INTERIM REPORT 3 - ANALYSIS OF FISH AND CLAM SAMPLES IInterim Report #3 -Analysis of Fish and Clam...

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INTERIM REPORT 3 - ANALYSIS OF FISH AND CLAM SAMPLES

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INTERIM REPORT #3- Analysis of Fish and Clam Samples

STUDY TITLE Analysis ofPeriluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, and Clams Using LC!MSIMS for the 3M Decatur Monitoring Program

DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792

STUDY DIRECTOR Jaisimha Kesari P.E., DEE

Weston Solutions, Inc. 1400 Weston Way

West Chester, PA 19380 Phone: 610-701-3761

INTERIM REPORT COMPLETION DATE June 17.2008

TESTING FACILITY MPI Research, Inc.

3058 Research Drive State Col1ege, PA 16801

Phone: 814-272-1039

STUDY SPONSOR 3M Company

3M Building 0236-01-B-10 St. Paul, MN 55144

Phone:651-733-6374

PROJECT MPI Research Study Number: 0137.0219

MPI Project Number: P0003267

Total Pages: 151

Interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0137.0219 MPI Project No.: P0003267

GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT

MPI Project Number P0003267, entitled "Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, and Clams Using LCIM:S/MS for the 3M Decatur Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by MPI Research, Inc.

Principal Investigator MPI Research, Inc.

Jaisimha Kesari P.E., DEE Study Director Weston Solutions, Inc.

Michael A. Santo Sponsor Repres ntative 3M Company

MPl Research

Date

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Interim Report #3- Analysis of Fish and Clam Samples MPI Study No.: 0137.0219 MPT Project No.: P0003267

QUALITY ASSURANCE STATEMENT

MPl Research's Quality Assurance Unit reviewed MPI Project Number P0003267, entitled, "Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Decatur Monitoring Program". All reviewed phases1 were inspected for conduct according to MPI Research's Standard Operating Procedures, the Study Protocol, the Study Method, and all applicable Good Laboratory Practice Standards. All findings were reported to the MPI Principal Investigator, Management and to the Study Director.

Raw Data, Protocol Amendments 5-8, and Draft Report Review

Final Interim Report Review

Date Inspected

05/27-29/08

06/04/08

Date Reported to Date Reported to Principal MPI

Investigator Management

05/29/08 05/29/08

06/04/08 06/04/08

Date Reported to Study Director

05/29/08

06/04/08

c£~ a. ~-Gn JU:i:) i.tJ -tl-0 8 Lynann Porter Date Quality Assurance Research Group Leader, Quality Assurance Unit

1Note: All in·lab inspections and the protocol review will be docwnented in the QA statement for the final analytical report at the conclusion of the study. This QA statement involves only the review of the interim report and associated raw data.

MPI Research Page 3 of.l51


CERTIFICATION OF AUTHENTICITY

This interim report, for MPI Project Number P0003267, is a true and complete representation of the raw data.

Submitted by: MPI Research, Inc. 305 8 Research Drive State College, PA 16801 (814) 272-1039

Director, Analyti Laboratory Operations MPJ Research, Inc.

Jaisimha esari P.E., DEE Weston Solutions, Inc.

Sponsor Representative, 3M Company:

toro Director of ~ gulatory Affairs 3M Company

MPI Research

obl n]o8 Date

Dat~#

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Interim Report #3 - Analysis of Fish and Clam Samples MPI Study No.: 0137.0219 MPI Project No.: P0003267

STUDY IDENTIFICATION

Analysis ofPerfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Decatur Monitoring Program

MPI PROJECT NUMBER:

MPI STUDY NUMBER:

TYPE Of STUDY:

SAMPLE MATRJX:

TEST SUBSTANCES:

SPONSOR:

STUDY DIRECTOR:

SPONSOR REPRESENTATIVE:

TESTING FACILITY:

ANALYTICAL PHASE TIMETABLE:

MPI Research

P0003267

0137.0219

Residue

Fish and Clam

Perfluorooctanoic Acid (PFOA)

3M Company 3M Building 0236-0 1-B-l 0 St. Paul, MN 55144

Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380

Michael A. Santoro 3M Company 3M Building0236-0I-B-10 St. Paul, MN 55144

MPI Research, Inc. 3058 Research Drive State College, PA 16801

Study Initiation Date: 06/14/07 Interim Analytical Start Date: 12/27/07 Interim Analytical Termination Date: 05/12/08 lnterirn Report Completion Date: 06/17/08

PageS of 151

Interim Report #3- Analysis ofFish and Clam Samples MPI Study No.: 0137.0219 MPI Project No.: P0003267

PROJECT PERSONNEL

The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc. The

following personnel from MPI Research, Inc. were associated with various phases of this

interim portion of the study:

Karen Risha Manager Analytical, Principal Investigator

Amy Sheehan Group Leader, LC/MS/MS Analysis

Christine Edwards Project Leader, LC/MS/MS Analysis

Krista Gallant Research Chemist Associate 2

Mark Neeley Research Chemist Associate 2

Gary Oden Research Chemist Associate 2

Ellen Dasbem Research Chemist Associate 1

Stacey Orso Research Chemist Associate 1

Nancy Saxton Research Chemist Associate 1

Mark Ammerman Project Leader, Sample Control

Eric Edwards Sample Custodian 2

MPl Research Page 6 of 151

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Interim Report #3- Analysis offish and Clam Samples

TABLE OF CONTENTS

MPI Study No.: 0137.0219 MPI Project No.: P0003267

TITLE PAG£ ....................................................................................................................... 1 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT .............................. 2 QUALITY ASSURANCE STATEMENT .......................................................................... 3 CERTIFICATION OF AUTHENTICITY ........................................................................... 4 STUDY IDENTIFICATION ............................................................................................... 5 PROJECT PERSONNEL .................................................................................................... 6 TABLE OF CONTENTS .................................................................................................... 7 LIST OF TABLES ............................................................................................................... & LIST OF FIGURES ............................................................................................................. 9 LIST OF APPENDICES .................................................................................................... 11 1.0 SUMMARY ................................................................................................................ 12 2.0 OBJECTIVE ............................................................................................................... 13 . 3.0 INTRODUCTION ...................................................................................................... 13 4.0 ANALYTICAL TEST SAMPLES ............................................................................. 13 5.0 REFERENCE MATERIAL ........................................................................................ 14 6.0 DESCRIPTION OF ANALYTICAL METHOD ........................................................ IS 6.1 Extraction Procedure for Fish and Clams ............................................................... 15 6.1.1 Smnple Preparation ........................................................................................ 15 6.1.2 Smnple Extraction .......................................................................................... 15 6.2 Preparation of Standards and Fortification Solutions ............................................. 16 6.3 Chromatography ...................................................................................................... l7 6.4 lnstrwnent Sensitivity .............................................................................................. IS 6.5 Description of LCIMS/MS Instruments and Operating Conditions ........................ 18 6.6 Quantitation and Example Calculation ................................................................... 19 7.0 EXPERIMENTAL DESIGN ...................................................................................... 20 8.0 RESUL T$ ................................................................................................................... 21 9.0 CONCLUSION ........................................................................................................... 22 10.0 RETENTION OF DATA AND SAMPLES ............................................................. 22

MPI Research Page 7 of15l

Interim Report #3- Analysis ofFish and Clam Samples

LIST OF TABLES


Table I. Summary ofPFOA in Fish Fillet Samples ..................................................... 24

Table 11. Summary ofPFOA in Re..extracted Fish Fillet Samples ................................ 27

Table ill. Summary of PFOA in Whole Body Fish Samples ......................................... 28

Table IV. Summary of PFOA in Re-extracted Whole Body Fish Samples .................... 31

Table V. Summary ofPFOA in Clam Samples ............................................................. 32

Table VI. Matrix Spike Recovery Summary of PFOA in Fish Fillet Samples ............... 33

Table VII. Matrix Spike Recovery Summary ofPFOA in Re-extracted Fish Fillet Samples .......................................................................................................... 38

Table Vlll. Matrix Spike Recovery Summary ofPFOA in Whole Body Fish Samples ... 39

Table IX. Matrix Spike Recovery Summary ofPFOA in Re-extracted Whole Body Fish

Samples .......................................................................................................... 44

Table X. Matrix Spike Recovery Summary ofPFOA in Clam Samples ..................... .45

MPI Research Page 8 of 151

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Interim Report #-3 - Analysis of Fish and Clam Samples

LIST OF FIGURES

MPJ Study No.: 0137.0219 MPI Project No.: P0003267

Figure 1. Typical Extracted Calibration Curve for PFOA in Catfish Fillet Matrix ...... .4 7 Figure 2. Extracted Standards of PFOA in Catfish Fillet Matrix, 0.025 ng/mL (0.1 0

ngfg) and 0.050 ng/mL (0.20 nglg), Respectively ........................................ ..4& Figure 3. PFOA in a Control Cartlsh Fillet, a 0.075 ng/mL (0.30 ng/g) Fortified Catfish

Fillet Spike A, a 0.50 ng/mL (2.0 ng/g) Fortified Catfish Fillet Spike B, and a 4.0 nglmL ( 16 ng/g) Fortified Catfish Fillet Spike C, Respectively ............. .49

Figure 4. Chromatogram Representing a Catfish Fillet Sample Analyzed for PFOA (ExyLIMS ID: C0227553, Data Set: 011108C) ............................................. 50

Figure 5. Typical Extracted Calibration Curve for PFOA in Bass Fillet Matrix ........... 51 Figure 6. Extracted Standards of PFOA in Bass Fillet Matrix, 0.025 nglmL (0.1 0 ng/g)

and 0.050 ng/mL (0.20 ng/g), Respectively ................................................... 52 Figure 7. PFOA in a Control Bass Fi11et, a 0.075 ng/mL (0.30 ng/g) Fortified Bass

Fillet Spike A, a 0.50 ng/mL (2.0 nglg) Fortified Bass Fillet Spike B, and a 4.0 ng/mL (16 ng/g) Fortified Bass Fillet Spike C, Respectively ................... 53

Figure 8. Chromatogram Representing a Bass Fillet Sample Analyzed for PFOA (ExyLIMS ID: C0227581, Data Set: 01 0308C) ............................................. 54

figure 9. Typical Extracted Calibration Curve for PFOA in Whole Body Catfish Matrix , ....................................................................................................................... 55

Figure 10. Extracted Standards ofPFOA in Whole Body Catfish Matrix, 0.025 ng/mL (0.1 0 nglg) and 0.050 nglmL (0.20 nglg), Respectively ................................. 56

Figure 11. PFOA in a Control Whole Body Catfish, a 0.075 ng/mL (0.30 ng/g) Fortified Whole Body Catfish Spike A, a 0.50 nglmL (2.0 ng/g) Fortified Whole Body Catfish Spike B, and a 4.0 ng!mL (16 nglg) Fortified Whole Body Catfish Spike C, Respectively ..................................................................................... 57

Figure 12. Chromatogram Representing a Whole Body Catfish Sample Analyzed for PFOA (ExyLIMS ID: C0227606, Data Set: 0321 08A) .................................. 58

Figure 13. Typical Extracted Calibration Curve for PFOA in Whole Body Bass Matrix ..... , ....................................................................................................... 59

Figure 14. Extracted Standards of PFOA in Whole Body Bass Matrix. 0.01 nglmL (0.1 0 ng/ g} and 0.02 ng/mL (0.20 ng/g), Respectively ............................................ 60

Figure 15. PFOA in a Control Whole Body Bass, a 0.03 ng/mL (0.30 nglg) Fortified Whole Body Bass Spike A, a 0.2 nglmL (2.0 ng/g) Fortified Whole Body Bass Spike B, and a 4.0 nglmL (40 nglg) Fortified Whole Body Bass Spike C, Respectively ................................................................................................... 6l



LIST OF FIGURES (Continued}

Figure 16. Chromatogram Representing a Whole Body Bass Sample Analyzed for PFOA (ExyLIMS ID: C0227637, Data Set: 042408B) ............................................. 62

Figure 17. Typical Extracted Calibration Curve for PFOA in Clam Matrix ................... 63

Figure 18. Extracted Standards ofPFOA in Clam Matrix, 0.025 ng/mL (0.10 nglg) and 0.050 ng/mL (0.20 ng/g). Respectively .......................................................... 64

Figure 19. PFOA in a Control Cl~ a 0.075 ng/mL (0.30 ng/g) Fortified Clam Spike A, a 0.50 ng/mL (2.0 ng/g) Fortified Clam Spike B, and a 4.0 ng/mL (16 ng/g) Fortified Clam Spike C, Respectively ............................................................ 65

Figure 20. Chromatogram Representing a Clam Sample Analyzed for PFOA (ExyLlMS lD: C0227658, Data Set: 050508A) ............................................................... 66

MPI Research Page 10 ofl51

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Interim Report #3 -Analysis of Fish and Clam Samples

LIST OF APPENDICES

MPJ Study No.: Ol37.0219 MPI Project No.: P0003267

Appendix A Study Protocol and Amendments .............................................................. 67


Interim Report #3- Analysis of Fish and Clam Samples

1.0 SUl'fiMARY

MP1 Study No.: 0137.0219 MP1 Project No.: P0003267

MPI Research, Inc. successfully extracted and analyzed fish and clam samples for the

determination of perfluorooctanoic acid (PFOA) according to 3M Environmental

Laboratory Method ETS-8-049.2 (V0003970) detailed in MPI Protocol P0003267

Amendments #3 through #8 (Appendix A, pgs. 124·151).

The limits of quantitation (LOQ) for the analyte in the fish fillet samples are listed in

Table I. The target LOQ for the method for fish fillet samples was 0.20 nglg. The limits

of quantitation (LOQ) for the analyte in the whole body fish samples are listed in Table

In. The target LOQ for the method for whole body fish samples was 0.20 ng/g. The

limits of quantitation (LOQ) for the analyte in the clam samples are listed in Tables V.

The target LOQ for the method for clam samples was 0.20 nglg. After evaluation of the

reagent blanks (method blanks) used for the analysis, the LOQ was determined. There

were no instances where a raised LOQ was required. A discussion of the process used to

evaluate the reagent blanks can be found in section 6.3 of the report. The LOQ for the

analyte in there-extracted whole body fish sample is listed in Table IV. The target LOQ

for the method for the re-extracted whole body fish sample was 0.20 ng/g.

Analytical results and assessed accuracies for the analysis ofPFOA found in the fish fillet

samples are summarized in Table I. Fortification recoveries for PFOA in the fish fillet

samples are detailed in Table VI. The average percent recovery± standard deviation for

PFOA in the fish fillet samples was 105 ± 23%. The results for one fish fillet sample

were not reported (NR) due to low spike recovery outside of the acceptance criteria range.

The sample was re-extracted and reanalyzed (Table ll), but matrix spike recovery of the

re-extracted sample (Table· VII) was also outside of the acceptance criteria range.

Analytical results and assessed accuracies for the analysis of PFOA found in the whole

body fish samples are summarized in Table Ill. Fortification recoveries for PFOA in the

whole body fish samples are detailed in Table VIII. The average percent recovery ± standard deviation for PFOA in the whole body fish samples was 99 ± 20%. The results

for one fish fillet sample were not reported (NR) due to low spike recovery outside of the

acceptance criteria range. The sample was re-extracted and reanalyzed, and the analytical

results and assessed accuracies for the analysis of PFOA found in the re·extracted whole

body fish sample are summarized in Table IV. The fortification recovery for PFOA in

the re--extracted whole body fish sample is detailed in Table Vill. The percent recovery

for PFOA in the re--extracted whole body fish sample was 89%. Analytical results and

assessed accuracies for the analysis of PFOA found in the clam samples are summarized

in Table V. Fortification recoveries for PFOA in the clam samples are detailed in Table

X. The average percent recovery± standard deviation forPFOA in the clam samples was

111 ± 190/o.

