Roy F Weston Inc 2 11400 Weston Way PO Box 2653 West Chester Pennsylvania 19380 610-701-3000 bull Fax 610-701-31 86 wwwrfwestoncom

27 October 1999

Mr Gary Lacroix Engineering Management Division New England District 696 Virginia Road Concord MA 01742-2751 Work Order No 10971-032-001-0132

Re Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY Final Quality Assurance Project Plan - Revised Appendix C of Volume III

Dear Mr Lacroix

Please find enclosed two copies of Appendix C of Volume III of the Final Quality Assurance Project Plan for the General Electric (GE) Housatonic River Project in Pittsfield MA Please insert this revised section behind the Appendix C tab in Volume I I I

Roy F Weston Inc (WESTONreg) is also providing five copies to Mr Chet Janowski at the EPA office in Boston MA three copies to Susan Steenstrup at MADEP in Springfield MA one copy to Andy Beliveau Massachusetts EPA Laboratory one copy to the HTRW Center of Expertise Document Distribution Center in Omaha NE and one copy to Holly Inglis EPA

This submittal has undergone WESTONs technical and quality control review and coordination procedures to ensure (1) completeness for each discipline commensurate with the level of effort required for the submittal (2) elimination of conflicts errors and omissions (3) compliance with project criteria and (4) overall professional and technical accuracy of the submittal

Please feel free to contact Sharon Nordstrom at 610-701-3948 or me at 610-701-7366 if you have any questions

Very truly yours

ROY F WESTON INC

~ Lee dePersm

Project Manager cc C Janowski EPA

S Steenstrup MADEP A Beliveau Massachusetts EPA Laboratory Document Distribution Center HTRW Center of Expertise 11

oH Inglis EPA ui DCN File -BGorman o oDCN Fi le-D Veilleux

LdPwp Enclosure o

o o

LJ M O

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1M9

APPENDIX C

QAPP ADDENDUM FOR TISSUE ANALYSES

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TABLE OF CONTENTS

C QAPP ADDENDUM FOR TISSUE ANALYSES

CI INTRODUCTION

C2 PROJECT DATA QUALITY OBJECTIVES

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LIST OF TABLES

Table C-l Analytical Measurements Quality Control Requirements

Table C-2 Spike Accuracy and Precision Limits

Table C-21 Spike Accuracy and Precision LimitsmdashPCDDsPCDFs

Table C-3 Surrogate Spike Recovery Limits

Table C-4 Valid Value List for Analysis Method

Table C-5 Required Containers Preservation Techniques and Holding Times for Tissue Samples

Table C-6 Appendix IX Pesticide Compound Reporting Limits

Table C-7 PCB Compound Reporting Limits

Table C-8 PCB CongenerHomologue Reporting Limits

Table C-9 PCDDPCDF Compound Reporting Limits

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Page 1of19

C QAPP ADDENDUM FOR TISSUE ANALYSES

C1 INTRODUCTION

Appendix C consists of text and table addendums as associated with the sections referenced in

the QAPP Appendix C addresses only those issues related to tissue sample analysis sampling of

which was performed at various OU locations as outlined in the specific Work Plan All tissue

samples are being managed by the US Fish and Wildlife Service Patuxent Wildlife Research

Center Primary analyses will be performed by the Geochemical and Environmental Research

Group College of Geosciences Texas AampM University The laboratory SOPs relevant to the

tissue analyses are referenced throughout the Appendix C addendums and are supplied in

Appendix D The general procedures established in the QAPP are to be followed except for

those analytical protocols specifically referenced in Appendices C and D

C2 PROJECT DATA QUALITY OBJECTIVES

The overall site data quality objective is to collect a sufficient quality and quantity of data based

on the OU such that scientifically based decisions can be made in order to

bull Determine the extent of contamination and migration of the primary compounds of concern Aroclor-1254 and Aroclor-1260 for characterizationremovalrisk assessment activities by content in various fish avian and mammal specimens

bull Determine extent of PCB weathering at specific OU locations with the examination of PCB congener results

bull Determine the absence or presence of other hazardous substances in addition to the contaminants of concern by OC pesticide and dioxinfuran analyses

bull Determine the extent of hazardous substance migration off-site by waterway or other mode of redistribution by content in various fish avian and mammal specimens

bull Make effective use of modeling tools to predict long-term trends and potential risks associated with location-specific PCB redistributiondispositionaccumulation in soil and sediment media as well as any inter-related biological tissues

bull Use as support in litigation against the Potentially Responsible Parties (PRP)

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Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCB Congeners

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt 50

Per Table C-2

Interspersed Calibration

Minimum of 4 concentrations

Calibration curve Rgt0 995

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per 20 or fewer samples

lt3 x MDL or analytes gt10 x blank

Ongoing Precision and Recovery (OPR)Standard Reference Materials

When required See Table C-2

Performance Evaluation Sample

As supplied Per Laboratory Data Validation Functional Guidelines for Environmental Analyses (99shyOIOO)

Corrective Action

NA

I As per SOP-9810 Section 3 3

1 Evaluate 2 Recalibrate when

QC criterion is not met

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 3

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Evaluate PE score report

2 Evaluate batch 3 Recommend action

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Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCBs and Organoshychlorme Pesticides

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt50

Per Table C-2

Interspersed Calibration

Four-point calibration for all analytes

Calibration R 20 995

Degradation Check Solution (DDT and Dieldrin)

Prior to initial calibration

Degradation of the labile chlorinated compounds in the injection port lt I5

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per each QC batch of 20 or fewer samples

lt3x MDL not more than 2 target compounds with concentrations gt3x MDL or analytes gt 10 x blank

Laboratory Blank Spike (LBS) and Laboratory Blank Spike Duplicate (LBSD)

When required 80 of the target compounds should have between 40 and 130 recoveries If the LBSD has been included the recoveries from LBS and LBSD should agree within an RPD of lt30

Corrective Action

As per SOP-9810 Section 3 3 4 2

As per SOP-9810 Section 3333

1 Evaluate 2 Recalibrate

when QC criterion is not met

1 Stop analytical run

2 Clean injection port

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 4 5 2

As per SOP-9810 Section 3 3 1

As per SOP-9810 Section 3 3

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Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9810 PCBs and Laboratory Laboratory When required RPD=S30 1 Recalculate or (GC-ECD) Organo-chlorme (cont ) Duplicate reanalyze the (Cont ) Pesticides duplicate and the

original sample

2 Recalibrate or re-extract the analytical QC batch

Performance As supplied Per Laboratory Data 1 Evaluate PE Evaluation Sample Validation Functional score report Standard Reference Guidelines for 2 Evaluate batch Materials Evaluating

Environmental Analyses (99-0 100)

3 Recommend action

SOP-9722 Polychlonnated Field Field Duplicate As supplied RPDlt50 1 Recalculate (HRGCshy dibenzo-p- Sampling andor reanalyze HRMS) dioxins the duplicate

polychlormated andor original dibenzofurans sample (PCDDPCDF) Compounds 2 Instrument

maintenance andor recalibration

Laboratory Matrix Spike and When required Per Table C-2 1 1 Recalculate Matrix Spike andor re-Duplicate analyze the MS

andMSD

2 Instrument maintenance andor recalibration

Initial and As per SOP-9722 As per SOP-9722 1 Evaluate Continuing Section 3 3 Section 3 3 2 Recalibrate Calibrations when QC

criterion is not met

Identification As per SOP-9722 As per SOP-9722 1 Evaluate Retention Times Section 3 2 Section 3 2 2 Rerun as Ion Abundance RatiosSignal to NoiseInterferences

