Roy F. Weston, Inc. 2 1 1400 Weston Way PO. Box 2653 West Chester, Pennsylvania 19380 610-701-3000 • Fax 610-701-31 86 www.rfweston.com 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 III. Roy F. Weston, Inc. (WESTON®) 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 WESTON's 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 1/1 o H. Inglis, EPA ui DCN File -B.Gorman o o DCN File-D. Veilleux LdP/wp Enclosure o o o LJ M O
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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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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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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
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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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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)
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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
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
Tissue reporting l imits are based on a 10-gram initial sample weight
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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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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
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)
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
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
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
TABLE OF CONTENTS
C QAPP ADDENDUM FOR TISSUE ANALYSES
CI INTRODUCTION
C2 PROJECT DATA QUALITY OBJECTIVES
MK01|0 M0971032 001QAPPAPPC-REV2 DOC 102099
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
Revision No 02 Date 1099
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
MK01|O M0971032 OOHQAPPAPPC-REV2 DOC 102099
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
Revision No 02 Date 1099
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)
MK01|0 M0971032 OOUQAPPVAPPC-REVZ DOC 102099
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
Revision No 02 Date-1099
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
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
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
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Page 9 of 19
Table C-21
Spike Accuracy and Precision LimitsmdashPCDDsPCDFs (Table 4-3 Addendum - Continued)
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
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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
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
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
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
MK01|O M0971032 OOHQAPPAPPC-REV2 DOC 102099
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
Revision No 02 Date 1099
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)
MK01|0 M0971032 OOUQAPPVAPPC-REVZ DOC 102099
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
Revision No 02 Date-1099
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
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
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)
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
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
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 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)
MK01|0 M0971032 OOUQAPPVAPPC-REVZ DOC 102099
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
Revision No 02 Date-1099
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
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
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)
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
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
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 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
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
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)
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
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
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 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
Contract No DACW33-94-D-0009 DON GEP2-060499-AAIY
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)
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
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
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 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)
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
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
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)
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
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
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)
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
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
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)
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
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
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)
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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