The assessed accuracy for the majority of the samples reported is +/. 30%. The

accuracies were assessed for each sample by reviewing the matrix spike whose spiking

level most closely matches the endogenous concentration found in the sample.

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2.0 OBJECTIVE

MPl Study No.: 0137.0219 MPI Project No.: P0003267

The objective of the analytical part of thls study was to detennine levels of perfluorooctanoic acid (PFOA) in fish and clam samples according to Protocol P0003267 and Amendments #3 through #8 (Appendix A).

3.0 INTRODUCfiON This report details the results of the analysis for the determination of PFOA in fish and clams using the 3M Environmental Laboratory analytical method ETS-8-049.2 (V0003970) entitled, "'Determination of Fluorocbemicals via Solid-Phase Extraction of Fish Tissues (Fillet or Whole Body) by High Performance Liquid Chromatography with Tandem Mass Spectrometry" detailed in MPI Protocol P0003267 Amendments #3 through #8.

The study was initiated on June 14, 2007, when the study director signed protocol number P0003267. The analytical start date for this interim report was December 27, 2007, and the analytical termination date for this interim report was May 12, 2008.

4.0 ANALYTICAL TEST SAMPLES

A total of one hundred and eighteen samples (ExyLIMS ID C0227544, C0227546 -C0227656, and C0227658 - C0227663 from login ID L00010436), one hundred and twelve fish and six clams, were received on dry ice on December 20. 2006 from Charles Young at Weston Solutions, Inc. The one hundred and twelve fish samples represented six sample sites: DLl, DL2. DL3, DOU, DMC, and DBC. Each site consisted oftwenty samples, with the exception of site DL2 which consisted of twelve samples. The twenty samples represented ten catfish samples (five catfish fillets and five whole body catfish samples) and ten bass samples (five bass fillets and five whole body bass samples). For the DL2 site, the twelve samples represented ten catfish samples (five catfish fillets and five whole body catfish samples) and two bass samples (two whole body bass samples). All samples were logged in by MPI personnel and placed in frozen storage. The sample IDs assigned by the client follow this formula: Dxx-x02-xxxxxx-x(x)-0612xx.

The first string begins with D for Decatur, Alabama and the xx defines the sampling area where: DL3 ==Up river Letter of Intent (LOI) sampling location LOC-3 DL2 => Cross river LOI sampling location LOC-2 DL 1 ~ Down river Fox Creek mouth LOI sampling location LOC- t

MPI Research Page 1 3 ofl51

Interim

DBC= DOU= DMC.,

These round' F02 = J 102=h

The thi and th(

sample

IP = ch MS=L CF=A

F = FiU W=W

001 thn

The fm.J 0 = Prir: 1 = Fiel RB""' E<

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fS Creek mouth ~ at 3M WWTP outfa;. nstream Mallard Cree mouth


';tring defines the gc :raJ category of the biota sample and the sampling

.:unple second round ,~brate sample second : md

'ng defines the specie tirst two characters), the sample type (third character)

ple number (last thr characters) within that sampling area and type of

: catfish (lctalurus pw :ltus) nouth bass (Micropter salmoides) ;; clam (Corbiculajlun Iea)

;sue sample body sample

1 005 =sample number vitbin the sampling area and sample type

;tring additionally defir ·s the sample type where: : field sample 1plicate sample 1ment rinseate blank sample

ring defines the sample preparation date in YYMMDD format.

Sample ~-in and chain of custudy information is located in the raw data package

associat·. with this interim report Storage records will be kept at MPI Research, Inc.

(State Ct ege).

5.0 REFERENCE MATERIAL

The req; :ition information, lot, purity, and expiration date for the reference material

used in t~ s study is listed below. The reference material was stored refrigerated.

Com pot. .J ExyLIMS

Supplier Lot# Purity ExQiration Received

Inventon: No. {%) Date Date

Oakwood No

PFOA SP0008065 Products, Inc.

YI6G 98 Definitive 09/08/06 Expiration


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Interim Report #J- Analysis of Fish and Clam Samples MPJ Study No.: 0137.0219 MPJ Project No.: POOOJ267

The molecular structure of the standard is given below:

PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight: 414 Transitions Monitored: 413 ----t 369

413 ..... 219 Structure:

F

F F F

OH F

6.0 DESCRIPTION OF ANALYTICAL METHOD

The 3M Environmental Laboratory analytical method ETS-8-049.2 (V0003970) entitled, "Determination of Fluorochemicals via Solid-Phase Extraction of Fish Tissues (Fillet or Wbole Body) by High Performance Liquid Chromatography with Tandem Mass Spectrometry" and details in Amendments #3 through #8 (Appendix A, pgs. 124-151) were used for the sample analysis in this study.

6.1 Extraction Procedure for Fish and Clams

6.1.1 Sample Preparation Before the samples could be weighed for the extraction, they had to be processed. To process, the frozen samples were placed into a food processor and homogenized with dry ice. The samples were transferred to one-gallon Ziploc bags and placed in frozen storage with bag left open to allow the dry ice to sublime. After sublimation. the sample bags were sealed and remained in frozen storage until time of analysis. Sample processing records are located in the Sample Information section of the raw data package except for those that were processed and supplied by the study sponsor as outlined in the protocol deviation found in the raw data package.

6.1.2 Sample Extraction

MPI Research

A 3-gram portion of each sample was weighed into a graduated cylinder, and the samples were brought up to 30 mL \·Vith acetonitrile. Each sample

Page 15 of 151

Interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0 l3 7.0219 MPI Project No.: P0003267

was then homogenized for -2 minutes. 5-mL aliquots of each sample were transferred to 15-mL centrifuge tubes, fortified as appropriate, and vortex mixed. The samples were placed into a freezer for -1 hour, and then centrifuged for -20 minutes at -3000 rpm at ~5°C. The supernatant was decanted into 100 mL of 2% H3P04 (aq) and vortexed. Next, the samples (catfish fillets, bass fillets, catfish whole bodies and clams) were loaded onto preconditioned HLB SPE cartridges (conditioned with 2 mL of methanol followed by 2 mL of water) and drawn through W1der vacuum, discarding the eluent. The whole body bass samples were loaded onto preconditioned tCI8 SPE cartridges (conditioned with 5 mL of methanol followed by 5 mL of water) and drawn through under vacuum, discarding the eluent. After the samples were drawn through the cartridges, the cartridges were washed with 2 mL of 5%. methanol (aq) (for the fillet samples) followed by 2 mL of 2% formic acid (aq) and suctioned dry. The HLB SPE cartridges were then eluted with 2 mL of 5% NH40H in methanol, and the tC18 SPE cartridges were eluted with 5 mL of 5% NH40H in methanol. The samples were then transferred to HPLC autosamplcr vials and diluted as necessary in 5% NH40H in methanol. Each sample was analyzed by LC/MS/MS electrospray.

6.2 Preparation of Standards and Fortification Solutions

A stock standard solution was prepared as specified in the method. The stock standard solution was prepared at a concentration of 1000 J..lg/mL by dissolving 0.1 g of the standard (corrected for purity and salt content, if necessary) in acetonitrile. From that solution, a 100 !lg/mL fortification standard solution was prepared by taking 10 mL of the stock and bringing the volume up to 100 mL with acetonitrile. By taking l 0 mL of the 100 !lg/mL fortification standard and bringing the volume up to 100 mL with acetonitrile, a I 0 llg/mL fortification standard was prepared. By taking 10 mL of the l 0 )lglmL fortification standard and bringing the volume up to 100 mL with acetonitrile, a 1.0 !lg/mL fortification standard was prepared. By taking 10 mL of the 1.0 J.lg/mL fortification standard and bringing the volwne up to 100 rnL with acetonitrile, tt 0.1 !lg/mL fortification standard was prepared. By taking 10 mL of the 0.1 f!g/mL fortification standard and bringing the volume up to 100 mL with acetonitrile, a 0.01 J..lg/mL fortification standard was prepared. By taking 10 mL of the 0.01 J..lg/mL fortification standard and bringing the volume up to 100 mL with acetonitrile, a 0.001 f!g/mL fortification standard was prepared.

A set of extracted calibration standards was prepared for each type of matrix (catfish fillet, whole body catfish, bass fillet, whole body bass, and clams). The extracted calibration standards were processed through the same extraction procedure as outlined above.


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Interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0137.0219 MPJ Project No.: P0003267

The following concentrations were prepared for the catfish fillet, bass fillet, whole body catfish, and clam samples:

Cone. of Fort. Aliquot Final Volume Final Cone. of Final Cone. of Solution Volume of Standard Calibration Std. Calibration Std. (nfimL) (ml} ~mq (n~mL} {ng/g)

1.0 50 2.0 0.025 0.10 1.0 100 2.0 0.050 0.20 10 25 2.0 0.125 0.50 10 50 2.0 0.25 1.0 10 100 2.0 0.50 2.0 10 125 2.0 0.625 2.5 100 25 2.0 1.25 5.0 100 50 2.0 2.5 to roo 100 2.0 5.0 20

The following concentrations were prepared for the whole body bass samples:

Cone. of Fort. Aliquot Final Volume Final Cone. of Final Cone. of Solution Volume of Standard Calibration Std. Calibration Std. {n&mq {mq !mL} {n~mq {n~s~ 1.0 50 5.0 0.01 0.10 l.O 100 5.0 0.02 0.20 IO 25 5.0 0.05 0.50 10 50 5.0 0.10 1.0 10 100 5.0 0.20 2.0 100 25 5.0 0.50 5.0 100 50 5.0 1.0 10 100 100 5.0 2.0 20 1000 25 5.0 5.0 50

The stock standard solution was stored in a freezer (~20• ± s·q when not in use. All other fortification and calibration standard solutions were stored in a refrigerator (4° ± 2°C) when not in use. Documentation of standard preparation is located in the raw data package associated with this interim report.

6.3 Chromatography

Quantification of the analyte was accomplished by LC/MS/MS electrospray. The retention time of PFOA ranged from 9.3 to 9.8 minutes. A method blank prepared for each data set was used to determine the LOQ. In instances where there were no peaks in the method blank, the LOQ was detennined by the concentration of the lowest standard injected in the analytical run that met the 70-130% recovery range of its known value. In instances where there was a peak detected in the method blank, the blank was evaluated. If the response of the method blank was Jess than 50 %of the response of the lowest standard meeting the recovery criteria, then the LOQ was detennined by the lowest standard. If the response of the method blank was greater than 50 % of the response of

MP I Research Page 17 of 151


the lowest standard meeting the recovery criteria, then the LOQ was raised to the standard that met the less than 50 % criteria.

6.4 Instrument Sensitivity

The smallest standard amount injected during the chromatographic run had a concentration of 0.025 ng/mL for the catfish fillet, bass fillet, whole body catfish and clam samples, and a concentration of 0.010 ng/mL for the whole body bass samples.

6.5 Description of LC/MS/MS Instruments and Operating Conditions

Instruments: Interface: Computer:

Software: HPLC:

API 5000 Biomolecular Mass Analyzer SCIEX Turbo Ion Spray Liquid Introduction Interface DELL Precision 360 DELL OptiPlex GX400 PE SClEX Analyst 1.4.1 Hewlett Packard (HP) Series 1200 Hewlett Packard (HP) Series 11 00

HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven

HPLC Column: Them10 Electron Betasil CIS, 100 nun x 2.1 mm, 5!J,m Column Temp.: -30° C Injection Vol.: 10 I!L Mobile Phase (A): 2 mM Ammonium Acetate in water Mobile Phase (B): Acetonitrile Gradient:

Time (min) %A %8 Flow Rat~ CLIVmLl

0.0 90 10 400 1.0 90 10 400 8.5 25 75 300 13.5 25 75 300 14.0 90 10 300 17.0 90 10 400 25.0 90 10 400

Total run time: -25 min lons monitored:

Analyte Mode Transition Retention Time Monitored (mjill

PFOA negative 413 ~ 369 -9.55 min. PFOA

Confirmation negative 413--t219 -9.55 min. Ion


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Interim Report #3 - Analysis of Fish and Clam Samples

6.6 Quantitation and Example Calculation


Ten microliters of sample or calibration standard was injected into the LC/MS/MS. The peak area was measured and the standard curve was genetated (using 1/x fit weighted quadratic regression) by Analyst software using eight or nine concentrations of standards. The concentration was determined from the following equations.

Equation 1 calculated the amount of analyte found (in ng/mL. based on peak area) using the standard curve (quadratic regression parameters) generated by the Analyst software program.

Equation 1:

Analyte found (ng/mL) = cc...J (82 + 4A y- 4AC))-B} X Dilution Factor 2A

Where: A = X variable 1 B = X variable 2 C = intercept Y= peak area

Equation 2 was used to e<>nvert the amount of analyte found in nglmL to nglg (ppb ).

Equation 2:

Analyte found (ppb) = [analyte found (ng/mL) x fmal volume" x aliquot factor(6)"'1 sample weight (3 g)

1\ Final volume of2mL for catfish fillet, bass fillet, whole body catfish, and clams. Final volume of SmL for whole body bass.

*Aliquot factor calculated by the following equation: [initial volume of sample (30mL)]/(extraction aliquot volume (SmL)] = 6

For samples fortified with kno"Ml amounts of analyte prior to extraction, Equation 3 was used to calculate the percent recovery.

Equation 3:

Recovery(%)= (total analyte found (ng[g}- average analyte in sample (nglg)) x 100%

analyte added (ng/g)


Interim Report #3- Analysis offish and Clam Samples MPI Study No.: 0137.0219 MPI Project No.: P0003267

An example of a calculation using an actual sample follows:

Bass fillet sample ExyLIMS ID: C0227547 Spike H {Set: 122707B), fortified at 2.0 ng/g with PFOA where:

Y (peak area) A (X variable I) B (X variable 2) C (intercept) dilution factor ng/g PFOA added (fort level) average amt in corresponding sample

From equation 1: Analyte found (nglmL) =

=

=

=

73943 -10600 147000 1250 1 2.0 nglg 0.370

((-./ {1470002 + 4(-10600)(73943)- 4(-10600)(1250)))-147000) X l 2(-10600)

From equation 2: Analyte found, wet weight (ng/g)

From equation 3:

%Recovery

0.514 nglmL

(0.514 ng/mL X 2 mL X 6) 3g

2.06 ng/g

= (2.06nglg-0.370ng/g) x 100% 2.0 nglg

85%

NOTE: Numbers may differ slightly from raw data due to rounding.

7.0 EXPERIMENTALDESIGN

For all fish and clam samples designated as laboratory matrix spikes, PFOA was added at a known concentration to the samples in the laboratory after the samples were weighed, homogenized and aliquoted for the extraction.

The fish samples were extracted in twenty seven sets. Each set included one reagent blank (method blank), two matrix controls, three matrix controls fortified at a lower level, three matrix controls fortified at a mid level, and three matrix controls fortified at a higher level of known concentrations. The catfish fillet samples were extracted in six sets. All six sets contained five catfish fillet samples, each from the same sample site. The bass fillet fish samples were extracted in five sets. All five sets contained five bass fillet fish

MPT Research Page 20 of 151

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-----·-·---------------------Interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0137.0219

MPI Project No.: P0003267

samples, each from the same sample site. The whole body catfish samples were extracted in six sets. All six sets contained five whole body catfish samples, each from the same sample site. The whole body bass samples were initially partially extracted in four sets. Tbe initial analysis was not reported due to quality control failures. The samples were then extracted using a modified version of the method (outlined in protocol amendment #6). The whole body bass samples were then extracted in six sets. Five of the sets contained t1ve whole body bass samples, each from the same sample site and one of the sets contained two samples> each from the same sample site.

The clam samples were extracted in one set. The set included one reagent blank (method blank), two matrix controls, three matrix controls fortified at a lower level, three matrix controls fortified at a mid level, and three matrix controls fortified at a higher level of known concentrations. The set contained six clam samples, one sample from each of the six sample sites.