SN exceeds 10 1 for all ions

Ion abundance ratio

3

necessary

Criteria must be met before

plusmn15 samples are run

Interference SN ^3

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Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9722 (HRGC-HRMS)

Polychlonnated dibenzo-p-

Laboratory (Cont )

Instrument Performance Check

As per SOPshy9722

As per SOP-9722 Section 3 1

12 Evaluate Retune instrument

(Cont ) dioxms polychlonnated

Section 3 1 3 Verify

dibenzofurans (PCDDPCDF) Compounds

Laboratory Duplicate

When required RPD S30 1 Recalculate or reanalyze the duplicate andor the original sample

2 Instrument maintenance andor recall bration

Standard Reference When required 70- 130 of the 1 Recalculate or Material (SRM) certified or consensus reanalyze the

value of the analyte SRM with no more than 13 2 Instrument of the analytes maintenance exceeding this criteria andor

recalibration

Labeled Compound All samples Recoveries within 1 Stop analytical Recovery 40- 13 5 run

2 Clean injection port

3 Rerun all affected samples

Initial Precision and Prior to any See SOP-9722 1 Evaluate Recovery (IPR) analysis by this

method Table 7 2 Repeat until

criteria are met

Ongoing Precision One per 20 or See Table C-2 1 Rerun and Recovery fewer samples 2 Evaluate batch (OPR) (Narrate)

3 If criteria are met reanalyze as necessary

Method Blank One per 20 or ltj POL 1 Rerun fewer samples 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

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Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

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Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

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Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

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Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

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Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

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Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

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Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

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Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

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Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

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Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

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Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

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Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

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Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

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Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

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TABLE OF CONTENTS

C QAPP ADDENDUM FOR TISSUE ANALYSES

CI INTRODUCTION

C2 PROJECT DATA QUALITY OBJECTIVES

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LIST OF TABLES

Table C-l Analytical Measurements Quality Control Requirements

Table C-2 Spike Accuracy and Precision Limits

Table C-21 Spike Accuracy and Precision LimitsmdashPCDDsPCDFs

Table C-3 Surrogate Spike Recovery Limits

Table C-4 Valid Value List for Analysis Method

Table C-5 Required Containers Preservation Techniques and Holding Times for Tissue Samples

Table C-6 Appendix IX Pesticide Compound Reporting Limits

Table C-7 PCB Compound Reporting Limits

Table C-8 PCB CongenerHomologue Reporting Limits

Table C-9 PCDDPCDF Compound Reporting Limits

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Page 1of19

C QAPP ADDENDUM FOR TISSUE ANALYSES

C1 INTRODUCTION

Appendix C consists of text and table addendums as associated with the sections referenced in

the QAPP Appendix C addresses only those issues related to tissue sample analysis sampling of

which was performed at various OU locations as outlined in the specific Work Plan All tissue

samples are being managed by the US Fish and Wildlife Service Patuxent Wildlife Research

Center Primary analyses will be performed by the Geochemical and Environmental Research

Group College of Geosciences Texas AampM University The laboratory SOPs relevant to the

tissue analyses are referenced throughout the Appendix C addendums and are supplied in

Appendix D The general procedures established in the QAPP are to be followed except for

those analytical protocols specifically referenced in Appendices C and D

C2 PROJECT DATA QUALITY OBJECTIVES

The overall site data quality objective is to collect a sufficient quality and quantity of data based

on the OU such that scientifically based decisions can be made in order to

bull Determine the extent of contamination and migration of the primary compounds of concern Aroclor-1254 and Aroclor-1260 for characterizationremovalrisk assessment activities by content in various fish avian and mammal specimens

bull Determine extent of PCB weathering at specific OU locations with the examination of PCB congener results

bull Determine the absence or presence of other hazardous substances in addition to the contaminants of concern by OC pesticide and dioxinfuran analyses

bull Determine the extent of hazardous substance migration off-site by waterway or other mode of redistribution by content in various fish avian and mammal specimens

bull Make effective use of modeling tools to predict long-term trends and potential risks associated with location-specific PCB redistributiondispositionaccumulation in soil and sediment media as well as any inter-related biological tissues

bull Use as support in litigation against the Potentially Responsible Parties (PRP)

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Page 2 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCB Congeners

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt 50

Per Table C-2

Interspersed Calibration

Minimum of 4 concentrations

Calibration curve Rgt0 995

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per 20 or fewer samples

lt3 x MDL or analytes gt10 x blank

Ongoing Precision and Recovery (OPR)Standard Reference Materials

When required See Table C-2

Performance Evaluation Sample

As supplied Per Laboratory Data Validation Functional Guidelines for Environmental Analyses (99shyOIOO)

Corrective Action

NA

I As per SOP-9810 Section 3 3

1 Evaluate 2 Recalibrate when

QC criterion is not met

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 3

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Evaluate PE score report

2 Evaluate batch 3 Recommend action

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Page 3 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCBs and Organoshychlorme Pesticides

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt50

Per Table C-2

Interspersed Calibration

Four-point calibration for all analytes

Calibration R 20 995

Degradation Check Solution (DDT and Dieldrin)

Prior to initial calibration

Degradation of the labile chlorinated compounds in the injection port lt I5

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per each QC batch of 20 or fewer samples

lt3x MDL not more than 2 target compounds with concentrations gt3x MDL or analytes gt 10 x blank

Laboratory Blank Spike (LBS) and Laboratory Blank Spike Duplicate (LBSD)

When required 80 of the target compounds should have between 40 and 130 recoveries If the LBSD has been included the recoveries from LBS and LBSD should agree within an RPD of lt30

Corrective Action

As per SOP-9810 Section 3 3 4 2

As per SOP-9810 Section 3333

1 Evaluate 2 Recalibrate

when QC criterion is not met

1 Stop analytical run

2 Clean injection port

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 4 5 2

As per SOP-9810 Section 3 3 1

As per SOP-9810 Section 3 3

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Page 4 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9810 PCBs and Laboratory Laboratory When required RPD=S30 1 Recalculate or (GC-ECD) Organo-chlorme (cont ) Duplicate reanalyze the (Cont ) Pesticides duplicate and the

original sample

2 Recalibrate or re-extract the analytical QC batch

Performance As supplied Per Laboratory Data 1 Evaluate PE Evaluation Sample Validation Functional score report Standard Reference Guidelines for 2 Evaluate batch Materials Evaluating

Environmental Analyses (99-0 100)

3 Recommend action

SOP-9722 Polychlonnated Field Field Duplicate As supplied RPDlt50 1 Recalculate (HRGCshy dibenzo-p- Sampling andor reanalyze HRMS) dioxins the duplicate

polychlormated andor original dibenzofurans sample (PCDDPCDF) Compounds 2 Instrument

maintenance andor recalibration

Laboratory Matrix Spike and When required Per Table C-2 1 1 Recalculate Matrix Spike andor re-Duplicate analyze the MS

andMSD

2 Instrument maintenance andor recalibration

Initial and As per SOP-9722 As per SOP-9722 1 Evaluate Continuing Section 3 3 Section 3 3 2 Recalibrate Calibrations when QC

criterion is not met

Identification As per SOP-9722 As per SOP-9722 1 Evaluate Retention Times Section 3 2 Section 3 2 2 Rerun as Ion Abundance RatiosSignal to NoiseInterferences

