTION, VALIDATION, AND REPORTING
Section No. 9
Revision No. l
Date 03/08/90
Pagel 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:
r = ( [N E 2 2 X; -(E X;) l
The acceptable values for the regression coefficient were given in Section 8. The
sample results are calculated according to the following formula:
y=mx+b
where y is they coordinate, xis the x coordinate, m is the slope, and b is 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No. 9
Revision No. 1
Date 03/08/90
Page 2 of4
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
value used in the calculation: 31 x 350.1 = 10,853.1, rounded off to 11,000.
9.2 Laboratory Data Validation
The Quality Assurance Department will validate all data prior to reporting. The
following procedures are used:
DCC#Q461
1) Standard curve is prepared prior to sample analysis
2) Standard regression coefficient is within the acceptable range
3) Standard reference materials are analyzed at proper frequency with
4)
5)
6)
7)
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
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. 1
Date 03/08/90
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 ~th the final report.
Laboratory data for transmittal to the U.S. EPA Region IV 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 exlubit 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
9.5 Independent Data Validation (Non-CLP Samples)
Section No. 9
Revision No. 1
Date 03/08/90
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
10.0 OUALl1Y CONTROL PROCEDURES
Section No: 10
Revision No: 1
Date: 03/08/90
Page 1 or19
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.
10.1 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 weli as other miscellaneous parameters analyzed in the
DCC#Q461 10-1
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 10
Revision No: 1
Date: 03/08/90
Page 2 of19
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 (DFfPP) for acid and base/neutral
extractable compounds and p-bromotluorobenzene (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 compounds must
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 (DITPP}
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. DFfPP must be analyzed separately or as part of the
DCC#Q461 10-2
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 10
Revision No: 1
Date: 03/08/90
Page3 oC19
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 procedures 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 10
Revision No: 1
Date: 03/08/90
Page4 of19
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 10
Revision No: 1
Date: 03/08/90
Pages ofl9
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 and 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 rn Table 10-6. When the
surrogate recovery level is outside of the control limits, the laboratory must take the
following actions:
0
DCC#Q461
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
0 Recalculate or reinject/repurge the sample or extract.
o Re-extract and reanalyze the sample.
Section No: 10
Revision No: 1
Date: 03/08/90
Page 6otl9
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 internal 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-d10
Chrysene-d12
l,4-dichlororbenzene-d4
10-6
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
o Naphthalene-dg
o Perylene-d12
o Phenanthrene-d 10
Section No: 10
Revision No: 1
Date: 03/08/90
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 blank will meet the criteria established in the current CLP
protocol. If a laboratory reagent blank exceeds criteria, the analytical 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
10.3 Organic Analyses -GC
Section No: 10
Revision No: 1
Date: 03/08/90
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 calibration 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
levels are given in Table 10-6.
Reagent B)ank and Matrix Spjke/Matrix Spjke Duplicate Analysis
These parameters will be run at the same frequency as stated for the GC/MS
procedures.
DCC#Q461 10-8
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Pesticide and PCB ONOC Requirements
Section No: 10
Revision No: l
Date: 03/08/90
Page9ofl9
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 I implemented by the laboratory.
I DCC#Q461 10 · 9
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Initial Calibration and Calibration Verification
Section No: 10
Revision No: 1
Date: 03/08/90
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
To verify inter-element and background correction factors an ICP Interference
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 specified 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 10
Revision No: 1
Date: 03/08/90
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 sample 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 Ieasf 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.
10.5 Metals by Furnace Atomic Absorption
Furnace Atomic Absorption (AA) analysis will be performed on metals 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No: 10
Revision No: 1
Date: 03/08/90
Page 12 of19
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 assurance/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 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.
10.6 Mercury by Cold Vapor Atomic Absorption
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
10.7 General Chemistry Parameters
Section No: 10
Revision No: l
Date: 03/08/90
Page 13 or 19
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
I Revision No: 1
Date: 03/08/90
Page 14 of19
I TABLE 10-1
I p-BROMOFLUOROBENZENE (BFB)
KEY IONS AND ION ABUNDANCE CRITERIA
I MASS ION ABUNDANCE CRITERIA
50 15.0 -40.0 percent of the base peak
I 75 30.0 -60.0 percent of the base peak
I 95 base peak, 100 percent relative abundance
96 5.0 -9.0 percent of the base peak
I 173 less than 1.00 percent of the base peak
174 greater than 50.0 percent of the base peak
I 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
177 5.0 -9.0 percent of mass 176
I
I
I
I
I
I
I
I
I DCC#Q461 10 -14
I
I Section No: 10
Revision No: l
Date: 03/08/90
I
Page 15 of 19
TABLE 10-2
I DECAFLUOROTRIPHENYLPHOSPHINE (DFfPP)
KEY IONS AND ION ABUNDANCE CRITERIA
I 51 30.0 -60.0 percent of mass 198
I 68 less than 2.0 percent of mass 69
70 less than 2.0 percent of mass 69
I 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
275 10.0 -30.0 percent of mass 198
I 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
I
I
I
I
I
I
I DCC#Q461 10-15
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
TABLE 10-3
Section No: 10
Revision No: 1
Date: 03/08/90
Page 16of19
VOLATILE INTERNAL STANDARDS WITH CORRESPONDING
ANALITES ASSIGNED FOR QUANTITATION
Chloromethane 2-butanone 2-hexanone
Bromomethane 1, 1,1-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 (surr)
1,2-dichloroethane·d 4 2-chloroethyl vinyl ether
(surr) Bromoform
DCC#Q461 10 -16
---------------TABLE 10-4
ACID ""'1ttlASFJNEUTRALl!XTRACTABLE INTERNAL STANDARDS WITH CORRESPONDING
TCL ANALYI'ES ASSIGNED FOR QUANTITATION
-
l,4-DICHWROBENZENE-d4 NAPTlfALENE-d8 ACENAPHTHENE-d1 o PIIENANTHRENE-d10 CHRYSENE-d12
Phenol
Bis(2-chorethyl)ether
2-chlorophenol
1,3-dichlorobenzene
1,4-dichlorobenzene
Benzyl alcohol
1,2-dichlorobenzene
2-methylphenol
Bis(2-chlorosopropyl) ether
4-methylphenol
N-nitroso-di-n-propylamine
Hexachloroethane
2-fluorophenol (surr)
Pheno1-<16 (surr)
Nitrobenzene
Isophoronc
2-nitrophenol
2,4-dimethylphenol
Benzoic acid
Bis(2-chloro-cthoxy)methane
2,4-dichlorophenol
1,2,4-trichlorobenzene
Naphthalene
4-chloroaniline
Hexachlorobutadiene
4-chloro-3-methylphenol
2-methylnaphthalene
Nitrobenzene-d5 (surr)
Hexachlorocyclpcntadiene
2,4,6-trichlorophenol
2,4,5-trichlorophenol
2-chloronaphthalene
2-nitroaniline
Dimethyl phthalate
Acenaphthylene
3-nitroaniline
Acenaphthene
2,4-dinitrophenol
4-nitrophenol
Dibenzofuran
2,4-dinitrotoluene
2,6-dinitrotoluene
Diethyl phthalate
4-chlorophenyl phenyl ether
Fluorene
4-nitroaniline
2-fluorobiphenyl (surr)
2,4,6-tribromophenol (surr)
4,6-dinitro-2-methylphenol
N-nitrosodiphenylaminc
1,2-diphcnylhydrazine
4-bromophenyl phenyl ether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di-n-butyl pthalate
Fluoranthene
Pryene
Butyl benzyl phthalate
3,3• -dichlorobenzidinc
Benzo(a)anthraccne
Bis(2-ethylhexyl)phthalate
Chrysene
Terphcnyl-d14 (surr)
---
PERYLENE-d12
Di-n-octyl phthalate
Benzo(b) fluoranthene
Benzo(k)fluoranthene
Benzo( a )pyrene
Indeno( 1, 2,3-cd)pyrene
Dibenzo( a,h )anthracene
Benw(g,h,l)preylene
I
I
I
I
I
I
I
I
I
I
Volatiles (GC or GC/MS)
1, 1 dichloroethene
chloroform
1,2-dichloropropane
toluene
ethylbenzene
vinyl chloride
Base Neutrals (GC/MS}
acenaphthene
1,4-dichlorobenzene
hexachlorobutadiene I N-nitrosodi-n-phenylarnine
fluoranthene I benzo(a)pyrene
I
I
I
I
I
I
I DCC#Q461
TABLE 10.5
CALIBRATION CHECK COMPOUNDS
Section No: 10
Revision No: 1
Date: 03/08/90
Page 18 of19
Acid Extractable Phenols (GC or GC/MS}
4-chloro-3-rnethylphenol
2,4-dichlorophenol
2-nitrophenol
phenol
pentachlorophenol
2,4,6-trichlorophenol
10-18
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
:I
I
! I
I
TABLE 10-6
Section No: 10
Revision No: 1
Date: 03/08/90
Page 19 of19
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-d8 88-110
4-bromofluorobenzene 86-115
1,2-dichloroethane-d4 76-114
EPA8270(CLP) nitrobenzene-d5 35-114
2-fluorobiphenyl 43-116
p-terphenyl-ct14 33-141
phenol-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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
11.0 PERFORMANCE AND SYSTEM AUDITS
Section No. 11
Revision No. 1
Date 03/08/90
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 system audits
to verify contract compliance or the laboratories ability to meet certification
requirements on methods of analysis and documentation.
DCC#Q461 11-1
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
12.0 ASSESSMENT PROCEDURES FOR LABO RA TORY DATA
ACCEPTABILITY
Section No. 12
Revision No. 1
Date 03/08/90
Page 1 or4
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 (RPD) of replicate spike samples or replicate sample
analyses according to the following equation:
RPD = Rl-R2
(Rl + R2)/2
12.2 Accuracy
X 100 where RI= 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Completeness(%)=
Section No. 12
Revision No. l
Date 03/08/90
Pagel of4
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 XI JJ
n•1
12 -2
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
standard deviation =
Section No. 12
Revision No. 1
Date 03/08/90
Page3 of4
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 12-1.
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
5 ·~ C .. I,
..
~ • I .. .. a
110
roo
10
10
IO
,o
i-, ,, ,.
I 7 ,. ,.
" 11
If
" ,.
• • ,
• ' •
1
2
0
FIGURE 12-1
I
I \
Section No. 12 Revision No. 1 Date 03/08/90
Page4 of4
I 2 J • I I 7 I f 10 II 12 II II II II 17 II It • ~ir--.a
~~ECISl<JN Pl.Of
'le.PaJ• ,...,.
DCC#Q46~ ...
1 I t 10 II 12 II II II II '1 'I If » U-4
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
13.0 PREVENTIVE MAINTENANCE
Section No. 13
Revision No. 1
Date 03/08/90
Page 1 of3
Periodic preventive maintenance is required for equipment whose performance can
affect results. Instrument manuals are kept on file for reference if equipment 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 miscellaneous 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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
g) Rinse three times with distilled water
h) Heat at soo0 c for 2 hours
Section No. 13
Revision No. 1
Date 03/08/90
Page2 of3
13.2 Routine Preventive Maintenance (Field and Laboratory Equipment)
(Keystone Environmental Resources, Inc., "Laboratory Standard
Operating Procedures", 5/88).
pH Meters
1)
2)
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
3) Replace filling solution as needed
Conductivity Meters
1)
2)
Keep battery fully charged
Replatinize cell when response becomes erratic or platinum black has
flaked off the cell
Liquid Chromatographs
1) Replace pump check valves every 6 months
2) Replace pump seals as needed
3) Use 3 to 5 cm pellicular guard columns
columns
Gas Chromatograpbs
1) Change septa daily
2) Periodically clean detectors
to protect the analytical
3) Replace columns when instrument response deteriorates
DCC#Q461 13-2
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Inductively Coupled Plasma Spectrophotometers
Change pump tubing every 4 hours of operation
Clean nebulizer daily
Section No. 13
Revision No. 1
Date 03/08/90
Page3 of3
1)
2)
3) Periodically clean and replace torch and chimney extension
Atomic Absorption Spectrophotometers
1) Periodically clean sample cells
Auto Analyzers
1) Clean platen daily
2) Change tubing and wipe pumprollers weekly
3) Clean colorimeter monthly
4) Grease pump and gears every 6 months
Analytical Balance
1)
2)
Check daily with class S weights
Oean and calibrate once per year
Mass Spectrometers
1) Periodically dismantle and clean the ionizing source
DCC#Q461 13-3
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
14.0 CORRECTIVE ACTION
Section No. 14
Revision No. l
Date 03/08/90
Pagel of3
Corrective action procedures are divided into two subgroups, notably, methods
corrective action and systems corrective action.
14.l 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 corrects 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 initiated 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.
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 from more
DCC#Q461 14-1
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Section No. 14
Revision No. 1
Date 03/08/90
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
1 I
i
!1
Laooratory Group: □ a
D
D
D
a
FIGURE 14 - 1
INVALID CATA NOTIFICATION
GC Date of Notification:
GC,MS
HPLC
Metals
Parameter:
Wet Chemistry
Mlscellaneous QC BalcnNo.
Section No. 14
Revision No. 1
Date 03/08/90
Page3 ot3
Data for the following samples. which have been submitted on ____ _ are not
valld.
TRAVELLER SAMPLE
NUMBER IDENTIFICATION
p I +r:_ ________________________ _
Submitted ti, _______ _
DCC#Q461
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
15.0 OA REPORTS TO MANAGEMENT
Section No.: 15
Revision No.: 1
Date: 03/08/90
Page 1 of 1
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
I
I
I
I
I
I
I
I
I
I
I
I
I
I
REFERENCES
Ackers, P., White, W.R., Perkins, J.A., and Harrison, AJ.M., Weirs and Flumes for
Flow Measurement, John Wiley & Sons, New York, NY (1978).
Federal Register, Vol. 49, No. 29, 1984, p 43260.
Keystone Environmental Resources Standard Operating Procedure. 1986.
Packa~ni and Shippini of Samples. Number 502.
Keystone Environmental Resources Standard Operating Procedure. 1986. Quality
Assurance/Quality Control for Groundwater Samplini. Number 504.
Kirkpatrick, George A., and Shelley, Philip E., Sewer Flow Measurement -A State-
of-the-Art Assessment, EPA Environmental Protection Technology Series,
EP A-600/2-75-027 ( 1975).
Mougenot, G., Measurini Sewar Flow Usini Weirs and Flumes, Water & Sewage
Works, July 1974, pp. 78-1.
Open Channel Flow Measurement Handbook, Isco, Lincoln, Nebraska (1988).
Scalf, M.R., J.a. McNabb, W.J. Dunlap, R.L Cosby and J. Fryberger. 1981. Manual
of Groundwater Samplini Procedures. U.S. EPA Robert S. Kerr.
Environmental Research Laboratory. Ada, OK: NWW A/WP A Series 1981.
Smoot, G.F., A Review of Velocity Measurjn~ Devices, United States Department of
the Interior, Geological Survey Open ile Report (April 1974).
Stevens Water Resources Data Book, 2nd Edition, Leupold & Stevens, Inc.,
Beaverton, Ore. (1974).
U.S. Environmental Protection Agency, Region IV, Environmental Services Division.
Engineerin~ Support Branch, Standard Operatini Procedures and Quality
Assurance ManuaI. April 1, 1986.
U.S. Environmental Protection Agency. 1982. Test Methods for Evaluatini Solid
Waste. 2nd ed. SW-846.
U.S. Environmental Protection Agency. 1984. Characterization of Hazardous Waste
Sjtes, A Methods Manual. Volume 2.2nd ed. EPA-600/4-84-076.
U.S. Environmental Protection Agency. September, 1986. RCRA Technical
Enforcement Guidance Document.
U.S. Environmental Protection Agency. February, 1988 with revisions September,
1988. Contract Laboratory Program (CLP), Statement of Work for Organics,
Multi-media, Multi-concentratin.
U.S. Environmental Protection Agency. July 1988 with revisions September 1989.
Contract Laboratory Program (CLP), Statement of Work for Inorganics,
Multi-media, Multi-concentration.
DCC#Q-461 -1-
.~·.
I
I
I
I
I
I APPENDIX A
I EXPORT PROTOCOL FOR
TOXICS COMPLIANCE
I MONITORING DATA
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
f ,.::, (
T1:1Ai ,: s :: ,.:iri-11 . .i ~ i an,:~ M1:,n it ,:,r· i r1g
Da '; c,
T~1is dc,cu~1~r,t e~t~bli~~l~s, fG( EPA P2gl.~tl r·; PC'PA . .,_ • · ·· _.. ,--c::-F•1-·LA -

.