One catfish fillet sample was re-extracted in one set. The set included one reagent blank (method blank), two matrix controls, three matrix controls fortified at a lower level, three matrix controls fortified at a mid level, and three matrix controls fortified at a higher level of known concentrations and the one catfish fillet sample.

One whole body bass sample was re-extracted in one set. The set included one reagent blank (method blank), two matrix controls, three matrix controls fortified at a lower level, three matrix controls fortified at a mid level, and three matrix controls fortified at a higher level of known concentrations and the one whole body bass sample.

Accuracies were assessed for each sample by reviewing the individual QC results obtained for each sample.

8.0 RESULTS

The limits of quantitation (LOQ) for the analyte in the fish fillet samples are listed in Table I. The target LOQ for the method for fish fillet samples was 0.20 nglg. The limits of quantitation (LOQ) for the analyte in the whole body fish samples are listed in Table III. The target LOQ for the method for whole body fish samples was 0.20 ng/g. The limits of quantitation (LOQ) for the analyte in the clam samples are listed in Tables V, The target LOQ for the method for clam samples was 0.20 ng/g. After evaluation of the reagent blanks (method blanks) used for the analysis, the LOQ was determined. There were no instances where a raised LOQ was required. A discussion of the process used to evaluate the reagent blanks can be found in section 6.3 of the report. The LOQ for the analyte in the re-extracted whole body fish sample is listed in Table IV. The target LOQ for the method for the re-extracted whole body fish sample was 0.20 nglg.

Analytical results and assessed accuracies for the analysis of PFOA found in the fish fillet samples are summarized in Table I. Fortification recoveries for PFOA in the fish fillet


Interim Report #3 - Analysis of Fish and Clam Samples MPI Study No.: 0137.0219 MP1 Project No.: POD03267

samples are detailed in Table VI. The average percent recovery ± standard deviation for

PFOA in the fish fillet samples was 105 ± 23%. The results for one fish fillet sample

were not reported (NR) due to low spike recovery outside of the acceptance criteria range.

The sample was re-extracted and reanalyzed (Table II), but matrix spike recovery of the

re-extracted sample (Table VII) was also outside of the acceptance criteria range.

Analytical results and assessed accuracies for the analysis of PFOA found in the whole

body fish samples are summarized in Table ill. Fortification recoveries for PFOA in the

whole body fish samples are detailed in Table vm. The average percent recovery ± standard deviation for PFOA in the whole body fish samples was 99 ± 20%. The results

for one fish fillet sample were not reported (NR) due to low spike recovery outside of the

acceptance criteria range. The sample was re-extracted and reanalyzed, and the analytical

results and assessed accuracies for the analysis of PFOA found in the re-extracted whole

body fish sample are summarized in Table IV. The fortification recovery for PFOA in

there-extracted whole body fish sample is detailed in Table Vlll. The percent recovery

for PFOA in there-extracted whole body fish sample was 89%. Analytical results and

assessed accuracies for the analysis of PFOA found in the clam samples are summarized

in Table V. Fortification recoveries for PFOA in the clam samples are detailed in Table

X. The average percent recovery ± standard deviation for PFOA in the clam samples was

111 ± 19%.

The assessed accuracy for the majority of the samples reported is +/- 30%. The

accuracies were assessed for each sample by reviewing the matrix spike whose spiking

level most closely matches the endogenous concentration found in the sample.

9.0 CONCLUSION

Except as noted above, the fish and clam samples were successfully extracted and

analyzed for PFOA according 3M Environmental Laboratory analytical method ETS-8-

049.2 (V0003970).

10.0 RETENTION OF DATA AND SAMPLES

All original paper data generated by MPI Research, Inc. (State College) that pertains to

this interim report will be shipped to the study director. This does not include facility~

specific raw data such as instrument or temperature logs. Exact copies of all raw data, as

well as a signed copy of the fmal analytical report and all original facility-specific raw

data, will be retained in the MPI Research, Inc. (State College) archives for the period of

time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792.

MPI Research Page 22 of151

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TABLES

MPI Research


Page 23 ofl5l

interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0137.0219 MPI Project No.: P0003267

Table I. Summary of PFOA in Fish Fillet Samples r ' C3Acld PFOA !

Perfl•orooctanolc Mid i

Analyt& Ac:ceptabla Ass&eaed

C~ent Foul'l(l lOQ A<:C\ncy r . E LIMSIO Sam 10 b, (+/-% t

I: C0227544 OL3-F02-MSF001-Q-D61207 0.434 020 30 t:•

C0227544 Rep Ol3-F02-MSF001-0-0a1207• 0.503 020 30

C0227546 OL3-F02~F002~1207 NO 0.20 30 f ! C0227546 Rep DL3-F02~SF0024061207' NO 0.20 30 I

C02275.c7 OL3-F02-MSF003-0-061207 0.359 020 30 '"< ~

C0227547 Rep DL3-F02·MSF003-0-061207* 0381 0.20 30

C0227548 DL3-F02-MSF004-0-06 t 207 0.319 020 30 I~ C0227548 Rep DL3-F02-MSFQ0.4-0-001207' 0270 0 20 30 J C0227549 DL3-F02-MSF005-0-061207 NO 0.20 30

C0227549 Rep Dl3-F02-MSF005-0-061207' NO 0.20 30

C0227550 DL3-F02-lPF001-0-061211 NO 020 30 f1 C0227550 Rep Ol3-F02-lPF001-0..{)61211* NO 020 30

C0227551 Dl3-F02-IPF002-0.001212 NO 020 30

C0227551 Rep DL3-F02-IPF002-0-06121 2" NO 020 30

C0227552 Dl3-F02-lPF003-0-061212 NO 0.20 30 f1 C0227552 Rep Dl3-F02·1PF003-0-tl61212' NO 0.20 30

<;{)227553 Dl3-F02-IPF004-0-061212 NO 0.20 40 C0227553 Rep DL3-F02-IPF004-0-061212* ND 0.20 40

' C0227554 Dl3-F02-IPF0054061212 NO 0.20 30 C0227~!54 Rep DL3-F02-IPF005-0.001212• NO 0.20 30

C02275~5 Dl2-F02-IPF001-0-061209 1110 020 30 C0227555 Rep Dl2-F02-lPFOOHl-061209• NO 0.20 30 Jl C0227556 DL2-F02..JPF002-0-061209 NO 020 30 C0227556 Re,> DL2·F02-tf'F002-0-00 1 209* 1110 0.20 30

u C0227557 Ol2-F02-IPF003-6-061209 NO 0.20 30

C0227557 Rep OL2-F02-IPF003-0-0&1209* NO 0.20 30 n C0227558 OL2-F02-IPF004-0-061209 NO 020 50 ;,.J C022755<48 Rep DL2-F02-IPF00+0-061209* NO 020 50

C022755B Dl2-F02-IPF005-0-061209 NO 020 50 C0227559 Rep Dl2-F02-!PF005-0-061209* NO 0.20 50 {1 C0227560 OBC-F02-MSF001-0-061207 1.05" 020 30 C0227580 Rep OBC-F02-MSF001-0-06120r 0.787' 0.20 30

C0227561 DBC·F02·MSF002·0..061207 0.327 020 3()

~ C0227561 Rep DBC-F02-MSF002-0-061207" 0.381 0.20 30

C0227562 D6C-F02-MSF003-0-061207 NO' 020 30 C0227562 Rep DBC-f02-MSF003-0-061207• 02or 0.20 30

C0227563 DBC-F02-MSFOQ.4.0-061207 ND 0.20 30 n C0227583 Rep DB~02~F0~1207• NO 0.20 30

<;{)227564 OBC-F02-MSF005-0-061207 0 3-47• 0.20 30 C0227584 Rep DBC-F02-MSF005-0-001207* 0.266" 0.20 30

C0227565 DBC-F02-IPF001 ~-061211 1.42 020 30

[! COZ27565 Rep 08C-F02-lPF001-0-061211• 1.42 0.20 30

C0227566 DBC-F02-l?F002~-061211 0.429 0.20 30 C0227566 Rep DBC-F02-lPF002..0-06t211• 0.511 020 30

C0227567 OBC-F02-lPF003-0-061211 0367 0.20 30 [; C0227567 Rep OBC-F02-lPF003-0-061211* 0.436 020 30

'Laboratory Ouplieate

'Relative Pefc:eni Oiffv111r>U > 20~ ( ~ 'Rtialive PMant Oifferance wat not calculat.d due to the pre$.001 of • nondeiBct aod rulftina Uneenaif\ty.

NO • Not deteQ!e<f at or aboYe tile acceptable LOO.

MPI Research Page 24 of 151 r If'

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Table I. Summary ofPFOA in Fish Fillet Samples (continued)

C8 AcidPFOA ,.,~..,., ....... cl

Acceptable As~ed P·.

Client LOQ ArxtJtiiC'f f

t : E UMSIO Sam leiD +1-%) .. C0227568 06C-F02-IPFOQ.4-Q-061211 0.441 020 30 C0227568 Rep OBC-F02-IPF004-Q-o51211" 0.423 0.20 30 f! C0227569 OBC-F02-IPF005-0..Q6121 1 0.726 0.20 50 ~ l L; C0227569 Rep OBC-F02-IPF005-0-061211" 0.760 020 50

C0227570 DOU-F02-MSF001·0·061209 ().89&' 0.20 30 C0227570 Rep DOU-F02~SF001~1209" 1.12" 0.20 30 n C0227571 DOlJ..F02-MSF002-0-06121 2 0.748A 0.20 30 k; C0227571 Rep OOU-F02-MSF002-0-QS121 2" 0.329" 0.20 30 C0227572 00lJ..F02-MSF0034-061212 0.61711 0.20 30 C0227572 Rep OOU-F02-MSFOOl-0-051212" 0.502" 0.20 30

~ C0227S73 OOU-F02-MSF004-0-061212 0.501 0.20 30 C0227573 Rep 00U-F02-MSF004-0-06121~ 0 584 0.20 30 C0227574 OOU-f02-MSF005-0-061212 0.422" 0.20 30 C022757-4 Rep DOU-f02-MSF005-0-06121~ 0.343" 0.20 30

~ C0227575 DOU-F02-IPF001-Q-061212 0.319 020 30 ' C0227575 Rep OOU-F02-IPF001-Q-061212" 0.295 0.20 30 C0227576 OOU-F02-IPF002·G-061212 0.540 0.20 30

I C02Z7576 Rep OOU-F02-IPF002-Q-061212" 0.526 020 30

C0227577 DOU-F02-IPF003-0-061212 0452 020 30 C0227577 Rep OOU-F02-IPF003-0-061212" 0.530 020 30 C0227578 DOU.F02-IPF004-0-061212 0.696• 0.20 50

[} C022778 Rep OOIJ.F02-l PF004-0-061212" 1.05" 0.20 50

C0227579 DOU-F02-IPF005-0-061211 NR' C0227579 Rep DOU-F02-IPF005-0-061211' NR*

C0227580 OU-F02-MSF001-o-061209 NO 0.20 30 n C0227580 Rep OU-F02-MSF001-0-0G 1209• NO 0.20 30 : i C0227581 DU·F02-MSF002-0-061209 NO 0.20 30 l . t.~:-;

C02275581 Rep DU-F02-MSF002-0-06 1 ~ NO 0.20 30 C0227582 OU-F02-MSF003-0-06 1209 NO 0.20 40

~ C02275582 Rep DU·F02-lASf003-0~1209" NO 020 40

CQ227583 DU-F02-MSf004-0-061209 0.201' 0.20 30 C0227583 Rep DU-F02-MSF004-0-061209* NO' 020 30 C022758-4 OU-F02-MSf()()5.1)..0& 1209 NO 0.20 30

m C0227564 RE!fl DU-F02-MSF005.0-061209" NO 020 30

C0227585 Dli-F02-IPF001-0-061212 NO 0.20 30 C0227585 Rep Dll..f02-IPF001.0-001212" NO 0.20 30 11"'\ C0227586 DLJ..F02-IPF002-0-001212 NO 0 20 30 'I C0227586 Rep DLI..f02-IPF002-0-061212' NO 0.20 30 I, LJ C0227587 DU-F02-IPF003-Q-061212 NO 0.20 30 C0227587 Rep OU-F02-IPF003-0--061212' NO 020 30 t C0227588 OU-F02-IPF004-0-061212 NO 0.20 30 ~! • j C0227588 Rep DLI-F02-IPF004-0-0G1212* NO 020 30 I

C0227589 OU-f'02-IPF006-0--061212 NO 0.20 30 ~'

C02275S9 Rep DU-F02-PF005-1).061212" 00 0.20 30 T' C0227590 DMC-F02-MSFOO 1-o-o61209 NO 0.20 30 C0227590 Rep DMC-F02-MSF001-0-061209' NO 020 30

"tabo.-attlly Oupt~eat• 'Relativa Pereenl Oilferer>ee ,. 20% 'Relatl,.. Percent Dm«ence- not Clll~l.ted due 10 the presenee Cf 1 nonc!etuct anc1 retU1t1ng oocertalnty. NO = Not detectea 81 or «>ove the~~ ~00. NR' =Not reported due to qulll~y~ fllilurea;- Table II for re-edraded IIMTlpiereauils.

,.


Jnterim Report #3- Analysis ofFish and Clam Samples MPI Study No.: 013 7.0219 MPI Project No.: P0003267

Table I. Summary ofPFOA in Fish Fillet Samples (continued)

C8Acld PFOA Perftuorooctanal~ Acid

Analyte Acceptable Assessed Client Found LOQ Accuracy

IMSID Sam le 10 b. (+/-%

C0227591 OM C-F02-MSF002-0-061209 0.29011 30 C0227591 Rep DMC-F02-MSF002-0-061209* Q.218A 30

C0227592 0 M C-F02-M SF003-0-061209 0.221' 0.20 30 C0227592 Rap DMC-F02 -MSF003-0-061209* NO' 0.20 30

C0227593 OMC-F02-MSF004-0-061212 NO 0.20 30 C0227593 Rep DMC-F02 -MSF004-0-061212* ND 0.20 30

C0227594 DMC-F02-MSF005-0-061212 ND 020 30 C0227594 Rep DMC-F02-MSF005-0-061212• ND 0 20 30

C0227595 DMC-F02-IPF001-0-061212 ND 0.20 40 C0227595 Rep DMC-F02-IPF001-0-061212* NO 0.20 40

C0227596 DMC-F02-IPF002-0-061212 0.284 0.20 30 C0227596 Rep DMC-F02-IPF0024061212• 0.245 0.20 30

C0227597 DMC-F02-IPF003-0-061212 0.22611 0.20 30 C0227597 Rep DMC-F02-IPF003-0-061212* 0.381" 0.20 30

C0227598 DMC-F02-IPF004...Q-00 1212 NO 0.20 40 C0227598 Rep DMC-F02-IPF004-0-061212" ND 0.20 40

C0227599 DMC-F02-IPF005-0-061212 NO 0.20 30 C0227599 Rep DMC-F02-IPF005-0-081212* NO 0.20 30

*laboratory DupliCate 'Relative Percent Difference > 20% 'Relative Percent Difference was not calculated due to the presence of a non detect and resulllng uncertalnty. NO • Not detected at or above the acceptable LOQ.


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Table II. Summary of PFOA in Re-extracted Fish Fillet Samples

Ex LIMS 10 Client

Sam leiD

C0227579 DOU-F02-IPF005-0-061211 C0227579 Rep DOU-F02-IPF005-0-061211"

•Laboratory Duplicate NR = Not reported due to quality control failures.

MPI Research

Analyte found

NR NR

C8Acid PFOA Perfloorooctanoic Acid

Acceptable LOQ

Assessed

Page27of151

Interim Report #3- i\nalysis ofFish and Clam Samples MPT Study No.: 0137.0219 MPI Project No.: ?0003267 ' I

Table III. Summary of PFOA in \Vhole Body Fish Samples L

' . C1!Acld PFOA f ·.