SN exceeds 10 1 for all ions

Ion abundance ratio

3

necessary

Criteria must be met before

plusmn15 samples are run

Interference SN ^3

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Page 5 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9722 (HRGC-HRMS)

Polychlonnated dibenzo-p-

Laboratory (Cont )

Instrument Performance Check

As per SOPshy9722

As per SOP-9722 Section 3 1

12 Evaluate Retune instrument

(Cont ) dioxms polychlonnated

Section 3 1 3 Verify

dibenzofurans (PCDDPCDF) Compounds

Laboratory Duplicate

When required RPD S30 1 Recalculate or reanalyze the duplicate andor the original sample

2 Instrument maintenance andor recall bration

Standard Reference When required 70- 130 of the 1 Recalculate or Material (SRM) certified or consensus reanalyze the

value of the analyte SRM with no more than 13 2 Instrument of the analytes maintenance exceeding this criteria andor

recalibration

Labeled Compound All samples Recoveries within 1 Stop analytical Recovery 40- 13 5 run

2 Clean injection port

3 Rerun all affected samples

Initial Precision and Prior to any See SOP-9722 1 Evaluate Recovery (IPR) analysis by this

method Table 7 2 Repeat until

criteria are met

Ongoing Precision One per 20 or See Table C-2 1 Rerun and Recovery fewer samples 2 Evaluate batch (OPR) (Narrate)

3 If criteria are met reanalyze as necessary

Method Blank One per 20 or ltj POL 1 Rerun fewer samples 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

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Page 6 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

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Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

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Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

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Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

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Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

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Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

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Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

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Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

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Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

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Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

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Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

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Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

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Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

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Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

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LIST OF TABLES

Table C-l Analytical Measurements Quality Control Requirements

Table C-2 Spike Accuracy and Precision Limits

Table C-21 Spike Accuracy and Precision LimitsmdashPCDDsPCDFs

Table C-3 Surrogate Spike Recovery Limits

Table C-4 Valid Value List for Analysis Method

Table C-5 Required Containers Preservation Techniques and Holding Times for Tissue Samples

Table C-6 Appendix IX Pesticide Compound Reporting Limits

Table C-7 PCB Compound Reporting Limits

Table C-8 PCB CongenerHomologue Reporting Limits

Table C-9 PCDDPCDF Compound Reporting Limits

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C QAPP ADDENDUM FOR TISSUE ANALYSES

C1 INTRODUCTION

Appendix C consists of text and table addendums as associated with the sections referenced in

the QAPP Appendix C addresses only those issues related to tissue sample analysis sampling of

which was performed at various OU locations as outlined in the specific Work Plan All tissue

samples are being managed by the US Fish and Wildlife Service Patuxent Wildlife Research

Center Primary analyses will be performed by the Geochemical and Environmental Research

Group College of Geosciences Texas AampM University The laboratory SOPs relevant to the

tissue analyses are referenced throughout the Appendix C addendums and are supplied in

Appendix D The general procedures established in the QAPP are to be followed except for

those analytical protocols specifically referenced in Appendices C and D

C2 PROJECT DATA QUALITY OBJECTIVES

The overall site data quality objective is to collect a sufficient quality and quantity of data based

on the OU such that scientifically based decisions can be made in order to

bull Determine the extent of contamination and migration of the primary compounds of concern Aroclor-1254 and Aroclor-1260 for characterizationremovalrisk assessment activities by content in various fish avian and mammal specimens

bull Determine extent of PCB weathering at specific OU locations with the examination of PCB congener results

bull Determine the absence or presence of other hazardous substances in addition to the contaminants of concern by OC pesticide and dioxinfuran analyses

bull Determine the extent of hazardous substance migration off-site by waterway or other mode of redistribution by content in various fish avian and mammal specimens

bull Make effective use of modeling tools to predict long-term trends and potential risks associated with location-specific PCB redistributiondispositionaccumulation in soil and sediment media as well as any inter-related biological tissues

bull Use as support in litigation against the Potentially Responsible Parties (PRP)

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Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCB Congeners

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt 50

Per Table C-2

Interspersed Calibration

Minimum of 4 concentrations

Calibration curve Rgt0 995

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per 20 or fewer samples

lt3 x MDL or analytes gt10 x blank

Ongoing Precision and Recovery (OPR)Standard Reference Materials

When required See Table C-2

Performance Evaluation Sample

As supplied Per Laboratory Data Validation Functional Guidelines for Environmental Analyses (99shyOIOO)

Corrective Action

NA

I As per SOP-9810 Section 3 3

1 Evaluate 2 Recalibrate when

QC criterion is not met

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 3

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Evaluate PE score report

2 Evaluate batch 3 Recommend action

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Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCBs and Organoshychlorme Pesticides

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt50

Per Table C-2

Interspersed Calibration

Four-point calibration for all analytes

Calibration R 20 995

Degradation Check Solution (DDT and Dieldrin)

Prior to initial calibration

Degradation of the labile chlorinated compounds in the injection port lt I5

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per each QC batch of 20 or fewer samples

lt3x MDL not more than 2 target compounds with concentrations gt3x MDL or analytes gt 10 x blank

Laboratory Blank Spike (LBS) and Laboratory Blank Spike Duplicate (LBSD)

When required 80 of the target compounds should have between 40 and 130 recoveries If the LBSD has been included the recoveries from LBS and LBSD should agree within an RPD of lt30

Corrective Action

As per SOP-9810 Section 3 3 4 2

As per SOP-9810 Section 3333

1 Evaluate 2 Recalibrate

when QC criterion is not met

1 Stop analytical run

2 Clean injection port

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 4 5 2

As per SOP-9810 Section 3 3 1

As per SOP-9810 Section 3 3

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Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9810 PCBs and Laboratory Laboratory When required RPD=S30 1 Recalculate or (GC-ECD) Organo-chlorme (cont ) Duplicate reanalyze the (Cont ) Pesticides duplicate and the

original sample

2 Recalibrate or re-extract the analytical QC batch

Performance As supplied Per Laboratory Data 1 Evaluate PE Evaluation Sample Validation Functional score report Standard Reference Guidelines for 2 Evaluate batch Materials Evaluating

Environmental Analyses (99-0 100)

3 Recommend action

SOP-9722 Polychlonnated Field Field Duplicate As supplied RPDlt50 1 Recalculate (HRGCshy dibenzo-p- Sampling andor reanalyze HRMS) dioxins the duplicate

polychlormated andor original dibenzofurans sample (PCDDPCDF) Compounds 2 Instrument

maintenance andor recalibration

Laboratory Matrix Spike and When required Per Table C-2 1 1 Recalculate Matrix Spike andor re-Duplicate analyze the MS

andMSD

2 Instrument maintenance andor recalibration

Initial and As per SOP-9722 As per SOP-9722 1 Evaluate Continuing Section 3 3 Section 3 3 2 Recalibrate Calibrations when QC

criterion is not met

Identification As per SOP-9722 As per SOP-9722 1 Evaluate Retention Times Section 3 2 Section 3 2 2 Rerun as Ion Abundance RatiosSignal to NoiseInterferences