'· · --'--t -· ,... · "I • • · · • . # -P-----~.-1l ,., .;.:-.:.·."5 ,_,J,._. ,_._ ·-· ,;>., •.,,: ,_,_,nr4ra1_ ,_,( ~, tht:" r"t:"ql_.l, ... ,_.d ,,_1(111at
•.::•li.:-,:tr"•.::.,·1.i,: t~•p•:•r"ting ,:,f t,.::i:,:i,:s r1 .. :it1it,:,ring data.
STA:::::N.DAT
WELL.DAT
SAMPLE.::.:
F·APM.DAT
,::,.:,nt . .=1.ir1~ Wa~i,: ir1f,.:,t·r,·1<:1.ti.,.:,n ab,:,ut
r1 .. :1t1it,:,ring 3tati,:,,·, l,: .. :dti,.:,n ,~ . .r-,d
type. Detailed description of
tht:" stru,:tur~ is ,:,:,nt . .3.int"",j in
appendi :, A.
,:0r1tains d~tail~d ir1f,)rmati•~r1
about constructi,~n at1d c~1arac-
:.:tiz:::. . .::: 1.:.f ~;-·,.:,:-t,·1(!,..3+;er r,)a:ini-
i..,,.:,..-.i...-',g ~•,.;,.;:1'..,.,_,i,~. :.'ll;''C' i."'\~~-=-ndi x B.
ccr,~~in: basi,: irif,~rmati,Jn ab1Jut
th~ coll~ction and ,:~iaracteris-
ti,:s ,:,f sampl~s. s~~ .app-==-ridi:< C.
,:i:1ntains m1;,..asw·(,i•d valut:·~ C\i1d
r~p1,rti~,g unit= for sp~,:ifi-:
par:.1i"1et-=-rs. s~e app~-:·,.::!i:,; D.
These file&~•• ~ob• transmitted in ASCII f,,,·mat using 5.25 itic~, fl~xible di~~, r1in~-track magnetic tape (1600 •~r 6:50 bpi) or, in th future, via communications chann•ls yet to be defined. Hardcopy reporting requirements will ,:~ntinue as curr·~ntly requir~~ ~:,ti! furt•ier n:;tic~. ~~~iti,~nal fi:~~ may be defin~d ir1 th@ f-~~r, for non-groundwat•r station typ•s should the need arise.
Sev•ral of these files will contain data that is usually static in nature. ~or example, t•,e basic ir1formati,~n ,:or,tair,~d in STATION.OAT will not normally change for any single station, th•r•fore one• th• data has b••n submitted for a particular station, it will not be requir•d to resubmit that information. ,If, however, the stati•Jn r<1t•:ord is updated or ,:,Jrrected the record would have to be r•submitt<1td, After the initial report
then, STATION.OAT would be subh·,itt•d ,Jnly. wh•n new stati,~ns are 2reated, or when an old station r•cord is modified, and need ,:,nly ,:i:intain the' new ,..Jr r,·.,:,.iifil:"J i-""..-c,:,rds. The :sarnc> i:. truc:-,_,f file WEL:...DAT. S,'\MFLE.C,•.T w•~uld, •~f ,:,Jurse, b,. .submitted .-a,~h time on~ or mor~ n~w sampl•s ~•rt:' to b~ reportt:"d, or dny sampl~ record required updating. Again, th• fil,. need onlt contain the n~-1o1 ,:,r u.:,Jc1t"d ,·e,:,~rd·~. FARM.OAT is exp .. ,:ted t,~ be subn1itt•d at t:."a,:h rot:"quirt:d r:?p;::,rtir·1g irit-;:r..-~l, ~iti1:t:" it i...iill ,_,:)1·,tain the-analyti1:a.l result~ r,c:-c:t;.it:""J L1:i det~rr.-1ir1e c,::implianct:". It mu3t contait1 all r1ew ~esults for t•,e rep,Jrting interval, arid mdy
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Datafil~ STATION.DAT
fit" 1 d f: .· l d
1 STATION fO:EY t
TYPE :t
3 LATITUDE
4 LONGITUDE
I :t required field
fi.:-ld
Dt:>s•:r ipt i,:,n
Un·iqll1:" stati,:1n ide,ntifie,r. C,:insists i:,f a ti..it:"nty-s~vt."r1 character alphanum&ric fi•ld, l•ft justifi•d, ,.:,:,ntaining:
,: ,:, l 1 .. u.-ir1 :
1-12
13-17
1S
des-: r i pt i ,:in:
Uniqu• site identifi•r as assigned by EPA. Must b• alphanum•ric.
Unique, s,~:id ~~~~~ ma,,age,me,nt unit de,sign~t,~r. Must b~ ~:p•1anume,ri,:.
Mejia statu5 indi,:ator. Must contain •~ne ,Jf t•,e folloi..iir,g:
C ,:,:,fr1p 1 i an 1: ~ r11or1i t,::r i ng st at i ,:in
B -b~~elir,~ ~•Jnit.~rir,i ~tation
A -ot•1e,r ambie,r1t monitoring ~tati-~r,.
Uniqu,:-:;it-3ti,:,n "idt:ntifi~·r. Mw5i: t-.~
al phat1Lu.-,e,r i ,: •
Type, of mot1itorin~ station. Consists of a f,~ur·· character alphanumeric fi•ld, l•ft justifi•d, containing one of th• following: AIR, SWTR, GWTP, SOIL, SEO, and SLOG. The meanings of these abbr•viations ar• as follows:
SWTR
131,.rrR
SOIL
SED
·-('.~~ ::ar,,plir,;; ;:;',-ati.,:,,,
--Surfa•:t!' watt!'r samplit1g stati,:,,1
-g~,~~r1d ~at~r =~mpling ztati~r~
-s,:,i l sc1mpl ing ,;tc1ti,:•t1
-Str•am bed s•dim•nt
SLOG -process sludg• sampling
Geographic po~iti~n Qf t•1• station il1 degrees north 1~f th& •quator. Mu~t be in the format DCMMSS. :<:co;, wh•r• DD repr·e:.;;nts d•gr;,es, MM repr&sent~ mir1ut&s, and SS.xxxx represe,1t3 ~•conds, with availabl• precision to four
c:j e,: i ma l p 1.21: es.
Geographic p1~sition of th~ ~t~ti~t, i~, Jegrecz · .. ·,:-st ,:,f th,: Pri;;,.: M.:.; >.:i.an. Must b•: in tho:-
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I .
f ~ :.-1 d
r·1afr1•.:
':TATION : :EY t
., AQNAM
1 DRMTH
5 ~RFLD
Ur1iqut:> st6t~•:•n idtl-t1ti fi~r. C,:insists ,:,f a t1.J1:"l'ltj'-·=it:"ver1 ,:~iara,:t~r alphanumeri,: fi~ld, l~ft _justifi~d,
,: ,:,n ta in i ng:
,: ,:, 1 Llf11n !
1 --• ,-,
13-17
18
1 '3 -27
d ·,.:s,: r i ~ti ,:,t,:
:.Jni:,t..:-,: .. ::i"::~ i,:!~r:ti fi-=-r -•·= ..:1.=-:i-;:·:.: . .-..: :,~
EPA. Mus.t b•.? alphanuri.:.::ri,:.
Uniq~lt:' s,:,lid •...ia~te r.-1anagement L1nit
d~sigr,at,Jr. Mu3t b1:' alp~1ar1umeri,:.
Medid ~tatus indicator. ~1ust ,:ot1t~ir1
or1e ,:if the following:
C compliance monitorir1g station
8 -baseline mor1itorir1g station
A -other ambier,t monitoring station.
Unique station identifier. Must be
alphanuroer i ,: •
USGS Aquifer Code for aquifer from which samples are obtained. Alphanumeric field with up to eight
,:hara,:t~rs.
T,:.tal depth to ...,rli1:h t:,e hole was Jr ~lled, b,:11~c:-~ ,:.,r-dug in f•et below !and surfa~• da~um. DEC!~~L NUMERIC fi~ld with a maximum of twelv~ cfiaracters (it,cluding
th.:-d'"•:imal p,:,i11t) and roay f1av• up t,:, tw,;, digit:; .:.:t·e·,
the decimal ~oint.
Method bj whi,:~, wel! wa~ con~truct~d. Must be
ALPHANUMERIC, ,:,:.t1si a.t.i.ng ,:,f a a.ingle ,:hara,:ter.
character must b• on• of the following:
Th'C"
H holl•:.w st•r,·, auger
C -,: ab l e t ,:,,:, l
S -solid stem auger
R -r,:,tary
V -reverse rotary
J -water J•t
D dug
A -air percussi•)n
F::..Jid used t,:, lubri,:att:> ,:utting ti:ii,l and/1:.r r-:r11,_,.,~
material;; fr,:,rn h•:.1..-. Must be ALPHANUMERIC, ,:,:,nsi~ti,1g of a single ,:•iaracter. The character Must b~ ,,~,~ •~f th• f.:,1l,:,wi,1g:
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
App;,ndi ,,_ B
14 STELVl
15 STEL•,::::
17 SBELVl
S9EL\.'3
::o NOCAS
:: 1 TCELV1
,.,,., TCELt./=
.-,'"'I TCELV3 _..,
I :t. r,;,qui r,;d field
decimal p•~ir,t), arid n~ay ha·~e LlP ta tw,J digits
f 1Jll0wir·;g t~,~ d~•=i~1al poir,t.
The d2pth t,~ t~~~ t,~p •~f the flr~t ~•~re ~,.~1: se,: ti ,:,n •
n,,.. d,;,ptf, t,:, tf1;, t,:,p ,:,f th;, ~,;-,:,c,nd bor;, h,:,le
S~•: ti ,:,n •
The depth to th;, top of th• third bor,;, hol;,
·3-="•=t i•:•n
Each of th;, STELVx fi;,lds is DECIMAL NUMERIC ~itf1 a maxirou~~ ,~f t~elve ,:hara,:t-=-rs (ir1,:luding the de,:in~3l point) and may have up ta two digits after the decimal poir,t. T~1ese depths are measured relative t,:i lar1d sur fa•:e datL1ir1.
The depth to the bottom of the first bore hole se,:tiein.
The depth to the b~ttoro of tt,~ ~~•:orid b,~re t1ole se,: ti ,:,n.
Tf1e d,;,pth
se,.:. ~ i ,:in.
Each of the SBELVx fields is DEC:MAL NUMC~IC with d rna:,;imur.-1 ,:if ti..ielve i:hara.,:te-rs ::ir1,:lwding t~,t: :j~,:i,,·,:;~ point) and may have up to two digits after th• d;,cimal point, These d•pths are measured relative to la,,d sur fa,:• datum.
Number of casing sections. A casitig s••:tion is
d•fined as a l~r,gth of casing of ~0nstant dia~~~~r and ut1iform mat~,i~l.Ca~it1g ~~•.:ti~r,~ ~;-~ ~~s~g~~~~~
numeri,:a!l; fi·•:im t,:,p ~,:. ~.:itt,:,m ,:if •~ll. !~JTEGER NUMERIC field containing~ value of one or tw~.
The deptfi t ·~ th,;, t ,:,p ,:, f t ht: fl r ,,t Sil:'•.: ti 1:,in Q f
,:a~ing(ir1 feet).
Th• d,;,pth t ,:i the t ,:,p ,:, f the se-1: . .:.fld s,-,: ti ,:.n • .• ) f ,:asir1gCit1 f ,;,et) •
The deptfi t,::, th• t ,:,p ,:if tf1• third se,: ti ,:in of
,:asir1g(it1 feet),
The TCELV:,, flelds are DECIMAL NUMERIC, e-a,:h with _,
r11a. ;.•; i mu1r1 ,_, f 'c •...J~ l ve-,:h.:\·r ~•: t '.:-r:; (in,: 1 i...:.J i :--.g t ~-. ,.: d,:-,: i. ri1a l ,:;,:,int) ~rid c,,ay !~ave up t,::, two digits after the de,:ir,,al point. These depths ar• measur&d relative to land
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
App,;ndi:,; 8
35 CMATR3
37 TOELV
3'3 OMATR
40 OWIDT
41 OLENl'.:i
De-s1:ripti,::in •:ir namt-i:,f ,:asing ri",att::"rial fr,:,r.-, 1,,,1hi,:h tht:-third St::'•:ti,Jt1 ,~f-casir1g is mad~.
Th<, CMATR·,. fi<,lds ar,; ALF'HANUMEF:IC, .-a,:h 1,,1ith a ,:1:::.:-.i.,·,.urn ,:,f •.:ight ,.:h2..ra,:tt::'rs.
CF·CN INTE;,7:VAL -any p1:.l'"ti,:,n ,:if tt1t;" •...i1:;:: ~.1 '..,;lii. ::. i n t -:: y· i ,:, r ,:, f th ,2--~.: l 1 i ~ ;·, . .:, t i 3 .:, l .:\ ~ -~ d f ':" ,: ~:: t h-:
sur'r•:1Lii",ding 5,:,i l .3.tid r,:.,:k by unbrc-21,.:;:·.~d ,:a31;·(~.
!rid~-=~tor ,~f th~ typ~ ,:if ,~p~~irig ir1 ~~,~ .:p~r, int.-,~al. Th<, field is ALPHANUMERIC, ccnsisting cf A ~ir1il~ ,:t,ara~ter. Tt,e •:•1ara~ter rou~t be ,:.r,~ ,Jf tf,~ f,:,11 ,:,!.,,Ji. ng:
0 -,:ip1:."t1 1?t1d p -pttr f,:,rat'C'd ,:,r :al ,:,t t <,d ~ -s,: r o?o?tl e,d T -sat1d p•:ii nt ~
w 1,,1al l <,d X -,:,pet1 h,:,l e z -,:,thc.-r
Th<, depth to th.-top of th,; op<,n it1t.-rval. Th~ TOELV field is DECIMAL NUMERIC 1,,1ith a ,·;,a>~~;:,:...:~.-, ,:,;f t· .. ·~!.\"i:-1:ha.;·~,..:~1::1"5 :.~;-·,,:..:udin,; t:,t" j~.:im~l p1Jint) and may hav• up tot~~ digits ~fter t~1~ decimal point. ~easui-t"d relativ~ L•~ land sur fa,:e.
The d<,pth to th.-bottom of the op9n it1t~~·.3l. Th,; BOELV fi.-ld i~ DECIMAL NUMERIC ~ith ~ ma:,imum of twelve c•1aracters (including the ~~•:imal p~it1~) and may hav.-up t,:, tw,:, digit :a a ft,;r th.-d.-,: i ,,,al p,:,i ;-, , • M•asur.-d r.-lativ,; to land surfa,:e.
D•scription or t1am,; of mat.-rial us.-d to scr••n th• ,:.p•n int.-rval. Th,;, OMATR fi,;ld is ALPHA~::.mE~IC _., ch ,, maximum of ~i;ht ~•1aract~r=.
Width or sh1~rt dimension of slot or mesh of ~creen material f,:,r th<, open irit,;rval, in iri,:h,;s. Tl,9 OWIDT fi•ld is DECIMAL NUMERIC with up t,::, t1,,1<,lve ,:hara,:ters (includit1g th.-decimal), and may hav.-up to 3 digits following th,; d.-cimal point.
Lttngth •::ir l,Jng dimensi,::,n ,::,f sl1::it ,:1r mesh ,:,f s,:r\:en mat,;rial for the op•n Lnt•rval, Ln Lnch&s. Th• OLENG field is DECIMAL NUMERIC with up to tw,;,lv.-charact.-rs (including th• d.cimal), and roay hav,; up t,:, 3 digits follo1,,1it1g th,;, d&cimal point.
FILTER PACK -mat<,rial plac<,d in th.-Q,-,n:.1lc..~ -~ r ~: . ., w&ll bea-t~C"'=',i the b1:ire~·11..:.le wall and ~:11? ~el~ ~,:rel;"n t! . .:,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Appe,ndi 8
TSLELV
51 SF:FSL
5.2 DNGRAD
5·-\ LTHU:,
55 WLUSE
I* required field
• I'•' I I •
T~,e ~:~t~, to th~ t-~~ 0f tt,e
Ti-h:.• T3LEL \/ f ii.: l J i ~ DEC I ~1,'\L
::.~..,~· . ._;!. ar
~~:..::1ER ! •:
ma~imum of twelv* ,:hara,:t~r3 ,:including t~,~
de,:imal p•Jint) arid m~j •1a·,~ up t,J t~•:. digit:
3ft~r tt1e de~im~! p,J~r1t. Measur~d r~l3t~.-:
t,) l~r,d ~urfa.:·~.
The dept~·i t,) th~ bottoro of tht:" dt1r1ula,· seal. Th,; 8SLEL'l fi;,ld ·is DECIMAL NUMERIC .iith a r,·,a:<ir,,ctr,,
,Jf twel·;e ,:haracters (including tt,e decimal point)
and ma; ha,a up to t.io digits after th• decimal
p,.:,il'1'+;. Mt:>a:Sured 'ft:lative t.:i lai·,~ ~ .... r·f~-:.:.:.
Surf.3.,:e -:.e.:.: !r1di,:-.ltor. Indir:..at.-~ 1.Jh•!'t ►1er ,.;;ir n,:it th::;o upper portion of the borehole is sealed ta prevent infl,)w ,)f surfa,:e water. Single c•1aracter
ALF'HANUMEF:IC, ,:,:,ntaining "Y" if .iell is sealed. Ott,eruise contains 11 N'1
•
D,:,wngradie-t1t indi,:at,:,r. Indi,:at1:"s i,,..hi:-the-r ,;ir 1-1,:it, the .iell has been installed hydrauli,:ally d,:,w,·,9,.a.di,:,c,t
of th~ sour,:~ of pot~ntial groundwater pollution, and is c~pable of detecting the migration of contaminants. Single character ALPHANUMERIC,
~o,1tainir1g ''Y'' if w•ll is downgradi~nt from wast2 disp,~sal site. Otherwis<t •=•~ntains "N".
Drill~rs l,~g it1Ji,:ator. Indi~at~s a·✓a~l~bil~tj· dri::•rs le;. Single charact .. r ALPHANUMERIC,
,:ontaining "Y 11 if li::ig is a.··ia.i labl'=-". Oth~r•..,ii-s•:
,:ont ai ns "N11
•
Lithalogic log indicator. Lithologic log showc distribution of lithologj with depth in the bore fie!~. Single character ALPHANUMERIC, containing ''Y'' if !,,~ is available. Other.iise contains ''N".
W<tll use indicator. Must be ALPHANUMERIC, consisting
of a single character.
the f,:,11,~.iing:
The character must be ,,na of
• •
j·:r.-.~s.i..:::.: ~i,J1 i·.-~te) \.Jc:lt~f
industri3l ~~ter supply
~ monit,:i·it1g w~ll
P -µubli,; \.J~t•r· 3U~pl~
0 -,~ther
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Appendi :,; C
Oatafil• SAMPLE.DAT
field
l
f ~ ~ l d
nan·1~
OELn:
DATE
:t
*
fic·ld
D•Z:-:;,:r i pt i ,:,n
Ut1iqu• sa~1Pl• identifier. Consists ,~fa f,~rtJ·-t~•~ ,:~1ara,:ter fi~ld, !~ft ,justifi~d, ,:,~ntainir,g:
1-1:::
13-1 7
18
:::e -4:::
=,;;:51:,~pti,:1t1:
Ut1iqu~ site 1d~r,t1f1~r 3; as3:~~~-~ ~i EPA. Must be alphanumeric.
Unique solid waste Mat1ag+m•r1t unit designator. Must be alphanumeric.
Media status indi,:ator. Must contain
or1e ,~f tt1e foll,~wing:
C c,Jmplian~e m,Jr1itcrir1g station B bas~lin~ ~onitcrir1g station
A -other ambient monitoring station.
Ur1ique station i"dotnti fier. ML,st be al phanun·,er i ,: .
Unique sample identifier.
al phanumer i ,: •
Must be
·.·~,-ti~al di~plac~Mer1t ~f 5~mple from th~ r·~f•r~n~~ el~vati-~n (in f~:t) of the sampli·ng stati,Jn. F,Jr surfac~ water, ~oils, and groundwater stati:ns thi5 would be the depth 1Jf the sampl• and for air ~,)ni~~rit1g staticns, the height above ground. Must be DECIMAL NUMERIC 1.:,:ir1·~i-~ting ,:,f a m.:l:Ai:imum 1:if 3ix -1:hara,:t-a,r5 (includit1g the d:,:im=!) arid may hav~ up to two diiit3 aft~r the deciffial point.
Date of sample collection.
field consisting of:
Eight character integer
1: 1:, l urr1n s
1-4
5-E,
7-8
1: ,:,n t t."ti t
year including century, e.g.
r1um413-r i1: 111,:inth
numeric day of mon~h
Column ,,umb~rs are relative to th~ b~ginr1ir1g ,:,f tt1~ DATE Field, Each subfield described above ffiust be right justifiad, and ffiay contain leading ~eros.
I I I I I I I I I I I I I I I I I I App,;ndi.-: '.) Datafil~ PARM.DAT f i -2-l ,j ' I<.• o ! -. -3 f i •2-1 d n ari"1t: !=',\!=::\!'--: ~ :::v '.:'!J!\Lc \/ALUE I * r~quired fi~ld l fi.-ld D•s•:ripti,~1r1 Ur1i41-:.:.· dai:;:l r~•::. .. -~ :.=.:.•tit:~:-~:--. C,:,n:.i.:3t=. ,:,fa fift/-f,:,ur ,:~1ara,:tt:r fit""ld, l~ft justi fi-a-d, ,:,:,ntaining; ,.: ,:, l lir11n ~ 1 -1 ·.:: 13-17 18 1 ') -.::7 .-.. ~ -~ ◄ .-. ·-t~ 43 -54 55 -58 des,: l'" i pt i ,:in: Ur,iqut" sit~ idt:"nti fit"r· as assignt"d b., EPA. Must b~ alphanumt"ric. Ut1iqut" s,:11 id 1,,,,1a'3t>: mat1agt"H1e-nt ur1i t desigt1at,:,r. Must bi:-alphcanurn~ri_c. M.-dia status indicator. Must contain one of th~ following: C -,:,~mpliance monitoring stati~n B -baselin& monitorit1g station A -ot~1t"r ambier,t monit,Jrir,g station. Unique station id.-ntifi.-r. Must b.-alphanum&ric. Ut1ique ~arnpl~ id~t1Lifi~r. ~!~~13num~ri,:. Muzt '· ~~ Paramet~r id~ntifi~r. F,:,r ,:~1~mi,:3l con3titu~r,ts f,~r ~hie~, CAS r1umb•rs .-xist, the CAS numb~r will bet~• identifier. For other constituents, the id•ntifier ~il~ t~ d~t~rmin~~ •~nan ~s-r,~~d~d ~asis. P•plicat.-number. Identi fi•~ th,'" valu• as on~ of two or mor• analyitical results for th• same parameter on the same sample. INTEGER NUMERIC, up t,:, f,:,ur characters. Not used unless replic3te results ar• ••ported. C\.i3li f:~( fi=ld. ,\LPHAt~UMERIC, r,,ay 1:,:intair1 up to fo~r S~□RET qu~:i!i~r coda3. * The r.-ported analytical result for the chemical. Mus~ b~ DECIMAL NUMERIC, consisting of up to tw.-l~e ,:har~ctcr (includi~;i t~,~ deciffial), ~nd m~j-:,ave up ~o
I
I
I
I
I
I APPENDIX B
I U.S. EPA FUNCTIONAL
GUIDELINES FOR EVALUATING
I ORGANICS AND INORGNIC
ANALYSES
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
• I
r
I
J..ABOR.ATORY DATA VALIDATION
FUNCTIONA.1. GU!D~ FORE.VALUATING ORGANICS ANALYSES
Prepared for the
HAZARDOUS SITE EVALUATION DrYISION
U.S. ENVIRONM:ENTAL PROU.CTION AGENCY
Compiled by
Ruth Elleyler
Sampk Mallage.ment Office
The USEPA Dais Review Work Group
Scott Siden -EPA HQ -Co-Chairpenon
Jeaue lunlcins -EPA Reaion m -Co-Ctiairpenon
Deborah Suro -EPA Region I
Leon Luarus -EPA Region D
Charles Sands -EPA Region m
Charles Hooper -EPA Region IV
Patrick Churilla -EPA Region V
Debra Morey -EPA Region VD
lbleiah Farlow -EPA lle&io.o X
••
·-
: -
•· .
•
I'
I
I
I
I
I
I
I
I
I
I
I
I:
I
I
I
I
I
I
TABLE Of CQ!'i:ul,J:S
fut'
l1''TROOUcnON ___ , _____________ _ .I
PR'ELlMlJ--!.RY RE~· _______ ---··-··-·····-----.. 3
VOLA Til.'ES AND SI.MJVOLAlll.ES .PllOCEDUll ____ _ ···-·4
L Holding Times ______________________ _ .s
Il. GC/MS TaniJlg ______________ _ __ 6
__ 9
m. Calibn.t»"-----------------------
IV. Bl.a.ala.-.·----------------------12
V. Sum>gate Recovery ____________________ _ 14
VJ. Matrix Spike/Matrix Spike Duplicate ______________ _ •• 16
VIl. Field Duplica~----------------------
VDL ln°tenial Standm!s PerfonlWICe-----------------
IX. TCL Compound ldenti!icatio11 -----------------
X. Compound Quantiution and Reported Detection Limits--------
17
II
19
0
XI. Te11catively Identified Compounds-----·----------.-21
:xn. System Performance-------------~------
xm. Overall Assessment of Daca for a ease _____________ _ 4
PESTICIDES PROCED
25
26 L Holding Tim,A--------------'---·------·
n. Pesticides lllstrument Performance _______________ _
m Calibrs..,·...._ ______________________ _
IV. Blanb----------------------
V. Surropte Recovery·--------------------
VL Matrix Spike/Mattu Spike Dvplie1te-------------
vn. Field Duplicates ____________________ _
Vlll
IX.
X.
CompollDd Identification _________________ _..
Compound Quanticatioli ad llepoTted Deteetion Limits---------
Ovenll Armmen1 ot t>aca for a Case--------------
::--
GLQl.'SA.'RY A: Data Qualil"tet Dermitiou-------------I --~
CiLOSSARY B: Otber TerDU'------------------
6
30
3
34
35
36
37
38
39
40
41
2/18
I
I
I
I
I
I
I
I
I
I
I
LAB.ORATORY DATA ',Ai.LIJAIIV,"'
FUNC"nO~AL CUlDELINr.S FOR EVALUATING ORGANICS ANALYSES
INTRODUCTION
Thu doc,unnt is dai1.11ed to offer ~ce in labontory data evalu.ation I.lid
validation. 111 some ISQem, it ii eQlliftleJlt IO • SD11d.ln1 Openti11g Procedure (SOP). 111
other, more ~bja.::ti+"c areas, a)y geaenl p"t noe is t1l'fcnd due to the complexities I.lid
uniqueness o( data relative ID spec:irJC 111!:1~\es. Tiiait Guideline\ have been updated to
include Lil reqwremeJ11S in tile 10/16 SlatemeJII ltC Wort (SOW) for Orgwcs aad 10/16 SOW
for Volatiles.
Th05e areas wbue ll)tciric SOi's are possible are primarily areas iJI which deffujtive
performance T~IS -me emblismd. lbese aJUS also correspond ta specific
requirements in Age11c:, coatncu. These nquirements are concerned wilh specificatiom that
are not sample dependent; they specify performance requirements 011 manen that should be
fully under a Jabontory"s control nese specific areas include blanks, calibration standards,
performance -1mtiOI' mndtrd materials, 1.11d hmina. ID particular, mistall:es such as
e:alC'lllatio-11 and tnnscription em:m mast be rectified by resubmission or corrected data sheets.
This d~menr k ia1lmded f11r tech.lucal ~w. Some areas or overlap between
technical review and Contnc:t Compliance Screeoi111 (CC:S) es.ist; however, contract
compliance is not intended to be a 1oal or these 1uideli0es. It is assumed that the CC:S is
available and can be utilized to assist .ill the data review procedure.
Some requirements are DOI identical for every Case· or batch or samples.
Requirements £or frequency of Qual.iry Control (QC) actiom are dependent OD the number of
samples, sample preparation rec:hnique, time of analysis, etc. Specific Case requirements 1.11d
the impact of noncom ormaDce mmt be addressed 011 a case by c:ue basis; 110 specific
guidance is provided. For eumple, there is a contract requirement that a bll.llk Ulllysis be
performed a minimum of once every twelve houn of analysis time. This requirement must be
translated into the number of bll.Dks nquired for a ~ific set of aamples; the data reviewer
may have to consider the impact on data qllllity £or a umple analyzed thirteen houn after a
bla.Dk. iD terms of the aca:eptability of that particular umple.
At times, there may be -1lf'ICIII Deed to -data which do DOt meet all CODtl"ICI
requirements and technical criteriL Use or these data does am constitute either a new
requirement IU!ldard « Cull acc:epllDce or the data. Ally decision to utilize data ror which
perfon:D111ce criteria lla'fl aot beea met b suictly to racilitate the pro1ress of projects
requiring the availability or die data. A ccn,tnc:t 11!,orau,ry nbmirting data which are out or
1pecificatio11 IUJ lie nqvind to IW1III or resubmit data even if' the previously 111bmined data
11ave beea atllized due to mpnt prolfflll Neds; data which do not meet specified
requirements are never flllly acceptable. TIie oa.ly uceptioD to this nquiremeat b iD the
area or requirements £or individual ample analysis; If the nature or the sample itself limits
the attahunent or specuatiom, appropriate lllowtnces must be made. ne ovenidi.Dg
CODCCTD of lhe A1eacy is to obtaill data w~h are techAic:ally Yllid ud legally defensible.
AU data reviews mast .. -ve, as a cover sheet, the Oraaoic lle&iollll Dita A.aessment
form. If mandatOTy actions are nquind, they 1hould be 1pecifically aoted on this form. hi
addition. this rorm is to be med to 111mmariz.e overall dericiencia requiriD1 ane11tion; as well
u general laboratory perf'ormuce 1114 uy discernible treads iJI the quality or the data. (This
I 2/11
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
form is Dot a replacement for the dat.a reviev,·,) Sufficient 1upplemeat.ary docume11tation
must accompany the form to clearly identify the problems associated •·ith I Case. Tbe form
and any attach.meats mu.st be 1ubmitted to the Contract Laboratory Procnm Quality
As.sura0ce Officer (CLP QAO), the Re1io0al Depury Project Officer (DPO), and the
Eoviroamenca.1 Moo.itoriag S)'1tems Laboratory il:a Las Vecas (EMSL/L V).
It i, t"1! ,apo...;biliTY of the data re~ to aotify the Recioml 1>PO concerning
problems aiid ahmCOBUap ,nib regud' cc labontory data. If then ir a11 argent ~uireme01,
the DPO may be C0111X:12<i by ldcJ)floae ID nped.i&r corrective acuo0. It is recommended
that all items for DPO ac:tioa tie 1"'Dal~ at -time. Ill uiy case, the Or&aiiic Regional
Data As.seua,ent form amt lit~ llDd abmined.
.-
..
: '
2 2/11
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
PR[LlhllNUY REYU:W
In order to use this document errectively, the reviewer should have a aeneral
overview or tbc Case a, Jund. The exact number of amples, their assiaaed 11umben, their
matrix, n:l lbe aumber of laboratories i.Dvolve4 ill their aml~~ ve esseatia.l i.Dformatioa.
Background m!ormatioo on the rirt is ltclpful bur of'le11 this mrorm1tio11 is Tery 4i!ficult to
locate. Tlte site pro~ officel ii Ole best 'IIOWet fen DSWen or further direction.
CCS 'A a ,om;::e of a large quutity d l1IJlllD■rized inf'ormatioa. h can be med to
alert the reviewa of problems in tbt Case or wllal may be umple-1pe,;ilic problems. ThiJ
information m.ay be utilmd ia dau -nlidation. If' CCS is 11D&vailable, those criteria affecting
data valiclity must be addressed by the data reviewer.
Cases routinely have unique amples which require special attention by the reviewer.
Field blanks, field duplicates, ud per{onnuce auclit samples Deed to be identifie4. The
sampling records should proYide:
..
I. Projec-t Off acer for site
2. Complete list or samples with 11otatiom on
a) Alllple matrix
b) l>lanlcs•
c) field duplic:ates•
d) field spikes•
e) QC audit sample•
f) shipping dates
1) labs involved
• If a;,plic:able
ne chain-o(-c\lStody record includes 1&111ple descriptioas and date or sampling.
Although ~ling date is not addressed by contract requirements, the reYiewer must take
into account lag times between sampling and shippi11g while usessina sample holding times.
Tbe Case NUT1tive is another source or 1eae1'111 laform.ation. Notable problems with
matrices, insufficient ample volume for analysis or nlllllysis, ud uusual events should be
found in the NarratiYe.
I .
3 2/U
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
VOLA TILt.S AND StMIVOLA TILts
PROCtDURI
The requiremenis t.o be checked in "nlidatioa are listed below: ("CCS" iadiC3te5 that
the contractual requirements for t.heM! items will also ~ c:heclr.ed by CCS; CC:S requirements
are not always the same as the data review criteria.)
I.
n.
m.
IV.
V. ,.
VJ.
vn.
Holding Tam.es (CC:S • ull lloldiq times only)
GC/MS Tull.ing
Calibntion
0 lnm:a1 (CX::S)
0 Continuins (CC:S)
Bww (CC:S)
SUrTOgate Recovery (CC:S)
Matrix Spilte,'Matru Spike Duplic:ate (CC:S)
Faeld Duplicates
vm. Internal Standards Performance (CCS)
-IX. TCL Compound Identification
X. Compound Quantitation and R.eponed Detection Lim.its
XL Tentltively Identified Compounds
xn. System Performance (CC:S)
:xm. 0ftrall Ass meat or Dau lor a Case
4
·.:·
. . --... I .
·4
·.t'• ....
Ao
2/1&
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
A.
B.
I. HQLDJ>;G Il'ltS
Objccll•c
The objecli~e is 10 a.scerta.i.a tlle validity or mutts based 011 the holcliDa time or the
sample from tjme of collec1jon D:> time of analysis or sample pRpantioc, as
appropria\t.
Crlurl.l
T"lui.ical requirements for ample hold.ma times have only bee11 established for water
matri~. The holdiA& times Cor IOils are nnudy uder illvestigatio11. Y,he11 the
results are available they will be incorponted into the data evaluation prcxess. On
October 26, 1984 ill Volume 49, Number 209 or the Federal Register, page 0260, the
followin& holding time requirements ftl"e established uder .CO CFR 136 (Clean Water
Act):
..
Purgeable,: If unpreserved, aromatic wlatiles must be analyzed within 7 days
and non-aromatic volatiles must be ualyzed within 14 days. If preserved with
hydrochloric acid and stored at .C-C, dle11 both aromatic and non-aromatic
"Olatiles must be analyzed within 14 days •
Extn;nb)e> (IDcludes BasefNeutnls and Acids): Both samples ud extracts
must be preserved at .c•c. Samples mast be extracted within 7 days ud the
ntraet must be ualyzed within .CO days.
C. Enluatlo11 Procedure
-ActlW holding times are established by comparuia sampling date OD the EPA Sample
Traffic Report with dates of ualysis ud/or ntrac:ti011 on Form I. Eumine the
sample records to determine if samples were properly preserved. (If there is 110
.indication or preservation, it must be assumed that the samples are unpreserved.)
J>. Actlo■
I£ -40 CFR J36 boldiq times are esceeded. flaa all positive results as estimated (J)
and sample q111.11mation limits u estimated (UJ) ll!ld document that holding times
were exceeded.
The following uble Dlmtrata wbe11 the qaalir,en are IO be med for volatiles:
J.
Mattia
Wat.et No
Yes
?7PID > 14 Pin