PerfluoroO<Otanolc Acid \ i

Analyu. A~ptabl• Aueue<l Client Found LOQ Accuracy ' '

IMSID Sam 1e 10 b.

C0227600 DL3-F02~SVV001~61207 ND 020 30 C0227600 Rep OL3..f02~SW001~61207 NO 0.20 30

C0227601 OL3-F02-MSW002-0-061207 NO' 0.20 40 I;

C0227601 Rep Dl3-F02~SVV002~1207 0.386' 020 40 t ; '' l i

C0227602 Dl3-F02-MSW003-0-061207 ND 0.20 30 C0227602 Rep DL3-F02-MSW003-Q-o61207 NO 0.20 30

C0227603 OL3-F02-MSW004-0-D61207 ND 020 30 [} C0227603 Rep Ol3..f02~S~061207 NO 0.20 30

C02276C4 Dl3-F02~SVV00~061207 NO 0.20 30 C0227604 Rep Dl3-F02-MSW005-0-061207 NO 020 30

C0227605 OL3..f02-IPW001..0-061212 NO 020 30 D C0227605 Rep OL3-F02·1PW001-0-061212 NO 0.20 30

C022760S Dl3-F02-IPW0024M1212 ND 0.20 30 C0227606 Rep DL3..f02-IPW002-o-o61212 NO 020 30

n C0227607 DL3..f02-IPWOOJ..0-061212 NO 020 30 C0227607 Rep OL3..f02-IPW003-0-061212 NO 0.20 30

C0227608 OLJ..F02~PW004-0-061212 NO 0.20 30 C0227605 Rep DL3-F02-IPW004..0-D61212 NO 0.20 30

I C0227609 DLJ..F02-IPW005-0-061212 NO 0 20 30 C0227609 Rep OLJ..F02-IPWQ05..0.061212 NO 020 30 ..

C0227610 OL2-F02-MSW001..0-061211 0.522A 0.20 30 C0227610 Rep DL2-F02-MSW001-D-061211 Q2J1A 0.20 30 f' ~

C0227611 Dl2-F02-MSW002-Q..(l61211 0.591 0.20 30 f I C0227611 Rep DL2-F02-MSW002-0-061211 0.509 0.20 30

C0227612 Dl2·F02-IPW001..0-00 1209 NO 0.20 30 C0227612 Rep DL2-F02-IPW001~061209 NO 020 30 n C0227613 Dl2-F02-PW002 -0-061209 NO 0.20 30

'-·~ C0227613 Rep Dl2..f02·PW002-0-o6 1209 NO 0.20 30

C0227614 DL2..f02-PW003-0-D61209 ND 020 30

u C0227614 Rep DL2-F02 -IPWOOJ..0-061209 NO 020 30

C0227615 Ol2-F02-iPW004-0-061209 NO 0.20 30 C0227615 Rep OL2-F02-PW004-0-061209 NO 0.20 30

C0227616 DL2..f02-PW005-0-061209 NO 0.20 30

~ C0227616 Rep DL2..f02·PW005-0-061209 NO 0.20 30

C0227617 DBC..f02-MSWOO 1-0-061207 2.95 0.20 30 C0227617 Rep DBC-F02-MSW001..0-061207 2.83 0.20 30

C0227618 DBC..f02·MSVV002-0-061207 2.72 0.20 30 [1 C0227618 Rep 0~02~SVV002~1207 2.67 020 30

C0227619 DBC..f02~SW00~1207 1.30 0.20 30 C0227619 Rep DBC..f02~SW00~1207 1.30 0.20 30

C0227620 DBC-F02-MSW004-0.061207 1.52 0.20 30 (! C0227620 Rep DBC-F02-MSW00~61207 1.60 0.20 30 C0227621 DBC..f02~SW00~61207 1.76 0.20 30

C0227621 Rep DBC..f02~SW005-0-061207 1.72 0.20 30

C0227622 DBC-F02-IPW001-0-061211 1.19 020 30 r: C0227622 Rep DBC-F02-IPW001..0..()61211 1.09 020 30 L

"'.aboratOJY Duplicate

•Retative Percent Olllere110e > 20% r 'Re!aW. P•rcont OilfOAOnc. was not ~ulated duo 10 lhe Pf••ence of a nondelect ancl resultln11 Yr~e!ll't!linty. NO =Not detected at 01 above the! ecceptablelOO.

MPI Research Page 28 of151 L r· l

Interim Report #3- Analysis of Fish and Clam Samples MPI Study No.: 0137.0219 MPI Project No.: P0003267

Table Ill. Summary of PFOA in Whole Body Fish Samples (continued)

CSAcld PFOA Penlu-onolc: AJ;Id

M~o AQ:eptellle As!KS$0\i Client FOill1d LOO IMSID Sam le 10

C0227623 DBC·F02-IPW002.0-061211 0.69<1 020 30 ,~'I

C0227623 Rep DBC-F02-IPW002-0-06 1211 o sae 0.20 30 r ' ~ !

C0227624 DBC-F02-IPW003-0-061211 2.0S 0.20 30

,.,t C0227S24 R&p OBC-F02-IPW003-Q-061211 194 020 30 C022782S OBC-F02-IPW004-0-061211 ND 0.20 30

,.) C022762S Rep OBC·F02-lPW004-0-061211 NO 0.20 30

! C0227626 OBC-f02-IPWOOS-Q-061211 1.47 0.20 30

,·J..

C0227626 Rep DSC-F02-IPWOOS-Q-061211 1.49 020 30 C02276:27 DOU..F0:2-MSW001-0-Q61209 123 0 20 30 u C0227627 Rep DOU-F02-MSWQ01-0-Q61209 1.05 020 30 C02276:2& DOU-F02~SVV002-0-Q61212 290 0.20 30 C()227628 Rap DOU-Ftl2-MSW00:2-0-061212 3.20 0.20 3()

fi C0227629 DOU-Ftl2-MSWOtl3-0-081212 NR' C0227629 Rep OOU-F02-MSW003-0-0612t2 NR• ' C0227830 00u-F02-MSW004-0-061212 1.04 0.20 30 C0227630 Rep OOU-F02-MSW004.C-06121 2 1.10 0.20 30

i C0227631 OOU-F02-MSW005-0-otl1212 3.75 0.20 30 C0227631 Rap OOU-F02-MSW005-0-061212 4.00 0.20 30 C0227632 OOU-F02-lPW001-(H)61 212 0634 o.:zo 30 C0227832 Rep OOU-F02-IPW001-o-o51212 0.619 0.20 30

fJ C0227633 OOU-F02-IPW002-C-{16 1212 o.are ()20 30 C0227633 Rap DOU-F02-IPW002-0-061212 0.874 0.20 30 C0227634 DOU-F02-IPW0034-06 1212 1.72 0.20 30 C0227634 Rap DOU-F02-IPW003-0-<J6121 2 1.79 0.20 30 fl C022763~ D<>U-F02-lPVV004-c-061212 NO 0.20 30 "fl C0227635 Rep OO\J·Ftl2·1PW004-o-()61212 NO 0.20 30 i. "' C0227636 D<JU-F02-IPW005-0-061212 1.11 0.20 30 C0227636 Rep OOU-F02-IPW005-0-061212 1.10 0.20 30 ~l C0227637 DL 1-F02-MSWOOt-o-06t209 0.291~ 0.20 30 ~J C0227637 Rep D\.t-F02-MSW001-0-o61209 0.337• 0.20 30 C0227636 DL 1·F02-MSW002-I;l-()61209 0.333" 0.20 30 C0227638 Rep OL 1 -FO:Z-MSW002-o-otH2011 0.485• 0.20 30

~ C0227639 Dl1-F02-MSW003-0-061209 0 3.42• 0.20 30 C0227639 Rep OL 1 .f'02-MSWOOJ.jl.C61209 o.<~sa• 0.20 30 C0227S40 Ol1-F02-MSW00-4-()..061209 0.351 0.20 30 C0227640 Rep DL 1-F02-MSW004-Q-061209 0.310 0.20 3() ;-l C0227&41 Dl1-F02·MSWOOS-0-061209 0.497 0.20 30 C02276-441 Rep DL t-F02-MS1N005-0-06120Q 0.462 0.20 30

' C0:2276.42 Ol1·F02-IPWo01-0-061212 0.262• 0.20 30 C0227642 Rep OL 1·F02..JF'W001-o-o61212 0.350-' 0.2() 30 C0227643 OL 1-F02-IPW002-0-o61 212 0.371• 0.20 30 C0227643 Rep Dl1-F02-IPW002-(H)61212 0.301• 0.20 30 C02276« DL 1-F02·1PW00~0-061212 0.285 0.20 40 C0227644 Rep Dl 1-F02·1PW003-0-061212 0 33.4 0.20 40 C0:227845 DL 1·F02-IPW004-0-061215 0 252 0.20 30 C0227645 Rep DL 1-F02-IPW004.0-06121S 0275 020 30

1-abOreiOf)' Oupllcale "Relative Pl!rcent Dilfttrence > 20% NO " Not c:Wecled a1 or~ ttw accaj!lable LOQ NR' =Not reported due to quality contrOl fail urea; se. Table IV for rl!-elllrac:ted sample tetull•

MPI Research Page 29 of15l


Table III. Summary of PFOA in Whole Body Fish Samples (continued)

C8Acid PFOA Periluorooctanolc Acid

Analyte Acceptable

Client Found LOQ

E IMSID Sam le ID I

C0227646 DL 1-F02-IPW005-0-061215 0.557 0.20

C0227646 Rep DL 1-F02-IPW005-0-061215 0.492 0.20

C0227647 DMC-F02-MSW001-0-061209 NO 0.20

C0227647 Rep DMC-F02-MSW001-0-001209 NO 0.20

C0227648 DMC-F02-MSW002-0-061209 0.536 0.20

C0227648 Rep DMC-F02-MSW002-0-<l61209 0.603 0.20

C0227649 DMC-F02-MSW0034061209 0.334" 0.20

C0227649 Rep DMC-F02-MSW003-0-061209 0.512" 0.20

C0227650 DMC-F02-MSW004-0-061212 1.48" 0.20

C0227650 Rep DMC-F02-MSW004-0-061212 0.202" 0.20

C0227651 DMC-F02-MSW005-0-061212 0.502' 0.20

C0227651 Rep DMC-F02-MSW0054061212 ND' 0.20

C0227652 DMC-F02-IPW001-0-061212 NO 0.20

C0227652 Rep DMC-F02-IPW001-0-061212 NO 020

C0227653 DMC-F02-IPW002-0-061212 NO 0.20

C0227653 Rep DMC-f02-IPW002-0-061212 NO 0.20

C0227654 DMC-F02-IPW003-0-061212 NO 0.20

C0227654 Rep DMC-F02-IPW003-0-061212 NO 0.20

C0227665 DMC-F02-IPWQ04.0..061212 NO 0.20

C0227655 Rep DMC·F02-IPW004-0-061212 NO 020

C0227656 DMC-F02-IPW005-0-061212 NO 0.20

C0227656 Rep DMC-F02-IPW005-0-061212 NO 0.20

"Laboratory Duplicate

"Relative Percent Difference> 20%

'Relative Percent Difference was not calculated due to the presence of a nondetect and resulting uncerteinty.

ND = Not detected at or above the acceptable LOQ.

40 40

30 :)()

30 :)()

30 30

40 40

30 30

30 30

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Interim Report #3 - Analysis of Fish and Clam Samples MPJ Study No.: 0137.0219 MPI Project No.: P0003267

Table IV. Summary ofPFOA in Re-extracted Whole Body Fish Samples

Ex llMS 10

C0227629 C0227629 Rep

"laboratory Duplcate

MPI Research

Client Sam leiD

DOU-F02-MSW003-0-061212 DOU-F02-MSW003-0-0S1212

Ana lyle Found

127 1.20

C8Acid PFOA P~rllucrooctanole Ac:id

Acceptable Assessed LOQ Accuracy

+/- %)

0.20 30 0.20 30

Page 31 of 151


Table V. Summary of PFOA in Clam Samples

C8Acld PFOA Per11uorooctanale Acid

Analyte Acceptable Client Found LOQ

E IMSIO Sam 10 b.

C0227658 DL3-102-CFW001·0-061219 0220 0.20 C0227658 Rep DL3-102-CFWOO 1-0-061219• 0.218 0.20

C0227659 OL2·102-CFW001-0-061219 0.424" 0.20 C0227659 Rep DL2-102-CFW001-0-061219• 0.295" 0.20

C0227660 DBC·I02-CFW001-0-061219 0.796" 0.20 C0227660 Rep DBC-102-CFW001·0-061219• 1.00" 0.20

C0227661 OOU-102-CFW001-0-061219 0.832 0.20 C0227661 Rep DOU-102-CFW001-0-061219* 0.857 020

C0227662 OLH02·CFW001-0-061219 NO' 020 C0227662 Rep DLI-102-CFW001-0-061219* 0.221' 0.20

C0227663 DMC-102-CFW001-0-061219 NO 0.20 C0227663 Rep DMC·I02-CFW001-0-001219* NO 0.20

*Labonotory Dupl~to

'Relative Percent Difference> 20%

'Rala!MI Percent Difference was not colculllted dua to the presence of a nondetect and resulting uncenalnty. NO,. Not clelectee at or above the aceeptabto LOQ.

MPI Research

As~~

Accuracy .,. %)

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30 30

30 30

30 30

30 30

30 30

Page 32 of 151

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Table VJ. Matrix Spike Recovery Summary of PFOA in Fish Fillet Samples

Dl3-F02-MSF001-~1207 {CtU7k4 Spl 0, U Holo opll<o)

Dl3-FI)2-M$F001-~1207 coom .... ,.. ~too.,.."""')

DL3-F02-MSF0024061207 (CIUZ7 ...... , ....... -

0L:l-F02·MSF002.0-G81~ (CDlVWI ... 0. 101 ppO -·

Dl3-F'02-MSF003-0-<l81207 !COJ21M1.,. tt. 2.0 ... tpll<t)

DL3- F02-MSFCJ03..0.0&1207 (COUTW s,t L '"' l'l'b •JIM!

Ol3-F02-M$Fil044061 ~rT7 ICIUI'UIS ... .J,U~·-

0l3-F02-MSF~1207 (CUID .......... ,. ..... _,

OL3-F02-MSF005-0-081207 tcOW' ........... u ppO.,..., Dl3-F02-MSF00&4a61207 (CtmUISpt M. UO ..... 11>~01

lll3-F02-IPF001 -0-MI ~II j01Zl1- .... D,Uppll•-

0l3-F02~Pf'll01401>121 t tct2VNO $00 1!. M w• tpllo)

Dl3-F02-lPF002-~1212 ~ .. 1.,. ..... ,._,

Ol3·F02-lt'F'0024<161212 ~Ulftt .... 0, 1ei!>PI>-

ot3-F'02-lPFfl03-li.OIS1212 (QOUlWI ... II.l.O ... _

DL3-F02-4PF~-c-081212 (COUUQ ..... l 1Ct ... J1>lhl

Dl:l-F02-IPFOO<I.Q.061212 ~7~ ..... J.U!P

DL).F02-IPF004.().()1!1212 iCG%ZTU2 apt K, '"',.-

Dl3-F02-If'FOO:i{l-a4121 2 !Cot21 ... - '- ..., ... -Dl3-F02·1P~1212 ~mc~t•l*•.loo,,.,....

OL2-1'02·1PF001.0.0$1 209 (COWRUj>ll D. U ,,.....,

DL2-F02·1PF001.Q.061209 jCOWICOI .... L •• ..,.,_

D~o:NPAJ02406120i

tQOZ>11M ''* '· ........ -DL2-F02·11'1'002-0-0&120i ~ .... 0. ,.,."'"' ..