SN exceeds 10 1 for all ions

Ion abundance ratio

3

necessary

Criteria must be met before

plusmn15 samples are run

Interference SN ^3

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Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9722 (HRGC-HRMS)

Polychlonnated dibenzo-p-

Laboratory (Cont )

Instrument Performance Check

As per SOPshy9722

As per SOP-9722 Section 3 1

12 Evaluate Retune instrument

(Cont ) dioxms polychlonnated

Section 3 1 3 Verify

dibenzofurans (PCDDPCDF) Compounds

Laboratory Duplicate

When required RPD S30 1 Recalculate or reanalyze the duplicate andor the original sample

2 Instrument maintenance andor recall bration

Standard Reference When required 70- 130 of the 1 Recalculate or Material (SRM) certified or consensus reanalyze the

value of the analyte SRM with no more than 13 2 Instrument of the analytes maintenance exceeding this criteria andor

recalibration

Labeled Compound All samples Recoveries within 1 Stop analytical Recovery 40- 13 5 run

2 Clean injection port

3 Rerun all affected samples

Initial Precision and Prior to any See SOP-9722 1 Evaluate Recovery (IPR) analysis by this

method Table 7 2 Repeat until

criteria are met

Ongoing Precision One per 20 or See Table C-2 1 Rerun and Recovery fewer samples 2 Evaluate batch (OPR) (Narrate)

3 If criteria are met reanalyze as necessary

Method Blank One per 20 or ltj POL 1 Rerun fewer samples 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

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Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

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Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

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(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

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Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

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Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

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Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

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Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

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Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

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Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

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Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

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Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

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Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

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Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

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Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

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Page 1of19

C QAPP ADDENDUM FOR TISSUE ANALYSES

C1 INTRODUCTION

Appendix C consists of text and table addendums as associated with the sections referenced in

the QAPP Appendix C addresses only those issues related to tissue sample analysis sampling of

which was performed at various OU locations as outlined in the specific Work Plan All tissue

samples are being managed by the US Fish and Wildlife Service Patuxent Wildlife Research

Center Primary analyses will be performed by the Geochemical and Environmental Research

Group College of Geosciences Texas AampM University The laboratory SOPs relevant to the

tissue analyses are referenced throughout the Appendix C addendums and are supplied in

Appendix D The general procedures established in the QAPP are to be followed except for

those analytical protocols specifically referenced in Appendices C and D

C2 PROJECT DATA QUALITY OBJECTIVES

The overall site data quality objective is to collect a sufficient quality and quantity of data based

on the OU such that scientifically based decisions can be made in order to

bull Determine the extent of contamination and migration of the primary compounds of concern Aroclor-1254 and Aroclor-1260 for characterizationremovalrisk assessment activities by content in various fish avian and mammal specimens

bull Determine extent of PCB weathering at specific OU locations with the examination of PCB congener results

bull Determine the absence or presence of other hazardous substances in addition to the contaminants of concern by OC pesticide and dioxinfuran analyses

bull Determine the extent of hazardous substance migration off-site by waterway or other mode of redistribution by content in various fish avian and mammal specimens

bull Make effective use of modeling tools to predict long-term trends and potential risks associated with location-specific PCB redistributiondispositionaccumulation in soil and sediment media as well as any inter-related biological tissues

bull Use as support in litigation against the Potentially Responsible Parties (PRP)

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Page 2 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCB Congeners

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt 50

Per Table C-2

Interspersed Calibration

Minimum of 4 concentrations

Calibration curve Rgt0 995

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per 20 or fewer samples

lt3 x MDL or analytes gt10 x blank

Ongoing Precision and Recovery (OPR)Standard Reference Materials

When required See Table C-2

Performance Evaluation Sample

As supplied Per Laboratory Data Validation Functional Guidelines for Environmental Analyses (99shyOIOO)

Corrective Action

NA

I As per SOP-9810 Section 3 3

1 Evaluate 2 Recalibrate when

QC criterion is not met

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 3

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Evaluate PE score report

2 Evaluate batch 3 Recommend action

102099 MK01|0 10971032001QAPPAPPC REV2 DOC

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Revision No 02 Date 1099

Page 3 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCBs and Organoshychlorme Pesticides

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt50

Per Table C-2

Interspersed Calibration

Four-point calibration for all analytes

Calibration R 20 995

Degradation Check Solution (DDT and Dieldrin)

Prior to initial calibration

Degradation of the labile chlorinated compounds in the injection port lt I5

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per each QC batch of 20 or fewer samples

lt3x MDL not more than 2 target compounds with concentrations gt3x MDL or analytes gt 10 x blank

Laboratory Blank Spike (LBS) and Laboratory Blank Spike Duplicate (LBSD)

When required 80 of the target compounds should have between 40 and 130 recoveries If the LBSD has been included the recoveries from LBS and LBSD should agree within an RPD of lt30

Corrective Action

As per SOP-9810 Section 3 3 4 2

As per SOP-9810 Section 3333

1 Evaluate 2 Recalibrate

when QC criterion is not met

1 Stop analytical run

2 Clean injection port

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 4 5 2

As per SOP-9810 Section 3 3 1

As per SOP-9810 Section 3 3

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Revision No 02 Date- 1099

Page 4 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9810 PCBs and Laboratory Laboratory When required RPD=S30 1 Recalculate or (GC-ECD) Organo-chlorme (cont ) Duplicate reanalyze the (Cont ) Pesticides duplicate and the

original sample

2 Recalibrate or re-extract the analytical QC batch

Performance As supplied Per Laboratory Data 1 Evaluate PE Evaluation Sample Validation Functional score report Standard Reference Guidelines for 2 Evaluate batch Materials Evaluating

Environmental Analyses (99-0 100)

3 Recommend action

SOP-9722 Polychlonnated Field Field Duplicate As supplied RPDlt50 1 Recalculate (HRGCshy dibenzo-p- Sampling andor reanalyze HRMS) dioxins the duplicate

polychlormated andor original dibenzofurans sample (PCDDPCDF) Compounds 2 Instrument

maintenance andor recalibration

Laboratory Matrix Spike and When required Per Table C-2 1 1 Recalculate Matrix Spike andor re-Duplicate analyze the MS

andMSD

2 Instrument maintenance andor recalibration

Initial and As per SOP-9722 As per SOP-9722 1 Evaluate Continuing Section 3 3 Section 3 3 2 Recalibrate Calibrations when QC

criterion is not met

Identification As per SOP-9722 As per SOP-9722 1 Evaluate Retention Times Section 3 2 Section 3 2 2 Rerun as Ion Abundance RatiosSignal to NoiseInterferences

SN exceeds 10 1 for all ions

Ion abundance ratio

3

necessary

Criteria must be met before

plusmn15 samples are run

Interference SN ^3

102099 MK01|0 M0971032 001OAPPAPPC-REV2 DOC

Table C-1

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 5 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9722 (HRGC-HRMS)

Polychlonnated dibenzo-p-

Laboratory (Cont )

Instrument Performance Check

As per SOPshy9722

As per SOP-9722 Section 3 1

12 Evaluate Retune instrument

(Cont ) dioxms polychlonnated

Section 3 1 3 Verify

dibenzofurans (PCDDPCDF) Compounds

Laboratory Duplicate

When required RPD S30 1 Recalculate or reanalyze the duplicate andor the original sample