AD aromatics AD compounds
None All compoW1ds
JI holding times are aroaly exceeded,. either oa the C"ust ualysis or upoa re-
ana!Y1is, the reviewer must 1111 professioaal Jud1ment co determine the
nliabiliry or the data ud the effects or additioaal storage OIi the ~pie
results. The reviewer may determine that DOIi-detect data are 1111aable (R).
.;.. ··t.,
5 2/18
-----------------·-·--
I
I
I
I
I
I
I
I
I
I
I
1~
I:_
I
I
I
I
I
I
A.
B.
C.
-2. Due 10 limited infonnatioc coccenung holding times for soil samples, it is left
to the discretion of the data ruiewer 10 apply water bolding time criteria to
aoil samples.
D. CCQJS JmlU:iG
ObJecthe
Tu!Wlg an4 performance criteria are established co ensure mass resolution,
. • -ide11tific:atio11 and: 10 some degree, sensitivity. Tbese criteria are 1101 sample specific;
c:onfonnance is determined using ltlllldazd IIIIIUials. Therefore, these criteria should
be met in all c:irc:WDSWlc:es. · ,
Criteria
1. Dec:aflaorotripbalytphosphlne (DFTPP)
,· . ma JON ABUNDANCE C'JUJDIA
51 30.0 -60.0 4Mi or m/z 191
61 less than 2. Qtlb of m/z 69
'70 Jess than 2.0 'Ill or m/z 69
127 ~.o -60.Qtlb of m/z 191
197 lest than 1.0 'Ill of m/z 191
198 base 1)eU.. I~ relative 1banda11c:e
199 5.0 -9.Qtlb of m/z 191
275 I 0.0 -30.Qtlb of m/z 198
365 areater than I.OO'III or m/z 198
-441 present, but less than m/z 443
442 aruter than 40.Qtlb or m/z 191
443 17.0 -23.Qtlb of m/z 442
2. Bromonuorobenzene (BFB) -ma ION ABUNDANCE cgm;grA
50 15.0 -40.~ or tu base peak
75 30.o -~.O'lb or 111e 1me peat
95 baa pcu. I OO'!rt relaliff abadaDce
'6 5.0 -'·°' ol die bee peak
173 Im dlu 2.Qtlb or m/z 174
174 irater Uwi ,O.D"' or die base peat
175 5.0 -9.Qtlb or m/z 174
176 1ruter than 95.Qtlb, bat lea dwl 101.()«M, or m/r. 174
177 5.0 -'·°' or m/r. 176 .• . -.... : ' . •.•
-~ -. !IAlg; As contncts are modiiied, new criteria would then apply.
Enluado■ P1 udaN
I. Verity Crom the nw data that the mass c:alibnuon b cornet.
6 2/11
I' L ' ,, 1;0 D. 2. 3. •• ,· Compare the data presented oa each GC/MS Tuning and Mass C&libraticn (Form V) "'ith each mass listiag aubmined. En.sure the following: a. Verify that Form V is present for ea.ch 12-ho-m period 11111ples are analyzed. b. The \aboratoTy w 904 !Ude ay tn.iucriptioo nron. C. d. The a.pproprim amnber ot ri&nif°JQZ!t fi,we, Jw been reported (oumber of 1ignific:ut C"iaures aiven for each ion ill the ion abuDCWJce criteria colu11111). The \abonlory Ji.u not made uy calc:ulatioa enon. For eu.mple;the ~ mass ot m/1 443 relative to the mass ot m/z "'42 is c:alculated asiD& the fouo .. i.ng equation: 'It, 1b1111dazlce • relative &b1111d&ace of m/z "'43 relative 1b1111d&Dce or m/z 442 z 100 <I. If pcmjble, verify that t.,«ba were aeoerated min& appropriate bacltarouad aubtnction t.echlliques. Since the DFTPP ud BFB spectr& are obtaioed from chromatognphic peaks dial should be free from coelution problems, background sabtra:tion should be straishtforwa.rd and designed ooly to eliminate column bleed or instrument bacltaround ioos. Bacltsrouad 1ubtr1ction actioos resultio& in spectn.l distortioos for the sole pwpose or meeting the contnct specificatioos are contnry to the quality us~ objectives and are therefore o:oacceptable. Acdoa 1. If ma.a calibration is ia error, classify all associated data IS unusable (R). 2. Jf ioa abllll<luoe criteria an 110t met and the data ia question are needed 011 a prioriry wis, proressioul Judameat may be applied to determ.ille to what extent the data may be 'ltilized. Ouideliaes to aid in the application of profeuioul Judameat to this topic are discuaed IS follows: L PfTPP -Tbe most cri1ic:ll 1111:ton Ill the DFJ'l'P criteria are the DOll-imtnmeat JpeCUIC requirements that are also IIOt 'IDduly alfected lly che loc:atioa m th spec.ta ...ii 011 the chromatoaraphic profile. The m/J 191/199 and "'42/4'43 ntios are critical. These ntios are based 011 dlt natural abuaduces or Carbon 12 and Cuboa 13 and should alwa11 be met. Similarly, die m/z 61, 70, 197, ud 441 relative abundances indicate the condition or the illstnimeot 111d the auitabilitY or the resolution adjustmeat ud are wry lmport111t. Note that all or the fore1oiA1 1bu11duces relate to adjacent iom -they are r,latively imeositive 10 difrereaca bi lmtrvmeat desiaa ud position or the apectnUD 011 the chromatoaraphic pror&Je. For the iollS at m/z 51, 127,. aad 275, the aetuaJ relative abuadlDce b aot u critical. for immce, ii m/1 275 1w .eO'i relative abundance (criteria-10-~) ud other criteria are met, the deficiency b miaor. The relative ab1111dance or , 2/IS
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
3.
.. •
b.
m/z 365 is an indicator or 111iable instr11ment zero adjustment. JC m/1
365 relative abwid&nc:e is zero, m.inimum detection lim.iu may be
aUected. OD the other ha.Dd, If m/1. 365 is present., but less Oun the
Jfjb minimum abund&Dte criteria, the deficiency is not as serious.
.IE& -M with DFTPP, the most i.mporu.at raeton to comidu an the
empirical ftS\1113 dlat are relatively insensitive to locaUO'II oa the
chn>autDSn?h.i.: p,ofi.l& ad &he sype of instn1meat1tioa. Therefore,
die uiuca1 ioD • bnodnN -:rilt:ria r ar BFB are the m/r. 9S/96 ratio, the
174/\75 mio. \11,t 176/JTI ntio, ud the 174/176 ntio. The relative
abuadallces of m/r. SO and 15 are or lower iaaponu,ce.
tu tiue w ilh the above diselwion, u explllSioa or minus 2SII& or the low limit
and plllS 25~ ol tlle luab limit Cot ael~ iom may be appropriate. For
example, hi DFll'P tJie m/r. 51 ion 1bwiduce eriwia miaht be expanded
Crom 30-60'llJ of m/r. 191 IO 22-75' or m/r. 191.
L 'Ille complete exi,aaded criteria ror DFTPP ud BFB are as follows:
l) Decatluorotripbeaylpbosphille (DFTPP) (Expanded Criteria)•
.m.!1 JON ,6JIUND6N0: QI I EJ!.16
SI 22.D -7S.OII& of m/r. 191
61 Im than 2.1111& of m/r. 69
70 less than 2.1111& or m/r. 69
127 30.0 -7S.OII& or m/z 191
197 less than I.OIi& or m/z 191
191 base peak, 100% relative 1bu11dallce
199 5.0 -9.1111& or m/r. 19&
27S 7.0 -37.1111& or m/z 191
36S irater dwl 0.7SII& or m/z 191
441 present, but less than m/z 443
442 areater dwl 30.0'1& or m/z 19&
443 17.0 -23.1111& or m/z 442
2) Bromofiuorobeuzeue (BFB) (E.lpuded Criteria)•
ma JON .6JIYNP.6NO: CBUEBl.6
50 11.0 -50.0'1& or the base peak
7S 22.D -75.1111& ot die llase peak
9.S lllse peak, IOO'!b Ttlathe abuDdallce
96 5.0 -9.K ot the base peak
173 Im 11m ~ of Che bue peak
174 paler dau ~ or the base peak
175 5.0 -9.0'1& or m/z 174
116 irater dlaD 951111, bat less than 1011111 or m/z 174
177 5.0 -9.1111& or m/z 176 -·--~ Does NOT dwl1e contract requirements.
.•
.;; •• ,
b. 1C results llll·widwl 1liese er.p&11ded criteria., data .... 7 .. acceptable.
IC. II resales ran outside t11ese exr,uded criteria, an data an 11111asable CR).
• 2/IS
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
A.
B.
d.
e.
r.
..
Objectl•e
These ~iteria do NOT estabwh new contract requiremeau. Coatnet
laboratories meewi& exp111ded cri1.cria but DOt mectiDa eo11~1
requin=meats an NOT ill eompliaace.
~isiom to ase ana.l)'Zi(:a] dara •ssoei• •ed w ilh DFTPP PDd BFB hl11es
DOl meeting CIDDtrlC"t reQIUICmeDts should be clearly aoted 011 the
C)rpJiic Reaioul Data Assessme11t Form.
If tlle reviewer bu reason to believe th.at hULiDg criteria were achieved
-ma tedllliq11eS th.at distuclltd or skewed the 1pee11~. run
doc::u l:IUIIII • 6t 1UiA\ qmlity coutrol ahould be obtauied. If" the
reehlli,ques emplored are (oud IO be •t ftl'Wlce with accepted
• ¢ae1im, -ihe quality esswuce prosram or the laboratory may merit
evaJ 111tio11.
Jr 11 vp tD tbe nviewer'1 d.iscretio11, based 011 professiollll Jad1me11t, IO
na, data essociated wi1h nmes -ting exp&11ded critem. but not basic
criteria. If" only one element Calls witblD the expuded critem. Do
qu•liric:ati01l mey be needed. 011 the other bud, Ir aevenl data
elerne11a are ia the expuded wiodows, ell essociated data may merit u
estimated naa (J). 1'ase D* daat the data reviewer is not required to
1151' expanded criteria. The reviewer may still choose to flag all data
associated with a tune 1101 moewi1 contract criteria u umable {R) Ir
it is deemed appropriate.
m. CALTJBADQN
Compliance requirements for 11tis(1ctory Jutniment c:alibration are established to
ensure that the instrument is capable or producing acceptable qautitative data.
lltitial calibration demomtnta that the illstrument is capable or acceptable
performance ill the begiuioa, and cootiaWJ11 aJibration checks dOCllllleDt
satisfactory m•ia1rn111oe and adjastment or the ios1nmleut on a day-ro-day !mu.
Criteria
I. lllitiel Calibratioa
L Volatile and Semiwlatile Fracliom
I) AD a-.e ltelatiw Jlapoaae Facton (RRF) for TCL
er ms w• ct, mat be ~ O.OS.
2) All Peroeat Jlelative Scudard Deviatiom ~) 1111111 be
:t3ft. ::,
,
-· .......
.1\ ·-•
2/11
I
'I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
C.
2. Continuing Cali'bratioa
a. Volatile and Semivolatile Fractions
1)
2)
All Relative Response Fac,on (RJtFJ for Ta. o:uni,ounds must
be' t,0.0S.
All Ptt:e..1 DifTereoce ('a,D) IWSt be$. 2511b.
Enhiatlon Proced1ue
1. Initial Calibntioa
r
L Ewluate the liF for all TCL compounds and verify the followiDa: -
1) Check and recalculate the RRF and RRF for one or more
volatile and temivolatile TCL compounds; verify that the
rec:alculated v.Jue(1) agrees with the laboratory reported
wlue(s).
2) Verify that &D volatile and aemivolatile TCL compo1111ds have
aven,e Relative Response Fai::ron or at leut 0.0S.
b. Ewluate the Percent 'Relative Standard Deviation ('IIIRSD) for Ill TCL
compounds and verify the followiDs:
C.
•
O•
fJ ~ JlSD • -:1 100 . 'i
ii • Scudard devialio11 or s response facton
~ • Meu or s response facton
J) Deck ud ncalculatie tile '6RSD lo, one or more TCL
compouds; wriff lllat die recalc:ulated fllue agrees with the
laboratory repor1IDd fllue.
2) Verify that ID TCL compounds (volatile and temivolatile) have
• ~ or~ 3()11. -
IC emn are detected bl the calculaliom or either Ille RRF or the
411iR.SD, perform I more comprehensive ncalClllatioL : 1
· .. -~ .. f:
10 2/IS
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
D.
2.
,.
Actloa
1.
2.
Co11ti11ui111 Calibr1tio11
a. E~luate the JlRF (or all TCL c:ompouads:
b.
C.
I) Veril'y that all volatile and aemivolatile TCL compouads have
Relative Req,011.K Faaon or at las\ 0.05.
1.Yahl:ate die Pertea! Dil'fc:mice and verify the followill&:
1) Oeck ~UOII fJI 'll> Difference ('ll>D) betwee11 initial
c:al.ibntm ...-e,qe Jle\ative Response Facton and c:o11tiDUU1g
calibratio11 Jlelatiw Response FICIOn for oae or more
c.;m1)0;uids, asin1 the followill1 equation:
wbere,
JlllFJ • JlJlF C --------x 100
ID1
-.
avenge relative response factor from
initial c:alibratioa.
RRFc • relative response (IC\Or from
coatiD ui.111 Rlibratioa ltllldard.
2) Verify that the 'MID ls s 25'1b for all volatile ud semivolatile
TCL compounds.
U erron ve detected iD the calculations or either the JlJlF or the 'MID,
perform I more comprebensive recalcutatioD.
lllitial Calibn tioa
L IC uy wlatile or aemivolatile TCL compound result 1w III average
Relative Response Factor or less tbaa 0.0~:
1) FJaa positive results for that compound u estimated (J).
2) FIii DOa-detee:U for that compoud u UIISlble (Jl).
V any -volatile or Rmr10latile TCI.. compoand 1w • 'Iii RSD or 1reater
Iha.a~
I)
2)
F1q positive results for that compound u estimated (J).
Noa-detects IIIIY be quali!"ied IISUII professioul Judgme11L
. • I
CoatiDui.111 Cllibntioa
L If uy wlatile or aemivolatile TCI.. compound 1w I llelative Response
FKtDr of less than 0.0S:
2/U
I I I I I I I I • I I I I Ii I I I I I I A. B. b. Objecd'l'e 1) 2) Flag positive resulu for that eompouod as estimated (J). Flag non-detects for that eompouod as unusable (R). If any ~btile or 1emivolatile TCL compound us a ~ DiUerence llec,,·eeJ1 IDitiaJ llld Continuing Ca.libntion or 1reater dwl 25%: 1) 11q all pwir;.., .aDlu for lhas c:om~11d as estimated (J). :) Nor 1 11 -Y be qaftfied ming pro(cssioul judgmeat. -• IV. BLANJS ~ The asse.ument of bllllk a.aalysis r=llla is to determilie the existence 111d 1112pit11de or corramioatwii probiam. ne criteria for evuaatic11 of blanks apply to uy blank qsociated with the amples. 1f problems with IDl bla.Dlt um. all dara associated with the Cue must be cvd'ully evaluated to dtterauDe wbe1llet or not there is &11 inherent variability m the data for the case, or If the problem is u isolated oc:cumnce not affectina other data. Criteria No co11t1min1n"' abowd be s,nseot in tile blallk(s). C. ·E,,.luad0& Plocab1re J). 1. 2. Acdoa • lleview the results or all associated blank(s), Form l(s) and nw da12 (chromatograms, reconstructed ion chromatognms, quutitation reporu or data system priruoua). VeriCy that Method Blank ualysis has been reponed per matrix. per concentnrion IPet. for each OC/MS system med 10 ualyze VOA umples, and for each eiuraetio1 llatcb for •mivolatiles. ne reviewer CID -the Method BlaAk Summmy (Fona IV) to mist in identifyiD& 11111ples associated with acb Method Bluk. Action ba tlle case d anitable b&anJt nsvlts depends 011 the circumstances and ori1in of the blank. No paaisi-Ye 111Dple J'esults should be reponed unless the concentration or the compowd ill die 11111ple uceeds 10 times the amount in any bluk for tbe common coi,tamin•nts listed below, or 5 times the amount for other compounds. IA instances where more tban 011e blank is associated with a aiven 11111ple, qualification should be based IIJ)On a CIOtllp&rison with the associated blult .. vinl the lushest concentration or a coi,tamlnant. The results mast IQ1 be corrected by 1Ubtnctlaa uy Illa.Ilk. \'Slue. Speci{'ic actiou are as r ollows: !. . !.~ 12 2/IS •·
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I.
2.
.. •
3.
1f a compou11d is found ill a blank bu1 AZ Couod io the sample, 110 action is
a.ken.
At1y ~mpouod (other than the five !isled below) de1ected ill the wnple
,.·fucll W'&S al.so dtte<:ted io a.cy as.,oc:ia1ed blank, m11SI be qualified wbe11 u,;
amplit CODCe.Olnt:ioci ii las tlw! five times die blaAlr. c:oncentration. For the
foDowia& f""" compouDds, me n:sula 1111' cpwified by elevatina the limil or
dtreaicr. wilft tM nmpir corrn1"tiou i\ les.s lha.o 10 cimcs the blank
C0DCeD!TIUOII.
Common lab co11t1minana:
L Methylene chloride -· -
b. Acetone
c:. Tolueoe
d. l-~
e. Common phtulale esin,
~ rniewer 1boa\d note that the blaok u.alyses may not blvolve the same
~lm. YOlvma. or dilutioo (IC'IOn as die associated 1&111ples. nese facton
mat be taken into considention wheo applyina the Sx and lOx criteria, 1ucb
dial • c:amparisaa or &be iotll amoUDt or contamination is "1Ullly DWle.
Additioully, 1here may be UIS1l!lces where little or no c:ontamlutlon wu
i,resent in the associated blallla, but qllllification or the a.mple was deemed
Decessary. Contamination Introduced throuah dilution water is one example.
Although it is not alway, possible to determine, insunca or th.ii oc:currin& can
be detected WMn cc,~nmin•nts an found ill the diluted 11111ple result, bat are
absent in tbe undiluted a.mple resulL Since both results are not roatinely
nponed, it may be impossible to verify th.ii aource or c:ontamiution.
However, it the reviewer determines that the contamination is from a aource
other th.La die sample, lae/1be should qualify the data. Ill th.ii ease, the Sx or
JOx nile does not apply; the l&ll!ple value alaould be reported IS a non-detect.
'TIie followin& an examples or 1pplyin1 the blank qllllification 1uidelille.s.
CenaiA ~ may wanut deviations from th'" 111idelines,
Ote t; Sample result is areater din the Contract Requited Quaatitation
Limit (CRQL), bat ii Jeu lbaD the required amount (Sx or JOx)
from the blanlt result.
Blank R.enlt
CRQL
Sample Result
Qualif"ied Sample Result
&Ilk
lli. ~
7 7 s s
60 30
60U .. JOU ...
Ill the eumple for die lOx rule, sample results less tlaaa 70 (or 10
s 7) would be qlllliraed IS aoa-deteets. Ill die case or die Sx rule,
ample results Jar IJaan 35 (or S & 7) would lie qualit'IOd as non-·
detee11. ·
J3 2/11
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
. -•
5.
6.
Sample result is less thaa CRQL, aad is also less thaa the required
.&mouat (51 or 101) Crom the blulr. result.
Blank Jlesuh
CRQL
5amplchra>t
Qa&lif.ied ~ Jlaalt
Rm
J.Q.g 1l
6 6
5 5
4J .,
5U 5U
Neu that data are not re,:,oned u 4U, u tlus ,vouJd be reponed u
a deteetioa limit l!ei9~e CP.QL.
Sample result is 1reaw than die required &mount (!ix or I0.1)Jro111
die bl&Ak reswL
BlaDk Remit
CRQL
Sample Result
Qualified Sample Result
l!.lll:
J.Q.g 1l
10
5
120
120
10
5
60
60
For both the 10x and 5x rules, 1&111ple results exceeded the
adjusted bluk RS111a of 100 (or 10110) and 50 (or 5110),
nspeetively.
It gross coatamination exists ("a.e-. saturated peaks by GC/MS), all compouads
attected should be naaaed II aasable (Jl), due to iaterfereace, i.D all samples
attected.
If iaordiaate &mouats or other TCL compouads are fouad at low levels in the
blank(s), it may be indicative or a problem at the laboratory and should be
Doted iD the data review COIIIIIWlts whicb are forwarded to the DPO.
S'mwar consideratioll should be v,e11 to TIC compounds which are found i.D
both the ample &Ad associated lllank(s). (See Sectioa XI tor TIC auidaace.)
V. IJZBBQGAU BECQYUY
ObJICtl"
Laboratory performance on iadividaal ampla is established by me1.111 or spikina
activities. All sampta are ■piked with nnoaate compounds prior to ample
preparation. Tbe evaluation or the results or daese ■um,pte spikes is 11ot 11e: 1111r :1y
ltraiahtfonvud. The ample itself' may prodace .«eets due 1D such racton as
buertereaces and lliah concentratiolll or ua1,tes. Si.Dee the effects or die ample
matrix are frequently outside the cootrol or die laboratory and may present relatively
IUlique problems, die review and fllidatioa or data based on speciric ample results is
14 2/1&
---------------------~·-------
I
I
I
I
I
I
I
I
I
I
I
I
I
••
I
I
I
I
I
B.
c.
D.
frel:luently subjective aad demands analytical experience aad i,ro(essional judgment.
Accordingly, this section C011Si.sts primarily or 1uidelines, ill some cases with several
optional approaches rugge.sted.
Criteria
Samele &Dd blw nn-o,ate recoverie.s (or volatiles ud aemivolatiles mu.st be within
limit! as per applicable SOil' (Form D).
i: .. 1uadoa Pr-ocdan
J.
3.
Cbeck nw data (u .• dromat.otnm.s, .-nt mt. eti:.) to Ylrify the recoveries
,011 the SclrToc,ate Recovery (Form D).
Tbe followi.111 ahould be detennilled from the SUffOlate Recovery rorm(s):
L
b.
tr any m runo11tes withln a bae/11eotnl or acid fraction (or one
11UTOgate ror the VOA Cnction) are out of 1pecificatio11, or if any one
ba.se/neutnl, acid or VOA 1unoaate 1w I recovery of less than ICYtli,
then there ahould be I rcamlysis wi.ila lllffOl&te results atill outside the
criteria. ~ WheA &lien are Dll&Q.ei)table 1uno11te recoveries
followed by 1uccessra1 re-lJl&lyses, the laba are required to repon oaly
the auccasful ru.11.)
Tbe lab has failed to perform ausractorily If 1unog1te recoveries are
out or apeciiacation with 110 evide11ce of repuraing, reilljectio11. or re-
e:uraction.
c. Verify that 110 blanks bave 1unoa1tes outside the criteria.
Ally time there are two or more analyses for a particular fraction the reviewer
must determine which are the best data to report.
Consideratiom should illclude:
L Suroaate recovery (JIWllll&) ff. poss deviation).
b. Holdm&rillles..
C. Comparito11 or 111e wlues or die TCL compounds reported bl each
fnctioe.
For sum,11te spike recoveries out or specuacatioa, the following approaches are
suggested based 011 a review or all da11 Crom the cue, especially comiderill& the
appare11t complexity or the ample matriz:
J.
. I
IC at least m nnoaates ·• a base/antral or acid fraction or GIie 111nog1te ill
tbe volatile Cractio11 are oat of' apecif"atioo. bat have nco'""es irater dwl
IO'lli:
L Positive results for diat Cractioa are f'laued u estimated (J).
u 2/11
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
A.
B.
2.
3.
,·
b. Negative RSulu for that rraction are ~gged with the sample
Quantit:ation limit as estimated (UJ).
Ir any surrogate ill a frxtion 1h0Yil less than 10% recovery.
L
b.
Pautive mlllu far tlw f~ an l'Aued as estimated (J).
Neptive mlllts for Wt fnaion art flaa~ as uusable (R).
No oualirica•ioa .-ith nsP«"t ID nrropt~ ffl:Oftry is placed 011 data 1111\ess at
least n.o 111noa1tes an: out of specification ill die base/neutral or acid
fraction, or one ill the vobtile fraciiou., or 1111less any aurTO&lle bas a less than
10% recovery.
ID the rpeciaJ case or a blal1k amlysi, w.itll sun-optts out or specificati011, the
nviewer must Jive ac,ec:ial colllideffoon to the validity or 1moci11ed sample
data. Tbe lluic cmceni is whether the blal1k problems represent an isolated
problem with the blank alone, or whether there is a fundamenw problem with
the ualytic:al proas:s. For ex.ample, if' one or more samples in the batch ahow
acceptable l'IIITO&IIC ,-,.erieJ. lbe reviewer may choose to consider the blank
problem to be an isolated ~mnce. However, even if' this judgment allowi
aome use or the affected data. ualytical problems remain that must be
corrected by the laboratory.
VI. MATR[X SPIXE!MAJJIIX SPIXE DUPLICATE
ObJectbe
These data are 1e11erated to determine long-term precis1011 and accuracy or the
analytical aiethod 011 various matrices. These daia WIit cannot be used to evaJuate
the precision and acc:uraq or illdividllll 11111ples.
Critula
I. Spike recoveries must be witlwl the advisory lim.ia esiablished ill the
appropriaaie lfl &Dd OIi Form m.
2. Relative Pen:at DifTereaca (llPD) bet• cu, matrix tpike ud mtrix spike ·
daplic:ate ,...,..ve,ia IIIIISt lie widt.iD die advisory limia esiablished in the
app,+atc IFI ud OIi F-DL
l. Jmpect nsula for die Matrh 5"ike/Matrh Spike Duplicate Recovery (Form
m). ' ,:; .
2. Vuil'y truacriptiom from nw data ud wrily calculatio~ ;
-
16 2/1&
I
I
I
I
I
I
I
I
I
I
I
I
I·
I
I
I
I
I ,,
D.
B.
Aclioo
No ai:tioc is takec 011 Matrix Spike~trix Spike Dllplicate (MS/MSD) data 1J.Q.n.t to
quali(y ac eatire Cue. However, usi.cg Wormed pnifessioll&I jud1me11t the data
revie,.·er Jl:3)" ~ lbe marri.1 1pilte and matrix si,ilte dup\icatt nswr:s ill cocjucction
with othe.t QC crituia and determine tbe Deed ror 10me quallfic:a6oa. or the da12.
T~ d.aA reviewer 1hould fint try ID determille Ill will! exwat 1he resulu of the
MS.'MSD a!(ect tJwo aDOCir•ed dam. n.i! de-tuminatioD abould be made with regard
to tht MS(MSD sample i.uc1f a.s "" as specific aDai,u:s (or all 1a111i,les associated
with the MS/MSD.
In those in.sta.nm where ii QII be de1c1 mined dttt t:le n:sullS o( the MS/MSD affect
O11\y the sample 1piked, thee qualific:atioc should be limited ro this umple alone.
However, it may be determiDed tbroag)I die MS,'MSD resu\lS that a lab is hrticg a
1y,tematic problem m the analysis oC ou or more ual)'t.eS, which affecu all
associated samples.
. -• Vil. DELP PJJPLJCAJES
Objecthe
Field duplicate samples may be taken ud analyzed as u indication of overall
precision. These a11al)'$CS measure both field ud lab precision; therefore, the results
may have more variability tlwl lab duplicates which measure only lab penorma11ce.
It is also expe:ud that 10il duplic:ate ruults will have a areater variance than water
matrices due to difficulties associated with collectin& identical field aamples.
Criteria
There are 110 specific review criteria for field duplicate ualyses comparability.
C. Enluatloa Pl'Kedura
D.
Samples wtaa are field daplic:ates should be identified IISUII EPA Sample Trafrac
Reports or sample field sheets. ne nviewer should compare die resulu reported ror
eKh ample and calculate the Relative PerceDt DiC(emace (RPD).
Acdoa
Any rnluation of die raeld daplic:ates llaould be provjded with the reviewer's
co-e11ts.
•
17
--•.
•• .. --I
2/U
I
I
I
I
I
I
I
I
1·
I
I.
•·
I
I
I
I
I
I
I
VIII. 17'TIB :-,; ,l.L STANDARDS ftBfPBMANCE
A. ObJetth~
B.
l.Dteni&l Saochrd.! (15) per(onzwice criteria flllllff 'dlat GC/MS temitivity and
response is suble d"1'iA& nery ru11.
Crllerla •
1. lwnw standard a.rea coll!lts mllfl 11oe ..,,-by more than I factor or two
(-~ Ill +JOO'llt} from tll.e wociated calibr1tio11 11111dard.
2. The rereotioD time of the iznenw 11111dard mllS1 IIOI \'II')' more thao :30
secoods Crom tm associated c:alibratioo 11111dard.
C. Enluadoa P,occdirn
1.
,· .
2.
3.
D. Actloa
Check raw data (i.e., chrom11ograms, q11&11titati011 lists, etc.) to veriCy the
recoveries reporud oa the l111enw Studard Am Summary (Form VlllA,
VllIB).
Verify that all retention times 111d IS ueu a.re acceptable.
Aay time then are two analyses for a i,articular fraction, the reviewer must
determine which a.re the best daCl to report. Comidentiom should include:
L Magnitude of the shiCL
b. Holding times.
c. Comparison or the values or the TCL compounds reported ill each
fraction.
l. If' an IS area coUDt is outside -5096 or +100Cl6 or die associated 1t111dard:
L Positive resula for compouads qaantitated ailla t1aat JS are flaaaed as
estimlled (J) ror lbat -pie fractioD.
C.
Noti-det«tr for compoonds quazrtitated IIIUII dial JS are flagged with
die sample q11111titalioa limit c:lassuied a eslizlllted (UJ) for that
tample fnctioD.
U extremely low area couats are reported, or if performance exhibits 1
major abrupt droP-OCf, theD a severe Joa or eemitivity is illdica1ed.
No11-detects lhould theD be flaued as 1111asable (R). . ·
-:£· ... . , .•. .,..
2. If an 1S reteatioD time mes by more thu 30 tee011ds, 111e·c1uvma101r1phic
11roriJe far lbat 11111ple must be examilled to determiae IC uy false positives or
11 2/11