DL2-F02-IPF003{)-0812Qe (CVW .. IIj>tH,U,,.._

Dl2-F02·1PF003-0-06120Q i<»227Rr s.- ~ \60.,. .. ~~~ ..

20

100

20

100

2.0

100

2.0

100

20

100

2.0

:z.o

100

tOO

2.0

100

!CO

2.0

tOO

2.0

100

NO • Net o.t.ctad «1 Of II1Wte 1M~ lOQ rw,ooMd 11 T•bkt I.

0.489

0.~

ND

NO

0 370

0 370

0295

0.2QS

NO

NO

NO

ND

NO

NO

NO

ND

ND

NO

ND

NO , ND

NO

NO

195

1.87

NA.

2.59

2.~

NA

2.eo

2.58

2.$1

2.4~

W. • Notopplio:oCJie. Thla mow op~<• <»_trion,.• nat•oecllO ...... moccurocy for lhlt .. tlytt.

107

NA

NA

115

130

NA

117

127

117

NA

129

Now: - IIIIo ••m,...O)' laolo olloWt -*" ,...,..,,~ .. , .... may WO)' "'ainly '""" 1119 ...... "'lito .. w dola.

MPI Research Page 3 3 of 151

Interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: Ot37.0219 MPl Project No.: P0003267

Table VI. Matrix Spike Recovery Summary of PFOA in Fish Fillet Samples (continued) r

I

t ' caAddPFOA

'IRl'f!u&f~C~td

Amount Ayg AIM F<>.Jntl Amo.mt r: Sa-n pie ~:~~ intS:Jie R~:;ad Re<:Ovary

' Oeocri<>tion l%1 ' ' ' . DLZ ..f02-lPFOOf.()..Q6 1209 lCIU7HIIpt. J, U ppllo cpJ:bt 2,0 1>0 484 1-42

Ol2-F02-IPFOOHI-CIS 1209 f ; tcanr"' op~o 1<.,...,.... ''"""' 100 1>0 Iii\ NA ~oJ Ol2-F02-IPF<IGS.c.Q91209 (C8U1UUpk l,.LO ppO -o! 2.0 00 2.~ 1~7

Dl2 -F02-PfOO!Hl·M 1209 t I (t;<2ZTH. Ci>kM, 1110 PI"> opllooj 100 It) NA NA u

DBC-F02-IJISFOOI-0451207 ICOIW ... lpl D. U ...... 'ul 20 0920 238 T3

OBC.f'02-MSF001.().061207 [] ;comw. .,.I!.-P~ <pibl 100 0_920 NA NA

DBC-F02-MSF0024001207 (UUJII'IIpl F,U oobtplllo) 20 Ol54, 22l 9-4

OOC -FIXI-MSF0024061207 n {COUflfr1 ·~ o, 1W ppO a.p-ibt 100 O_lS4 NA NA

OOC-F02-MSF00340e1207 (COU711Q Sf>~< K, U ,,. ol>l>ol 2.0 0,204 228 104

06C-F02-MSF0034001207

I tcGI'Il' JIU llpl l._ 1MI ppll• .-.a 100 0204 NA NA

DBC-F02-MGF004-0-061 207 (CJU11U Spt J, U IIIPD .,.a.) 2,0 ND 1n 69

DBc-F02-MSF004-0-061 207 f(»Witlt,.k,IOG .... - 100 NO NA NA r i OBC·F02-MSF(I(IS.I).OO 1207 .. ) r=znu '"' l. u,.... '""'" 2,0 0;)06 2 27 98

OBC-F02-MSFOOIHHlS1207

(CIN211U- .. - ... -100 0.306 NA Iii\

D 06C-F02-wf001 -<1.001211

(CQW'MUp' 0, U ..... - 2.0 1.42 385 122

OBC-F02·1PF001.Q-tJii1211 (CUifMUp> ~. 1 ....... •plkol 100 142 NA NA u 06C-F02-IPF002-0-061211 1CGU7-s.-,,u..,..~ 2.0 0~0 3.06 130

08C-F02 4Pl'002-0-061211 tctmiiM ""' o. *,.... _, 100 0.470 AA NA

08C-F02~PF003-0-061211 f] (aZ%1117 .......... __ 2.0 0402 295 127

DBC-F02-IPF~1211 !CO>Z1 ... 0 .. L_ ... _) 100 0102 NA Nil

r~ DBC-F02-IPF004.()~121 1 i

(c:n.JJ .. I'* J.UI ,_. ·- 2.0 0432 2.7& 116 ; DE!C-1'02-IPF004.().061Z,1 (C.UTMt lpk K, IN,.,. o.,;MI 100 0432 NA NA

OBC-F02·1PFOOS.o.o&1211 c t= ... ..,..~.u,. .. hl 2.0 01-43 360 143

08C.f'IXI-JPF0054061211 (caDl' .......... , ..... -et 100 0.74J NA NA

OOU-F02-MSF001.().061209 r (COUJin&pl D, U JOI'I>- 20 101 3 01 100

DOU-1'02-MSFOOI 4ll61209 (C!UZU"So01!.10t .... ~ 100 101 NA NA

NO, No! -·O<oboWtnt~lOO- in T-1. [' NA. c:; Not appit:.ttlM. Thl:f; n\H\1a:p1U (;Oncarrtrlttion WH not \116d ~ IJKNI '1M attutec; fCII' f\11 ·~

1\loi:a! lil\c:. thll• •UrMNJY tabM &hG1fit'll fOV1"'oChd f'IU.Uh:IP """"""YVIIihiN r"M}' 'tllf"t ti.t~y fnllfto tJ. Wf"" jn ttl• I'WW cl81&.

MPI Research Page 34 of 151 r t

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Table VI. Matrix Spike Recovery Summary of PFOA in Fish Fillet Samples (continued)

<=aAcldPFOA Pwrf'L.toroo~Ae14 r Mlount A~ Arnl Fou<1d Amour¥ \ Smlpill Spiked

'\=~ R..,.,_ed RecowJY I ~ loolal IMial 1%\

DO\J-F02·MSF002-0-ilet212

f I ICOZZ11<>1 ..,. '·'" ,~ ''"""' 2.0 0.535 233 90 OOU-F02..\1SF002.0.0Sl :m (COWI<>t S"" •. tOO poo1t ''"""' 100 0.53& N4 NA DOU-F02-MSF!lCJ3.0-M121 2 ~m..,.H,u.,.,_ 20 0.5~9 205 75

DOU-F02-MSF003-Q..061212 l,; ICOZzrm a,.~~ t. 1e0...,.. .,.Jil-t 100 0559 NA "" DOU-F02-MSFOI:l4-0-001212

(CQW17> apt .1. l.O ,.. ,,.., 20 05-43 1.94 70

f] OOU.f'02-MSF004-().()61212 (COU!I73 aplK, tiMI ......... 100 0.543 iliA NA

OOU-F02-MSFOOS-o-oo1212

~"' ""L. Ul,.,. -~ 2.0 0.383 1.114 73

f1 OOU-F02-MSF005~1212 fCO:&niUS~M. 1W-~ 100 0.383 ~-~~ NA t.t 00\J-1'02 -!Pf'OOl..o«Ei\21 2 C<;tU1171SptD,>.a ..... _ 2.0 0.307 2.83 110

*~·~ OOU-F02..f'F0014l.¢61212

I (QU!fl'l.,. E.- ... - 100 0.307 NA NA DOIJ.F02-IPF002.o.(IS1212 (COZ2Jf11 .... J.U ... oj>llool 2.0 0.633 l9'i 13 ~-li'F002..Q.OI!.1212 11 iCOWf7t ..,. o. toe """"""" 100 0533 lilA NA ·! DOU-F02-tf'Foo:J-0.061212 a;., !OOWm..,. H. u Pl'i> ~"' 20 0.491 2.01 78 00\J-F02-IPFQ03..0-Q61212

I!:' I i<'OmJn ""~ * ""' ...... 100 0.491 lilA NA 11 OOU-F02·1Pf~-081212 tctur m ,,. J. u ~ .pa..; 20 0.371 190 51 OOU-F02..PF0044Q;1212

f1 pctmln S,k II, IIMI ... .,alii 100 0.671 NA lolA OOU-F02-II'F00!-0.001211 ;J ~S,kt.U .......... 2.0 NR" NR' NR• OOU-F02..f'F0()54CJ61 211 {COmiAS,kM,- ..... "f''PP 100 NR" foR' NR' I 0~02-MSF001-C-C61209 fi'

t:: ~,.,..,,u.,..- 2.0 NO 2.2$ 113 Dl1-l'02·MSFDOI.().(le1209 fC~wtm ''* •. ,.. ......... 100 NO NA NA f) Oll-f<l2-MSF002-0-ile1209 ~. :

t' (\:.O"mh; s..- 11.1.0 ,..llpilt., 2.0 NO 2.:10 1111 ~ ;

OLI-F02-MSFOC2-o«EE1209 f<8UTIII a,tl G, 1110 .,,IIjllbll 100 NO No\ NA (-;:':'>

OLI-F02..MSfll034081209 ~ : ICOZZfD1 .... 11..t..CI .... - 2.0 NO 2.71 136 Dll-f02-MSF~12011

(CIIl27v.t ... '· ....... - 100 NO No\ NA

0U.f02-MSFIXJ44.0Ei120!1 ICOUT'A.,. J,t.O PI>~ 'l'lkl 2.0 •,< 0.201 219 99 Dll..f02-M~1209 (CIOUTin..,. II,,..-~ 100 0201 H" NA

HI): Not-"" at orabcwo ti>o ~ LOO roportod tnT- I I<IA • Not_.,__ Thlo moW ~k<l"""""""' -• 1\01 utt<l 10 •- tho -..recy fl>r 1f'd ~ ~· • Not ...,.,nod-~ quofily_,_,_ T- \Ill lo<....----_, &inc:. !IN ...,...ryloW. .~._.. ,.._ --· ,....,_, voluu ma~ ""'Y oljjllll,lrom 11M wluet in lito...., ato.


Interim Report #3- Analysis of Fish and Clam Samples MPI Study No.: 013 7.0219 MPl Project No.: P0003267

Table VI. Matrix Spike Recovery Summary of PFOA in Fish Fillet SampJes (continued)

C8H:Id'i'FOA P•~~ckld

Amount AvgAmiFound Mlourrt ~-

Sum pie Sp,hd tlr=-.r R~":f>d Re~v;'ry I !mcrtction ~~ ... Q) i.- i

OLI-FQ2-MS~12C9

lcn27114lH 1.. u,.,. -·l 2-0 ND Hill 98

OLI-f02-MSF~2D9 q

~ISUiolllll.110 .... """'"' 100 NO NA NA i ! k l

DLI-F02-IPF001-o.<le 121 2 {C02::r1AI 8st' D• U f~ 1p(lt .. 2.0 NO 1.9~ 100

DLI-1'02-IPF0014-051212 p (<»%%71M ... I, 100 ..... •I'IMI 100 NO NA HA tJ DL~f02-ff002-0-0&1212

!Ctm'M I!Ol P, U l'f'l' •Pibl 20 NO 2.18 109

Ol.l-1'02·1PF002-0$1212 u l"''u.t ..... IOt,.P- 100 NO NA NA

OLJ.F02-IPF003.o.o6121 2 ICOZZTMT .... K. U ppl> ... oi <-0 ND un 915

DU-F02-IPF003-0-061212

r1 ~IIJipk~1DOppb~ 100 ND NA NA

Ot.l-fll2-IPFOO~.o-o&121 Z j

1CI22UU .... J, JJI ... s- 20 NO 207 104

OLI-f'02-IPF004~1212 -!OHJ71UI .. It.101 .... < .... 1 100 NO "'A NA

' ()LI-F02-IPFOQ5.().(e 1212 !Camat Sf'IL 1.. ZJI,.. ""'-' :.l.O NO 2-00 ~~

OLI-~02-I'I'OO~-O-OI'll21: (CIIZZ7_.., ..... ..,..._ 100 NO NA ,., ...

[J DMC-F<I2-MSF0014051209 ~Dqa,IID.U .... •-l 2.0 NO 1.61 e1

OMC-F02~Fil01~12J:lt IC0%%71t0 ....... ,.,..,... 100 Hl) NA NA r DMC-F02-MSFCXI2400121»

!

ICID1it11oiiP,U .......... 20 0254 1_84 711 j

OMC.f02~.o.o61201l

.... UTU1 .......... .,. - 100 02.54 HA NA

DMC-F02-USF~1209 u ~..,,... ... """''- 2.0 0211 2.2'1 100

DMC-F02-MSF003-0-0EI1209 !c=I71H ... '· , ...... qlooj 100 0211 NA NA

OMC-!'024oi$RX)o4~1212 ~ tci1Z11H .._ Jl u,. ..... 2.0 NO 1e1 91

Dr.IC-F02-YSF004-().051212

(C012>1H .... K,,. ... ·-100 NO NA NA

DMC-1'02-USI'CKJS-.().051212 n t=U ..... \.. ....... - 2() NO \.~ 10

DMC-F02-MSF~1212 ICIUfUoiS,.It, , ....... .,. .. 100 ND NA NA

OMC-F02-lPF001~1212 f. ICIW., .... 0. JJI-- 2.0 r-ID 2.61 131

OMC-FQ2-1P!'OO,-O-ll612 \2 rcoti71N .... e. _p,. •ollool 100 ~0 NA NA

DMC-f'a2-J>F002.().061212 (' . tctmiN.,..,,u.,..,a., 20 0.2&1 2.~ 105

. DMC-F02-PF002.o-o&121 2 L (al!DIN .... Q,1GI,....,.,.. 100 0254 lolA NA

NO> ~cl-11<1 .. ..,-.. lho IICQOplaobloi.OQr-Ad;nT-1. r ; """~-- Tt\lt,....,..'l'll<a.............--IIOt•-to .. •ou1110-wtNoonolyio. IMto; a .... !hlo •• _,.- "" .... .-.. ......... .--owrywiwo rnor ...... ""~'""" ............. tho .... d- t.

MPI Research Page 36 of 151 f L

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Table VI. Matrix Spike Recovery Summary of PFOA in Fish Fillet Samples (continued)

C8AcldPFOA Perfluorooctanole Acid

Amol.l"lt Avg Ami Found Amount Sample Spiked in Sample Recovered Recovery Description (rnvq) {nqfq) (na/Q) (%)

DMC-F02-IPF003-0-061212 IC0%27$&7 Sp- H. 2.0 ppb $pll<•) 2.0 0.304 2.17 93 DMC·F02·1PFOOJ.O-Q61212 (C0%27617 Spk I, 100 ppb spike) 100 0.304 NA NA

DMC-F02·1PFoo..-0-061212 (COU7Stl Spk J, 2.0 ppb •pll<•l 2.0 NO 2.70 135 DMC-F02-IPF004-0-05121Z (COZ275U Spll K, 1~ ppb oplk•l 100 ND NA NA

DMC-F02-IPF005-0-001212 (C0227591 Spk L, 2.0 ppb sJ>ike) 2.0 NO 2.53 127 DMC·F02·1PFOIJ5..0-051212

(C0%%75&9 Spk M, 100 ppb spike) 100 NO NA NA

Averagt: 105 Standard Deviation: 23

NO : Not deted.O at Of above 11\e ~ble LOO ~In Table I. iliA v Not applicable. This mstri~ spike conoenntrion -• not""" IO IUIHISS the ac:curaey fer liltS analyte, Not.: Since this summary bible snows roui'ICI&d ruult$, rveov'"'f val~a may vary slightly from tha vallin In the raw data,

MPI Research Page 3 7 of 151

Interim Report #3- Analysis ofFish and Clam Samples MPI Study No.: 0137.0219 MPI Project No.: ?0003267

Table VII. Matrix Spike Recovery Summary of PFOA in Re-extracted Fish Fillet Samples

C8AeidPFOA Perflu oraoctanolt Acid

Amount AV9 Amt Foond Amount

Sample Spiked in Sample Recovered Recovery Oescrlp11on (1'\Q/Q) (nq/Q) (nq/Q} (%1

DOU-F02·1PF005·o-o61211 (COZ2T51t Spk F, 2.0 ppb spike) 2.0 NR NR NR

NR = Not r&pO(Ied due to quality control failures

Nottt: Since this summary table $!lows rounded ~lilt$, rtteovery Ylllues may vary ~lightly from the .-a"'nln the raw data.