2 Instrument maintenance andor recall bration

Standard Reference When required 70- 130 of the 1 Recalculate or Material (SRM) certified or consensus reanalyze the

value of the analyte SRM with no more than 13 2 Instrument of the analytes maintenance exceeding this criteria andor

recalibration

Labeled Compound All samples Recoveries within 1 Stop analytical Recovery 40- 13 5 run

2 Clean injection port

3 Rerun all affected samples

Initial Precision and Prior to any See SOP-9722 1 Evaluate Recovery (IPR) analysis by this

method Table 7 2 Repeat until

criteria are met

Ongoing Precision One per 20 or See Table C-2 1 Rerun and Recovery fewer samples 2 Evaluate batch (OPR) (Narrate)

3 If criteria are met reanalyze as necessary

Method Blank One per 20 or ltj POL 1 Rerun fewer samples 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

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Table C-1

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 6 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

102099 MK01IO 10971032 001QAPPAPPC-REV2 DOC

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Revision No 02 Date- 1099

Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

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Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

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Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

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Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

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Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

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Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

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Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

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Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

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Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

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Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

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Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

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Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

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Page 2 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCB Congeners

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt 50

Per Table C-2

Interspersed Calibration

Minimum of 4 concentrations

Calibration curve Rgt0 995

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per 20 or fewer samples

lt3 x MDL or analytes gt10 x blank

Ongoing Precision and Recovery (OPR)Standard Reference Materials

When required See Table C-2

Performance Evaluation Sample

As supplied Per Laboratory Data Validation Functional Guidelines for Environmental Analyses (99shyOIOO)

Corrective Action

NA

I As per SOP-9810 Section 3 3

1 Evaluate 2 Recalibrate when

QC criterion is not met

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 3

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Rerun 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

1 Evaluate PE score report

2 Evaluate batch 3 Recommend action

102099 MK01|0 10971032001QAPPAPPC REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 3 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCBs and Organoshychlorme Pesticides

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt50

Per Table C-2

Interspersed Calibration

Four-point calibration for all analytes

Calibration R 20 995

Degradation Check Solution (DDT and Dieldrin)

Prior to initial calibration

Degradation of the labile chlorinated compounds in the injection port lt I5

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per each QC batch of 20 or fewer samples

lt3x MDL not more than 2 target compounds with concentrations gt3x MDL or analytes gt 10 x blank

Laboratory Blank Spike (LBS) and Laboratory Blank Spike Duplicate (LBSD)

When required 80 of the target compounds should have between 40 and 130 recoveries If the LBSD has been included the recoveries from LBS and LBSD should agree within an RPD of lt30

Corrective Action

As per SOP-9810 Section 3 3 4 2

As per SOP-9810 Section 3333

1 Evaluate 2 Recalibrate

when QC criterion is not met

1 Stop analytical run

2 Clean injection port

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 4 5 2

As per SOP-9810 Section 3 3 1

As per SOP-9810 Section 3 3

102099 MK01IO M0971032 001QAPPAPPC REV2 DOC

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Revision No 02 Date- 1099

Page 4 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9810 PCBs and Laboratory Laboratory When required RPD=S30 1 Recalculate or (GC-ECD) Organo-chlorme (cont ) Duplicate reanalyze the (Cont ) Pesticides duplicate and the

original sample

2 Recalibrate or re-extract the analytical QC batch

Performance As supplied Per Laboratory Data 1 Evaluate PE Evaluation Sample Validation Functional score report Standard Reference Guidelines for 2 Evaluate batch Materials Evaluating

Environmental Analyses (99-0 100)

3 Recommend action

SOP-9722 Polychlonnated Field Field Duplicate As supplied RPDlt50 1 Recalculate (HRGCshy dibenzo-p- Sampling andor reanalyze HRMS) dioxins the duplicate

polychlormated andor original dibenzofurans sample (PCDDPCDF) Compounds 2 Instrument

maintenance andor recalibration

Laboratory Matrix Spike and When required Per Table C-2 1 1 Recalculate Matrix Spike andor re-Duplicate analyze the MS

andMSD

2 Instrument maintenance andor recalibration

Initial and As per SOP-9722 As per SOP-9722 1 Evaluate Continuing Section 3 3 Section 3 3 2 Recalibrate Calibrations when QC

criterion is not met

Identification As per SOP-9722 As per SOP-9722 1 Evaluate Retention Times Section 3 2 Section 3 2 2 Rerun as Ion Abundance RatiosSignal to NoiseInterferences

SN exceeds 10 1 for all ions

Ion abundance ratio

3

necessary

Criteria must be met before

plusmn15 samples are run

Interference SN ^3

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Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 5 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9722 (HRGC-HRMS)

Polychlonnated dibenzo-p-

Laboratory (Cont )

Instrument Performance Check

As per SOPshy9722

As per SOP-9722 Section 3 1

12 Evaluate Retune instrument

(Cont ) dioxms polychlonnated

Section 3 1 3 Verify

dibenzofurans (PCDDPCDF) Compounds

Laboratory Duplicate

When required RPD S30 1 Recalculate or reanalyze the duplicate andor the original sample

2 Instrument maintenance andor recall bration

Standard Reference When required 70- 130 of the 1 Recalculate or Material (SRM) certified or consensus reanalyze the

value of the analyte SRM with no more than 13 2 Instrument of the analytes maintenance exceeding this criteria andor

recalibration

Labeled Compound All samples Recoveries within 1 Stop analytical Recovery 40- 13 5 run

2 Clean injection port

3 Rerun all affected samples

Initial Precision and Prior to any See SOP-9722 1 Evaluate Recovery (IPR) analysis by this

method Table 7 2 Repeat until

criteria are met

Ongoing Precision One per 20 or See Table C-2 1 Rerun and Recovery fewer samples 2 Evaluate batch (OPR) (Narrate)

3 If criteria are met reanalyze as necessary

Method Blank One per 20 or ltj POL 1 Rerun fewer samples 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

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Page 6 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

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Revision No 02 Date- 1099

Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

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Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

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Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

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Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

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Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

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Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

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Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

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Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

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Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

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Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

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Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

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Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

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Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

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Page 3 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP Reference) Parameter

FieldLab Req

Quality Control Check Frequency

Acceptance Criteria

SOP-9810 (GC-ECD)

PCBs and Organoshychlorme Pesticides

Field Sampling

Laboratory

Field Duplicate

Matrix Spike and Matrix Spike Duplicate

As supplied

When required

RPD lt50

Per Table C-2

Interspersed Calibration

Four-point calibration for all analytes

Calibration R 20 995

Degradation Check Solution (DDT and Dieldrin)

Prior to initial calibration

Degradation of the labile chlorinated compounds in the injection port lt I5

Retention Time Window

Each calibration standard

plusmn4 sec for each analyte retention calibration standard

Surrogate Every sample Per Table C-3

Method Blank One per each QC batch of 20 or fewer samples

lt3x MDL not more than 2 target compounds with concentrations gt3x MDL or analytes gt 10 x blank

Laboratory Blank Spike (LBS) and Laboratory Blank Spike Duplicate (LBSD)

When required 80 of the target compounds should have between 40 and 130 recoveries If the LBSD has been included the recoveries from LBS and LBSD should agree within an RPD of lt30