A. B. C. 11egatives exist. For shifts of t large mag11i111de, the reviewer may con.sider partial or total rejection of the data for that sample fraction. DL IO, COMfOUND mrNTinc,4,nON Ob)ecthe ne ob~ or lhe criteria lor GC/MS qualitative analysis is to minimiR the 11umber of em>neous identifJcatioDS oC compounds. AA ~neous identification cu either be a falst positive (reporti.111 a compound preseal 1111111 ea it is 1101) or a false negative (1101 reporti.111 a compo1111d that is present). -'Ille identif'u:ation criteria cu be 1;19\ied ma more easily hi deteetina false positives than false 11egatives. More information is available due to the requirement for 1ubminal or data 111P110rtin1 positive Mie11tilicati0ns. Neaatives, or non-detected compounds, OIi the. other hand represent III absence or data 1.11d are, therefore, much more dil"ficult to assess. 'Criteria 1. Compo1111d must be within :t().06 relative retention time (RRT) IUlits or the IW!dard RR T. 2. Mass si,ecua or die ample compound 111d a current laboratory-1e11erated ltllldard must match acconSill& to the Coll0will1 criteria: L b. C. All iom present in the 1t111dard mus apec:tnim at a relative inte111ity &reater than 1°' J11J1S1 be present ill the ample spectrum The relative izltemities or 10111 specified above must agree within :t2°' between the 11&11danS 111d sample spectra. (Eumple: For 111 1011 with u abuduce or 5(1111, ill the 11111dard spectnlm, the corresponding •mple .ioll ~uduc:e must be between 3041111.11d 7°'-) Jons areacer tllaD 1ft hi die aroPle 1rr,,ec:a um but 1101 present ill the •flpdaal aped:lu.u must be co111idered ud accouted for. E•alaa&.l'lw:eun I. C11ect dlat the IUlT or reported compou11dl is within 0.06 JUlT allits of the nfeiace 111Ddard. --,, 2. Oect the laboBtory ltllldard spec.a, YS. the 11111ple compoud spec:tn. 3. The reviewer ahoatd be aware or sitvatiom (e-1,, luJII coace11tratio11 amples prec:edill& tow co11ce1uratio11 samples) when ample CIITJ-oflr is a poaibility and should me Jud1-11t to determine if uistn1me11t croa-co11tuu111tioD Ills affected uy positive ClOIIIPoaDd ide11tif'icatio11. ·..:. 19 2/11
I
I
I
I
I
I
I
I
I
1·
••
I
I
I
I
I
I
I
D.
A.
B,
C.
D.
Aclloa
I.
2.
The application or qualitative criteria ror GC/MS a:wysu of TCL compounds
requites professfooal judgment. lf it is determined Uiat illcorrect
ide.tltificauoos ..ere made, all mc:b data should be f'lagged as -detected (U)
01 aasable (R).
P7ofesrioc!11 j11d1ment 111ml be me4 \0 qalifJ the data if it Is determined that
cros.s-CO"nminotioll w oc:eurffd.
x. COMPOUND OUA"iTXIATION AND RtPQRUD prnmoN LIMITS
ObJectbe
The objec:til"e .is to ensnre that the reponed QIWltitation results and CRQl.s are
a.c:cunte.
Cntula ,· .
1. Cmnpound quantitatioa, IS well IS the adjustment or the CRQL, must be
calculated ac:conlina to the appropriate SOW.
2. Compound RRF must be calculated based on the IS specified iD the SOW ror
that compoDDd. Quantitatioa must be based on the QIWltitatioa ion (m/z)
specified in the SOW. The compound Quantitatioa mast be based on the RRF
from the appropriate daily standard.
E•aluatloa Proc1b"
1. For all (,actions, nw data should be eu.mined to verify the correct ealculation
. ol aD sam;,le results reponed by the laboratory. Quantication lisu,
chromatograms, and sample preparation lo& sheets should be compared to the
reported positive umple resales and quantitation limiu.
2. Verif'y that the correct internal atudard, Q1W1titation io11, and RRF were ased
to quutitate tbe compotu1d.
3. Verify that die CRQLI liaw beu adjasted to renect all ample dilutions,
CIODCeDtntiom, ,;,lies, cleu-ap 111:1mties, and dry weipt facton that are liot
-UDted for l,J die~
U there are uy discrepancies found, die laboratory may lie contacted by the
designated representative to obtain additional mronnadon tbat CI01lld resoJve any
difCereDCes. U a discrepancy remains 11Dresolved, die nvieww must decide which
nlue is the best 'ft111e. Under these drcumsta"Ces, tile l'Piewer. may determine
qualil'ication or data Is wuruted. .
20 2/1&
A. B. C. • XI. U"ITAD".tLY JPt'ffiOtP CO~!POl'ISDS Objective Chromatographic pc.aJc.s ill YOlatile ud aemivolatile fni:tio11 analyses that &re 1101 tarSH compo1111d list (TCl.) M&lyus, suno,.au:s, or illt.enw 1ta11dards are potential tent1tr1~ly idu.tiiied compoW1d! (TIC). TICs murt be qualitatively Identified by (GC/MS) ~-,nm ud tM ideatlf'icatiom wessed '>y the data re-rie..-er. Criteria 1. . . 2. For eadl sample, the labontory must conduct a mass spectral NClth er i.e NBS h"brvy and repor1 1ti.e possible ide11tiry for the 10 Jaraest VOA fraction peala ud tbe 20 brsest BNA fni:tio11 pea.l:s wlucb are not aurro11te, internal staDdud. or TCL compo1111ds.. b11t whiu liave aru/heiaht are.ater thu 10 perc:e11t of the 1m o( die Marat iDter1lll l1:lndard. TIC results are reponed for each sample 011 the Orpnjc AD&lyses Data Sheet (Form 1, TIC). ~ SOW Rvisio11 October 1916 does 11ot allow the laboratory to repon as teatativcly identified omipounds (TIC.) uy TCL compound which is properly reported ill LDOther fJVtioo. (For example, late eluti111 volatile TCL compowads must not be RPOned as BNA TICa.) Gyjdc!jges for tentative idelltif"acation are as follows: L Major ions (Ire.at.er tbu 10'!6 relative iDtensiry) iD the reference apectrwD should be present iA die sample spectrum. b. Tbe relative intensities of the major ions sbould agree within :20'!b bet,11ee11 the ample ud the referen~ apecbL c. Molecular ions present iD the reference si,ectnlm should be present 111 the ample spectnllll. d. Ions present ua the sample q,ectnim b11t 11ot ill the n!(ere11ce spectrum should be n!viewed for possible baclcgrou11d co11t1mmatio11, iDtederuce, or coelution • additioul nc or TC. compounds. e. When the above criteria are not met, but In the technical j11dgment or lhe datl ae,iewu or mass apectral illterpret1tion specialist the icfcntiracat1on is C011.C:t. die data reviewer may n!port the idelltil".::acion. r. II ill the data reviewer's Judament the identiracation is a11certain or then! are estenuati111 facton arrec:wa1 compowad Identifications, Cle TIC result may be reported u "ullkllown•. E'1llaatloa ,,_..,. .... ). . . I . Oieck the nw data to wrif'y that the labontory Jiu aenented a h"brary ICal'Ch for all required pealca ill Ille du'omal03J'I.IDI (samples and blallks). 21 2/11
I
I
I
I
I
I
I
I
I
I
I
••
I
I
I
I
I
I
2.
3.
Blanl. c:hromatocram.s 1bould be eumined to veri(y that TIC peaks present in
samples are not found ill bl&nks. Wben I low-level DOn• TCL compound that
is I common aruract or laboratory conta.m.u1111t is detected iD • samr:,le, 1
thorongh check or bllllk chromatograms may reqllire looking for peaks which
are len than JO percent of the illternal 1ta.11dard height, but present in the
bla.nlc c:hromat01nm at similar relative retention time.
AU mass ~D• ill every ample ud blank must be e:u..mined. •
Smee TIC h"'bnry wchcs often yield se\"Ual c:uididate compounds having a
dose matthilla ll0IS'e. all n:-,mblr dloic:es 'IIIIZSt be cons.idered.
__ ..._ __ The reviewer abould be 1,vare of common laboratory artifacts/contaminants
ud their aourcer (aldol prodDCU, IOlvect preservatives/reagent contami11111ts,
etc.). lbese may be praeD.t ill blu.b ud DOI rec,oned IS ample TlCs. ,
D.
,.
6.
Examples: ..
b.
c.
Common lab conamfaants: ~ (m/e 44), ailounes (m/e 73), diethyl
ether, heune, certain freom (T,l,2-trichloro-1,2,2-trinuoroetlwle or
nuoro-trichlorometlwle), phthalates at levels less th&A 100 u&fl or
4000 11g/k1.
Solvtnt preservatives: ~lobexene is a methylene chloride preser-
Y&tive. Related by-products include eycloheunone, eyclohexeaone,
~lohCllJlol, cyclohexeaol, cbloroc:yclohexene, chloroc:ycloheunol.
Aldo! tac:tioD products or acetone include: 4-hydroxy-4-methyl-2-
peaianaae, 4-methyl-2-pezuea-2-one, 5,S-dimethyl-2(SH)-runnoae.
0c:casioaally, a Ta. compouad may be ideatilied in the proper lllllytic:al
Crac:tion by non-target library search procedures, evea though it WIS ao1 round
on the quanti12tioa list. If the total area quaatiatioa method WIS used, the
reviewer ahould request that the laboratory recalculate the result usin1 the
proper q11&11ti12tion loa. ID addition, the reviewer ahoutd evaluate other
1&111,!)le chromatogruq ud check library reference retention times on
quantiiatioo lists 10 determine whether the Cabe 11e11tive result is an isolated
.OCCllrTellefl or whether data from the entire case may be affected.
7. TCL compoimds may be identiraed in more thu one fraction. Verify that
quuti11tioa is made C,om the proper Cni:don.
Actloa
I. AU TIC nnlts 1hoald be flaued as tentatively Identified with estimated
CODCeDtratioDS (JN).
2. General actioas related co the review or TIC results 1111 u follows:
L IC it is determined that • leDtative ldentlr1C1tiOD
0
=0r • JIOD•TCL
compound is aot ac:cepable, the leDtalivc ldentiratioa .abould be
clwl&ed to -...Uown• or u appropriate identuacatioa. ·
22 2/IS
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
3.
5.
6.
I.
b. If &II COD~Y required pew were DOI library aearched, the
designated repraenmtive could request these data from the laboratory.
TIC results which are not sufficiently above the level iD the blalk should not
be reported. (Dilutions aad IL!llple size mu.st be talten iDto account when
compui.ag the amounts prac111 ill bWlks a.ad ample:s.)
1''tta • CDa1po1111C! is aot fond DI any blanlu, bnt is a 1uspei:Ud artifact or
-labomur, -nmivn!, die nnt.11 aay be flagged a uuuble (R).
la <k.cicliz,.g wbedier a librvy lea1di result for a TIC represents a realistic
idealificatia:-, pro(emOll&I jlldgment must be exercised. II there is more than
oat ~h. die RSult may be reported as "either compound X or
compouod Y." Jf shere ii a Jaclt or isomer 1pecificity, the TIC result may be
cb&Aged to a 11on-1pecirJC ilomer result (1,3,S-trimethyl bellzene to tri111ethyl
benune isomer) or to a oompomul class (2-methyl, 3-ethyl benzene to
1ubstit11ted aromatic oompoud).
The reviewer may ele:t to report all 1imilu i.somen as a total. (All allwies
may be 1umizwi2ed ud rcponed as total hydroc:arbons.)
Odicr Oue Cacton may hilbaence TIC Judiments. It a a.mple TIC match is
poor bur other ami,la .i... a TIC wilh a &ood library match, timilar relative
.retention ~ and the a.me ions, identification information may be illf'emd
Crom the other sample TIC results.
Physical consants, tuch a boili.111 point, may be factored illto professional
judgme:11 or TIC resul11.
m. SYSTEM PERFORMANCE
During the period Collowill& lmtntmenl Performance QC checks (e.1. bl&Dlcs, tuning,
c:alibration), changes may oc:ear DI the system that dearade the quality or the daia. While this
degradation would iiot be directly sllowD by QC clleek, ntil the nut required aeries of
analytical QC nam, a dloroll&h review o( die naoia& data acquisition c:u yield illdicaton or
instrument performa.ace.
Sollll' enmptes or Jmlnameat perf'ormuce illdicaran ror 'ftrious Cac:ton are as
follows:
I. Abnlpl, dilc:reft lhifCI ia ._bca.d ion dlrvmatogram (IUC) buelille may
iadicate pin or dlresho14 dlaqes.
2. Poor cbrollllto&npbic performance atteeu both qulitative ud QUUtitative
resulcs. llldicatio111 or nbs1udard performa.ace iDclude:
I
L Hi&h lllC lleck&r0Ulld levels Of lhif'ts Ul 1blol11te ntentioD times or illtern.al
l1Uldardl.
•. ...... .
b. E&ceaive bueliDe rile at elevated aempe,.ture.
23 2/IS
I
I
I
I
I
I
I
I
••
I
I
1·
I'
I
I
I
I
I
I
c. E..uraneow ~ks.
d. Loss or resolutioa IS 1uggested by racton such IS aoa-resolution or 2,4-and
2,S· diDitrotoluene.
e. Pw ra.iJiag or peak splitt.in, may reralt iD wccunte QIWltitation.
Coatiautd anuytjcal ac,h·ity '11\tll dfgraclec! ptrionn&n~ 111uesa lack or aneation or
i,rofessiona.l e1pei-ieoee. Based 011 CM iastnlmtllt peri'Clnll.l.llee illdicaton, the data reviewer
must decidr ;r tM 1}'ltcm Im dcgnded 10 cu poilll or a!Tectin& data Q\llliry or Yllidiry. Ir
data qualicy zm.y U\'1: tws aO'ecud, data shoud be qmli{"aed wing the rtviewer'1 best
i,rofessional judgment.
xm. QUB ALL AS:SE SSYErIT Of DATA FOR A CASE
It is appropriate for the data rtviewer to make professional jud&ments aad express
conc:erns aad commeua oa the validity or the ovenll data package tor a Case. Tlw is
i,articulwy appropriale for Cases in which there are several QC criteria out of specification.
The additive nature of QC racton out or 1pecificatioD is clif'fie11lt to usess ill u objective
manner, but the RViewu bas a respomibiliry to Worm men con~ng data Quality ud
data limitations ill order to assist that mer ill avoidin& iDappnipriate me of the data, while
not precluding any comidentioa or the data at alL TIie data rtviewu would be areatly
assisted in this elldea vor if the data qm.lity objectives were provided.
2/11
I
I
I
I
I
I
I
I
I
I
B
g;
It
I
I
I
I
I
1.
PESTICIDES PRoctDURE:
The requirements to be chedted in validation are listed below. recs-indicates that
the con1nc:1 requirements for these items .,ill also be checked by CCS; CCS requiremenu are
DOI always the same as the data review criteria..)
L lioldin& Tiaies (CCS -Lab holdiag times only)
n. "enicide:! 'we u-.Al ht'fa,rm (CC:S)
o wtial (CCS)
o ADalytical Sequence (CC:S)
0 Coatu111mg (CCS)
IV. Bbnk• (CCS}
'V. Surrogate Recovery
VL Matrix Spike/Matrix Spike Duplicate (CC:S)
VIl. Field Duplicates
vm. Compound Ide11tificatioa
IX. Compound Quantitatio11 and Reported Detection Limits
X. Overall AJsessment or Data ror a Cue
...
'
25 2/11
I
I
I
I
I
I
I
I
I
I
I
I
••
I
I
I
I
I
A.
B.
C.
D.
A.
I. HQLP{NG D'Jts
Objecll°>e
Tiw: ob~~ti~ is to mcenam dat 1'alidity or results based oD the holding time or the
sample from J)m• qf Q!)c;'tkQ ID lime of &1Wysis or mple preparation, as
ap Pf'Oi'l'i:a r~.
Criteria
Technical requirements for AmOle holdmg times laave only been established for ,.,.,er
matrices. The holdiDg times for aoils are eurrently uder iD~o~ea, When the
results are available they will be incorporated into the data e,,alaation process. On
October 26, 1914 in Volllme 49, N11111ber 209 or die Federal Re1ister, paae 0268, the
boldi.Dg time requirelllen!J f01 pesticides were established ander -40 CFR U6 {Clean
Water Act). Samples mast be ei:tncted within 7 days aad the extnct must be
analyzed within 40 days. Both 11mples aad extracU must be atored at 4• C.
Euluatloa Proced11re
A~al holding times are established b7 comparing sampliD1 date on the EPA Sample
TBl'Cic Repon with dates of I.IW)'ID aad extnctioD OD Form L E11mine the umple
records to determine if samples were properly preserved. (1f there is DO indication or
preservation, ii must be assumed that the aamples are upreserved.)
Actloa
If 40 CFR 136 holding times are exceeded, fla& all positive results IS estimated (J)
and sample quantitation limits IS estimated (UJ) aad clocament to the effect that
holding times were exceeded.
I.
.2.
If holding times are 1rossly exceeded, either on the f"111t analysis or upon re-
analysis, the reviewer must ase professional Jud1ment to determine the
reliability of the data and the effect ol additional storage on the aample
results. The reviewer may determine DOD-detect data are uusable (R).
Due to limited information concernin1 holdill1 times for aoil samples, it is lert
IO 1lle cliscntiol ol the dlJa reviewer to apply water boldill& time criteria to
9oi.l nmpleL
n. PtsnQPts INSTJl\JMJNJ PEB[ORMANCE
ObJecthe I
Tlttse criteria are established to emare that adequate cllromatosrapu: resolutioa aad
iutrumeiit 1ensitivity are achieved by the chromato1npluc system. nese criteria are
DOI sample specif"ac; conformance is determined miq ltaDdard material,. Tberefore,
dlese criteria should be met ill all eir=ml1aaces.
26 2/11
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
'I
I
I
B. Criteria
2.
3.
,· .
DDT Rete11tio11 Time
DDT must have retention time on packed col1111111S (except OV-1 and OV-101)
IIUW' thaJI or equl to 12 IIIII.LIIII\!\.
Re1entio11 Time Windows
The laboratory must ft1)0rt retention time window datl OIi tbe Pesticide/PCB
Swid&rds S11mZDalJ' {Form IX) for each GC column 11Sed to analyu samples.
DOT /EDdrin Degradation Cbeck
The total percent breakdown for aejther DOT Dor endriD may exceect 20%.
~ pen::ent breakdoWII is Uic a:momit or decomposition dial endriD and 4,4'-
DDT llllderio •hen analyzed by the du~raphic 1yssem.
L
b.
C.
For endrizl. the percent breakdown is determfoed by the presence or
endri.n aldehyde ud/or endrin ketone in the GC chromatogram.
For 4,4'-00T, the percent breakdown is determined from the presence
of 4,4'-DOO ud/or 4,4'-DDE in the GC chroma1111ram.
A combined percent breakdown must be calculated If' there Is evidence
oC a peak at the retentioD ti.me of endriD aldehyde/4,4'-DOO, which
co-elute OD the OV-1 packed column (or u equivalent col1111111).
d. Percent breakdown Is calc11lated usina the followiq equations:
'Ill Breakdown •
for .C,4'-DOT
Total DDT dearadation peak area (ODE + DOD) z IOO
Total DOT peak area (DDT + ODE + DOD)
De,ndatioD Ptak Areas (ndrin aldehyde + eDdriD ketone) • 100
'Iii Breakdown • •
for endri.n Peak Area (endrin + endriD aldehyde + endrill ketone)
Combined •
'Iii BreakdoW11
NCM J;
Nptg 2;
Peak uea of endrin aldehyde mllll be measured during
die de&ndation check IO wrify ,ystem performuce •
.Eadrin alddlyde is DOI reported OD Form I because it Is
.-¥ed by alumi111 cleanup.
The tmn 9peak beipl" _, be Abltituted for the term
9peak area•.
Total degradatioa peak mas • ,
(DOE + DDD + endrill aldehyde + todriA ketone)
Total DDT 111d eDdria peak mas ·
(DDT+ DOE + DOD + endriD + eDdriD aldellyde + udriD ketoDe)
27 2/11
I
I
I
I
I
I
I
I
C.
D.
r:
2.
3.
Acdo■
1.
2.
DBC Retectioc Time Check
The retectioc time of DBC ic each &11.l!ysis must be compared 10 the re1e111i011
time of DBC iii E~uatioc SWldard Mu A. The Pcrc&111 Difference (%0)
must 1101 exceed 2.0% for packed coh1m111, O.l'il for 1WTOw-bore capillary
cohimas, ed 1.5% if wide-bore cap~ colum» an med.
ltTs
• z 100
• Absolute rete11ti011 time of dibutyldl!orudatc ill the initial sca.adard
(E ~ll&tio11 Stl.lldard Mix A). ~
• Absolute retention time or ch1,af)'lchlorelldate ill the subse(iue111
analyses.
Check raw data tD verify th.it DDT reteatioll time is 1reater tJwi 12 micutes
011 the standard c:moma101ram and tllat there Is adequate resolution between
pea.ks.
Check raw data to verify that rete11tioa time windows are reported 011 Form
DC. and that all pesticide studards are widu11 the established retention time
willdows.
Check nw data to verify that the perceat brealcdoWII for e11drill ud 4,4'
-DDT, or the combined pen:e11t breakdoWII, · does not exc:eed 20CI& ill all
EYSluati011 Stalldard Mix B ualyses 011 Form VDJ D.
Check nw data to verify 1hat the perce11t difi'ere11ce ill rete11ti011 time for
dibutylchlore11date ill all 1ta11dards ud amples is .s 2.0CI& for packed colum11
ualysis.. .s 0.31' for capillary colum11 ualysis, ud s 1..51111 for wide-bore
capillar]' collUllll aalysis Oil form VDJ E.
DDT lte1UDllll TJJDC
JI' Ill& fflntioli d.e of DDT is less dwl 12 millates (u.cept 011 OV-1 ud
OV-101). a close eumi11atio11 or the cllromatoaraphy is 11ecemry to emure
dlat adequate separation or individual components is achieved. U ad~uate
aepanti011 is 1101 achieved, f1q all affected compollJld data as anusable (R).
llete11tio11 Tame Willdows I
llett11ti011. time windows an ued ill Qualitative idelltiricatioa. U the ata11dards
do not fall within the retention time wiadows, die usociated sample results
lllould be carefally evaluated. AD rmples injected after die last in-control
a1Uldard are pocutially affected.
21 2/11
I
I
I
I
I
I
I
I
I
I
I
' q
I
~ •
I
I
I
I
I
I
3.
••
b.
For the .rrecied samples, check to see if chromatograms contain any
peaks within a.a expanded window 1111Tou11di11g the expected retention
time window or the pe.sticide of interest. U 110 peaks are present either
within or dou to lhe re1e11tio11 time window of the devwit target
pestic~ compound. there is usually 110 efr~t 011 the data. (Non-
detecled ~11es CUI be conside"-Cf valid.)
lf the atreeted aample chromatognms coat:w1 peaks which may be or
conceni (i.e., •bo~ lite CR.QL &Dd either dose 10 or within the
expected rett11tio1 time willdow of the pesticide or interest), then two
options are •~ to the reviewer to cleterawie lhe extent of the
eff«t 011 the dalL
1)
l)
IC 110 additional effort is 'Wllnllted by the reviewer, Oag all
positive results and qwuititation limia as unusable (R).~ The
un-ative ahould emphasize the possibility of either false
negatives or false positives, u appropriate.
Ill some cases, additional effort is wuranted by the reviewer
(e.1-, i£ the data are lleeded 011 a priority basis and if the
peak(r) present mi1ht represent a level of concern for that
partiC'lllar pesticide). In these situations, the reviewer may
widerulce the following additioul effons to determine a usable
retention time window for affected aamples:
(1) TIie reviewer 1ho11ld examine the data package for the
preunce of three or 111ore ,swidards containing the
pesticide of interest 1h11 were run within a 72-hour
period during which the -pie was analyud.
(b) IC three or 111ore 111ch standards are present, the mean
ud 11a11dard deviation of the retention time window c:an
be re-evaluated.
(c) If' all 1taJ1dards and 11111rix spikes fall within the revised
window, the valid positive or negative ample resula can
be detel'lllilled using this window •
(d) TIie unative should identify the additioul efforts·
1akft by the nv~wer and the resultant impact on data
-bility. la additioa, the support documentation should
coalaill all calc:ltlaoom ud comparisons generated by
die reviewer.
DDT /Endrill Degradation Claeck
L IC DDT breakdown is 1reater th8II 2(1116, begiuiD1 with the samples
following the last jg-control 1taJ1darlt ,
-: ..
I) Flag ID quantitative results for DDT u estimated (J). If DDT
-DOI detected, bul ODD and DOE ue positive, tben flag the
quantitatio11 limit for DDT u unusable {R).
2/18
I
I
I
I
I
I
I
I
I
D
I
I
I
I
I
A.
"·
b.
2) Flag results for DDD ILlld/or DOE LI presumptively present at
u estimated qu111tity (NJ).
If' endriD breakdoWD is greater than 20'1&:
J) Fh& all q11&.11titative resula for e11drui as esumated (J). If
•dml was aot detected, ,u, endrm aldehyde ILlld eDdriD ketone
an positive, &hea flag 1lle q11&11titation limit for endrill as
ausable (R).
2) flag raults for ndrin ketone as presumptively present at 1L11
. atima ted qantity (NJ).
Rete11tio11 'fime Check
L
b.
JI' tht l'dlllltioll cimc aJ:ai!r for dibvf)'JchJo~date (DBC) Is greater thaD
'2.0'lb for packed colvru, greater thaD 0.3q& for 11&1TOw-bon capillary
colvm.n, or greater thaD 1.5% for wide-bon capillary column, the
am.lysis may be flagged unusable for that sample(s) (R), but
cru-lification of the data is left DP to the professional judgment of the
reviewer.
ne retention time 1hift c:amaot be rtaluated ill the absence of DBC.
m CALIBRATION
Objecth·e
Compliance requinme11a for satisfactory illstrume11t calibntio11 are established to
ensure that the i.Dstrume11t Is capable of produciDg acceptable quutitative data.
Initial calibntio11 demonstrates that the i.Dstrument is capable of acceptable
performance ill the be1i11Dill1, IDd coati11uiD1 cah"bntio11 checks document
satisfactory maiDteD1L11ce ud adjunment or the iDstrume11t over apecif"ac time periods.
J. IAitial Calibration Linearity Oieclc
'tbe Percent Jlelative St111dard Deviation ('RSD) of calibntio11 facton for
aldriD, ndriD, DDT. ud dillutylchlorudlte mast DOI exceed IO'lb. If
maphe11e is ide11tiraed ud QUIDtiraed, a thRe-poiDt calibntio11 is required.
IC the calibntio11 fac&or for DDT or touphene is outside the IOC!li RSD
window, calibn&ioa auws m\lSt be med for QU1Dtitatio11 of DDT, DDE,
l>DD, • IDDphme.
Calibntio11 FICIOr • Total A[CI of' Prak
Mass Injected (111)
JO
.-. .. I
2/11
I
I
I
I
I
I
I
I; .,
I
1:
1t
11
1·
Ii
1:
I!
Ii
11
C.
2.
,· .
Cl
1 100
CF
wbere,
CS • 5tlndarJ Deviation
CI' • Me:u C&l.ibntion Factor
~ 1lw IO'i RSI> linearity chec.k is required only ror columns which are
used (or qaai,tita.tive ~tiom. Quutitation or the surrogate
reqaiaes die uc of• cioluma. ~ &o .meet the IO'li, linearity criterion.
Co\amm aed only 1D provide qalitati'" COAiumati011 are not required
&o meet tbis criterion. ·
All&lytical Sequence
L Primary All&lysis
At die llegiADing or each 72-hour period all standards must be
all&lyzed.
b. Coaiumation All&lysis
1) Evaluation Sludard Mix A, B, and, C are required ror the
c,uye.
2) Only the ltalldards containing the compound(s) to be confirmed
are required. These 1ta11dards must be repeated alter every five
amples.
3) Evalnatioa Mix B is required alter every ten samples.
3. ContiDuiD& Cahmtion
'Ille c:abmtioa r1C10r ror each 11Udard must be withiD J5q& or the standard at
die lle&imlm& ol Cfle U&lytical ,equence on quantitation columm (2011 on
COnf'"ll'lllatioD eolamm).
Emudo• Paoc,d■n
1. !Aida.I Cah11ratioa
L
b.
._pee( die r.ti:ide Evaluation Slud&rds Summary (Form VID) and
wrif'y qreement with die nw GC data (chromatoanmS and data
aynem printouts). .. ~· -
Deck 1lle nw data ud recalculate IOme or the c:ah11ratioD racton and
Clle perceat relative JtaDdard deviations {'RSD) for aldriA, endrill,
.DO'\" J.1>ec..
2/11
I
I
I
I
I
I
I
I
I
I
1·
I
I
I
6
I
I
I
I
D.
2.
3.
,·
Actloo
c. Verify that the 'loRSD for the calibntion factor or uch spe:iri;
pesticide is less than or eQual to IO'li. for each 72-hour period.
d. If en-on are detected, more comprehensive recalculation should be
petfonned.
e. Jr soupbeoe or tbt DDT series wv identified and quazrtitlt2d, verify
that 1. t'arer-point calib~t.ior. wu established.
Verif'y that ~ studards were uwyud in the 72-hour sequence.
Continuing ~ibntioa
a.
b.
Review the pesticide sample dau to verify whether the standard wu
wed u a qumticatio.o standard or as a confirmation standard. ,
For the qnantitatioa swidards, check the nw data to verify the percent
difference (111,D), ming 1he followina formula., for approximately tea
percent of the reported values by recalculation.
:i: 100
where,
R 1 • Calibncioa Factor from fine analysis
R2 • Calibntion Factor from subsequent analysis
'
1. lDitlal Calibntlon
tr criteria for linearity are 1101 met, Oaa all associated quantitative resuhs u
estimated (J).
2. AAalytical Sequence
3.
tr die proper mndards uve not been ualyzed, data may be affected. The
dau nviewer must nse professiollll judament to determine severity or the
effect uad qualify die data accordill1ly.
Oatiaum& C'alilndon
L If' die 41D betweai calibntion facton is areater than IS% for the
compouad(s) beiaa quantitaled (2041b for compounds bei111 coararmed),
fla& all usoc:iated positive quantitative results u estimated (J).
I
32 2/11
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
A.
B.
C.
D.
IV. BLA!l\iS
Objecti•e
~ -essm,,;it of bl.a.ak &ialysis results is to delm!Wle 1be nislUCe ud magnitude
of coc,nmim>:ioc problem4. l'lle criccria for •Yllluatio11 or Nulks apply ID any bbok
ass~ted with Che ~le1. l! problem! ,..jt)I au 'oDlak aist, all da12 assoeiated -.·ith
the Cue must bt c:amolly evahia!.ed ID determia,e wt.et!ltt or not there is an illhereot
vuia!rtlity .iD the data for tht. Case, or the problem is an isolated occ11rreoce 1101
af'ft.ctml otliu dalL
Crlteria----
No contaminants should be prescllt ill the bluJc(s).
Enlualloa Procedare
1. Review tu nnlu or all associated blank(s), Form l(s) and nw data