MPI Research Page 38 of 15l

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Table Vlll. Matrix Spike Recovery Summary of PFOA in Whole Body I

Fish Samples t CIAddPFOA

Pe~taoMAc/4 c

Amo<Jnl A~ Am! Found Amount 1· { !iam:>le Spri<eG ln(s,:;;'• R";'.=;-.1 RecoY"'Y t OescriP!iOn (~a/QJ (,.,,

OI..J.F02·MSW0014-061207 ( tcfU7000 Sp- ~. Z.t PIOII oplh) 2.0 NO 2.09 lOS { I

DL3-f'02-MSW00\-~0012C7 lJ (C0121'5CO lpl €, 400 Pill> -I 400 NO NA NA

DL3-I'02-MSW002-{).()61207

rr (CO!U"" Sp. P, U Pf>lt-1 2.0 0.293 1.8: 66 OL3-F02-MSW002-().061 7:07

' I lCW7W1 """a.-"""·- 400 0293 NA NA

I.:.J

Ol3-F02-MSWQ03-().061207

f'l l¢0ttnol ..... ~. :.0 ..... _, 2.0 NO 2 .• 5 123

OL3-F02-I.ISW003-!UI61207 ') (Cnz71Clllpll~40tl>f>ltopb) coo NO NA NA

OL3-F02-M~O!I1207 ICDZ2noJ Sl'l J. U,.,.. a,olkoj 2.0 NO 2.211 113 (1 DL3-F02-MSW0044061207 I lC~12710.0 llpll II,- ppo ->1 400 NO NA NA

OL3-F02-M$W0(15..0.061 1IJ7 (Ct:W- tp~ L, U llf'O •- 2.0 NO 2.-42 121 - Ol3-1'02-M~1Nl (CCW750flplt It, .U -·to) 400 NO NA NA Dt.J.F02-If>VI.001~1212 1(:0U7_1,..!>,J.A_opi .. ) 2.0 NO 2.13 107 (1 Dl3-F02·1PWl01.0.0S1212

' IG»tuUllpll. 1.10 PI'II•Pbl so NO NA NA ,, OL3-F02..JPIN002-0.001212 (COlt711111p. F, U,.,. IP<ioo) 2.0 NO \96 sa 4.: ~ Dl3-f'02-lPW0024061212

t (C0221401 """ ~. $0 - &p!Mj so NO NA NA DI..3-F02-If'W003.0.0&1212 tct1271011 ...... u-....... , 2.0 NO 2.2) 112 ~-:; DI..3-F02-lPWXI3-o-o6121 2 !J lC<>U7<07 -~ •• - _, 50 NO NA NA k DI..3-F02-IP'MJ().f.().OI1212 ICIIUTINII'lJ.:t.OIIII~I-.. 2.0 NO 1.51 91 if.:"1 DI.:J. F02-lPV\'004-!U161 21 Z ttl tcf2"'- ... It, 50 ..... ,,_, 50 !«) NA NA iJ Ol3-F02-1~12t2 tcf217tM ... L, z.• ..... opllo) 2.0 NO 1.68 8S i;f: Ol3-F02.JPW005-Q..061 212 (C01Z710t ~ "'·" pplt .,.,... 50 NO NA NA

Dl2-F02-MSW001-0-061211 (Ctt:Tfllllpj< D.l.l,... .,.., 2.D OST7 2.70 118

Ol2-F02-MSW001-().06f211 (C012Tt1U ... E. ........ ~ <400 O:n7 NA NA Ol2-F02-t.ISWOQ24061211 (CO'W"I11 ..... F, t.0,., .,... z.o o.550 2.04 75

DL.l-F02-MSW002-0-0612 1 1 tcoU7t11 """o. -,.,. ~ 400 0.550 NA NA

NO c Nt>! dltoe..:S 0101-. N-LC0 ,..~;,Tallie 1n. NA • Hot opplic..,._ Thio motTll< ~·· conctuwllr!On wu no1 "ft<IIIO ... _, tt>o eccuraov lor t\ls ar.otyta. Note: Slns:othia aurwm.wytabM ......,_.. roUI'Idlld ,.autt1. MCCIVIItynluM II'J.aY••rv•ll.ghtjyftDmU.V111uo i" tN r'I'W data,

MPI Research Page 39of151


Table VIII. Matrix Spike Recovery Summary of PFOA in Whole Body Fish Samples (continued)

CIAclcl PFOA hrfhlotooctmole AcW

MIOunl· Avg Ami Fouod N11ounl s.m,:l.o Spil>e4 inSamp• ~O<J ~~ D•ICI'IPfion (nalal (ml/.;) fna/ul

DL2-F02·1PWOO 14-061209 (C0227fU lpl< D, Z.O ppa UINI 2.0 NO 185 93

OL2-F02..Jf'W001-G-001209

tc0227f11l,O.I!. 2H ,.,. ·- 200 NO NA WI

DL2-F02..JP'Ml02-0-0e1209 tC0211"1 Spi<F,l.lt>P' ,,..., 2-0 NO 2.07 104

DL2-F02-If"AA02-G-00120U (COUTI13 Jp0 0, act ,at opllo) 200 NO NA WI

OU·f0Z-l~209 {C0211fl. Spk It, U l'f'lo ..-01 20 ND 1.« 72

Dl2-F02-IPIM)C3.{)..(Jij12()!1 !C<Iftrl1• Spit t, 100 "* apille) 200 NO WI NA

OL2-F02-1~1200 [CVlVOfl $pi< J,l.t ,..a-~ 2.0 NO 1.7e 91)

Dl2-F02-11'\'1004-0-061 209 fCIUTOU Stol< tt. ZOO ppll spllloj 200 NO NA HA

DL2-F02-IPWOOS-0-CG12og (CaUl'O<I $1*1-. JJ .... .,.., 2.0 NO 1.68 34

Dl2·F02·1~209

(CC22TI1l SpiiM,- ..... - 200 NO NA NA

OBC-F02-MS"W001-0-CG1207 (C0:2fl11-D, U ,..a- 20 2.89 5.13 112

06CF02-USW001-0-081207 ICOUI'f11 ... ~1-.0opilloj 10000 2.89 WI WI

OSC-F02-USWOOZ-G-001207 t<:Od711UpH, Ll ~ oplkoJ 2..0 2.119 ... 83 107

DBC-F02-MSW002-0-0e1207 I(:OUU1tlplt0.1-~op<koJ 10000 2.89 NA NA

D8C-F02-MSW0034001201 !eotnlu a,. ... 1..1 pp~~~..,l_, 2.0 1.:30 3.21 96

DBC-F02-MS\W03.0.0812IJ7 (t;tU1'011 SpO <. 1-ppa Ol'lt•l 10000 1.:30 NA NA

DBC-F02-MSWOIU-<HI61207 (CHVUO Sf*~ U ,..._ 2.0 Hill 4.07 12.S

OBC-f02-~061207

(Ca27Ut.,... 11,1-.... """"' 10000 1.61! NA NA

DBCf02-US~1207 (C0:21UI lpa I, U ,.,. ,,.... 2.0 1.74 3.9$ 111

DBC-F02-Ioo1~207

tctarm •ilk ... •- ''* a,WU~ 10WO 1.74 ""' ""' DBC-F02·1PYI'001.(1.06 1211

1Ql27Ul••t>. u""'- 2.0 1.14 3.25 106

DBC-F024PY\'001..J).()61211 ICO:W0128toi<E. -~lPli41 5000 1.14 NA NA

06C-F02-IPW0024-06 1211 (COHTUI lpO ,, z.o ..... tf'lool 2.0 0.640 2.67 102

D6C·Fot-JPW0024-06121 1 ICOWIU lpO 0,-~- 5000 0.640 NA NA

NO • Not~ al 0t -IM """PI- LOQ r.,x>Md "'Ttl>• IlL NA • Not .e.ppialtQ. Thil tnaui.l S~ ~ion Ml not u.Hod U> • ...._.. th• .a:t:Kaey fat tB1 ~~·· NOU: Sk'Joe lhjls &UJI!.flla'Ytabkl •~-.owe rout1CIH t6Cults, rwaovary valuu may vttr titiQ:I'I11yfrom tM ntuellln the raw d.m.


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Interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0137.0219

l MPI Project No.: P0003267

Table VIII. Matrix Spike Recovery Summary of PFOA in Whole Body

t Fish Samples (continued)

C8Acld PFO.A P•rlh,~e.v.a.no\~ .kW '<":

AJnount A~ Amt F ountt mount ! ; S"'"Plo Sptlted il1 Sompl~ Recovored RIICO~ \ i

Casaloli<ln IJlQ/al {nllill) i_ngl~) (~ .. ;

OBC-Rl2~PW0~061211

f ICGnlUA S,~ H, U ~ -~ z.o Z.QI ~n nt DBC..f04-IPW003-0-06121 1 I~U71%A llo>a ~soot pPio .,..._, 5000 2.01 NA NA

DOC-F02-IPW004-()..()61211 ,.. 1Qtl7i1U~ J, U pPio •pll<ot 2.0 NO 2.43 122 'i D8C-F02-I~1211 '! ICOU7US Spll K, -pPI> splbt $000 NO NA NA ';O<.J

D8C-F02·1PWOOS..o.o&121 I ~:tallp•L.UPJ>• .. .._l 2.D 1."6 2<113 n

~ DBC..F02..f?W005.0.06 1211 (C0227$M t,.C M, _,.,.. "l>'lool 5000 1.48 NA NA

DOU..f02-MSW001.0.0612QII tcGn7U7 tpk 0, J.l pJ>b ti'IUJ 2.0 , 14 3<17 102

~ DOU.f Ol·MSWool..o.<l!l 1 209 jCO>%JU7 Spa E, ,_ .... ..,. .. ) 25000 , 14 NA NA

00u-f02-MSW00240e 1212 (eiU7fJO .... f, u,... ....... , 2.0 3.05 4.9.5 95

I OOIJ.F02-!,ISW002.0-otil212 ~zum t,.c o. ZSIIII'Pb•l>'tel 25000 3.05 NA NA

DOu-1'02 ·MSWOOl-D-0& 1212 tcOW121 .... H. u """ .,.., 2"0 NR" NR" NR"

P"• DOU-F02-M~1212 _, CCOUnliiS ... ~- .... - 2.5000 NR• NR" NR" ft!

~J DOV-F02-MSW0Q4.0-06121Z

ICOWGII ... .I,U,.,.._) 2.0 1.07 3.82 12a ~'~ [)()IJ.J'02-MSW00+0-061212 t:;

fCOtttflll,. ... - """ .., ... , 25000 1.07 NA NA w DOU-f02-MSW~1Z1Z

t')IWIS1 ... &.. Up ... "f''bb 2.0 387 Ml 77

~ D0u-f02-MSWQOS.!l-Oii, 212 !COU7U1 ~II,_,. <t>J'"'I 25000 3!7 NA NA

OOU-F02-l!'W001~1212 JCmr-U tpl D, U .... •IIA•I 2.0 0.62!1 2.85 111

g DOU-F02-IPWOO 14061212 (CIUJIUIP!, .... PP• •-1 5000 0.62& NA NA

DOU-FD2-IPW002-1).001212 pwm ap~~ F. u f'Pb "'''bl 2.0 0.875 230 71

u oou-ro2-IPW002~DG1212 fCOllnU Sill<~.- pp1> ..,.._, 50()() 0.87!1 ,..,..

NA

001.,'.F02·1PW003-0-0612l2 ICIHrF.U Sl>i II. :U _,., ..,. .. , 2.0 1.16 •n 123

~~ oou-F02·1PW003-0-06121 z tcaU7i34 SpOt, Iiiio~ ppll """'") 5000 176 NA NA

H DOIJ. F02·1PW0Qo4.0-061212 (Cl>IJ71M SJIIt J, L1""' •-1 2.0 NO 2.21 111 DOU·f02·1PW004-0.061 212

tc•mw '"" K . ...,. """ '"'"' 5000 ND NA NA ·'

NO • !'lot·- ot 0< obow lhiK<:-blo LOO lllpOI1IOd "'T- II NA o,..., ~. '!1u m.U. .,. .. .....,..,.,_-not""~ 10 ......... ~10< ttQ ¥1aly1a NR" • Nol ,.poo1od dua t~ <JJOI!ItJ conlrallolufu: ... Tlble IX lor -.!radood ...,plo i'UUIIs.

''I Hole: Since !hit 0""""'1 I- lhowa- tuulto, .... OY«y vthiOS IMY '""' ~y frOIII!M YlluH lrl 1M taW~ l ' j


;

'"· lnterim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0137.0219


Table VIII. Matrix Spike Recovery Summary of PFOA in Whole Body Fish Samples (continued) ' ' t .

CS Acid PFOA Perflt.lillrCX>CUI"Oie Mid

Amo<lnt Avg Ar1\t FOII><I Am0U111 S4mple 'Spiked In Salllflle R~;~ R~';"'Y D•acriPtion (nQig) (,gig)

DO~F02-IPW00~1212

(C01UU6 tlf>l< L, 2.D ppb oolkal 2"0 1.10 2.62 76 f: DOV-FOZ--4PW00~()..06,l12

(COUTU& Spk M, 5000 ppiJ '""''I 5000 1.10 NA NA u Dl1-FC2-MSW001.()-06120i (COU7U7 &oJI 0, U ppb apAce) 2"0 0.339 2"37 102 {,

DL 1-F02-MSW001-0·061200 u (C0221Uf 81>111!, I !lOt> Pill> splkloj 1000 0.339 NA NA

OL 1-F02-MSW002.o-061201i (COUTUt tlf>l< F, 2.0 ppb aplklo) 2"0 0,399 2.99 130

~ OL 1-F02-MSW002.o-0612C$ tcom~n Spto G, 1000 ,J>b •t>ll<tl 1000 O.JW NA NA

DL 1·F02-MS'A'003400 1200 (COJ!7ut S,0 H, U ppb spil<oj 2.0 o.•os 3.t)1 130 n DL 1-F02-MSW003-0-081 ZOO

fCOU'IUI s-,t I, 1000 m -· 1000 O"ltDS NA NA

D\.1-F02-MSWOO<I.C.001 ZOO (C02%7UO Sflk .J,U ppb apltof 2.0 o.m 2.1S 121 -Dl1-F(I2-MSWOO<I-e.oe1209

I(:OU1r.oo .,... K.- ppiJ -· 1000 0.330 NA NA

DL 1-~-MS'A'OOS-0-061 Z09 tc4W'Ut spit L.!.G ~~~~~ .,..., 2.0 O.A90 3.05 128

[1 DL 1-F02-MSWll05-0-061209 (CNDUI SJ11 M, 1000 l'fl> 1pllat) 1000 0.490 NA HA

Olt-F02-IPW00140612, 2 ((;OUJMZ SpkD,:Z.OpPI> -~ 2.0 0.3011 1.H 72 'ill DL 1-F02-IPW001-0-06121 2 t \ fCOU7141 a,~! I!,-~~~~· opiU1 200 0.306 NA ~ u Dl1·F02-IPWOOZ4061212 (COU714.1 a,ll f', 2J1 ppb aot•l 2"D 0.338 2.N 98 u Dl1-F02-IPW002-0-061212 ICIZJTMI St* 0. 2M ppll- 200 0"33& NA NA

DL1-F02-If'WlXI3.0.001212 IC<lU7'"" St* H.UJOPI ....._.1 2.1) C.Wil 1.56 ~3 u DL 1-F02-IPW00).0-061212 (c:nzTW Spli ~.lAO~ tplko) 200 0.309 NA N.O.