Corrective Action

As per SOP-9810 Section 3 3 4 2

As per SOP-9810 Section 3333

1 Evaluate 2 Recalibrate

when QC criterion is not met

1 Stop analytical run

2 Clean injection port

1 Evaluate 2 Reanalyze all

samples analyzed since the last retention time check

As per SOP-9810 Section 3 4 5 2

As per SOP-9810 Section 3 3 1

As per SOP-9810 Section 3 3

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Page 4 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9810 PCBs and Laboratory Laboratory When required RPD=S30 1 Recalculate or (GC-ECD) Organo-chlorme (cont ) Duplicate reanalyze the (Cont ) Pesticides duplicate and the

original sample

2 Recalibrate or re-extract the analytical QC batch

Performance As supplied Per Laboratory Data 1 Evaluate PE Evaluation Sample Validation Functional score report Standard Reference Guidelines for 2 Evaluate batch Materials Evaluating

Environmental Analyses (99-0 100)

3 Recommend action

SOP-9722 Polychlonnated Field Field Duplicate As supplied RPDlt50 1 Recalculate (HRGCshy dibenzo-p- Sampling andor reanalyze HRMS) dioxins the duplicate

polychlormated andor original dibenzofurans sample (PCDDPCDF) Compounds 2 Instrument

maintenance andor recalibration

Laboratory Matrix Spike and When required Per Table C-2 1 1 Recalculate Matrix Spike andor re-Duplicate analyze the MS

andMSD

2 Instrument maintenance andor recalibration

Initial and As per SOP-9722 As per SOP-9722 1 Evaluate Continuing Section 3 3 Section 3 3 2 Recalibrate Calibrations when QC

criterion is not met

Identification As per SOP-9722 As per SOP-9722 1 Evaluate Retention Times Section 3 2 Section 3 2 2 Rerun as Ion Abundance RatiosSignal to NoiseInterferences

SN exceeds 10 1 for all ions

Ion abundance ratio

3

necessary

Criteria must be met before

plusmn15 samples are run

Interference SN ^3

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Table C-1

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 5 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9722 (HRGC-HRMS)

Polychlonnated dibenzo-p-

Laboratory (Cont )

Instrument Performance Check

As per SOPshy9722

As per SOP-9722 Section 3 1

12 Evaluate Retune instrument

(Cont ) dioxms polychlonnated

Section 3 1 3 Verify

dibenzofurans (PCDDPCDF) Compounds

Laboratory Duplicate

When required RPD S30 1 Recalculate or reanalyze the duplicate andor the original sample

2 Instrument maintenance andor recall bration

Standard Reference When required 70- 130 of the 1 Recalculate or Material (SRM) certified or consensus reanalyze the

value of the analyte SRM with no more than 13 2 Instrument of the analytes maintenance exceeding this criteria andor

recalibration

Labeled Compound All samples Recoveries within 1 Stop analytical Recovery 40- 13 5 run

2 Clean injection port

3 Rerun all affected samples

Initial Precision and Prior to any See SOP-9722 1 Evaluate Recovery (IPR) analysis by this

method Table 7 2 Repeat until

criteria are met

Ongoing Precision One per 20 or See Table C-2 1 Rerun and Recovery fewer samples 2 Evaluate batch (OPR) (Narrate)

3 If criteria are met reanalyze as necessary

Method Blank One per 20 or ltj POL 1 Rerun fewer samples 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

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Revision No 02 Date 1099

Page 6 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

102099 MK01IO 10971032 001QAPPAPPC-REV2 DOC

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Revision No 02 Date- 1099

Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

DACW33-94-D-0009 GEP2-060499-AAIY

Revision No 02 Date 1099

Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

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Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102799

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Revision No 02 Date 1099

Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

MK01|O M0971032 001QAPPAPPC-REV2 DOC 102699

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Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

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Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

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Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

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Revision No 02 Date- 1099

Page 4 of 19

Table C-1

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9810 PCBs and Laboratory Laboratory When required RPD=S30 1 Recalculate or (GC-ECD) Organo-chlorme (cont ) Duplicate reanalyze the (Cont ) Pesticides duplicate and the

original sample

2 Recalibrate or re-extract the analytical QC batch

Performance As supplied Per Laboratory Data 1 Evaluate PE Evaluation Sample Validation Functional score report Standard Reference Guidelines for 2 Evaluate batch Materials Evaluating

Environmental Analyses (99-0 100)

3 Recommend action

SOP-9722 Polychlonnated Field Field Duplicate As supplied RPDlt50 1 Recalculate (HRGCshy dibenzo-p- Sampling andor reanalyze HRMS) dioxins the duplicate

polychlormated andor original dibenzofurans sample (PCDDPCDF) Compounds 2 Instrument

maintenance andor recalibration

Laboratory Matrix Spike and When required Per Table C-2 1 1 Recalculate Matrix Spike andor re-Duplicate analyze the MS

andMSD

2 Instrument maintenance andor recalibration

Initial and As per SOP-9722 As per SOP-9722 1 Evaluate Continuing Section 3 3 Section 3 3 2 Recalibrate Calibrations when QC

criterion is not met

Identification As per SOP-9722 As per SOP-9722 1 Evaluate Retention Times Section 3 2 Section 3 2 2 Rerun as Ion Abundance RatiosSignal to NoiseInterferences

SN exceeds 10 1 for all ions

Ion abundance ratio

3

necessary

Criteria must be met before

plusmn15 samples are run

Interference SN ^3

102099 MK01|0 M0971032 001OAPPAPPC-REV2 DOC

Table C-1

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 5 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9722 (HRGC-HRMS)

Polychlonnated dibenzo-p-

Laboratory (Cont )

Instrument Performance Check

As per SOPshy9722

As per SOP-9722 Section 3 1

12 Evaluate Retune instrument

(Cont ) dioxms polychlonnated

Section 3 1 3 Verify

dibenzofurans (PCDDPCDF) Compounds

Laboratory Duplicate

When required RPD S30 1 Recalculate or reanalyze the duplicate andor the original sample

2 Instrument maintenance andor recall bration

Standard Reference When required 70- 130 of the 1 Recalculate or Material (SRM) certified or consensus reanalyze the

value of the analyte SRM with no more than 13 2 Instrument of the analytes maintenance exceeding this criteria andor

recalibration

Labeled Compound All samples Recoveries within 1 Stop analytical Recovery 40- 13 5 run

2 Clean injection port

3 Rerun all affected samples

Initial Precision and Prior to any See SOP-9722 1 Evaluate Recovery (IPR) analysis by this

method Table 7 2 Repeat until

criteria are met

Ongoing Precision One per 20 or See Table C-2 1 Rerun and Recovery fewer samples 2 Evaluate batch (OPR) (Narrate)

3 If criteria are met reanalyze as necessary

Method Blank One per 20 or ltj POL 1 Rerun fewer samples 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

102099 MK01IO 10971032 001QAPPAPPC REV2 DOC

Table C-1

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 6 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

102099 MK01IO 10971032 001QAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

DACW33-94-D-0009 GEP2-060499-AAIY

Revision No 02 Date 1099

Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

MK01|0 10971032001QAPPAPPC REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102799

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

MK01|O M0971032 001QAPPAPPC-REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

MK01|O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Table C-1

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 5 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method