(chromatoJ)'mlS. qmnti12tio11 re90ns or data sy1tem printouts).
·:i Verify tbat. the melbod blaAk ualysis(es) co11ca.im less th.an the Co11tnct
Required Quutitatio11 Lim.its (CRQL) or cy Pesticide/PCB or hltert'eriDa
peak.
3 ..
Acdoa
Verify that method blank a11alysis bas bee11 reported per matrix, per
co11ce11tntio11 level, for each GC system ased to analyze 11111ples, and for each
extractio11 bat.ch.
Actio11 in the case of ansuitable blank results depeads oa the circums1111ces cd the
origi11 or the blank. No positive sample results should be reponed a11less the
c:o11ce11tratio11 or the co111pou11d ill the sample exceeds 5 times the amou111 i11 the
blmJc. I.II instances where more thall 011e blank is associated with a 1ive11 sample,
qualific:atio11 should be based vpoa ■ compariso11 with the 11SSOCiated blank havi11g the
highest coace11tntio11 or a C011tamiD&J1t. ne results must mu be conected by
svbtr&Cti111 die b1uJc value. Speciiac ■etiom are os follows:
I.
2.
If a Pesticide/PCB is row ill the blallk bvt mu foU11d ill the ample(s), ao
aclioa is takeD.
Aay Pesticide/PCB ~ ia die -pie ud also detected ID any associated
•hnk, must be QualiiJed wlia die ■ample c:oace11tntio11 is less tha11 5 times
1M WaAk coacentnlioL
ne reviewer should aote that the bhnk ualyses may aot illvolve the ■ame
-iahts, \IOlumes or dilutio11 racton as the usoci■ted amples. nese r■cten
must be taken illto eonsider■tion when applyin1 the 51 criteria, sach that a
compariso11 or the total amount or coat■miatioa is acnzally made. ·
-:.
Additionally, there may be instlJICa where link or ao co1111miutio11 was
present iD th-' UIOciat.ed blanks, bvt qualiricatioa of the ample was deemed
33 2/IS
I
I
I
I -.:
I
I
I
I
I
u
I
I
I
I
I
I
I
, I
I
I
necessary. CoDta.miDatioD iDtroduced through dilutioD Wlter is ODe example.
Although it is 1101 alw.ys possible to determiDe, i.nsC&Dces or this occurrin1 caD
be detected wheD co11t1miD•D•s are fouDd in the diluted umple result, but
absent iD the undiluted sample result. Si.Dee both resuhs arc 1101 routiDely
reponed, it may be impossible to verify this 10111cc or COD1aminatio11.
Ho-"cr, if the ff.-ie11Tr deteno.iiies that the coDtamlution ii Crom a source
other \ba.n the amplt, k/lAc uaauld q,w.if"y the data. 111 this ease, the 51 rule
does aot a;,plr; the am,:>Jt "ll\lC sllouk! be reported as a non-detect.
3. The follOWUIC are eum;iles of applyulg the blank quslificanoa 1uidelilies.
.. '
Cera.iA eirrmnsnn:a aiay wwnsi cleviatioDJ Crom tbese 1uidelliies.
:i.Co11•~•e,~J·-----c:..,1...,mple result is 1reater thall the CllQL, but is less tha.a the
required amount (51) from I.be bb.nk result.
o,, 2;
BlanJc R.esult
CJlQL
Sample Result
Qaalified Sample Result
a
1.0
.5
4.0
4.0U
IA this case, sample results less dwl S.0 (or S :& 1.0) -uld be
qualified as non-detects.
Sample result is pater thu the required amount (51) from the
blank raalt.
Bink Result
CJlQL
Sample Result
Qualified Sample Result
V. SURROGATE RECOVERY
.. a
1.0
.5
6.0
6.0
OIIJecdM
l.abaratDr7 ,iert'ormuce OIi iDdlriduaJ IUlples ii embliued by me&DS or IPWIII
activities. All rmples an apiud widt a nm,pte compound prior to umple
p,epanlioa.. 'Ille ..-aliatioa ol 1M nnlts or dMse IVffllllle spikes is DOI nee V ;ily
maipdon.anl TM anpe hse1f -Y produce erreccs due to auc1I facton u
iaterfuaas ud hip CODCeDtntioDS of tulyteS. Since die etteets or the rmple
matrix are frequently outside the CODtrOl of the laboratory ud may praeat relatively
llllique problems, the review ud nlidatioD or data based OD specusc rmple results is
frequently subjective ud dem•ads Ull)'tic:11 experiellce ud prof'essioul J1id1meat.
AccordiD1ly, di.ls NCtioD CODSistl primarily of &wdelilla, ID 101De .cues witli aeveBl
optioul approeches 111uested. ·
2/IS
I
I
I
I
I
I
I
I
I
I
1·
I
I
I
I
I
B.
c.
D.
A.
••
Crllerla
Sample and blank recoveries or dibutylchlorendate must be· within limiu as per
applicable SOW (Form II).
I.Y&ludoa ?,oced .. ,e
I. Chdt nw data (i.e~ ehromatognms, qant list, etc:.) to YCCuy the recoveries
OJI CM San-ogur llec:ovef) (Form U).
2. lf recover~ vi 11ot 'Withia limits, c:bec:k nw data for possible interferences
whicb may have arfec:ted surrogate rec:overies.
It pestic:ide sum:,gate recoveries an outside of advisory wizldows, the following
guidaDc:e ii aggened:
1.
3.
If low ncovaier are obrai!ied, f'laa usoc:iated positive results and quantitation
limits 11S estimated (J).
If high recx,veries an obtaiaed, professioul judgment should be used to
determine appropriate ac:tioa. A hip bias may be due to co-elutlag
.interferences.
If' iero pestic:ide nm,pte recovery is reported, the reviewer should examine
the ample c:hromatogram to determine if the surrogate may be present, but
al.ightly outside its reteatioa time window. It this is the case, in addition to
assessing surrogate recovery for quaatitative bias, the overriding c:onsidel"ltion
is to investigate the qualitative validity or the aaalysis. If the surrogate is aot
present, flaa aJ1 aeptive results u unusable (R).
VJ. MADJX SPm{MAJB(X SPIKE DUPLICATE
ObJeedYe
These dala u. a,uented to detumiae lolls-term prec:isioa ud accurac:y of the
analytical method n 'ftrious maaice. Tbere data llgJll cauot be ased to evaluate
the I>"• • • • and aceuracy or illdmdual ,1 ....
Crileda
J. Advisory limits are es11blished ror spike recovery limits iD the appropriate
SOW a.ad OD Form Ill.
2.
• I
Advisory lisaits are established ror relative percent difTereace between matrix
11>ike a.ad matrix spike duplicate .-veries ill the appropriate SOW ud oa
Form Ill. ·
3S 2/11
I
I
I
I
I
I
I
I
I
I
I
I
I
••
I
I
I
I
I
C.
D.
B.
C.
D.
I.,alyatioo ProcedMrt
I. lllspect results for the Matrix Spike/Matrix Spike Duplicate Recovery (Form
Ill).
2. Verify~ froa n,. data ud vmfy caiculatica.s.
No action is taken on Matrix Spike/Matrix Spike Duptic:ate (MS/MSI)) data Wt to
qu&lify an entire Case. Howeve,, miJ11 informed profession.al Jud&ment, the data
reviewer mw, me the inatriJ. q,ilce an4 Jll81ris. spike duplicate results in conjunction
with other QC criteria and detm11ine the n~,cation of the data.
The data reviewer should rm cry to determine to what extent the results oC the
MS/MSD affect the IS$0Ci••e4 data. 'Ibis determination should be made with re1ard
to the MS/MSD ample itself u wen u specific ualyteS for all amples associated
with the MS,'MSD.
In those imtaDces wberr it can be dem1n.iAed that the results of the MS/MSD affect
on_ty the ample spiud_ then qalif"ication should be limited to this ample alone.
However, i:t may be delU1!Wled throu&h the MS/MSD results that I Jab is bavin& 1
systematic problem in the ualysis of one or more analyteS, which affects all
associate4 samplea..
VII. DtJ,P DUPLIC:ATES
ObJectl..e
Field duplicate samples may be lalcen and analyzed u an illdication of ovenll
precision. nese analyses measure both field and Jab precision; therefore, the results
111&y have more variability thaD Jab daplicates which measure only Jab performance.
It is also expected that soil duplicate nsults will have I areatei ~ce than water
matrices due to ditrieuJtia usoc:iated with collectina identical raeld samples.
Criteria
nae .. -tpeCaJC aevi.:■ criseria ror raeld daplicate analyses CIOmplRbility.
Sample:a which are C-aeld duplicata should be identiraed mina EPA Simple Traffic
Repons or sample f"ield sheets. The reviewer should compare the results reponed for
each sample and calc:ulate the Relative Percent Differuce (IU'D).
Actloa
. -: (
. AzJy evaluatioa of the ("aeJd duplicates uould lie provided .-Ith the nviewer's
comments.
2/IS
A. B. C. D. \"III. co,,row,p ID[l\"TlfICATIO~ ObJretlH QuaL tatin crilffia {or compound identificatiaii lnve been esnblished to mi.D.imiz.e the nu■ber of efTOtleous idt.otific:atioas of compoands. An erroneous identification c:an eitlle-:~ be • fuse pou:i~e (~g a compoW>d presevt wllea it is not) or a false nep1ive (IIOf ~ma, a O>IIIJ)OQJl,d &hat .is presur). Crltarla 1. Retention times of reported compognds mmt fall within the calcu.ut1.1a.ure~d1-. __ retention time window, for the two chrllllWDs;npluc collllD!IS. ~ 2. GC/MS conrU1111tion is requ1nd if the CODcenu.tion of a compound exceeds 10 nlfuL in the fin.al ample extnct. E,ahadoa Pncedan ,J, 2. Jlrnew Fona I. the associated nw data (chromatoanm, ud data l)'ltem piotoau) ud t.be Pesticide/PCB Jde.atificatiaa Summary (Form X). CourlrlD rec,oned positive deu.:ts, asiD1 appropriate retention times ud retention time windows, ud verify that the compounds listed u "not detected" are correc:t. Verify that positive identifications have dissimilar collllll.D &D.aly,is. (The 3% OV-1 column ca.anot be used for courU111ation iC both dieldri.n ud DOE are identified.) 3. For multipeak pesticides (chlordane ud touphene) ud PCBs, the retention times ud relative peak height ntios of major component peaks should be compared against the appropriate 1tudud chromatograms. 4. Verify that GC/MS coarirmatiou wu performed for pesticides/PCB f"OIICJMIU"WODS ill the rma1 aample extract which exceeded 10 Dl/UL A.ctlo■ l. 2. JC the qualitative criteria for two column courumation -re not met, all nponed positive desectl abould be co111idered ■on-deleell. The reviewer lliould ue prof'essioml Jnct,men• to usip u appropriate Q11UtitatioD limit 1lliA& the followiJi& 1uidlnc:e: L 1f' die aisi4entaied peak -nfT'Jdendy oll1Side the taraet pesticide retadoa time window, daeJI the CRQL cu be reponed. b. JC the misidentified peak poses u iDterfaeuce with potential detection or a taraet peak, then the reported wlue should be co111idered ud flaged U die estimated QllUtitatioD limit (UJ). 0~ . .. ,. ... _ IC PCBs or muttipealt pesticides uhibit 11W1iul patten1-matchin1 quality, pn,reaion.al judgment 1ho11ld be ued to establish whether the differences are attributable to environmental -..therillg•. If' the w,resence or a 37 2/11
I
I
I
I
I
I
I
I
I
I
I
•·
I·
I
I
I
I
I
A.
B.
C.
PCB/multipulc pesticide is ltrongly 1uuested, resula should be reponed u
presumptively present (N).
If an observed patten, closely matches more \hall one Aroclor, professional
j...ii&ma:.t s~ld be med ex, decide-whethet tbe aei,hborio& Aroc:lor is a better
-tch., Ol ii .,.Jtiple ArocJoa &n pruuL . .
3. 1f GC/MS c:onf'irmaoon was reqaind but DOl performed, 1he reviewer should
notify the DPO.
IX. CQMPQUND QUAfillIAJJQN Ab'P BtPQBitP PtitCTJQN LJ~OJ'S
ObJecdN
Tbe objectne • to -aree that 1ht. 1epo1te4 QQIUltitation results and CRQLs are
accunte.
Criteria ,•
Compoud quantiution, u well u the adjustmCllt or the CRQL, must be cali:ulated
acairding to the appropriate SOW.
E,aJuadoa Procedun
1. Jlaw data 1ho11ld be examined to verif'y the c:onect 'cali:ulation of all sample
resula reponed by the labontory. Quantitation reports, chromatognms, and
sample prepantion lo& sheea should be compared to the reponed positive
sample results and q11&11titatio11 lilll.its.
Verify that the CRQLs llave been adjasted to reflect all sample dilutions,
cio11ce11tntiom, spliu, clean-up aetivities, ud dry weight faeton that are 11ot
.aiunted for by die •thod.
D. Acdo■
Quutitatioa limits a!fected by Jarae, off-teah peaks uould be flagged u unusable
(R). IC the illteri'ereace is on-scale, die rewiewer cu provide u estimated
quutitatioa Jim.it (UJ) for each al'fected composmd
tiasr; Gm~peal( pesticide ,wults cu lie cllecbd for ~ugh agreement between
Quutita ve results c-boieed OIi die a-GC CICllamm. The reviewer should use
professional judgment to decide wbether a mucll laraer conceatntion obtained 011 one
column 'Venus the other indicates the preeace or u illtenerillg ciomp0uad. If an
mterfuillg compound is illdicated, die lower oldie two values should be nported and
qualified u presumptively present at u eetinllted quutity (NJ). nis necessitates a
determination or u estimated co11Ce11tntioa n die collf"armatioa columll. The
narrative should iDdicate dial die presence ol lDterferuces llal obscured die attempt
at a NCODd COIU.lllll coDf"armatioa.
2/11
.-
I
I
I
I
I
I
I
I
I
I
I
I
I
••
I
I
I
I
I
X. QYJ:BALl ASS!'.5-$HE""7 Of PATA fOR A CASE
It is appro::,ria1e far tile data revie..,er CD make professioul judpeots and express
concerns and CIOIIIJMDt. OD ~~ nlidjry o{ die ovua.1.1 data package for a Cue. This is
particularly appro;iri:He lcr Oms s ... ~ ~ an •¥Cnl QC criteria out of IP"ificatioo.
The additi"e natun or QC (.etan 011t of ~ic:arloe .is difT.r.ult to assess iD an objective
manner, but &ht reviewer 1w • responsibility to Worm -asea CODCU!1ill& dau quality and
data limitatiom in order to mis1 WI mer iD avoidiA& .inappropriate iw or the data, while
not precludinr, any com:idera.tioa of the data . al all TIie data rniewer would be areatly
assisted in this endeavor if the data quafity o'ojectr,es were provided.
.-
. . 14:,,.
i~:
,, 2/11
I
I
I
I
I
I
I
I
I
I
I
.
••
;
••
I
I
I
I
II
I
'
! I
-·-
GLOS.SARY A
Data QuaJIOer DeOaltloas
For the purposes or tha diaimac the fo\lowt Cllldt lenen ad associated definitions are
provided.
U -TIie muerial was ua.1-,zed {or, but -Dot deiecud. TIie associated
numerical value is the sample q1W1tit1tio11 lim.it.
J -The associated n11!!1trical valne is III estimated q11-111tity.
Jl -TIie data are Wlusable (compoUDd maJ ar -Y not be prese11t). ResampU111
ud mmlysis is &'ecesnry rcn: ~-tioa.
N -Pn:sm:aptm evide11ce of presence or Jll&leria1..
NJ -Presumi,tive evide11ee or the pw or the material at III estimated
quantity. ·
,•
UJ -The material wu analyzed ror, bat was not detected. ne ample
quantit1tio11 limit is III estimated q11111tity.
The reviewer may determine dist qualifien other Wit those ased iD this docume11t are
necessary to descn"be or qualify the data. l11 these imtlllces, it is the responsibility or eac:h
Region to thoroughly dOCW11e11t/e:i:pw11 the qualifien med. '
_,,
2/11
I
I
I
I
I
I
I
I
I
I
I
I
• r I
I·
I
I
I '
I
i
1
I
BFB
BNA
Case
CLOSSAR\' B
Otber Term,
BromoOu.on>belW:lle -\OOlalile tasw11 ~
Ba:se/Ne11tral/Aeid Compouads -oc,mpom,ds a.ulyud by semivolatile technique
A finite, anally pl"ldttel'11lined number or amples collected over a 1iven time
period for a s,anic'l1ar aite. A c:ax CODSists or one or more Sample Delivery
Gron;,(s).
CCC Calibntion Qec:k Compaimd
cc:s Colltm:t Coml)f1111ce Sc:reaiill& -proceG iD which SMO inapeea ualytical data
for contnctml compliance and provides res'llla to the Regions, labontories and
EMSL/LV.
CF
CRQL•·
DFTPP
Calibntion Factor
C.ontract R.eqv.ind Qautiiation Limit
Decall11orotripbenylphospbine -Rmivolatile tllllin1 compound
DPO Deputy Project OCficer
ElCP .Extrxted Jon Current Prorile
GC/EC Gu Chromato1nphy/Electron Capture Deteetor
GC/MS Gu Chromatoanph/MISI Spectrometer
GPC Gel Permeation Chromato1raphy -A ample dean-up technique that separates
compo1111ds by size and molec1ilar wei1ht. Generally ased to remove oily
materials from ample utracU.
IS latenial Smduds -Ovnpounds added to every VOA and BNA. 111.Ddard., blank,
aairiz spike dapJic:aa. Dd ample extract at a known concentration, prior to
Jaso ..-.ill! am.tysa. 1 • iill '1IDdards are used u the basis for qwuitiiation
or die taraet compoaads
MS/MSD Matrix Spike,'Matria Spike Duplicate
m/z The ntio or mm (m) to cJw-ae (:r.) or ions measured by GC/MS
OADS
J'CB
Oraanic Alla.lysis Daza Sheet (Form I)
l'olychlorimte4 biplieayl
I
2/11
I
I
I
I
I
I
I
I
I
I
I
••
I
I
I
I
I
Primary
Analysi.s
QA
QC
RJC
JlPD
RllF -RRF
RR.T
RSI>
RT
SDG
SMO
SOP
sow
SPCC
sv
TC.
TIC
VOA
. -•
011e or two types or pesticide/PCB Lll.llysi.s by c;cfEC tecll11iques, the other
1,eioa ~llfirmation analysi.s. lf the two analyses are '11D a1 aepu11e limes, the
primary analysis is the rint lllalyii.s cb.ro110logically, and is used to ~tabli.sh the
Uatative ide11tifiati011 or &D)' ,aticide:,,/1'CBs deteeted. Tbe ide11tifica1i011 i.s
the11 confirmed ill che C0Gfinzmio11 sfr;siL If lht rwo ualyses are d011e
liaiuliueoasly, eitller may be c:mridet~ u, primary ID&lym. Either may be
med for quuwatio11 if contl'K\ ~iteria are met.
Quiliry A.lslUUce -Total prognm for assuriD1 die ftli&bility of data.
Quality Control -Ro11tine applicatlo11 of procedures fOT co11trolli11g the
mo11itoria1 process.
hconstn1cted 1011 Chromatoan.m -
ltelatM l'en:eDt Diffue11ce (betwee11 mauix spike ud matrix spike duplicate)
Relative RespoDSe Factor
Avenge Relative RespoDSe Factor
Relative Rete11tlon T1111e (with relatl011 to illterul ltlDdard)
Relative Sta.11dard Deviation
Retentloa Time
Sample Delivery Group -Defined by one of the following, whichever occun
fine
o Cue of field amples
o Eaeh 20 field 11mples :within a Cue
o Eada 14-day c:alendar period duri111 which field samples ill a Cue are
received, be&inniD& with receipt of the fint ample ill the SDO. (For VOA
COlltncU, the c:aJeadar period is 7-day.)
Sample Muaaemeat Office
SlaDdard Operatina Procedure
Statement of Work
System Perf'onDDCe Cbeclt Compound
Semiwlatile llllfJ'sil -~ IIUed u ualysis by OC/MS ror BNA orpnic
co""'°""tb.. I
Taraet Compoad List
. ·-. -.
Tentatively ldeDtif-.ed Compou11d -A compouDd 110t OD die TO..
Volatile 0rpnic Aaalysis -Method bued OD the parse ud cnp tecbDiq111 ror
orpnic: compouud ualysis.
2/1&
~ VTSR I a r • •' . . .. --:~_-_ ----.. . -Validated Time of Sample Receipt -T'1111e of sample receipt at the laboratory u recorded oil the shipper'• delivery receipt 111d Sample Tnl'fic R.epon. StlDdvd Deviwoll Ett1m11e (of a ~le) -
I
I
I
I
I
I
I
I
'-
I
I'-,
I
I
I
I
I
I
I
I '
LA~URATURY DATA VALIDATION
t"UNCTlUNAL GUIDELINES FOR t:VALUATlUN INURGANICS ANALYSt:S
Uniteo States ~nvironmental Protection Aweney
ottiee ot ~mer~eney ano Remedial Response
..
'
I
I
I
.--
I
I
I
I
I
I , ,-
I
I
I
I
I
I
I
I \
Table of Contents
section
Title Page
Page
i
Table of Contents
ii
Introduction
l
Responsibilities of ~ey Individuals/Offices
Communication System
2
9
Preliminary Review 11
Procedure
13
I. sample Holding Times 13
II. Calibration
16
A. Initial Calibration• Calibration
Verification
16
B. Continuing Calibration Verification 19
III. Blanks
22
IV. ICP Interference Check Sample Analysis 25
v. Laboratory Control Sample Results 30
VI. Specific Sample Results 33
A. Duplicate Sample Analysis 33
~. Spiked sample Analysis 37
C. t·urnace AA QC Analysis 40
D. ICP QC Analysis 45
E. Sample Result Verification 46
VII. Field and Other 0C 51
VIII. Quarterly Verification of InstrUlllent Parameters 53
Report
IX. Overall Assessment of Data for a Case 54
Appendix l Contract Required Deliverables SS
Appendix ll Contract Required Detection Limits 64
Apenndix Ill Spiking Levell for Spiked sample Analysis 66
Appendix JV Furnace Atomic Absorption Analysis Scheme 67
Appendix V CLP Telephone Record Log/DPO C0111111unication 68
Appendix Vl
SullllDary
Regional DPU List/Report Distribution 70
Addresses
Glossary
72
ii
'
I
I
I
I
I
I
I
I
I
I
I'
I
I
I
I
I
I
I
I \
~ORATORY DATA VALIDATION
FUNCTIONAL GUIDELINES FOR EVALUATINU INORGANICS ANALY~ES
Introduction
This document is designed to offer guiaance in labor•tory
data evaluation and validation. In some aspects, it 1• equivalent
to a Standard Operatin~ Procedure (SOPI 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 ~ossible are primarily
areas in which definitive performance reQuirements are established.
These requirements are concerned with specifications that are not
sam~le devendent; they sr,,ecify performance requirements on matters
that should be fully under a laboratory'• control. These specific
areas include laboratory preparation blanks, calibration atandaras,
calibration verification standards, laboratory control standards
ana interference check atanaards, Failure to ■eet the contract
,.
performance requirements warrants that corrective action be taken
by the laboratory,
At times, there may b4t an urgent need to use data which do not
~eet all contract requirements, Any decision to utilize data for
vhich non-sample specific criteria have not been ■et is strictly
to facilitate the progress of projects requiring the availability
of the aata and such decisions should be clearly noted on the
summary review for111, Use of this data does n2! constitute
acceptance (contractually) of the data nor does ~t release the
I
I
II
'-I
I
I
I
I
I
I
I '-
I
I
I
I
I
I
I
I \
contractor from the obligation to perform aa per the terma of
the contract. A contract laboratory aubrllitting data which ia out
of apecification may be required to -re-run or reaubmit data. The
only exception to this is in the area of requirementa for indivi-
dual aample analysis, if the nature of the aample itaelf limits
the attainment of apecifications, appropriate allowance ■ must be
made. An overriding concern of the Agency ia to prevent non-aample
apecific data validation requirement ■ from adveraely affecting
overall data valiaation activities. There ia ultimately no
Justification for noncompliance on requirements for performance
relative to such areas as blanks, calibration and performance
verification standards; data validation activities 1houla only be
concerned with subJects requiring professional JUO~ment on
indiviaual sam~le results.
With these concept& in mind, this Guideline is designed to
permit atructurea data review, and to include aut0111atea data
I
checkout procedures when auch capabilities are available.
ObJective, unambiguoua requirements are easily and efficiently
rele~ated to peraonnel other than experienced profeasionals and
to automated procedures for verification of compliance with
requirement•. To thia end, the guideline is arranged in order,
with the most objective, atrai~httorward validation elements
given firat.
Responsibilities of Key Individuala/Office1
The data reviewer ia a critical link in the chain of people
and event• involved in the collection, analysis, and interpreta-
I
I
~
I
I
I
I
I
I
I
I
I
I
I
I ,
tion of Superfund environmental ■easurement. The aucceaa, useful-
neas, and validity of the data review depends on the techn_ical
expertise ot the data reviewer and communication with otnu key
individuals. Although each Region ia aet up aomewhat differently
from an organizational point of view, the following individuals/
offices should be known to the reviewer,
(11 National Pro~ram Office (NPO)
(21 National Program Manager (NPM)
(31 CLP CA Officer (CAO)
(41 ProJect Otficer (PO)
(51 Sample Management Office (SMO)
(6) Deputy Project Officer (DPO)
(71 Regional ~ample Control Center (RSCC)
(ij) on-Scene Coordinator (OSCI
Each of the above is responsible for a particular set of
tunctions related to sampling, analysis and/or management of
the CLP. The data reviewer ahould be aware of the responsibilities
of each in order to ensure effective communication. The following
hi~nlights the responsibilities and authorities of each of the
above and includes the type;of information likely to be communicated
to and from the data reviewer.
(1) National Program Office (NPO)
The CLP i• directed by the National Pro~ram Office (NPO), in
EPA Headquarter'• Analytical Support Branch (ASB), Hazardous
Response Support Diviaion (HUD), Office of Emergency and Remedial
Response (OERRl, in Washington, D.C. The NPO is comprised of the
National PrOiJram Mana~er, organic and Inorganic Technical Officers,
and a oualitf Assurance Officer, who also provide• OA aupport to
the OERR.
•
I
I
I
r
I
I
I
I
I
I
t
I
I
I
I
I
I
I
I\.
NPO responsibilities include: overall aanagement of the
CLP in terms of vro,_ram obJectives, expansion ana interface
with clients and other groups; policy and bud~et fonaation-and
implementation; administration of analytical and aupport
contracts; development and technical review of analytical
protocols; review of analytical special aervice1 subcontract• and
CLP generated laboratory data; development of CLP analytical
and support services contracts, monitoriog and formal evaluation
of analytical and 1upport contractors; and in direction of CLP
quality assurance (OA) in coordination with overall OERR OA
activities.
(2) The National Program ManaQer (NPM), in addition to
directing proc,,ram staff, is responsible tor the for111ulation of
program policies and direction, communicates with the Rec,iional
and A,_enc~ communities on a continuing basis, keeping all
parties apprised of program,.activities and receiving input on
program effectiveness, administers several program support
contracts, and handles financial and contractual aspects of the
pro11ram.
The National Program Manager i1 responsible for the
overall success of CLP operations, identifying Superfund
analytical requirements, and establishing Program obJectives to
meet the analytical requirements. POs end DPO• assist the
Program Manager in achieving Program objectives and aanaging
the CLP on a day-to-aay basis, Program issues which cannot be
resolved by the POa, or which arise between the POa and DPOs
will be referred to the NPM for resolution. ,
I
I
l
I
I
I
-s -
(31 Ttl• Quality Aaaurance COAi Offi~T coordinate ■ all aapecta
of pro<;iram application of 0A procedurea. _ The (IA Officer works
cloaely with EPA Headquarter'• Office of Reaearch and Development
..
(ORO) and the ORD'• Environmental Monitoring Syatema Laboratory
in Las Vegas (EMSL/LV) which provides 0A aupport to the CLP.
The 0A Officer also coordinates with the POs and EMSL/LV in
refininw and updating analytical ■ethod 0A procedures.
I (4) The Organics and Inorganics Technical Officer ■ aerve as
Project Officers (POsl on laboratory analttical contracts. The
I
I
I
I
I
I
I
I
I
I \
POs are responsible for technical program deci1ion11, contract
aoministration, and contractor performance evaluation. The POs
work closely with the Regional Deputy Project Officers (DPOs)
ano laboratories on a daily basis in resolvin<;i technical
issues. The POs direct the ongoing effort to improve contract
languawe and analytical methodologies, and conduct technical
caucuses for purposes of CLP data and protocol review.
The Pos have primary reaponsibility for all administrative
,.
aspects of contract formation and procurement, and will
adJniniater all CLP contract ■ on a Program level.
The PO ia reaponaible for the following activitieaa
l) Defining the Government'• requirement• and initiating
the procurement proce11 by developing appropriate
procurement packages.
2) Technical and programmatic evaluation of laboratories
for possible contract award.
?) Award of contract.
4) Implementation of contract modification ■ and change
order ■• s> Resolution of Program level iasuea between Re;ions.
6) Resolution of iaaues between DPoa and contract labora-
tories.
I
I
I
I
7)
8)
9)
1~
-