OL 1-F02-IPW004-0-0a1215 (CcmTW Spli .J. U1 ppll .... a) 2.0 0.263 DO 102 fi DL 1-F02--lf'WlXM-0.06 121 ~

[Cl>UlW6 &plo K, lilt ppl> "P"'"" 200 0.263 NA NA

Dl1-F02-IPW005-0-061215

~ ~ (CUW!A5 "'* L. u ~,pb aotllel 2.0 0.~24 1.7! 63

Dl1-F02-IPWOOS-0-081215 i (Cittl'MI Spli II,..., 1'1'& lpii<O) 200 0.524 NA NA

l

DMC-F02-MSW001-C-Oe1209 f. (COUl'ln a,ll D, U Pill> lpllool 2.0 NO 239 120

~ DMC-F02-MSW0014061209 t ICC~ Spli 1!, tOGO pllb '''""' 1000 ND NA NA

NO~ Not d<ltectadll Cit-"-~& lOQ reported In Tobie fl. f W. • N<lt ~ Till• l!'latnll Ojllk• conotnlt1lli1on wu lllJt UH<t to aueulhe OCQnC)' lor 11111 analyte. llotb·. 5I.--_...,~a .. ..-arounc~e<~. multi. ,.,..Wl'Y-11\&'i toty lllgl\tiVIr<>WI 1M -In 1M row ftta. L

MPI Research Page 42 of 151 [_

fl

i


Table VIII. Matrix Spike Recovery Summary of PFOA in Whole Body r Fish Samples (continued) r

C8AeidPFOA f'erfluarooctanok; Ackl

Amount Avg Amt Found Amount < ' Sam pia Spiked In Sample Recovered Recovery

Description {OQIJI) (1)QIO) \nQIID~ . (%_l '-'·"•

DMC-F02-MSW002-0.061209 ,. \

tot 1' \ (C022T144 Spk F, 2.0 PPb tpiu) 2.0 0.570 2.29 86 ~~-'

DMC-F02-MSW002-0-061209 (C0227144 Spk G, 1000 ppb •!Hk•l 1000 0.570 NA NA r !

I DMC-F02-MSW003-G-061209 I I (C0221'14t Spk H. .2.0 ppb apike) 2.0 0.423 2.47 102

DMC-F02-MSW003-0-061209

fl (C0227W Spl< I, 10011 ppb 1plka) 1000 0.423 NA NA ,J DMC-F02-MSW004-0-061212

(C0227650 Spk J, 2.0 ppb aplh) 2.0 0.842 2.23 69

fi DMC-F02-MSW004-0-061212 (C0221'850 Silk 1<, 1000 ppll1pike) 1000 0.842 NA NA

DMC-F02-MSWOOS-0.061212 ..,. (C022TG$1 SQII L, 2.0 P1>b 1plke) 2.0 0351 2.56 110 I DMC-F02·MSW005-0-061212 (C0227811 Spl< M, 1to0 ppb aplko) 1000 0.361 NA NA

q DMC·F02-IPIN001-D-061212 {C022TH2 Spit D, 2.0 ppb *Pihl 2.0 NO 1.72 86 DMC-F02-JPW001-0-061212 {C0Zl78$2 Spk E. 200 ppb lplkel 200 NO NA NA

'1 DMC-F02-IPIN002-().()61 212 ~j (C02275U Spk F, %.0 ppb apike) 2.0 NO 1.83 92 DMC-F02-IPW002-0-061212

u (C0227653 Spk G. 200 ppb •pike) 200 NO NA NA

DMC-F02-4PW00~-001212 (C0221'654 Sf* H, 2.0 ppb lplk&) 2.0 NO 1.50 75

OMC-F02-IFW003-0-061212

D (C0Zl7654 Spl( I, 2tO ppb I~IIA) 200 NO NA NA

DMC-FQ2-IPW004-0-061212 {00227155 Spk J, 2.0 ppb apll<•• 2.0 NO 2.42 121 n OMC-F02-IPN004-D-061212

~. 1 (C02ZT51i5 Spk K. 200 ppb •pike-) 200 NO NA NA

DMC-F02-IFW005-0-o61212 i'') (C022765f Spk I.. 2.0 ppb ~k•l 2.0 NO 1.42 71 I DMC-F02-IP'N005-0-o61212 ~- I

(COZ2704t Spll M, 200 ppb Spike-) 200 NO NA NA

; ' Average: 99 ' ·J Stanc:fard OevlaUon: 20

NO • Not detected at or at>Qve the acceptable LOO report*<~ In Tabla 111. NA • Not appl•cabla. ThiS matrix spike ccooenlratnor\ was not usee~ to 8llaess the accuracy lot 1tlla analyte. Note: Sinco thla aurnmaty table &bows rovndea rKtllts, recovery valun may YafY sii;Mly from 1he values In tht raw data.



Table IX. Matrix Spike Recovery Summary ofPFOA in Re-extracted Whole Body Fish Samples

ce Acid Pf'OA PertfuontOC1a:nOIC JJJ:~

Amount Avg Amt Found Amount Sample Spiked if\ Sample Recovered Raeovery

Oeocr1pt>on fng/g) _(nglg) (no/al (%)

DOU·f02-MSW003-0-001212 (CP227&21 Spl< ~. :LO ppb oplko) 2.0 1.23 3.01 99

AveraQO: 89 Standard Dav~tlon: NA

Not•' Slftce thi. oummuy tabla shows tOUnd~ rasutto. rec:o.ary val"" may vary slightly !<om thtl v.U...s In the raw dat&


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Table X. Matrix Spike Recovery Summary of PFOA in Clam Samples

C8Acld PFOA PllffluoiiXI~olc kid

Amount Avg Amt Found Amount Sample Spiked in Sample Recovered Recovery

Oescril)tioo (~gig) 1ngfg) (r.g/g) (%)

DL3-I02-cFW001..()-()61219 (COU71i68 Sp\ D, 2.0 j>l>b Spikt) 2.0 0.219 2.95 137 DL3-102-CFW0014061219 ii::0%27658 8pk 1!, 20 ppb Spill&) 20 0.219 NA NA

Dl2-102..CFW001-0..Q61219 (COUTI>5e Spit F, :Z.O ppb Splh) 20 0.360 2.78 121 Dl2-102..CFW001 Q-061219 (C022T6H Spk G, 20 ppb Splltet 20 0.360 NA NA

DBC-102-CFWOO 1-0-061219 (COU76GO SpK H, 2.0 ppb Sp••l z.o 0899 3.215 118 DBC-102-CFW001.0-o61219 (C022T&a0 Spt ~ 24 ppb Spike) 20 0.899 NA NA

DOU-102.CF'N001-0-061219 !COU7M1 Sp\ J. 2.0 ppb Spike) z.o 0.6<45 3.04 110 DOU-102-CFW001.0-061219 (C0227tf1 Spk 1(, 20 ppb Sp!M) 20 0.8-45 NA NA

DU-102-CFWOOt-o-061219 (C0%27662 Spk L, 2.0 ppb Spike) 2.0 0.211 2.08 93 DU-102-CFW001-Q-061219 (COU7662 Spk M, 20 ppb S!>iMI 20 0.211 NA NA

OMC-102-CFW001.0-001219 (COUTMS Spk ~. 2.0 ppb Splk•l 2.0 NO 1.73 87 OMC-102-CFW001-C·061219 (COU7at! Spk 0, 20 ppb Spiktl 20 NO NA NA

A~erage: 111 Stllndard Devlltlon: 19

NO "' Not d&leclod at or above fle ~ptable LOQ reported in Table V. NA • Not ~b~. Thia matrix $pike concentratrion was not use<l to auea1 Die accur.cy for lhi• •n11yte. Not&: Since ltllt 1umma.y toable •t.ow. ro~mdad ruultl, lliCCNtry valuH rnay VI'Y 111gtrtty from tii4J vafua In the raw data.



FIGURES


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Interim Report #3- Analysis ofFish and Clam Samples MPI Study No.: 013 7.0219 MPI Project No.: P0003267

Figure 1. Typical Extracted Calibration Curve for PFOA in Catfish Fillet Matrix

• tl1110QC C.ftf~ fil"'t S•t 1,r.Jb(FF'OA)'. "Ou~dr.atl~ R•orun~('t I '>I' w.itl'ltJI\Q): '/• 2.29.-+003 ~ • O.oga+004: x+ EI.J3t+003 (1• OQQ19)

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40o4

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OJ} 0.2 04 0.11 o a ~.o <.2 ,_4 1~ ~.s 2.0 2.2 2.4 2.0 :a 3.0 32 3.4 3.0 3.e 4.0 4.2 4.4 4.0 4.8 &o Conet"trlfion, rt...,..J,..

MPl Research Page 47 ofl 51

Interim Report #3- Analysis ofFish and Clam Samples MPl Study No.: 013 7.0219 MPI Project No.: P0003267

Figure 2. Extracted Standards of PFOA in Catfish Fillet Matrix, 0.025 ng/mL (0.10 ng/g) and 0.050 ng/mL (0.20 ng/g), Respectively

I XC<>1-·1·PFOA (Stlllltlllrtl}41111~'-•••• •n•pl•1oiSSfrotrr 0111ttC.wif1 Aro11: !ltlaJ <II» II~ Holfllll: 1.4'->+H~ cpe RT: t.J2 •ill

·~ !Xl 2000

14.00

1500

"' 3' c:n

~ 1000 11.!6..' "' 3

e~ E. ®a

&!13 7~ Q

J 4 5 e 7 a ' g 1G 11 12 1J 14 1!1 18

Time. ~~nfn.

I '-CG~·2 · PrOA(Sbnd••d)413.Df.l8Q 0 "''" • .. m,lo 2 oi55f<on> 0111()91;,...;11 Att .. 11017 eour.ts .,.•lgM.: Q.OSt+l:lll opt RT· 0 e2 miq

11!52

1000 02~ 1585

eoo "' :;}

~ !100

"' ., <0) s 200

oeo 0

2 ~ • 0 e 0 10 H 12 13 14 i5 18

lim•. mill


. ' l' t . I ' '

p I;

Li

[J

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f:

f' I

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' u

fl . '

I r . I ~-- J

r .. I : . ' }_! ,._'

Interim Report #3 -Analysis of Fish and Clam Samples MPI StudyNo.: 0137.0219 MPI Project No.: P0003267

Figure 3. PFOA in a Control Catfish Fillet, a 0.075 ng/mL (0.30 ng/g) Fortified Catfish Fillet Spike A, a 0.50 ng!mL (2.0 nglg) Fortified Catfish Fillet Spike B, and a 4.0 nglmL (16 ng/g} Fortified Catfish Fillet Spike C, Respectively

I cnt2S03 C..•t••t 1 .l't'O/I turh•-.rJ .fnf46t.t ,,.,. ·cn"'pl* n"' ~H'""' ~111tte.wiff ,.. .. , 4TS2CDM4C. llai~l: T.I.:O+UUJN RT: l.UMi.

1000

4

Tl~t~t. nti" I COM00311)kA1· PfO,& (QC)413,0130Q.O arnu • 1.4..,PI• t3 o1" tfo~ 011100C.Nff Are•: IMIIil eouMt Ht~ht: 1.42•+003 C9t fU: Ql.42 rnin

2 3

1~·"'"'

o . .v

I Cf2!1Mlll~i B.l·PFOil (fJCJ413.IIoOO.t•••· .. .,.l.lt«55fro. tttr.c.Wiitr ~ .. :JZF.flt<>•.,. ~lgM: 5.tS.+fQ<:p RJl J..fl•l•

Tl""•· rnl• I ~liP< C1 · PfCU.(ClC)413.cv.lOej)...,. • ,..,,,. 21 otGO "'"' 011 10tC.ANa: 32e715 oovrf• ~ .. "o._t .a.44•+00a ept AT· a.42 l'l"tirl

1000

3 4

MPI Research

0.42

10 11

14.i1

12 13

Page 49 of 151

Interim F

Figure

I ~Z7~

A¥u:

2000

1900

1000

1400

e 1200

;z;

I !000

000

800

400

:1 #3- Analysis ofFish and CL'm Samples MPI Study No.: 0137.0219 MPI Project No.: P0003267

Chromatogram Representing a Catfish Fillet Sample Analyzed for PFOA (ExyLIMS ID: C0227553, Data Set: 011108C)

·FOA ~kllt>lffll)~1er.J$J.f• .. • ·H-S. 4Sof51HfOM ff11gtC.wit1 <<~Mil» Hoigltt: J.Z7•~•f2 c~ RT: t.-13 •i•

12.()6

12l 14111

Q<O

0.2k

803..,

Timt. min.


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f:l •... .J

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Interim Report #3- Analysis ofFish and Clam Samples MPI Study No.: 0137.0219


Figure 5. Typical Extracted Calibration Curve for PFOA in Bass Fillet Matrix

.13 "' "' 8 ,; e "'

~.3.~

e.oo6

4.~.5

40>6

3.s.e

3.o.e

2~~

2.0~ •

u~

• 1.0~

O.Oo4

o.o 0.2 0.4 0.111 oe 1.0 1.2 L4 1 e 1.a 20 z.:~ 24 2e 2.a ~.II 3.1 3.4 3.~ 3.8 4.0 4.2 4.4 4.11 4.e ~.o Cone.ntutilu· •. ft.O,ImL


•

Interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0137.0219 MPl Project No.: P0003267

Figure 6. Extracted Standards of PFOA in Bass Fillet Matrix, 0.025 ng/mL (0.10 ng/g) and 0.050 ng/mL (0.20 ng/g), Respectively

I XCfZZ7e1·1- PFCIA lS'411dlll<l) 41l.fl".l'!.llllllllt - ,.;wpa 1 "' SS froM l)l,;JfK'."'''II' At .. : fe,illc<>•""- HHtJIIC 1."•..-IIJ<fM RT: '-'3111111

003 1~53

200) ..-1e.o1

"' 5' 1500 ..,: i1i <: 1000 ..-10.14 ~ s

500

0 4 5 e 8 ~ 10 11 12 13 14 15 1&

Time. 11\ih:

I XC122707·2 • P'FOA (SUr~C.JJ.d)•1~.1)13t1Q.O llft\11· '""-P'i• 2 .t" hm 01030iC.-n At4!.1; 132• oounb: Me1ght. 2.74..oo3 09'" RT; Q.C411Hf'r

0!14 3000

~

"' 2000 "' " ;,; 1600 1~.48 'a!

~

~ '1£100 ~ . ..:~...

&l) 11.13...

0 :l 3 4 e 0 9 g 1Q 11 t2 1l 14 1S 1CI

Tlmt. rJ~Irt


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r, k. '

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'. t; ~;

Interim Report #3- Analysis ofFish and Clam Samples MPI Study No.: 0137.0219 MPJ Project No.: P0003267

Figure 7. PFOA in a Control Bass Fillet, a 0.075 ng!mL (0.30 ng/g) Fortified Bass Fillet Spike A, a 0.50 ng/mL (2.0 ng/g) Fortified Bass Fillet Spike B, and a 4.0 nglmL (16 ng/g) Fortified Bass Fillet Spike C, Respectively

I cnutn c-tuii1·PFOtt (Uik.,._J 413. f/JRI .,,. .,..p,. not 55,.,.~, cno:uotG.IOil1 l>t•.tlff>lft>IUti}

2000

.. 1000 e 1ll()l]

7.37 ill&

0 Tlr.-•. rr-!n

I C021l<I!IO'J Spi<A1· PfOA(Oc:)"'13.tl.llCWj) '"'" • ""''I• Ia •IIIII from0103011CArcf: 111i83 IIGI.lfttl l'lt~g~t A.01a"'{J()3 tfC RT: g,O;J: min

I ~ *.t Ill· PFOA IQC) .nl._,_, .,.. •HIIIPH 2t <>I 55 t;o• Of*JOIIC...., -· S'lnfN·- Haig., 1.1 .. __ RT: 1.&3•1•

.. fK)OO,(II)

a. ... ~ eooo.CIIl

i .QQOO.OO

H!llt,tnln.