(SOP FieldLab Quality Control Acceptance Criteria Reference) Parameter Req Check Frequency Corrective Action

SOP-9722 (HRGC-HRMS)

Polychlonnated dibenzo-p-

Laboratory (Cont )

Instrument Performance Check

As per SOPshy9722

As per SOP-9722 Section 3 1

12 Evaluate Retune instrument

(Cont ) dioxms polychlonnated

Section 3 1 3 Verify

dibenzofurans (PCDDPCDF) Compounds

Laboratory Duplicate

When required RPD S30 1 Recalculate or reanalyze the duplicate andor the original sample

2 Instrument maintenance andor recall bration

Standard Reference When required 70- 130 of the 1 Recalculate or Material (SRM) certified or consensus reanalyze the

value of the analyte SRM with no more than 13 2 Instrument of the analytes maintenance exceeding this criteria andor

recalibration

Labeled Compound All samples Recoveries within 1 Stop analytical Recovery 40- 13 5 run

2 Clean injection port

3 Rerun all affected samples

Initial Precision and Prior to any See SOP-9722 1 Evaluate Recovery (IPR) analysis by this

method Table 7 2 Repeat until

criteria are met

Ongoing Precision One per 20 or See Table C-2 1 Rerun and Recovery fewer samples 2 Evaluate batch (OPR) (Narrate)

3 If criteria are met reanalyze as necessary

Method Blank One per 20 or ltj POL 1 Rerun fewer samples 2 Evaluate batch

(Narrate) 3 Re-extract as

necessary

102099 MK01IO 10971032 001QAPPAPPC REV2 DOC

Table C-1

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 6 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

102099 MK01IO 10971032 001QAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

DACW33-94-D-0009 GEP2-060499-AAIY

Revision No 02 Date 1099

Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

MK01|0 10971032001QAPPAPPC REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102799

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Revision No 02 Date 1099

Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

MK01|O M0971032 001QAPPAPPC-REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

MK01|O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Table C-1

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 6 of 19

Analytical Measurements Quality Control Requirements (Table 4-2 Addendum Continued)

Analysis Method (SOP FieldLab Quality Control Acceptance

Reference) Parameter Req Check Frequency Criteria Corrective Action

SOP-9722 Polychlonnated Laboratory Laboratory Blank As required 70- 130 recoveries 1 Recalculate (HRGC-HRMS) dibenzo-pshy (Cont ) Spike (LBS) of the spiked amount andor reanalyze (Cont ) dioxins the LBS

polychlormated 2 Instrument dibenzofurans maintenance (PCDDPCDF) andor Compounds recalibaration and

re-extraction of the analytical batch

Performance As supplied Per Laboratory Data 1 Evaluate PE score Evaluation Sample Validation Functional report

Guidelines for 2 Evaluate batch Evaluating Environmental Analyses (99-0 100)

3 Recommend action

102099 MK01IO 10971032 001QAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

DACW33-94-D-0009 GEP2-060499-AAIY

Revision No 02 Date 1099

Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

MK01|0 10971032001QAPPAPPC REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102799

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

MK01|O M0971032 001QAPPAPPC-REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

MK01|O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 7 of 19 Table C-2

Spike Accuracy and Precision Limits (Table 4-3 Addendum)

Fraction

Chlorinated Pesticides

PCB Congeners

Spike Compound

1 245-tetrachlorobenzene

1 234-tetrachlorobenzene

penlachlorobenzene

hexachlorobenzene

pentachloroanisole

alpha-HCH

Aew-HCH

delta-HCH

gamma-HCH (lindane)

heptachlor

heptachlor epoxide

apM-chlordane

gamma-chlordane

oxychlordane

cij-nonachlor

trans-nonacMor

24-DDE

44-DDE

24-DDD

44-DDD

24-DDT

44-DDT

aldnn

dieldrm

endosulfan II

endnn

mirex

PCB-8V5

PCB-1817

PCB-28

PCB-29

PCB-44

PCB-52

Tissue (MSMSD)

Recovery RPD

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

40-130 30

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

DACW33-94-D-0009 GEP2-060499-AAIY

Revision No 02 Date 1099

Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

MK01|0 10971032001QAPPAPPC REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102799

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

MK01|O M0971032 001QAPPAPPC-REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

MK01|O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Fraction

PCB Congeners (continued)

Contract NoDON

Table C-2

Spike Accuracy and Precision Limits

DACW33-94-D-0009 GEP2-060499-AAIY

Revision No 02 Date 1099

Page 8 of 19

(Table 4-3 Addendum

Spike Compound

PCB-66

PCB-87ll5

PCB-IOl90

PCB-105

PCB-HOV77

PCB-H8

PCB-128

PCB-138VI60

PCB-153V132

PCB-170190

PCB-180

PCB-187

PCB-195-208

PCB-201157173

PCB-206

PCB-209

Continued)

Tissue (MSMSD)

Recovery

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

40-130

RPD

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

30

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

MK01|0 10971032001QAPPAPPC REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102799

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

MK01|O M0971032 001QAPPAPPC-REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

MK01|O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 9 of 19

Table C-21

Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)

Tissue (MSMSD) Tissue (OPR)

Fraction Spike Compound Recovery RPD Concentration pguL

PCDDsPCDFs 2378-TCDD 40-130 30 67-158

12378-PeCDD 40-130 30 35-71

123478-HxCDD 40-130 30 35-82

123678-HxCDD 40-130 30 38-67

1237-89-HxCDD 40-130 30 32-81

1234678-HpCDD 40-130 30 35-70

OCDD 40-130 30 78-144

2378-TCDF 40-130 30 75-158

12378-PeCDF 40-130 30 40-67

23478-HxCDF 40-130 30 34-80

123478-HxCDF 40-130 30 36-67

123678-HxCDF 40-130 30 42-65

234678-HxCDF 40-130 30 35-78

123789-HxCDF 40-130 30 39-65

1234678-HpCDF 40-130 30 41-61

1234789-HpCDF 40-130 30 39-69

OCDF 40-130 30 63-170

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102799

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

MK01|O M0971032 001QAPPAPPC-REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

MK01|O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 10 of 19

Table C-3

Surrogate Spike and Labeled Compound Spike Solution Recovery Limits

Fraction

PCB Congeners amp Pesticides

DioxinFuran

(Table 4-4 Addendum)

Surrogate Compound

PCB- 103

DBOFB l3C12-2378-TCDD nC2-2378-TCDF

3C2-l2378-PeCDD

3C12-l2378-PeCDF

3C2-23478-PeCDF

3C12-l23478-HxCDD

3C2-l23678-HxCDD 13C2-l23478-HxCDF 13C2-l23678-HxCDF

3C12-l23789-HxCDF 13C2-234678-HxCDF 13Cl2-l234678-HpCDD 13C|2-l234678-HpCDF

3C|2-1234789-HpCDF 13CI2-OCDD

Tissue Recovery

40-120

40-120

25-164

24-169

25-181

24-185

21-178

32-141

28-130

26-152

26-123

29-147

28-136

23-140

28-143

26-138

17-157

MK01|O M0971032 001QAPPAPPC-REV2 DOC 102699

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

MK01|O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 11 of 19

Table C-4

Valid Value List for Analysis Method (Table 5-4 Addendum)