6

-
Certification of invoice voucher ■ for es, prC>Qreaa payment.
Evaluation of collective laboratort performance.
Recommending to the Contracting Officer that aanctions be
imposed for laboratory non-compliance or non-performance.
Other tasks normally performed by ProJect Officvs.
(S) 6&111ple Mana~ement Office (SMO)
I The contractor-operated Sample Management Office functions
I in direct support of the NPO, providing management, operations,
and administrative support to the CLP. The primary objective
I
I
I
I
I
I
I
I
I
of the SMO operation is to facilitate optimal use of program
analytical resources. SMO activities fall into the following
areas: (l) sample scheduling and tracking1 (21 Special analy-
tical Services (SAS) subcontracting, (3) laboratory invoice pro-
cessin~: (41 maintenance of CLP records and management reportinw:
and (5) NPO management and administrative support.
SMO routinely receives analytical reQuests fr0111 the Regions,
coordinates and schedules sample analyses, tracks sample shipment
and analyses, receives and checks data for completeness, and
maintains a repository ot sampling records and prOc,Jram data. In
response to client reQuests for non-routine types of analyses,
SMO subcontracts for SAS, performin~ scheduling and tracking for
tiAS eftorts as outlined above. SMU maintains a comprehensive
data base of CLP services, performance and utilization, and
generates a variety of management and usar reports,
(6) Contract Deputy Project Ofticers
In January 1984, Regional Administrator• appointed a CLP
technical Deputy ProJect Ofticer (DPO) for each Regional office.
,
I
I
I
f
I
I
I
I
I
I
r
I
I
I
I
I
I
-

7

-
Under direction ~f the NPO, the Regional DPO assUJDes a portion of
the responsibility for ■_onitoring the laboratory contractor ■
physically located in the Region.
DPOs will have overall responsibility for ■onitoring the
aay-to-aay technical performance of assigned laboratories, for
improving that performance where necessary, and for re ■olving
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 yeneral, DPO
responsibilities are ■pecific to contracts, protocol ■, and
laboratories and.are related to ensurinl,l the ■uccessful performance
of the laboratories under his/her jurisdiction. More specifically,
DPOs have responsibility for:
1)
iJ
Participation in audits of laboratories within his/her
Region.
Recommending contract changes. Rec0111111endations ot technical
contract modifications~·
Monitoring contractual terms and condition ■•
Resolution of issues between CLP c!ients and the laboratories
within hi ■/her Rel,lion.
Evaluation of individual laboratory perfo~ance within
his/her Rel,lion.
Recommending to POs that ■anctions be impo ■ed on laboratories
tor non-c0111pliance or non-performance.
POs' ana DPO■' role ■ will overlap in area ■ requiriny inter-
pretation of contract language or re■olution of conflicting
contractual re~uirements, and in the impo■ition of laboratory
■anctions ■uch a ■ rec0111111endation ■ of non-payment for
I non-performance. There will be a cooperative eftort between the
POs and DPOs when the settling of individual i■sues will
I reflect cnanges that will benefit the entire CLP.
I
I
I ,--
1
I
I
I
I
I
I'
I
I
ii
I
I
I
I
I
I
-8 -
It will be the data reviewer•• prero~•tive and reaponaibility
to notify the Regional Deputy Project Officer (DPO) concerning
problems and ahortcomings vi th regard to laboratory data. -If
■anaatory actions are reQuirea, they should be specifically
noted on the DPO Action Report, Thia form ahould also be used to
note overall deficiencies reQuiring attention a ■ well a ■ comnients
on general lab performance and any aiscernible trends in the
Quality of data, It is rec0111111ended that the DPO be notified of
all problems and reQuirements for a case at one time, If there
is an urgent reQuirement, the DPO may be contacted by phone to
expedite corrective action. Yowever, it is appropriate to submit
a Data Review Summary in any event to provide documentation of
the Data Review,
(71 Regional Sam~le Control Centers (RSCC)
In January 19H4, each Region established a Regional
•'
&ample Control center to centralize ordering of CLP sample
analyse ■ within the Region, The RSCC is comprised of three or
more indiviauals deaignated as CLP Authorized ReQue ■tor ■, with
one individual named a• the Primary Authorized ReQuestor (AR)
directin~ the IUiCC, The JlSCC is responsible for coordinating
the level of Regional sampling activities to correspond with
monthly allocations of CLP analyses, The Primary AR makes final
determination ■ re~arding Regional analysis priorities when
con~lict ■ occur. RS~C AJta routinely place all Re~ional
reQuesta for CLP analyses, coordinate with SMO during sam~lin~
I
I
I
t
I
I
I
I
I
I
I
I
I
I
I
I
I
I
1,
and aample ahipment, and reaolve any problems which ariae
concerning the aamples •. The RSCC aerves as the central point
of contact for Questions concerning Regional aampling efforts.
(81 un-scene Coordinator
This individual may have various titles (e.g., On-Site Team
Leader) but, whatever the title, the person is primarily
responsible for the sampling effort. This person is a good
aource of information related to the sample collection ( i.e.,
ioentity of blanks, duplicates, etc.).
Communication System
several communication networks and .links have been
established to assist in the transfer of information to the
appropriate individual. Data reviewers should be aware of
these links and utilize the procedures as is appropriate to the
issue at hand.
' .
(ll Regional/Laboratory Communciation System
In Janua~y 1983, the NPO established a •tstem of oirect
communication between the R•~ions and contract laboratories as
a routine ■ethoa for Regional data review staff to obtain
answers to technical Questions concerning program data in the
timeliest end most direct manner possible. In this system,
desi~nated Rewional communication contacts call designated
laboratory c0111111unication contacts as needed to resolve technical
data question~. This communication link also benefits the
laboratory by providing direct feedback on its data product.
I
I
~
I
I
I
I
I
I
I
I
I
I
I
I
I
I
-10 -
Issues warrantin~ further investigation by the reviewer correipond
to areas where the contract requirement• were not ■et, une_xpla ined
discrepancies between report forms and raw d1t1 exist or ~ere
analytical problems and/or concerns were discovered in I case.
Reviewers are reminded of the ground rules for this system:
o Regional contact of laboratories is permissible only after
laboratory data submission.
o Re~ions 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 recommendations, and other
general matters continue to be referred to SMU or Pr0<,1ram
management (i.e., DPO), as •~propriate.
o unly authorized Re~ional personnel ■ay contact laboratories,
and they may contact only the specified laboratory
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 Record Log is forwarded by the
Re~ion and the laboratort to SMO on a weekly basis, and
becomes part of tne Case File 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 copt to the
Region.
(2) DPO Communication syst~m
Similar to the above, DPO c0111111unications with POs, labs,
SMU, and data reviewers are docUJDented 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
review will be torwarded to reviewers•• appropriate (i.e.,
Quarterly verification of InstrUJDent Par1111eters Report). The
DPus will also provide updates to protocols a• they are received.
lnter-Rewional questions or problems with laboratory
performances are referred to DPOs for resolution. For instance,
I
I
I
'--
I
I
I
I
I
I
I
I'
I
I
I
I
I
I
I
-11 -
it Region V data reviewer• uncovered a possible contamination
problem in a laboratory assigned to Re~ion II, the problem 1•
first referred to the Region V DPO w.ho then contacts the DPO in
Region II,
(3) Report distribution (See APP!ndix VI for addresses)
A copy of each data review should be sent to1
Duane Geuder, QAO
koss Robeson, EMSL-LV
DPO for the laboratory
Preliminary Review
In order to use this document effectively, the reviewer should
have a general overview of the case at hand, The exact number
of samples, their assigned traffic report and laboratory numbers,
their matrix, and concentration level, the identity of an, tield
QC samples (blanks, duplicates, apikea, •~lita, perfor111ance
,'
auoit samples), sampling dates and the number of lab• involved
for their analysis are ••••ntial information, Backgrouno informa-
tion on the site ia helpful but oftentimes it 1• very difficult
to locate. The site project officer is the beat source for
answers or further direction. The aafflpl• tracking record which
ia initiated in the field providea1
al ProJect Officer for site
bl Complete list of sample• with notation• on1
I
I
I
1'--
1
I
I
I
I
I
I·
I
I
I
I
I
I
-12 -
1 I aample matrix
21 field blanks
3) field duplicates
41 field spikes
SI OC audit
6 I anippinr;i dates
71 labs involved
The chain-of-custody record provides sample descriptions
and the ciate of sampling, Althou1,1h the sampling date is not
addressed by contract requirements, the reviewer 1hould be
aware of any lar;i time between samplinr;i ana shippinr;i, The case
narrative which is submitted bJ "'~ laboratort 111 another
source of general information, Notable ~roblems with matrices,
insufticient sample for analysis or reanalysis, and unusual events
should be found here.
The requirements to be checked in validation, in order, are as
follows:
l,
11,
111,
IV,
v.
VI,
sample Holdinr;i Times
Calibration
a. Initial Calibration and Calibration Verification
b, Continuing Calibration Verification
c. Calibration Blank
l:llanks
a. Laboratory preparation blank
b. 1''ield blank
Interference Cheek Sample Analysis
Laboratory Control Sample Analysis
S"9cific Sample Results
a. Duplicate ~ample Analysiu
b, bpikeo ~ample Analysis
C. Gt'AA 0C Analysis
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
.....
VII.
VIII.
IX.
-13 -
l. Duplicate Injection•
2. Analytical Spikea
d. ICP 0C Analysis
e. Sample Result Verification
Field and Other 0C
Quarterly Subllliasions
Overall case (Batch) Assessment
Procedure
I. ~ample Holding Times
A. ObJective
The obJective is to ascertain the validity of results
based on the holding time of the ■ample frcm time of
collection to time ot analysis or ■ample preparation, as
a~propriate. From the atandpoint of contractor
( performance, the time trom Veritied Time of Sample
Receipt (VTSR) until analysis or ■ample preparation is
needed to determine compliance with contract requirements.
~. Requirement ■
The followinw holding time requirement• were established
under 40 CtR 136 (Clean Water Act) and are found in
Volume 49, Number 20~ of the Federal Rewi ■ter, page 28,
issued on october 26, 1984.
NETAUil 6 month ■
NERCURYl 28 days
CYANIDE& 14 day ■
I
I
•c
I
I
I
I
I
I
I
I \.
I
I
I
I
I
I
I
I \_
-14 -
The 40 CrR 136 requirements are rec0111111ended for use in
determining dat~ usability, With the exception of ■ercury, -
the contract follows these 40 CFR 136 requirements, The
contractual holding ti■e for ■ercury i• 30 daya, Technical
re~uirements for •ample holding times have only been
established tor water matrices, however, they are also
suggested for use as guidelines in evaluating aeoiment 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
Verified Time of Sample Receipt (VTSR) with dates of
analysis,
Exceeding the holdi~g time for a sample generally
affects• loss ot the analyte(s), This occur• through
any number of ■echanisms auch as deposition on the
sample container walls or precipitation. Therefore,
from a usability atandpoint, when holding tiae violations
occur, the reaults which are aost severely callea into
question are those which fall below or cloae to the detection
li■it, Relatively apeaking, analytical result• which fall
aignificantly above the detection li■it could be ■inimally
affected by a holding ti,e violation, Determinati,-,n of
the effects of holdin~ time violations on the usability
,
I
I
I .~
I
I
I D.
I
I
I
I ~
I
I
I
I
I
I
I
I ~
of analytical results is extremely aubJective. The
degree and nature of the eftact 1• dependent on aultiple
factors, such as the nature ~f the analyte and aauix,
the degree of the violation (days), and the concentration
of the analyte in the sample. Ultimately, the decision
whether to acce~t the data is best left to the data
reviewer's/user's professional Judgment.
Action
If 40 CYR 136 holding times are exceeded, flag all positive
results (J) and mini■um detection limits (UJ) as estimated
and annotate data to the effect that holding times were
·exceeded. In the review narrative, state that the
possibility of false negatives may exist and indicate that
the aetection limit for that sample ■ay be elevated over
what is reporteo. Reanalysis of samples which occurs
after holdinw times are exceeded must also be evaluated
,
for the ramifications of sample age in the interpretation
of the re-analysis results.
In that analytical holding times for soil• or sediments
have not been statistically determined, do not reJect
data that have exceeded the contract holdin~ ti■••• If
contract holdinw times are exceeded, aU111111ari1e the defi-
ciency on the DPO Action Report and forward to the appro-
priate DPU tor that laboratory upon completion of the
review.
'
I
I
I t
I
I
I
I
I
I
I
'-.
I
I
I
I
I
I
I
I (
-16 -
II. Calibration
A. Initial Calibration and Calibration Verification
l. ObJective
The obJective in establishing com~liance re~uirements
for satistactory instrument calibration is to insure
that the instrument is capable of producinw acceptable
~uantitative data. Initial calibration demonstrates
that the instrument ia capable ot acceptable .,ertormance
at the be.,_inninw ot the sam~le analysis runs.
2. Re~uirements
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.
o Calibration veritication shall be made by the
analysis ot ~PA Quality Control ~o!utions.
wnere an EPA uc ~ample is not available tne
accuracy ot the calibration shall be conducted
on an indeV41ndent standara at a concentration
otner tnan that used tor calibration, but
within the calibration range.
•> lCP Analysis
o Calibration blank and at least one
standard must be usea in eatablisninij
tne analytical curve.
o calibration veritication results must tall
within tne control limits ot 90-1101 of
the true value.
bl Atomic Absorption Analysis
o Calibration blank and at least three
standaras must be used in establishinw
the analytical curve.
o Calibration veritication r~sults must
tall within the control limits ot ~O-llUI
,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
-17 -
for all AA analytes with the exception
of tin and mercury for which the l~mits
of 80-1201 apply.
cl Cyanide Analysii
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 90-110\
of the true value.
3. Evaluation Procedure
al Verity that the instrument was calibrated
at the proper frequency using the correct
number of standards and a calibration blank.
b) Verity that the calibration verification
source used met contract requirements.
C) Review Form II for failure to ■eet acceptance
criteria. Spot check calibration verification
checks for each case/batch by recalculation of
the percent recovery from the raw data, verify
that the recalculated value agrees with the
laboratory reported values. To allow possible
rounding discrepancies allow results to fall
with 11 of the contract windows (i.e., BY-1111).
4. Action
The inability of a laboratory to perform acceptably
on the calibration criteria indicates severe problems
exist in the analytical system which ■ult be resolved.
An) data generated under such conditions should be
considered suspect. If contractual windows are
'
I
I
I
1 "--
1
I
I
I
I
I
I '-
I
I
I
I
I
I
I
I \
-18 -
exceeded or if improper calibration procedures were used,
all data a1111ociated with that calibration ■hould be re-
analyzed, su111111arize any deficiencies on the DPO Action
Report, If the data in question are needed on a priority
basis, professional judgment may be applied to determine
to what extent the data may be utilized, Guideline11 to
aia in the application of profe ■aional judgment to this
topic are as follows.
o If the initial calibration verification falls outside
the contract windows but within th• ranges of 50-891
or 111-1501 the flag the positive bit data a■ estimated
(J) •. In the review narrative, give an indication to
the data user as to the percent bias of the re1ults
(i.e., if the initial calibration verification for an
analyte is 1501, then it could be stated that the
reported results for that analyte could be biased
I
approximately 501 high).
• If an analtte is not detected in a sample and the
initial calibration verification result is greater than
1101 then the usability of that analytical sample
determination is acceptable,
9 If analyte i ■ not detected in a sample and the initial
calibration verification result is less than 901,
then the detection limit may be biased low. If the
I
I
I .~
I
I
I
I
I
I
I
'-
I
I
I
I
I
I
I
I {
'
-111 -
IDL ana CRDL fall cloae to each Other the poa1ibility
exists that the CRDL was not ■et. In the review
narrative, report that the·aeteetion limit tor that
■am~le may be elevated ana wive an estimate of the
bias. flag the data tor these samples as estimated
( UJ) •
If initial calibration verification results fall less
than ~o, or greater than 1S01 this is indicative of
severe analytical aetieieneies ana the data should be
reJeeted as unusable (R).
~. Continuinw Calibration Veritieation
1. UDJeetive
Continuin11 calibration verification aoe\llllenta satisfactory
instrument pertonnanee (calibration accuracy) over
speeitic time periOds.
i. Keyuirements
I
t·or each of the catewories listea below, the tollowin..i
criteria appl)I
• Continuinw calibration checks and calibration
blank analysis must be pertormed at a ainimlJIII
freyuency of 101 or every 2 hours aurin..i an
analysis run, whichever is more tre~uent, ana
atter the last analytical sample.
o Continuinw calibration cheeks must be performed
with one of the tollowinw aolutiona1 EPA O<.:, NS~
tiAA 16•Ja, or a contractor prepared •1n0ependent
atandard• (i.e., from a ditterent aource than that
I
I
I
I\._
I
I
I
I
I
I
I\_
I
I
I
I
I
I
I
I (
-20 -
used for the initial calibration standards).
o Continuinw calibration verification ■u ■t occur at
or near the ■id•range level of the calibration
curve.
o The calibration blank result ■ust be leas than the
CROL.
a) ICP analyses
o continuin~ calibration results must fall within the
control limits ot ~0-1101 of the true value.
b) Atomic Absor~tion analyses
o Continuin~ calibration results must tall within the
control limits of 90-1101 for all M analytea with
the exce~tion ot tin and ■ercury for which the limits
ot so-1~0, apply.
c) Cyanide analysis
o Continuin~ calibration results must tall within the
• control limits of 90-1101 ot the true value.
3. ~valuation Procedure
a) Review the aupportin~ raw aata to verify that
continuinw calibration verification and calibration
blank analysis were performed at the proper
tre~uency.
bl ~erity that the atanaard used tor pertorminw
the continuinw calibration ■et contract
criteria.
cl Review ~orm II for any results outside control
limits.
I
I
I
I
I
I
I
I
I
I
I,
I
I
I
I
I
I
I
I ._
-21 -
d) Verity •~proximately 101 of the re1,10rtea
values by recalculation trcm the raw data;
4. Action
follow ~uiaelines as presented under Initial Calibra-
tion ana Initial Calibration Veritication.
I
I
I
1'-
1
I
I
I
I
I
I
I
I
I
I
I
I
I '
-22 -
I I I. tllanka
A. UbJ•ctive
The assessment ot resul ta .on blank analyaea 1• rt>r the
purpose of detennininw the exiatence and ■agnitude of
contamination problems. The criteria for evaluation
ot Blanks applies to all blanks, including reawent
blanks, method blanks, field blanks, etc. The
responsibility tor action in t_he case ot unsuitable
blank results depenos on the circumstances ano the
ori~in of the blank. If problems with any blank
exist, all data associated with the caae must be
caretully evaluated to determine whether or not there
1• an inherent variability in the oat• tor th• Caae,
or the problem is an isolated occurrence not affectin~
other aata.
ti. Re~uirements
I
1. The laboratory preparation blank (r••~ent blank)
i• the only in-houae blank th• laboratory is
responsible tor reportinw ands
al At least one preparation blank must be
prepared ano analyzed for every 20 samples
received, or for each batch ot samples
oiwesteo, whichever is ■ore trequent.
bl It the concentration ot the blank is less than
the CRUL (see Appendix Ill, no corrective action
is re~uired to be taken by the laboratory.
cl It the concentration ot the blank is above the
contract r•~uired detection levels for any
wrol·~, of sample• associated with a particular
blank, the concentration of the sam.-le with tile
I
I
I
'--1
I
I
I
I
I
I
I'
I
I
I
I
I
I
I
I ~
-23 -
least concentrated analyte au ■

t

be lUX the
blank concentration, or all ■amplea a11ociate0
witn the blank •no leas than lU time ■ tne blank
concentration aust be redige1ted and reanalyzed
with the excevtion ot an identified aqueous '
■oil field blank, .~he ■amvle value i ■ m:,t
to be corrected tor the blank value.
dl Result ■ must be reverted to the in■truaent
detection limit,
2, No contractual criteria apply to the levels ot
contaminant in tield blank ■,
c. ~valuation Procedures
1, Review tne results reported on the Preparation
~lank ~UIMlary (t'orm 111) as well as the Pre~aration
blank(&) raw data (ICP ~rintout ■, ■trip charts,
printer tapes, bench sneets, etc,) and verity tnat
results were accurately reported,
i. It any blank contaminant ■ were identitied at levels
greater than the CRUL, determine it rediyestion/
reanalysis was necessary by comvarinw blank levels
with the reported sample results,
D, Action
If contaminant analytes are detected in samples
at a concentration of less than~ times the concentration
touna in the hiwhest associated blank (pre~aration,
field), th••• results ahould be consioereo su ■pect.
coae the reycrted results as estimated (Jl. In this
instance, a atatement should be included in tne nar-
'
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
g
-24 -
rative that indicates that it ia not possible to
verify whether the level of analyte aetected in the
aam~le was due to contamination,
To minimize error in interpretinw blank levels in the
range of the IDL, which ia aubJect to noise tluctuations,
tne 5 times criteria is •~plied only wnen the level of
the contaminant in tne blank is greater than i times
the IOL or wreater than the CRDL tor the analyte,
whichever value is lower.
If contract criteria were not met, summarize the aeticiency
on tne DPU Action Re.x>rt for that case and submit to
tne appropriate DPo upon completion of the review.
It con~aminants were identitiea in the field blank
which were aosent trom the laboratory preparation blank,
this could be indicative of a potential field OC problem,
a aeficiency in the bottle preparation procedure or that
the laboratory newlected to prepare the laboratory
blank in a ■anner aimilar to the field blank,
,
I
I
I ,~
I
I
I
I
I
I
·~
I
I
I
I
I
I
I
I
-25 -
IV. lCP Interterenee Cheek ~amvle Analysis
A. UbJeCtive
The ICP Interference Cheek ~am~le Analysis is pertormeo
to verity the contract laboratories interelement ano
baekwround correction taetors.
b. Requirements
l. ICP Cheek sample must be run at the bewinning
and eno of each sam~le analysis run (or a minimum ot
twice per 8 hour workin~ shitt, whichever is
more trequent).
~. If available, the cheek sample must be obtained
from EPA. Utherwise, it must be ~repareo at the
contract s~eeitieo levels.
3. Results for the cheek samvle analysis must fall
within the control limits ot ! ,u, of the establisheo
mean value.
•• The cheek •11111~le results as veil as the mean values
ano stanaara deviations must be reeoraea on ~orm Iv.
~. corrective measures are speeitiea in the contract
when cheek sample results fall outside the control
limits (i.e., termination of analysis, recalibration,
reanalysis).
c. ~valuation Procedure
1. Review rorm IV ana verity that results ■eet the
contract criteria.
.I
I
I
I
I
I
I
I
I
I
I
I
I
I
•
I
I
I
I
-26 -
spot check raw aata (lC~ printout) to verity the
accuracy ot the recoveriea reportea on ror'ID 1v. -
~. s.,ot check aample raw aata for negative results.
4. If results do not aeet the apecifiea criteria,
verity that all atfected samples were reanalyzed,
D. Action
lt the lCP interterence check sample analysis results
tall outsiae the contract winaows, aUJ1U11arize the deti-
ciencies on the DPu Action Report for that case ana sub-
mit to the appropriate DPO upon com~letion ot the review.
~rofessional JUO~ement may be appliea to aetermine to
what extent tne aata may be utilized in the event that
the lC~ interterence check sample results exceed the
contract winaows. Guiaelines to aio in the application
ot protessional )UOyement to thia to~ic are as follows:
' o t·or SU11,>les witn concentrations ot Al, ca, t·e, and
Mw which are c0111parable to or wreater than their
rea1,19ctive levels in tne Interference Check ~ample:
al lf the ICb recovery for an element is> 1201
and tne reyorted a1111ple result• are < lDL then
tnis aata is acceptable for use.
b) It the IC~ recovery for an element is > 1201
and the re..,ortea sample results are > lDL then
t.lay the attect•a aata as estiaated (J) ana
inaicate in the review narrative the potential
bias in the results.
I
I
I
I
I
I
I
I
I
I
I ,
I
I
I
I
I
I
•
I
-:n -
cl If the IC~ recovery for an element tall•
oetween 30 ano 7VI ana reportable quant•-
ties of the analyte were detecteo then rtaw
the aata aa eati■ated (J). In the review
narrative, give an inaication aa to the
potential bias of the reaulta.
a) It an analyte ia not detectea in the •am~le
ana the ICS recover) for that analyte tall•
within the ran~• of 3U-7YI then the ~ossi-
bilitt of falae newativea ■ay exiat. In the
review narrative, report that the aetection
limit for that ■ample may be elevatea and
give an eatimate of the biaa. tlaw the Oata
tor these aamplea as eatimatea (UJ).
el It ICs recovery result• tor an element fall
<3UI, this is inoicative ot aevere analytical
aef icienc'ies and the data ahoula be reporteo
as unuseable (R),
o If u.,on review ot the ICs raw data poaitive reaults
are observea tor element• which are not present in
the EPA provideo ICs solution then the poaaibility ot
talae poaitivea exiata. An evaluation ot the associatea
■ample data tor the atfecteo element ■ ahould be made.
t·or sample a vi th c011_para0le or hiyher level a of inter-
terenta, poaitive samples results, which approximate
those level• touno in the ICS (talae positives>, ahoula
be tl•~wed es esti■ateo (J). ,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
0
0
-ie -
It upon review of the ICti raw aata, newative reaulta
which are> than CiU>L or -