Analytical Code Description Matrix

EPA1668TI PCB Congeners (GC-ECD) Tissue

SW8081TI Organochlorine Pesticides (GC-ECD) Tissue

SW8082TI PCBs (GC-ECD) Tissue

SW8290TI PCDDPCDF - High Res (HRGC- Tissue HRMS)

MK01|O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON- GEP2-060499-AAIY

Revision No 02 Date 1099

Page 12 of 19

Table C-5

Required Containers Preservation Techniques and Holding Times for Tissue Samples

(Table 6-1 Addendum)

Analytical Reference Maximum

(SOP Sample Holding Parameter Reference) Sample Container Volume Preservation Time

PCB Congeners SOP-9810 Aluminum foil metal Approximately -20 degC 2 years glass 200 g of

Organochlorme PesticidesPCBs SOP-9810 sample for all analyses

DioxmsFurans (PCDDsPCDFs) SOP-9722

Matrices consist of whole fish fish filets amphibians (frogs) turtles water fowl small mammals andor earthworms

Archives of Environmental Contamination and Toxicology 1990 19748-781 (fish tissue analyzed over approximately a 2-year period with no changes in concentrations)

MK01|O 1097103200nQAPPAPPC-REV2 DOC

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date- 1099

Page 13 of 19

Table C-6

Appendix IX Pesticide Compound Reporting Limits (SOP-9810) (Table 7-6 Addendum)

Analytical Parameter CAS Number

1 2 34-tetrachloro benzene 95-94-3

1 245-tetrachloro benzene 634-66-2

24-DDElaquo 3424-82-6

24-DDD 53-19-0

24-DDTraquo 789-02-6

44-DDD 72-54-8

44-DDE 72-55-9

44 -DDT 50-29-3

Aldnn 309-00-2

alpha-BHC 319-84-6

alpha-chlordane 56534-02-2

beta-BHC 319-85-7

Chlorpynfos 2921-88-2

cis-nonachlor 129303-29-3

dclta-BHC 319-86-8

Dieldrm 60-57-1

Endosulfan I 959-98-8

Endosuifan II 33213-65-9

Endnn 72-20-8

gamma-BHC (Lmdane) 58-89-9

gamma-chlordane 5566-34-7

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene 118-74-1

Mirex 2385-85-5

Oxychlordane 27304-13-8

Pentachloroanisole 1825-21-4

Penlachloro benzene 608-93-5

trans-nonachlor 39765-80-5

Toxaphene 8001-35-2

Target analytes included in the calibration mixtures

bull Tissue reporting limits are based on a 10-gram initial sample weight

Tissue Reporting Limit

(ppb)

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

10

MK0110 M 0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 14 of 19 Table C-7

PCB Compound Reporting Limits (SOP-9810) (Table 7-7 Addendum)

Tissue Reporting Limit

Analytical Parameter CAS Number (ppb)

PCB-Aroclor 1 242 53469-2 1 -9 50

PCB-Aroclor 1 248 1 2672-29-6 50

PCB-Aroclor 1 254 H097-69-1 50

PCB-Aroclor 1 260 1 1 096-82-5 50

Total PCBs 1 336-36-3 50

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|O M0971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 15 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum)

Tissue CAS Number Reporting Limits (ppb)

PCB-1 001

PCB-79 001

PCB-85 001

PCB- 15 001

PCB- 1632 001

PCB-1817 001

PCB-2251 001

PCB-2427 001

PCB-25 001

PCB-26 001

PCB-28 001

PCB-29 001

PCB-30 001

PCB-31 001

PCB-3320 001

PCB-39 001

PCB-40 001

PCB-4164 001

PCB-425937 001

PCB-44 001

PCB-45 001

PCB-46 001

PCB-4775 001

PCB-48 001

PCB-49 001

PCB-52 001

PCB-53 001

MK01 |O 10971032 001 QAPPAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 16 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB-6056

PCB-63

PCB-66

PCB-67

PCB-69

PCB-70

PCB-72

PCB-7461

PCB-77

PCB-81

PCB-82

PCB-83

PCB-84

PCB-85

PCB-87115

PCB-9155

PCB-92

PCB-9580

PCB-97

PCB-99

PCB-10190

PCB-105

PCB- 107

PCB- 11 0777

PCB- 114

PCB- 11 8

PCB-119

PCB- 126

PCB- 128

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01|OM0971032001aAPPAPPC-REV2DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DCN GEP2-060499-AAIY

Revision No 02 Date 1099

Page 17 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 1 29

PCB-130

PCB-135

PCB-136

PCB-138160

PCB-141179

PCB- 146

PCB- 1491 23

PCB-151

PCB-153132

PCB-156

PCB-158

PCB- 166

PCB- 167

PCB- 169

PCB-170V190

PCB- 17 1202

PCB- 172

PCB- 174

PCB- 175

PCB- 1761 37

PCB- 177

PCB- 178

PCB- 180

PCB- 183

PCB- 185

PCB- 187

PCB- 189

PCB-191

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

001

MK01IO 10971032 001 QAPPAPPC-REV2 DOC 1 MO99

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 18 of 19 Table C-8

PCB CongenerHomologue Reporting Limits (SOP-9304) (Table 7-8 Addendum Continued)

CAS Number

PCB- 193

PCB- 194

PCB-195V208

PCB- 197

PCB- 199

PCB-200

PCB-201V157173

PCB-203196

PCB-205

PCB-206

PCB-207

PCB-209

Total monochlorobiphenyl

Total dichlorobiphenyl

Total trichlorobiphenyl

Total pentachlorobiphenyl

Total hexachlorobiphenyl

Total heptachlorobiphenyl

Total octachlorobiphenyl

Total nonachlorobipenyl

Tissue Reporting Limits (ppb)

001

001

001

001

001

001

001

001

001

001

001

001

10

10

10

10

10

10

10

10

Target analytes included in the calibration mixtures Indicates co-eluting congeners on a DB-5 column The order of co-eluting congeners is given according to their relative contribution in common Aroclor mixtures

Tissue reporting limits are based on a 10-gram initial sample weight

MK01|0 VI0971032 001VQAPPWPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099

Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY

Revision No 02 Date 1099

Page 19 of 19 Table C-9

PCDDPCDF Compound Reporting Limits (SOP-9722) (Table 7-11 Addendum)

Analytical Parameter

2378-TCDD 1746-01-6 1 5 5

5 5 5 10 1 5 5 5

5 5 5 5 5 10

12378-PeCDD 40321-76-4

123678-HxCDD 57653-85-7

123478-HxCDD 39227-28-6 123789-HxCDD 19408-74-3 1234678-HpCDD 35822-46-9

12346789-OCDD 3268-87-9 2378-TCDF 51207-31-9

12378-PeCDF 57117-41-6 23478-PeCDF 57117-31-4

123678-HxCDF 57117-44-9

123789-HxCDF 72918-21-9

123478-HxCDF 70648-26-9 234678-HxCDF 60851-34-5

1234678-HpCDF 67562-39-4 1234789-HpCDF 55673-89-7

12346789-OCDF 39001-02-0

Tissue Reporting Limit

CAS Number (ppt)

Tissue reporting l imits are based on a 10-gram initial sample weight

MK01|0 10971032 OOHQAPPVAPPC-REV2 DOC 102099