l

• IDL, whichever is less
neyative are obaerved for el .. enta wtlich are"°'
preaent in the EPA ICS aolutiona, tben tbe poaaibility
ot talae newativa ■ ■ay exi ■t, An evaluation ot tne
associateo ■ample data 1hould be ■ade. ror aample1
with comparable or hiyher level• ot interterent ■, all
results for the attectea analyte1 which are reported
as< IDL ahoula be flagged as eati■atea (UJ), In the
review narrative, atate that the detection limit for
these ■ample ■ ■ay be elevateo.
In weneral, the ■ample data can be acceptea without
turtner evaluation it the concentrations of Al, ca,
~e ano Mw in the ■•m~l• are tound to be 1ignifi-
c1ntly less tnan tneir re ■pective concentration ■
in the Interterence Check ~ample (i,e,, ~Oil, How-
ever, if other element ■ are pre ■ent in the ■ample
at ~reater than 10 ppm the reviewer 1hould inves-
tiwate the poaaibility ot other interterence effects
by uain~ the table given on pawe D-41 ot the ~ow
or one ot the reterences li ■ted below, Analyte
concentration equivalent• preaentea in th•••
reterence ■ ahou1a be conaidered only aa eatimateo
value• aince the exact value ot any analytical 1y1tem
will ae..,end upon a variety of factor ■ auch a ■ tne
viewinw position, ahape ot the plasma ,nd back-
ground compenaation technique ■ employee. Theretore,
'
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I \
-29 -
in the instance where interterinw el-enta produce
an equivalent analyte concentration greater than·
l ti-• the CRDL and greater than lUI of the analyte
concentration identitied in the ■lllllple, flaw the
aftected results as estimated (J).
Additional References
a. Ml~ wavelenwth Tables, 1969, Massachusetts Institute of
1·echnolo1,1y.
b. Table of Sl,)tlctral Lines, iaioel et.al., Ifl/Plenum, New York,
1!17U.
c. Inductively l:ou~led Plasma -Atomic Emission Sl,)tlctroscopyi
Prominent Lines, u.s. EPA, Environmental Research Labs, Athens,
~eorgia, EPA 6UU/4-7Y-017, 1~79.
d. Tables ot spectral Line Intensities, Part II -Arranweo by
~avelenyths, inc ~a., W.F, Me~yess, et.al., National bureau ot
stanaaras, May 1Y7~.
e. A Table of ~'mission Lines in the vacuum Ultraviolet for All
~lements, Ul:RL ~4612, R,L. kelly, University ot l:alitornia,
Lawrence kaaiation Laboratory, Livermore, California, 195Y,
' t. Line l:oincioence Tables for Inauctivel) Cou~led Plasma Atomic
~inission s1,19ctrometry, Vols. I, II, J.M. boumans, Perwamon
Press, New York, 198U,
I
I
l
I
I
I
I
I
I
I
' I'
I
I
I
I
I
I
I •
I '
-30 -
v. Laboratory Control tialllple Analysis
A. ObJective
The laboratory control aainp1• analysis is desiwn•~to
serve as a monitor ot the etticiency ot the aigestion
proceaure.
b. Re~uirements
l, one ayueous LCS must be analyzea tor every 20
aam~les receivea or tor each_batch ot samples digestea,
whichever is more fre~uent, Results for each analyte
should be reported on t·orm VI I.
2. The a4ueous LCS must be an ~PA OC solution or a
standard which satisfies criteria tor use as an
initial calibration standard.
J. t"or c:,anide, at least one mia-ranliJe atandard must be
distillea ana com~ared to the calibration curve to
insure that tne distillation technique is reliable,
The distillea s{andara must a~ree within~ lUI of the
unaistillea stanaaras.
4. An a4ueous LCS tor mercury i• not required in that all
tne calibration standaras as well as OC stanaards
must be diwestea prior to analysis.
), une solid LCS must be preparea ana analysed each
month tor each analyte and results must be reportea
on t·orm v 11 •
6. The solid LCS aust be obtained from tPA.
I
I
I
I
I
I
I
I
I
I
11
I
I
I
I
I
I
I
I
-31 -
7. All aQueous LCS results aust fall within the control
limits of 80-1201 otherwise analyses should have been
terminatea, problem correctea and all batch asioeiatea
samples reanalyzed.
H. All solid LCS results aust fall within the control
limits establishea by ~PA, sam~le analysis aust be
terminated until satisfactory LCS results are obtainea.
c. Evaluation Proeeaure
l. Review form VII ana verity results fall within contract
control .limits.
2. spot cheek raw data (ICP printout, strip charts, bench
sneets) to verity the reverted recoveries on form VII.
3. If results 00 not meet criteria, verify corrective
action was taken.
D. Action
Tne inability of tne laboratory to successfully analyze
..
a known UC cneek sample (LCS) is indicative of an anaJ.y-
tical problem relatea to tne diyestion/sam~le prevaration
~roceaures ana/or instrwnent operations. Any data assoeiatea
witn tnat LCS snould t>e considerea suspect. lt the control
windows are exceeded, all data associated with tne LCS
should be reanalyzed. A summary of the aeficiency should
be included in the DPU Action Report for the case and tor~
waraea to the appro~riate DPU upon com~letion ot the review.
It the data in question are needea on a priority basis,
protessional Judyement may be ap~lied to ae~ermine to what
extent the Gata may be ~tilized.
I
I
I
'
I
I
I
I
I
I
I
' I
I
I
I
I
I
I
I ,
-32 -
o lf the .LCS recovery tor any analyte tall ■ within the
range ot 30 -791 or> 1201 then flag th• po■itive hit
aata as eatiaated (J). In the ·review narrative wive
an indication to the data u ■er as to the "°tential bias
ot the result ■ and the aetection limit■,
o It an analyte is not detected in a ■ample and the LCS
recovery is wreater than 1201 then the uaability of
tnat analytical ■ample determination i ■ acceptable,
o It an analyte is not oetectea in a ■ample and the LCS
recovery falls within the ran~• of 30 -7~1, then tne
reportea detection limit may be bia ■ed low, It the
IDL and CRDL tall clo■• to each other then the pos-
sibility exists that the CRDL was not aet. In the
review narrative, report that the detection limit tor
that sam~le ma1 De elevated and wive an estimate ot
the bias. t·law the data tor these ■ampJ.es as estimated
( UJ I•
o It LCS recovery results tall la ■■ than 301 thi ■ is
indicative of severe laboratory or ■ethod aeficienciea
and the data ■hould be reported a ■ unusable (R).
I
I
~
I
I
I
I
I
I
I
'
I ,
I
I
I
I
I
I
I
I ,
-33 -
VI. ~pecific ~ample Results
A. Duplicate Samp~e Analysis
l. UbJeCtive -The ~rcent.ditterence data will be
useo Dy EPA to evaluate the lonw term precision of
the methoos for each parameter. The data reviewer
can use the results ot the duplicate analyses as an
inoicator of the precision of the sample results.
2. tte.,.uirements
a) At least one auplicate sample must be analyzed
trom each wroup of samples of a similar matrix
type (i.e., water, soil) ano concentration (i.e.,
low, meoium) tor each case ot samples or for
eacn iu samples receiveo, whichever is more
tre,..uent.
bl ~amples iOentitieo as tield blanks cannot be
used tor auplicate sample analysis.
c) Uu1,1licate results must be reportea on t·orm VI.
a) A control limit ot ! 201 tor kPD shall be useo
tor aample values>~ times the CJUJL.
•> A control limit ot ! the CRDL shall be usea
tor sample values less than S times the CkDL.
t J t·or samples leas than the CRDL the RPO is
not calculatea.
vi All results which tall outside the acceptance
criteria must be flaw~•a with an••• on
t·orms l and VI.
'
'• -34 -J, Evaluation Proceaure al keviev J'orm VI and verify re■ult■ fall within the control limit■, bl ti~t cneck the rav data to verify tnat re■ult■ nave been correctly reported on form VI, cl t·or durilicate result■ vnicn fall outaide the control limits verity the correct usage of tla~ on both t·orms VI and I, 4, Action/Discussion Actions taken as a result of duplicate ■ample anaiysi■ must be veiwhed carefully since it may be ditticult to determine if poor preci■ion ia a re■uit ot samr'le non-homogeneity, method detect■ or lat>oratory technique, The non-homogeneous nature ot ■oil samples often makes it more aitficult to achieve wooa auylicate results compar~~ to a~ueous ■ample■, Kovever, aQueous aam~l•• containinw hi~h level■ ot aoliaa can produce erratic auplicate results a■ well, In yeneral, tne result■ ot au~licate sample analyai■ anoula be usea to support conclusion■ dravn about the Quality ot tne aata rather than as a baaia tor tneae conclusions, tiince only one auylicate ia generallt 1,19rformed per matrix tyl,18 (i.e., LU AO, M~D AO, LU tiUL, M~U bUL) tne precision result■ anoula be appliea to all otner sample■ ot the same matrix type. An exception to thi■ can be made vnen it appear■ evident that the duplicated aamyle vaa ot a aifterent chemical and,
I
I
I,
I
I
I
I
I
I
I
-
It
I
I
I
I
I
I
I
I '
-lS -
phy ■ical nature than other ■ample ■ wiven tne aame
■atrix clas ■ification. Unfortunately, oe■criptive
intormation rewaraing cntain a ■pect ■ of the iaMple
nature (i.e., appearance) ia currently li■itea ana
not reaaily availaDle to the reviewer.
The tollowinw guiaelines are offerea to enable the
reviewer to make a usability determinations
o It the proper nuMber ot duplicates for each matrix
type nave not been analyzed, reject the data ana
notit) tne DPU immediately to initiate reanaly ■is,
o If a~ueous duplicate analysia reault• tor a
particular analyte fall outside the control
vinaows of! 201 or! CRDL, whichever is ap~ropriate,
the results for that analyte in all other aamples
ot the aame ■atrix type ■houla be flawwea as
estimated I ~I. (Limits of ♦ lSI or ♦ CkUL apply --
for aoil/aediment duplicate result■.)
o hhen aQueous auplicate analysis results for a
particular analyte exceed SO JlPD and the sample
concentration level in the ouplicate 1• > S x the
CRDL, th• result• ■hould be considered Quanti-
tatively questionable (J). However, the nar-
rative ahould ■tat• that the qualitative pre-
aence ot the analyte was confinaea.
I
I
l
I
I
I
I
I
I
I
(
I
I
I
I
I
I
I
I'
o When aoil/aediaent du~licata analya1a for a
~articular analyte exceed lUU llPD and the sa111ple
concentration level irt the duplicate 11 > fa the
CRDL the result ■ should be considered quantita-
tively questionable (Jl. bowever, the narrative
should state that tne Qualitative pre1ence ot
the analyte was confirmed,
o Althouwh there i1 no contractual ba1i1 for
requiring laboratory reanaly1i1 baaed u~n submit-
ted du~licate analy1i1 re1ult1, reanalyaia requests
can be made if the reviewer/uaer deems the informa-
tion ia critical, Reanalysia occur• at ~PA'a
ex~ense and theretore all requests must be processed
throuwh the DPO not by airect contact with the
laboratory.
I
I
I
I
I
I
I
I
I
I
I (
I
I
I
I
I
I
I
I ,
-37 -
~. bpiked bample Analy ■i ■
1. UbJective -The Spiked ■ample analyai ■ 1 ■ deaigned
to provide information about the eftect ot thl
■ample matrix on the diwestion and ■ea ■ure■ent
■ethOdO.loWY•
2, kequire111ents
a) At leaat one ■piked ■ample analy ■i ■ must be
performed on each wrou~_ot ■ample, of a
■imilar matrix type (i.e., water, ■oil) and
concentration (1,e., low, hiwhl tor each
case of ■a111ple1 or tor each 20 ■ample,
received, whichever is more fr•~uent.
bl samples identitied as field blanks cannot be
used tor ■piked ■ample ana.ly ■il,
c) The analyte ■pike must be added prior to
diwestion ana in the a111ount1 ■tJ41cifiea in
• the contract (Apl,,l9ndix Ill).
dl If the ■pike recovery 1 ■ not within the
limit ■ of 1s-12s,, the data of all the
■am~les a

■
■
ociated with that ■pikea ■ample
mu ■t be tlawwed with th• letter •R• (by the
contract laboratory). An exception 1 ■ wranted
when ■ample concentration exceed■ the ■pike
concentration by a factor ot 4 or ■ore.
e) When ■ample concentration i ■ l••• than the
CtWL, SR•u is to be uued for tho purpo ■e
of calculatinw recovery.
I
I
I .,
I
I
I
I
I
I
11·
I
I
I
I
I
I
I
1,
-311 -
ti tipiked ■aml,)le re ■ult• ■uat be reported on
rorm v.
3, Evaluation Procedure
a) Keview rorm V and verify re ■ult• fall within
tne a1,19citie0 limit■,
Dl ~pot cneck raw data to verify r••ult• were
correctly revorted on rorm v.
c) t'or ■piked ■am"le result• which fall outaide
tne control limits verity the correct usa~e
ot tla,;is on l"orms I ana v.
•• Action/Discussion
ln oroer to properly assess ■pike ■am~le analysis
results, it is necessary tor the reviewer to consioer
a variety ot factors whicn could impact tneir outcome,
such as:
o "atrix ■uppr,ession effects
•
o "atrix enhancement effects
o Duvlicate presicion results
o Diyestion efticiency
o contamination
o Relative level ■ ot analyte in the ■pike and ■ample
ror exam1,>le, it the end~enou■ ■amvl• level is
yreater than 4 times th• ■pike level the percent
recovery result• ehould not be con■idered accurate
or used to Jud~• the accuracy of the ■am1,>le results,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
\.
-39 -
As with the duplicate analysis results, the accuracy
statement implied by the s~ike recovery should be
applied·to all other ■ample• of the ■ame ••trix
. -
t;rpe. An exception to thi ■ can be ■aae when it
ap~ars evident that the ■pikea ■ample was a dif-
terent chemical and phy1ical nature than other
samyles given the same matrix clasaitication.
o It the proper number of •ample lpikes have not
been procesaeo, reJect the data and notify the
DPU i111111ediately to initiate reanalyai ■•
Tne followinw guidelines are recommended for u1e in
evaluatin~ oata usability when the ■pike recoveries
Clo not fall within contract limits1
o It the spike recovery ii >1251 and the reported
sample re1ult1 are le11 than the IDL then this data
is acceptable for use.
o It the ■pike recovery 1• >1251 and the rei)Orteo
•am~le levels are yreater than the IDL then tlaij
the aata as estimated (Jl and give an inaication
in the review narrative as to the potential bias
in the result ■•
o It the ■pike recovery fall ■ between JU and 741
and reportable quantities of analyte were detected,
flaw the data as eatimatea (J). In the review
narrative, wive an indication as to the percent
bias ot the results. ,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
.....
/ ,
'·
'
-40 -
o It an analyte 1• not detected in a ■ample and
the ■pike recovery fall• within the ran~• ot
30-741 then the detection limit ■ay be bia■ea
low, In the review narrative, report that the
aetection limit tor that ■ample ■ay be elevated
ana give an estimate of the bias. rlag the aata
tor these ■amples as e1timate (UJ),
o t·or ■

a
m
,
i
l
e

results reportea as < IDL, if ■pike
recovery results fall <301, the data ■hould
be reportea as unuseable (R), Thi ■ i• indica-
tive ot ■evere analytical deticiencie ■ and the
reviewer ■houla ■tate in the narrative that the
possibility ot a false newative exists and that
the aetection limits are elevatea over what is
rei;,ortea,
o t'or po ■itive hit aata, if the ■pike recovery
re ■ult• tall <lOI, the data ■hould be reportea
L
as ~uantitatively que ■tionable (J), The
reviewer ahoula atate in the narrative that
the result• could be bia ■ed •i~nificantly low
and that the reported concentration i• the
minimum concentration at which the analyte i•
pre ■ent.
<.:, t·urnace Atomic Absorption OC Analy•i•
1. UbJ8Ctive
Duplicate inJection• and analytical ■pike■ were
incorporatea into the UC ■cheme in order to establish ,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
-41 -
a aecnani•m vhereby the reviewer could better e•ti-
aate the preci•ion and accuracy ot the indiv'idual -analytical determination relative to the overall
aetnod preci•ion and accuracy.
2. Requirement•
In addition to the previou•ly described OC
reQuirementa, the follovin1,1 adaitional criteria
apply to •·urnace AA determi-nations:
a) Du~licate inJectiona are required for all
furnace analyaea except durin~ Yull Methods
ot btandaro Addition. Averawe result is
to be reportea, rav aata must contain all
reaain1,1a.
b) for concentrations> CltDL, duplicate
inJections muat •wree within+ 201 R.SD
or the sam~le must be rerun at least once
' (tnird inJection).
c) All analyses must tall vithin the calibration
ran1,1e.
dl ~•en sample (includinw the methoa duplicate,
LCb ana blank) requires at least a sin~le
analytical spike to determine if MbA is
necessary tor quantitation.
el 'l'he spike is required to be at a concentration
tvice the CRl)L.
I
I
I
I
I
I
I
I
I
I .~
I
I
I
I
I
I
I
I ',
-42 -
f) The percent recovery of the ■pike aeterminea
hov the ■ample ■uat be quantitatea (alao aee
Al,)~naix IV) I
o If the apike recovery ia le11 than 401,
the aample ■ult be diluted by a factor of
5 to 10 and rerun vith another apike,
Tnis atep must be verformea only once.
If, after the ailution, the apike recovery
is still <401, flaw aata vith an•~• to
inaicate interterence ~roblems,
o It the s~ike recovery is wreater than
40\ ana the sample absorbance or
concentration is less than ~u, of the
spike, report the sample as le11 tnan the
CkUL or less than tne CRUL times any
dilution factor.
o If tne,sample absorbance or concentration
1• >~u, ot the •~ike ana the apike
recovery ia between B~I ana 1151, the
aamp!e should be ~uantitated directly
from the calibration curve.
o It the aample absorbance or concentration is
> 501 ot the apike and the spike recovery is
less than a~, or wreater than 11~1, the
aample must be quantitated by MSA,
1) MSA data ■Ult be vithin the
linear ranwe eata0li1hea by the
,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I I \
-43 -
initial calibration curve.
i) The ■

a
m
.
,
l
e

ana tnr•• ■pike ■.
■u■t be analy1ea con■ecutively
for MSA quantitation. (The
initial mample ana spike data
cannot be u ■ea.) Only ■inwle
inJections are re~uirea for MSA
quantitation.
3) Tne spikes ahoula be prepared
at approximately ~u, luu ana
1501 of the •am~le absorbance.
4) It the correlation coetticient
is less than 0.995, the MSA
analyses must be repeated once.
5) Tne data for MSA QUantitation
ahoula be recoraea in the raw
aata with the ■lope, intercept
ana correlation coefficient tor
the line ana the re ■ult■ ahould
also be recoraea tor t'orm VI I I.
kevcrtea va!ues obtained by MSA
ahould be tla~wea with a •s•.
6) If the MSA ha ■ been rerun a
■econa time ana the corre!ation
coefficient still i ■ le ■■ than
u.995, the re ■ult■ on torm I
ahould be fla~wed with a•+•.
I
I
I
I
I
I
I
I
I
I
I ,
I
I
I
I
I
I
I
I \
-44 -
3. ~valuation Procedure
•> Review rurnace AA raw data and tona VIII to
verity that all analy ■i ■ re~uirement ■ have
been met (i.e., ouplicate inJection ■, NSA,
etc.).
bl Verity re~orted results by recalculatin~ at
least 10\ ot the oata tor eacn varameter.
4. Action
a) If ouplicate inJections have not been
performed, reJect the oata, notity the UPO
and re~uest reanalysis.
bl lt du~licate inJections are out ■ioe tne !2U\
kSU limits and a third inJection has not
been maoe as re~uirea, tla; the data as
estimated •J•, ana ■ummarize the oeticiency on
the DPu Ac~ion kel,)Ort.
cl If the thiro inJection aoe ■ not •vree with
either of the tir ■t two inJections (! iu,
RSD), tlaij the Oat••• e ■timatea (JI.
O) If the analytical spike recovery i ■ less than
401 ano a dilution has not been analyzed,
tl•~ the data a■ estimated (J), ano ■ummarize
the oeticiency on the DPO Action Rel,)Ort tor
that ca ■e.
e) J• the analytical ■vike recovery i ■ less than
lUI the oata ■noula be re~rtea as unuseable lkl.
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
~
'
\
-4S -
fl If MSA 1• reQuired but na• not been aone,
fl•~ the data a• e•timatea (J), and aummarite
the deticiency on the DPU Action Report for
that ca•e.
g) If the correlation coetficient 1• <0,99S and
a duplicate MSA has not been .,erformea, flaw
the data as estimated (JI ana au111111arite the
aeticiency on the DPU Action Report for that
case.
h) If au~licate MSAs nave been performed ana
Doth correlation coetficient• are <0,99~,
the aata ahould be reported a, estimated (J).
ii It au~licate MSAs nave been "41rtorme0 and
00th correlation coetticients are <D.99S,
tlaw the data as unuseable (~).
o. ICP QC Analysis
l. ObJective
.~erial dilution analysis ii re~uirea 10 that the
reviewer can ascertain whether 1iwniticant physical
or chemical interferences exist due to aample matrix,
i. Meguirement1
a) une sample fr0111 each ~rou~ of 1ample1 of• similar
matrix ty.,e and concentration (i,e,, low, meaium),
for each case of aam~les, or for each 20 aamples
received, whichever 11 more tre~uent, must underwo
at least one aerial ailution.
'
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
-, .
,
'-
-46 -
bl Re1ult1 ot the ailuted ■ample 1n1ly1i1 and the
oriwinal 1na1y1e1 ■ult a~ree within 101. It_the
dilution analy1e1 i ■ not within 101, a chemical
or pny1ical interference effect ■hould be 1u1pected,
and the data ■u

■

t

be flaww•d with an •t• by the
laboratory. The 101 criteria apply only if the
analyte concentration i ■ ■ini■ally factor of 10 above
the IDL after dilution.
3. ~valuation Procedures
a) Review raw data to insure that aerial dilution
analysis was 1,>41rformed at the pro1,>41r fre~uency
tor each matrix type.
·bl ~~ot check the raw aata and verity, by recalculation,
that tne Dilution analysis results com~are within
101. verify that the correct flaw wa ■ added to
l"orm I, if requirea.
4. Action
a) It the 101 criteria i ■ not ■et, fl•w the associated
data as e ■timatea (J).
b) If ~•rial Dilution Analysis was not performed
111111111ari1e the deticiency on the DPO Action Report.
E. ~am~le Result Veritication
l. UbJective -The sample Result Verification process
checks the correctne ■

s

ot the data c0111putation and
transcription, the validity ot the calibration and
M~A curve construction, and the corre~t u■e of the
'
codes described on the cover page of the data report. i'-"2-<i
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
J.
\
-4'7 -
Re~uirementa -It 1 ■ 1•~11cit within the so~ that all
re~uired data reduction, reportinw and documentation
au ■

t

be performed and pre ■ented in ■uch a ■anner a■
to insure the data package i ■ both complete•• well
as free of computational and/or transcription error ■•
~valuation Proceaure
It is o~timal to perform a 100\ valiaation of the
data package. It ia reco._nized however, that instances
exist wnere this level ot effort mat not be practical
aue to resource constraints. The tollowinw wuidelines
snoulo be ap.i;,lied in determinin~ the minimum level ot
cata valication required to assure the acce~tability
ot the cata packawe:
a. furnace AA Parameters
cnoose at least two furnace AA parameters for
comflete valiaation. If any errors are identified
in the review of these parameters it will be
necessary to evaluate all case associated turnace
data.
b. IC~ Parameter ■
cnoo■• at least two ICP parameter ■ for complete
validation. If any error ■ are identified in this
review then evaluate an additional two parameters.
It error ■ are still encountered then all remaininw
ICP parameters aust be evaluated.
c. t'lame AA Parameter11
At a minimum, lU\ ot the flame AA parameters must
I
I
I
I
I
I
I
I
I
I
I'
---
I
I
I
I
I
I
I
I \
-41:1 -
be verified, __ .ll enora ere iaenttftect N•i-
addition.l ,.r ... tera ere required unaer tbe
prev ioua ••et ton,'
d, Mercury ana Cyaniae
U.ta for th••• ~r--tera ahould be ••lidated 1001.
e, Percent ~olia1
Due to the impact an error could have on the
results for an entire aample the data for the
percent aolida determination ahoula be validatea 100\,
In addition to the evaluation procedure, previously
outlined within this document, the apecific elements
ot the data validation process ahoula include the
tollowin1,11
a. A review ot all the deliverable• tor completeness
as aescribed in Appendix I -Contract Re~uired
Deliverables,
' •
b. An evaluation of the calibration/M~A curve in
rewarda to linearity, ran~•• outlier• and coetti-
cient of correlation. Ascertain that the CRUL
has been met.
c. verification that result• tall within the linear
ranw• of the lCP (reter to ouarterly rorm ~II and
within the calibrated range for the non-ICP para-
metera.
u. An examination ot the raw data for any anomalies
(i,e,, baseline 1hifts, newativ• abaorbance,
omi1sions, etc.I '
I
I
I,
I
I
I
I
I
I
I
1(
I
I
I
I
I
I
I
I \
-49 -
e. Verification that all the codes used on the Porm
I'• submitted for the ca•• are appropriat,.
f. A comparison of furn.~ce and ICP results fo.r the
same element. When a furnace analyte ia also in
the ICP analytical scheme, and ia identified at a
concentration greater than the ICP detection
limit, compare the results with the ICP. (This
frequently occurs for Pb and Cd.) This is•
useful method for verifying these values or
determining if• problem exists in the analysis
of the parameter. Professional judgment will be
required for both evaluation and action.
4. Action
•• If differences are identified between the reported
result and the reviewer calculated result and the
reported result is:
l) within 101 of the reviewer calculated result
and the difference could be attributed to
rounding, then no action ii required.
2) 9reater than 101 different from t.he reviewer
calculated re1ult, or le11 than 101 but not
attributable to rounding, contact the labora-
tory for verification. If an error ii con-
firmed, reque1t resubmi11ion of corrected
data 1heet1. Summarize all contact ■ with the
labordtory u1ing the CLP Telephone Log Record.
Attach copie1 of all phone l09s to the final
Quality A11urance Data Review Report.
I
I
~ '--·
I
I
I
I
I
I
I
•· '--
I
I
I
I
I
I
I
I \
-so -
b. When the improper u•e ot flaw• i• identifiea or when
~roblems are noticed with the calibration/MsA·curve ■,
contact the laboratort tor re ■ubmi ■■ion ot the correctea
aata.
I
I
I
1"
I
I
I
I
I
I
I· '
I
I
I
I
I
I
I
I \
-Sl -
VII. t'ield and Uther oc
This section is provided for guidance onl)' and as such
no tonnal evaluation procedures or actions are set torth,
ObJective, Oetinitions ana Assessment1
t'iela vt: consists ot field blanks and fiela duplicates •
. Other types of QC samples incluae split samples, blind
blanks ana blind spikes.
These types ot OC are not a part of the ijUw, but are a
usetul tool that the Rewional aata reviewer can take
advanta~e ot to monitor the performance of a laboratory,
The extent to which these types ot OC are used is lett up
to the Re~ional field and laboratory personnel,
A tield blank is 01 water that has been •run throuwn•
all the sampiinw e~ui.:,inent, The intent of a tield
blank is to monitor fot contamination introduced by
samplin~ .,eraonnel, althouwh any laboratory introducea
contamination will also be present.
A blind blank is bottlea ana ~reserved in the Rewionai
lab and shipped •a• is• to the contract lab, The
purpose ot a blind blank is to monitor tor contamination
introduced by the contract lab. A blina spike is pre~ared
by the Mewional lab. Usually the epike is inorganic atanar-
daras spiked into Dl water. Thia procidea an interterence
tree matrix with which to monitor the lab's ability to reach
I
I
I
I
I
I
I
I
I
I .(
I
I
I
I
I
I
I
I
-52 -
the CRDL or the lab'• ability to quantitatively recovar an
analyte, l:iV9citic •pikes can be pre.,ared to aonitor. •~cific
areas ( e .1,1., orwanic mercury, lCP interferant•, etc .4
A aplit sample is one that 1• divided between the
contract lab and Re~ional lab, When analyzinw a aplit
sample it is important that the aame methodology is
useo by both labs •o that there i& a basis for the
comparisons ot the results.
~lanks, spikes and splits are usetul as aupportin~
evioence in the overall assessment of a case. blanks
ano spikes are samples ot a known composition and
matrix, As such, they are usetul in assessing a
laboratory's ~•rformance independent ot •am~le or method
problems wnich ma~ arise in a real sample.
~xce~t in the case of gross errors, blanks, spikes and
I
•~lits ahould not be the basis of accepting or reJectin~
data, but rather as aoditional evidence in aupport ot
these conclusions arrived at by a review of the total
.,ackawe, tslank, apike and •Jrllit oample results often
will point out areas that the reviewer needs to look at
more caretully,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I '
VIII.
-SJ -
Quarterly Verification of Instrument Paruetera Revort
The contract laboratory must pertorm ana report
.veritication ot the follovinw ~arameters1
o Instrument Detection Limits (Mana ICPI
The contract requires that before any fiela samples
are analyzed under the contract, the instrumental
detection limits (in uw/LI must be dOCWDented and
must meet the specified levels (CROLi. The
instrumental detection limits are determined by
multiplyinw by 3, the standard Ceviation obtained
tor the analysis ot a 1tandard ■olution (each
analyte in reawent vaterl at a concentration 3-) times
the IDL on three (31 non-consecutive days vith 7
consecutive measurements ver day.
o Linear Manwe (ICPI
The linear ranwe veritication check standard must
De analyzed and reported tor each element on rorm
XI. The ■tanaara must be analyzed durinw a routine
analytical run pertormed under this contract. The
analytically determined concentration of the standard
must be within! )I ot the true value. This
concentration i ■ tne upper limit of the ICP linear
ranwe beyond which results cannot be reportea under
this contract.
o Interelement Correction factor ■ (ICPI
o wavelenwths used (ICPI
o Intewration Times (ICPI
,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I'·
IX. uverall Assessment of Data tor a caae
It is a~~ropriate tor the aata reviewer to aake
protessional Juawmenta ana express concerns ana c01111D1nts
on the valiaity of the overall aata pack•~• for a
Case. Tnis is particularly appro~riate tor Cases in
which there are several QC criteria out of specification.
The aoditive nature of QC tactors out of specification
is aitficult to assess in an ObJective manner, but the
reviewer has a responsibility to intorm users of the
data of all concerns in oraer to assist that user in
avoiain',I inap~ro~riate use ot the aata, while not
precludin._ any consideration ot the data at all. The
data reviewer would be ~reatly assisted in this endeavor
if the s~ecitic expected use of the data was provided.
t·or instance, if the reviewer was aware that the primary
element ot concern at a su~ertund ~ite was tor exam~le
,'
lead, then less eftort and resources would have to be ex-
penaea than be necessary to do a COID~r•hensive review of
the entire aata case. It is important for the reviewer to
have all &,Artinent information available.
I
I
I
1'---
1
I
I
I
I
I
Ir
I
I
I
I
I
I
I
I '
-55 -
Ap..,endix 1
Contract ReQuired Deliverable•
Contents
A. Inor~anic cover Pa~e
l!. Data Report in11 -rorm l
c. Oualitt Control SUJ11111ary
l. Initial ana Continuin\j Calibration Veritication -rorrn 11
:.I. lllank Report in.,i -t·orrn l I I
3. lCP Interference Check -t'orrn IV
4. s~ike Sam~le Recovery -Form V
5. Dui,;l icates -t·orm Vl
6. lDL and Laboratory Control Standard -Form Vll
7. Stanaard Aadition Results -t·orm VIII
D. Raw Data
1. IC~ sequential Measurement Readout Record
2. t·lame AA SeQuential ,Measurement Readout Record
3. c.a·AA SeQuential Measurement Readout Record
4. ~ola va~or Mercury se~uential Measurement Reaaout Recore
s. CN SeQuential Measurement Reaaout Record
6. Diweation low• tor M, ICP and H11 digestions
7. Percent solids raw data
~. sample Trattic ke1,10rts
Data Completeness
A. Inorwanic cover Paw•
1. submitted ~ith Case
2. Pro..,erly comvleted
a. Laboratory name
I
I
~·
I
I
I
I
I
I
I
1r
I
I
I
I
I
I
I
I •.
b, Case number
c. Date
d, !>OW No,
e, QC Report No,
-56 -
t. EPA/Laboratory sample ID numbers
y. Indication of use or non-use of ICP interelement
and backyround correction
~. Data Reportiny -t'orm I
1. Ensure that form I has been submitted
~. Proper !y com,;leted with the tollowin,,i:
a. Laboratory name
b. Case number
c. EYA bilffl~!e No.
d. Lab IU bam~le No.
e, bUW NO,
t. QC keport No,
g. Date
h, Correct units
i. Instrument used (P-ICP/t·1ame or r-t·urnace
J• ~ample results tor each parameter corrected for percent
101101 on 10111
k, Values reported to IDL'• and bracketed between
IUL's and CRDL'•·
1, Correct use ot footnotes for M~A, ■pike recovery
outside winaowa, du~licate R~U outside windows and
r < U,995,
I
I
1.
\_
I
I
I
I
I
I
I
I r
"-
I
I
I
I
I
I
I
I \
-S7 -
c. Quality control summary Yorms
l. Initial and Continuin~ Calibration Verification -
a) t:nsure tnat t'orm II has been submitted with a
minimum ot one continuing calibration veritication
per every lU samples.
bl t:nsure tne torm is ~roperly com~leteo by evaluatin~
tne fol.I.owing:
o Laboratory name
o Case number
o Units
o bcope of work
o Acce~table initial calibration source (EPA
stanoard or otner inoe1,19ndent standaro)
o Continuin~ calibration source (t:PA stanoard or
otner indepe~dent stanoard)
o Instrument used
i. t1lank tteporting -1-·orm Ill
al Ensure that the laboratory has submitted Form
III witn ~r•~aration b.l.anka tor each matrix
and continuin~ blank checks tor every 10
samples.
bl Check that Yorm III contains the tollowinw
information recorded ~ro.,er.l.y1
o Laboratory name
o case number
o Date '
I
I
I(
I
I
I
I
I
I
I
I (_
I
I
I
I
I
I
I
I '
3.
-58 -
o Unit•
o Matrix
o Values reportea to IDL'•
ICP Interterence Check -t·onn 1\1
a) ~nsure that term IV has been •ubmittea by the
laboratory it ICP analysis is used on tne
case. The form must contain analy•is ■ t tne
be~innin~ ana ena of each •am~le analysis run
(or a minimum ot twice per ~-hour workinw
snitt, whichever is more treQuent).
bl cneck that t'orm IV is properly com~letea by
evaluatin~ the tollowin~:
0
0
0
0
0
0
0
Laboratory name
case number
Date
cneck •am~l• ID
• Check sam~le source
Mean and stanaara deviation or true values
for all re"uirea elen,ents
Means ba•ea on~ or more measurements (it
UNLV ICP check solution i• not uaea).
c. keQuired elements ■re defined as all element•
analyzea by ICP, excluain~ the interterence
elements of Al, ¥e, Ca, and Mw,
o. The ICP check solution •hould be u•ea it it
is available to the laboratory. It the ICP
check solution is not available, the labOratory
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
..__
'
4.
-!i!I -
■noula prepare their ovn ana determine tne
true concentrations Dy analyzinw the aolution
a minimum ot five times.
bpike bam~le Recovery -rorm v
a) Ensure that the ■pike aam~le recovery form(■)
has been submitted.
b) At least one pre-diwestion ■pike analysis
must be performed on each wroup ot ■am,i;>les ot
a simi!ar matrix type and concentration tor
each case or tor each 2U aam~les, vnichever is
more trequent.
c) cneck that the t·orm V ( s l are pro,i;>er ly comr1leted
Dy eva!uatin~ tne tollowinw:
0
0
0
0
0
Laboratory name
Case number
Date
EPA sample number I
Units
o Matrix
o b~ikes at the contract apecifiea levels
d. The levels to •~ike both veter and ■oil
aam~les betore aiwestion i ■ apecitiea in
t:xh ibi t E, 'l'able 3 1 aee A~pend ix 2.
el bpikea are not re~uirea tor Al, ca, re, Mw,
K, or Na on aoil/aeaiment aamples.
Uu,i;>!icates -rorm VI
al Ensure that rorm VI(■) have been aubmitted
,
I
I
•c
I
I
I
I
I
I
I
I ',
I
I
I
I
I
I
I
I \
-60 -
with at least one ouplicate analy1i1 for each
wroup of aample1 of a similar matrix and
concentration or for.each group ot sa111yles
receivea, whichever i1 ■ore frequent.
bl Check that the Form VI(I) have been properly
completed with the followinw information:
o Laboratory name
o case number
o Uate
o EPA sam~le number
o Units
o Matrix
o Correct tootnotes
c. Duplicate results shoula be fla~wea with a
••• on r·orm VI if the results are out1iae the
control limits. A control limit ot 20\ MPD
on sam~les yreater than ~x CORL or! CMDL on
sam~l•s less than )X CRDL.
4. IDL ano Laboratory Control ijtanaaro -rorm VIII
al t.nsure that t·orm VII has been submitted with
instrument detection limits for each element
usinw tne instrumentation used in this case,
and laboratory control sam~le results tor a
.li~uid sam~le.
bl cneck that t·orm VII is pro~rly completed by
evaluatinw the tollowinw:
o Laboratory name
'
I
I
I'
I
I
I
I
I
I
I
Ir
I
I
I
I
I
I
I
I
-61 -
o Case nWllber
o IDL'• below CkDL for eacn parameter
o Units on the LCS _.
c) It an element 1• analyzed by both ICP/.V. ana
turnace AA, instrWllent aetection limits must
be supyliea tor both methoas.
5. stanaara Aaaition Results -t·orm VIII
11J J:;nsure that t·orm VIII has been submitted.
b) Check that t·orm VIII is properly coml,)letea by
evaluatin~ tne followinw:
o Laboratory name
o Case number
o uate
o Units
o t'ootnotes torr values less than 0.99!>.
c) All turnace analyses that are done by the
method of stanaaro aaaition must be recoraed
on t·orm v I I I •
a) correlation coetficients below o.995 should
be tlawwea with an••••
o. Raw I.late
1. A lewible ~notocopy ot raw data (sequential
measurement reaaout recora) clearly labeled
with sufficient information to une~uivocally
identity the followinw intormation ■ust be
su0111ittea with each case.
,
I
I
I/
I
I
I
I
I
I
I .(
I
I
I
I
I
I
I
I ,
-62 -
2. ~nsure that the tollovinw rav oata elements
are presents
o Digestion lo~ tor ICP preparation•
o Digestion log tor·M preparations
o Di~e1tion log for Hw preparations
o Distillation 1~ tor CN pre~arations
o Measurement readout record for ICP analyses,
it ICP is used.
o continuinw calibration recora in ICP raw
data, if ICP is usea.
o Initial and final l~P interference check,
it lCP is used.
o Dilutions tor sample out1iae ICP linear
ranwe (checked awainst laboratory's
~uarterly linear ranwe values).
o Measurement reaaout record tor turnace M
I
ano flame AA (it tlame AA is used) •
• o kecord ot tour point calibration on all
non-ICP analyses (3 standaros ano blanks).
o aecora ot parameter, oate, stanoard preva-
ration date, and analyst tor AA, Hw, and CN-.
o correlation coetticients, ~rep. blanks,
spikes, continuinw calibrations, ouplicates,
MSA, and dilutions clearl~ indicateo in
the rav oata,
o Percent solids rav data,
o Dual burns on rurnace M, not required on MSA.
'
I
I
I
I
I
I
I
I
I
I
I ,
I
I
I
I
I
I
I
I \
-63-
3. All aample results ■ust be recorded in
aeQuential order.
4. Check that raw data intensities and/or AA
absorbances are contained in the raw data
unless the instrument io in concentration ■ooe.
5. Check that all metals were analyzed within
holdin~ time (6 months).
6. Check that H~ was analyzed within holdin~
time (2ij oa;s).
7. Check that cN-was analyzed within holdin~
time (14 days).
~. sample Trattic keports
1. Ensure that copies of com~leted SHU sam~le Tratfic
Re~orts svecitic to the Case are included.
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I ,
Plu111
LleMnt
Alu11lnu11
Anti■ODY
Aueoic
llarium
llerylliu11
C.dtlium
Calcium
Chromium
Cobalt
Copper
lron
-64-
APP!RI>ll 11
El••nt1 lleterwined by lnductl•ely Coupled
E11i111on or Atoaic Ab•orption Spectro,copy -·--------'-Ontract laqulred
betectiOD 1.ev,11,2
(u1/L)
zw •u
10
2UU s s
suuo
10
SU
2)
lW s sooo
lS
0.2
40 soou
s
lU
)UUU
10
SU
2U
Leid
Nagnuium
~ngane1e
Mercury
Nlclr.el
Pota11lu111
Selenium
Silver
Sodlulll
Thallium
Vanadium
Zinc ____ -;;.;~------------------------------
I
I
I
I
I
I
I
I
I
I
I t
I
I
I
I
I
I
I
I '
Cyanide Dataraiutioa
ElaMnt
Coatract laquirad
Detection Levell, 2
(u1/L)
Cyanide 10
l: Any analytical Mthod 1pecifiad ln SOW Ezhibit Duy be utili&ad a•
long a, the documented in1truaent or aethod detection limit• aeet
the Contract Required Detection Laval (ClDL) taquiraaent1. Higher
detection level• uy only be u1ad in the followin& circum1tance:
2:
lf the aample concentration axteed1 tvo ti•• the detection liait
of the 1n1truaent or aethod in u1a, the value UJ be reported even
though the in1tru•nt or aethod dataction liait uy not equal the
contract required detection level, Thia la 1llu1tratad in the
example belov:
For lead:
Method in uae • lCP
ln1tru11ent Detection Lillit (lDL) • 40
Sample concentration• 8)
Contract lequirad Detection Laval (ClDL) • ~
The value of 8) uy be reported even thou1h 1natruMnt detection
limit 11 1raater than required detection level, The 1n1trument or
Mthod detection li~t aitt be docu•ntad 11 de1cribad in Exhibit L.
The•• CllDL ara the 1natrument detection llait1 obtained in pure
vater that ai1t be Mt u1in1 the procedure in Exhibit E, The
detection llmlt1 for 11mple1 uy be con1ldar1bly hi1her depandin&
on th• •••Pl• utrlx,
I
I
~
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
·-
APPENDlX lll
SPIKING l.EVELSI fOR SPIKED SAMPLE ANALYSIS
for ICP/11.A for· furnace AA Other
Eleaent (u&IL) (1111/L) ~u&IL)
Water SediuntI Water Sedi111entl
Alu111in11111 2,000 •
Antiaony soo soo 100 100
Ar■anic 20 40
Barium 2,000 2,000
•• ry U i 11111 so so
Cadmium so so s s
Calctua • •
Chromium 200 200
Cobalt soo soo
Copper 2SO 2SO
Iron 1,000 •
Lead soo soo 20
M&ane ■iua • •
M&n&ane ■e 200 soo I
Mercury
I
Nickel 400 soo
Pot ■Hiua • •
Selenium 10 10
Silver so so
Sodillll • •
Thalliua so
Vanadiua soo soo
Zinc 200 sou
Cyanide
100
·-------···----------·--·--·-
IIOTE: Ele-nt ■ vithout ■ptlte level ■ and not de ■i&n ■ted vith an a ■tetl ■k, ■hould
be ■piked at appropriate level ■•
lThe level• 1hovn indicate concentratlon1 tn the final dt,e■tate of the •plked
aaaple (lUO al. FV)
*No ■pike required.
,
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I \
-67-
APPENDIX IV
P'tllHACE ATOMIC .USORnlOH AIIAI.YSlS IOWtt
Pl\£Pu.t AND A!W.Y7.E SAMPLE
AND ON!:: SPIK.E (2 l C,l,D,L,) 'llll◄r--------------r
(double lnjection1 required)
_AM_Al._Y_S_l_S_W_lT-:-l-N_CAL __ l_B_RA_T_l_ON_UN_G_E-.. _____ No ___ ...Jr-1 Dll.UTE SAIU'L£ l '.
I U.COVERY OF SPIK.E )40i
if NO, repeat only once
't Yl::S
if ~111 ►! FLAG DATAW1T11 Ali ·r I
I SAMPLE A.ISORBANCE >S01 of SPltCl:: USORBANCl:*I--N_o ____ ~:~
SPIKE IU::CUVERY (8S% OR )!IS%
QUANTlTATE MY MSA WlTII 3 SPIUS
AT SO, 100 AND IS01 OF SAMPLE
AB!;llllJlANCE
'
(only 1incl• lnJection• required)
CORll£1.ATlON COEFFlCl!NT >0,99S
NO
•
1f IIU,
repeat only ooce
llPOIT SAMPLE AS
(C,l,D,L, l ANY
DILUTION fA<."TUK
QUANTITATE FllUM
CALlBRATlUN
CIJRVE AND U:PORT
I fl.,U; DI.TA WlTH -.-,
L,l ___________
••I fl.AC UATA WITH A-♦-
u ■till NU
*•pike abaorbance defl,.ed •• (ebaorbance of 1pike 1a■ple) ■inu1 (ebaorbance of the
1a■ple)
I
I
~-
I
I
I
I
I
I
I
1(
I
I
I
I
I
I
I
I I
-68-
APPEHDIX V
Contract Llbcratary Program
ltEC.JONAL/LA80RATORY COMMUN1CAT10N SYST!.11
Telqiae ll&Cllrd Loe
Date of Call:
Laboratory Name:
L&b Contact:
Region:
Regional Contact:
Call Initiated By: _ Laboratory _Region
In reference to data for the following 11mple 11Jmberi1):
Summary of Questions/Issues Disc:\lssed:
Summary of Resolution:
Signature
Distribution: (I) Lab Copy, (2) Region Copy, (3) SMO Copy
Dlte
'
I
I
I
I
I
I
I
I
I
I
I(
I
I
I
I
I
I
I
I '-
-69-
CONTRACTLABORATORYPROCRAM
Deputy Project Officer Comml.S\ication Swnmary
Date DPO Notified of Issue: ____ _ DPO Notified 8y1 ________ _
SYbject lAboratory: ____________ _ C&se /S&s No:
Cont.act for Resolution: --------.,.,..-,-----,,.,,.--------(lAboratory or PO)
Date of Cont.act: C&ll or Vi.lit (Circle One)
Summary of Issues & Resolutions:
Document the ilsue(s), resolution(s), and action deadlines, if any._
Signature
Region
(I) DPO Copy (2) Project Officer Copy
Date
()) SMO Copy (It) Lab Copy
}/14
I
I
I
I
I
I
I
I
I
I
I'
I
I
I
I
I
I
I
I '
APPDIDll VI
UCIOHAL DEPUTY PllOJECT OFFICEllS
FOR
Q.p TECHNlCAL AOMJNISTRA T10N
USE PA Region I
Edward Taylor
Chief, Chemistry Section
USEPA Region I
Envlronmenul Services Division
60 Westvlew Street
Lexington, MA 0217)
,1111,11700
USE PA Region D
William Coalcley
Superfund QA CoordiNtor
USEPA Region n
!nvironmenul Services Divlslon
Woodbridge Avenue
Edison, New leney 01137
201/)21-6702
USEPA Rttion m
Patricia Krantz
QA Officer
USEPA Region m
A.M&polis Field Office
Central Regional Office
139 Bestga te Rd.
Annapolis, MD 211J0 l
30l/221t-271J0
USEPA Region IV
Tom a. Berv,ett, lr.
Chief, Chemistry Section
USEP A Region IV
Environment&! ServlcH Dlvllion
College Station Road
Athens, Cieor&la JCkilJ
.o,1m-,112
USEPA Region V
Chuck !Uy
SMO Coordinator
USEPA Reclon V
JJ6 s. Clarie St.
Tenth Floor, CRL
Chicago, Illinois 6060J
)12/JJ)-,017
•'
USEPA Region VI
William Lan&leJ .
USEPA Re&ion vt _
Monterey Park Plaza, lld&, C
U0I Hornwood Drive
Houston, Texas 7707•
7U/9.k-17"
U5EPA Region Vil
Dr. Robert Kleopfer
Chief Chemist
USEPA Region VU
Environmental ServlcH Division
2J Fi,nston Rd.
Kansas City, Kanas "lU
· fU/23'->111
USEPA Region vtD
.John Tilstra
Chief, Laboratory Services Sectlon
USEPA Region Vlll • Laboratory
Denver Federal Center
luildin& '3, !ntrance W-1, 2nd Floor
Denver, CO 1022J
,03/,_,i..,2,,
USEPA Region IX
Harold Takenaka
Chief of Laboratory Support Section for OES
USEPA Region IX
21' Fremont StrNt
San Francisco, California ,,10,
,ut,1-.1,1,
USEPA Region X
Arnold Cahler
Chief, Laboratory lrandl
USEPA Region X
P.O, lo1 S.t
Manchester, ,r A tlJJJ
206/,,2-0,10
•
I
I
I(
I
I
I
I
I
I
I -
I
{
I
I
I
I
I
I
I
I '
-71-
Data keview Ui1tribution Addre11e1
1) Duane Geuder
Analytical ~upport branch (WH-~48A)
Hazardous kesponse sup~rt Divi1ion
401 •"• st., s.w.
Washinwton, 0.c. io46O
:.t) llos s kobeson
t::M:.L-LV
P.O. box 1~027
Las Vewas, NV ijYll4
3) Co~nizant DPO
LaDoratory/DPO Assi~nntents (by Reyion):
kewion I:
Rewion II:
Cambridge Analyticl Associates
Chemtech Consultinw Group, Ltd.
u.s. Testin~ com~any
llewion III: Centec Analytical services
Hittman-LDasco Associates, Inc.
JTC t::nvironmental consultant,, Inc.
Mack Laboratories
llewion IV:
kewion VI:
Ver1ar Laboratorie1, Inc.
comvuChem Laboratories, Inc.
Anacon
Radian
S1>9ctrix Corvcration
'l·oxicon Laboratories, Inc.
llewion VII: Wilaon Laboratory
llewion ~Ills Accu-Labs Research
Rewion IX1
Rewion Xs
Rocky Mountain Analytical Laboratory, Inc.
calitornia Analytical Laboratoriea, Inc.
weyerhaeuaer Company
I
I
1-
·-
I
I
I
I
I
I
I
Ir"
I
I
I
I
I
I
I
I '
-72-
Gloaaary
Data Oualitier Definitions
t·or the 1,>urposes ot this document the ·tollowinw coae letter• ano
asaociated definitions are provioed, use of these apecitic code
letters is not manoatory1 use ot ditferent cooes with the same
qualifier definitions is o~tional,
u -Tne material was analyzed tor, but was not cetecteo, The
associateo numerical value is the estimateo SAID~l• quantitation
limit.
J -The associateo numerical value is an estimated quantity
because Quality control criteria were not met,
K -Quality control inOicates tnat the data are unusable (com~ouno
may or may not be present), Kesamplinw ano/or reanalysis is
necessary tor verification.
2 -No analytical result
I
I
If
I
I
I
I
I
I
I
,.
I I ,
I
I
I
I
I
I
I
I '
-73-
Other Terms
AA -Atomic Absorption
CLP -Contract Laboratory PrO<,jram
CIWL -contract Re~uired Detection Limit
DPO -Deyuty ProJect Otficer
G~'AA -liraphite •·urnace Atomic Absorption
ICP -Inductively Couvled Plasma
IUL -Instrument Detection Limit
LCS -Laboratory Control a;am1,1le
M:.A -Metnod ot Standard Addition
IIIPO -National PrO<,jram Utt ice
use -on scene Coordinator
PU -l'rOJeCt utticer
OA -Quality Assurance
uc -Quality Control
Rscc -Mewional samfle control Center
a;Mu -sample Manawement ottice
v1:sR -Validated Ti•• of a;am1,1l• Receipt
'
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
U.S.E.P.A. Region
INORGANIC QUALITY ASSURANC"E~D"""A""'TA ....... R.EVIEW REPORT
Case No. _________ _ Project Namr ____ _
Laboratory ________ _ DPO for Lab _____ _
Applicable Sample Nos.
Date Sampled: ________ _
Date Data Received: ______ _
Review Date: _________ _
Contact of laboratory required (yes, attach CLP logs) (no) --

-
-
Resubmissions requested Received --
Data Oualifers:
U -The material was analyzed for but was not detected. The associated
numerical value is the sample quantitation limit. NOT DETECTED.
J -The associated numerical value is an estimated quantity because one
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.
'
DPOAction FYI
I
I Quality Assurance Data Review Report (Cont.)
I
I Case No.
Laboratory
I
I
Comments
I
I
I
I
I OPO Action Items
I
I
I
I
I
I Reviewed by: Phone No. Date:
Attachments
I CC:
I Regional OPO (for laboratory)
Contract Laboratory Program, QAO ,
-------------------DATA S .IMARY
M No.----------
boratory
Matrl ■----------
Uni1, ________ _
COMMENTS
m,num
imon,
tnK
iu,n
yllium
lmium
.,ium
rofflium
bait ,.,,.,
n
ad
-
1allftium
anoa,_
"'"" , ....
,taniulft ·~
lwf
~
.. niuffl
n
....clium
in<
yanide
~ Solich
CawNO._
l-•to,y -llfGIONAl OC \AMPU FIHOOC OlMHI MATIUX \P(CIFIC 0C WIClflCQC
OVfllAU CA\f OC ..... --·= COMMUITS
:,)-:i ·r~ -'t:,· .. .., ... '"-...... ...... --·~', ....... ...... ..,,,_ -... •Ii•~ , --'" ,o .. ... AO .... -,... ... -·--... -1~-;; :~4-.. AO ....... ... AO Mil -· , .. _ ......
' . ·-----... _ ._.,..._ ,,_
I -. , ......
:!c,._
ljc-
;j<-..... . :,l ...
.
1 ... , ..... !1~--
I , ....... u,rr
' ....... I. ; ..,_ -I "'---·-, .. v-, ...
c, ....
--
,
•
.. ...____ -----------

-
• ----.. --