I ~ S~C1- PfOA(OC)4131l05Q_I) Jme~~l•2i M5!1 fr•*010308CJillrlli'ft .WV.J: 30WO O'l'uo.~tl ~"tilt: 0.46....003.,. JH: ~.153 mN\

MPI Research

11

15.61

1l 13 14 Hi

Page 53 of 151


Figure 8. Chromatogram Representing a Bass Fillet Sample Analyzed for PFOA (ExyLIMS ID: C0227581, Data Set: 010308C)

J C0227Sn ·PFOA (f.lllt-)41:l.IY.!n.f••• •• ,.,p,. J4of55fiY>Ifl OffJOfC.wltf Ana: t7T2eo.,.c.- H>ttJIII> 1.S~+mw- R.T: !J.52•JII

1100

1000

1t500

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Ul

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700

000

600

400

300

200

100

MPI Research

4 6 9 Q Tkf\t, mll'l

15.43

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10 11 12 '3 14 '16 til

Page 54 of 151

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Figure 9. Typical Extracted Calibration Curve for PFOA in Whole Body Catfish Matrix

~ "' e e <

gs.s

g(>d!

e~e

80•~

re.e

'7,o.~

e.th5

eo.~

~ . .,.::s ~.Oe!

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1.~.5

1.0al5

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a o 0.2 0.4 o.c 0.11 1 o 1.2 1.4 1 e t.e 1.0 z:z 2.4 2.e 2.e :J.I) '.2 3.4 3.0 i.ll ~.o 4.2 4.4 40 "~·• e.c (orll""tr.cl•n. r.~mL


Interim Report #3 -Analysis of fish and Clam Samples MPI Study No.: 0137 0219 MPl Project No.: P0003267

Figure 10. Extracted Standards of PFOA in Whole Body Catfish Matrix, 0.025 ng/mL (0.10 ng/g) and 0.050 nglmL (0.20 ng/g), Respectively

I XCPJ2f ... f -PFOA {Shtrd#NI}#3.0!3C'Af•lllll ·#6Mpl•1ofSSrrUI IJ3210M.wilf Aro•: 17P4 ct>llll,. 1*/gllt: 1J ... •f03 <p• RT: 9.62 mi•

4000

"' 3000 :'} ~ ·o; ZOO()

"' !!! s;

1000

0 3 5 & 8 Q 10 11 12 1J 14 1:5 '8

Time, ~ln

I XC032108·2 · PfOA {'iUf\IS.,4) 413.CU"JflQ Q •mv · Ut'nJ\•l 1>f 00 tro~ 1);3~108~~

A'••: 26408 cto\Jnk M•!-&"t 4.10.-+003 ops R!: Q e.!J min

0000

; 400C

t 3000 c: .!! 2000 .s

1<lXJ

0 2: 3 4 e • 1 a g ID .. u 13 14 15 1tS

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Figure 11. PFOA in a Control Whole Body Catfish, a 0.075 ng/mL (0.30 ng/g) Fortified Whole Body Catfish Spike A, a 0.50 nglmL (2.0 nglg) Fortified Whole Body Catfish Spike B, and a 4.0 ng/mL (16 ng/g) Fortified Whole Body Catfish Spike C, Respectively

I Clr.192:5s• C...trof t • PFOII (1Mb~-) 413.oV.lUJ ""'" •n~~tpl. 1% ~f SSft- ll.l21ttA.will' An.r.2,ffc11MIItlt HolgH:l.JJt+fGJcPI RT: '-~llfilf

Ttflfl.•.~m I C02'Q2568' &:aM .A1 .. PF"OA (OC)413.Q131)S.O .,.u • un~~~•• 13 et&5 froJII'I 032t08A..Mft Ar•~: 3o41CJ7 eo"~:tts H•ifht 7..00t+003 o;ps RT. QI.OO l"'lift

nmt.,.lll

0.~1

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I U212S51Spt 113·PFOA IOC).tr.lfi3Ut••• ... ,.. 21oi5SfTollf r:RJHA."""' m.~t: 114-Ufe~~~tlltl Holg/kt: 2.M•+H4~ RT: I.SIMIIt

20o4

Cl.

n, ••. ..,,. I IXI:!G~ $pi< C1 PFOA (Qt)413.01!!111;i,O •m• · Slmpl•l1 .. "f""' 0321~ AI••: eoaucz cowrtJ H••l&fht 1.n.....co:s ert R"T: g.a7 ,..,,.

8.41

MPI Research

CI.5G

0.81

u 13 14 15 ~

Page 57 of 151


Figure 12. Chromatogram Representing a Whole Body Catfish Sample

Analyzed for PFOA (ExyLIMS ID: C0227606, Data Set:

032108A)

I C~227SK·PFOA jUr.t.o-}4'13.CII3H.fiiiiW """'P'* ~of S5frt>m fJRf~M.wltr Ar•l: 11312co;nr~ Holgll(: 1.1-f••HJ ~ Rf: lt.S4•11f

2000

1600

1COD

"' 1q)() e ~

~ 1200

];

1000

90C

MPI Research Page 5& of 151

f

r. ! : ' ! t :

f'' ~ : t;

;


Figure 13. Typical Extracted Calibration Curve for PFOA in Whole Body Bass Matrix

., E

" 0 <> •• e <

l.4•5

22t5

20ol!

•.e.s

l.ec5

1.4•1!1

1.~.5

1.0<6

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4.00'1

~0~~~~~~~~~~~~~~~~~~~~~--r-~~~T-~-,--~-r~--~ o.o 02 o.4 o.e o.a 1-0 1.2 1.4 ~~ u 2.0 2.2 24 25 2.8 J.o 3.2 J.-4 a.e 3.8 4.0 42 4.4 45 4.8 ~.o

Coo~n1u1lon. lllii/~


Interim Report #3- Analysis offish and Clam Samples NfPI Study No.: 0137.0219 MPI Project No.: P0003267

Figure 14. Extracted Standards of PFOA in Whole Body Bass Matrix, 0.01 ng/mL (0.10 ng!g) and 0.02 nglmL (0.20 ng/g), Respectively

I .XC042ZOII·1 • PFOA (St•INI•rd} 411 flll"-f .,., • nwpl• 1 ot SS fNiff 11424ff!B.wtff At.,; Uff C04!1ft:t Hciwltt: 2-''*..o2,.,. liT: 9.55 ,[,

QM 1~.21)

300

zoo ., fr 200

~ 100 " ~ •oo

~

0 s 4 II 7 $ g 10 11 12 13 14 ~~ ~~

Tim•. m.Jft

I ;t.CI)42:209.2 · PfOA (etand•rd)41~.013MI.O '"'"· saropl• Z <I~$ from 042-11-Ate.t: 1Q37 counts: Htieht. 2.1~ee+002 qa:s RT: Q.e6 milll

Q~~

300 i3.23

Z60 ., fr 200 ~ II! 1~ c ., :s 100

00

0 ) 4 ~ e ~ 10 11 12 1:1 14 15 "' llmc. lflllf'l


I, I

l

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Interim Report #3- Analysis of Fish and Clam Samples MPI Study No.: 0137.02\9 MPI Project No.: P0003267

Figure 15. PFOA in a Control Whole Body Bass, a 0.03 nglmL (0.30 ng/g) Fortified Whole Body Bass Spike A, a 0.2 ng/mL (2.0 ng/g) Fortified Whole Body Bass Spike B, and a 4.0 ng/mL ( 40 nglg) Fortified Whole Body Bass Spike C, Respectively

I C-.305047 Ci>IIIJ'•I1- PFOA (Uirt-) 41l.MU. f.,., ·••"'P,. 12 t>I5Sfr- UUOIIJ..wttf An•: tnco.v,.u lfll.fgii'C ,_24it••t2~ R"l': l.U"';,.

Tl"'•· mtn-

1 C()3()&147 SpkA1· PFOA(CC)'\13~0 •mu.,.,.pto13 ol641<om042-IP ... If .AHa: 23W tounb Hti;ht 4.$2•.-oo2 epj ~T: O.e3 f'l'lll'l

I ~ S,. 83 • PFOA (QCJ 413.1130.1 ••• •• ..,.,. ~ "'~ II'•• U24Htl.wRt IIIN: 1153f-•• Hti9tt: Z.66fo+ftJ- RTI aO•I•

1000

Ti.lt\e, l'Jiilll

I C0305041 Splc C1 • PfOA(OC) 413DIJaQI.O .lt:rl\1· Utftl'-1• 21 •164 f'Jo.w'l 0424089.writ Ate •. '~~\If)~ Jiejfl'lt 4.3e.+oo4""' ,::tt; o.ee 11'\l~

10o4

1imt. mta


Interim Report #3 -Analysis of Fish and Clam Samples MPI Srudy No.: 0137.0219 MPI Project No.: P0003267

Figure 16. Chromatogram Representing a Whole Body Bass Sample Analyzed for PFOA (ExyLIMS ID: C0227637, Data Set: 042408B)

I Gf227637 • PFOII(IJdlfoww} ~1J.IIf.JSU ••• -u .. pl• JO ~~ S5 frrn• UU.'III.wifl An-1: 2214 <<l•- 111>/gltl: 4.35. +-H2 q» RT: :I.U ,.;,

~

:)00

~ ;,;

~

~ 200

1~

'100

~

0

MPI Research

3 4 8 g

Tu"t.l'lfln

13.23

13.015 .....

Page 62 of 151

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Figure 17. Typical Extracted Calibration Curve for PFOA in Clam Matrix

~ r: ::> 3 .r ., <

7.00'1 • 7.()0'1

e.eo4

Mt4

MO'I

~1)0'1

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1.00'1 • 2.~t'l

• 2.0t4

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1 Oo4 • OCWO

0.0 0.2 0.4 0!1 08 1D 1.2 1.4 1.8 1.8 2D 2.2 2.4 2.ll 2.t ;),0 l-2 3.'1 3.$ 3.$ 4D .. .2 4.4 40 ... 50 Co~ntJ•tiM, nQil'JIL


-----------------------------------Interim Report #3 -Analysis of Fish and Clam Samples MPI Study No.: 0137.0219


Figure 18. Extracted Standards of PFOA in Clam Matrix, 0.025 ng/mL (0.10 ng/g) and 0.050 ng/mL (0.20 ng/g), Respectively

1 xcrntsoi-1-PFOA tst""""'"' 41J.(J(J~f ••• ·u•pl• 1 """"'"' 03~m Ar~•: 111l<o••lll*lgllt: 1.~+1102 ep1t RT: f.4J .,,.

200

fr 150

~ Ul 1(X) c: s s

50

0

tlme, rrlr.

I .X.Cflei0006•2 • HOA ('St.1ndard) 4 t3,01300.D amt.t ~ ~,....,fwl' vf 0111em ~A .... n Alt.l: 1Mlli o-urttl 1-l•JoM: 2..B'2~r+002 ... RT· I) 63 m!J'I

250

<II 2(X) e-~ 1!!10 ;a c:

~ 100

50 034

0

MPI Research

2.40

2 3 4 8 g Tll'l'lw-. min

13.41

10 13 15

Page 64 of 151

t:

tl Fl L ~--:,

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Figure 19. PFOA in a Control Clam, a 0.075 ng/mL (0.30 ng/g) Fortified Clam Spike A, a 0.50 ng/mL (2.0 ng/g) Fortified Clam Spike B, and a 4.0 nglmL {16 nglg) Fortified Clam Spike C, Respectively

I c•mn• eo,trol1· PFOA turk-.) 4r.J.w:JU.I ••• .n,.,.,. n "' 6f rr.,. o5ci-. ..;IJ ~•: 1otu;m JltfiJ/It.!J.3•-2q>a RT! i.S1•J•

Ill) ..0.00 UIJ IIIII

4 0 8 Tim., 'fhilf

I =711 Spi<A1 • ~~OA(QC)413.D/38Q.O •m• · ,.,,,_ 13 of &I f!om ~"""' Alu: 2e40 010~o~nCJ H•ioht o4.47.....oo2 C!Jl" ~r·g.• lfll-n

Q.!\1

I Cf2Stm.S,.tt13•Pf'Oit!QCH1:Lw.JA.f••• ·oa.-p~t 2hiC1rn.. fSISIIA.Aru: rru~ ... - ftH~ f.Tio....,_ RT: '-4t•l•

nm.e, mJ,

I CC12:1:1Q27t lplli'C1 • t"P:OA(QC)413-013:eG1.0 J!fftV• Ul"f'l~a 2'1 fl'tft1 fretn CII5CIII5C&A-*" Aiu;41a!5Mo.~.~nt.: lftJ.t~ 1.01••00..cs- Rl;Q.<C ~t~~lt~

eooo.oo

2000.00

r-. •• min

MPI Research

13.52

Page 65 of 1 51


Figure 20. Chromatogram Representing a Clam Sample Analyzed for PFOA (ExyLIMS ID: C0227658, Data Set: 050508A)

I Cf227C,_ • PF()A (Urklt-W} 4f3.f<JU.t ••• • IIIMpt. 3t of •1 fro• t$t$t8A.wilf Al't•: 1~1 co•lrl» Heig.ta 1. PC.. •lit? op.r RT: 'I.«<"''"

280~ lOG

z.., I 220

200

160

~ •eo \ ;:; 14Ch'

-~ I

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100

eo

2 3

MPI Research

12.il7

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Page 66 of 151

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ATTACHMENT 2

GROUNDWATER SAMPLING TECHNICAL PROGRESS REPORT

August 2008

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GROUNDWATER SA1'\1PLING TECHNICAL PROGRESS REPORT

JM AND DYNEON DECATUR, ALABAMA

As part of the groundwater assessment associated with the former sludge incorporation area, 17 monitoring wells were constructed from November 2005 through April 2006 to evaluate groundwater conditions associated with the perimeter of the property. The locations include two well clusters located west of the former sludge incorporation area (monitoring wells 601RJ601S/601L and 602RJ602S/602L), two well clusters south of the former sludge incorporation area (monitoring wells 603R/603S/603L and 60IRJ601S/60IL), one well cluster at the east side of the former sludge incorporation area (monitoring wells 138RJ138S/138L in Field 11), and one well cluster on the east side of Bakers Creek (monitoring wells 605RJ605L).

Initial sampling and analysis of groundwater for PFOA was performed in April 2006 and reported in the October 25, 2006 Quarterly Status Report and the 2008 Data Assessment Report. A second round of groundwater sampling of the off-site monitoring well clusters 60 I through 605 was performed in September 2006 prior to the abandonment of the 60 I R/60 I S/60 1 L wells before commencement of construction activities at that location. In addition, groundwater samples were collected from the 605R and 605L wells in April 2008. Analytical results for the September 2007 and April 2008 sampling rounds are tabulated in Table I and shown in Figure I. The groundwater laboratory data packages for PFOA (Interim Reports 4 and 5) are provided in an appendix to this attachment.

Table 1 Off-Site Groundwater PFOA Concentrations September 2007/April 2008

Sample ID Well Sample Average PFOA

Date (ng/mL, ppb)

DAL-GW-601R-0-070920 601R 20-Sep-07 0.179 DAL-GW -601 S-0-070920 601S 20-Sep-07 0.221 DAL-GW -601 L-0-070920 601L 20-Sep-07 11.0 DAL-GW -602S-0-070920 602S 20-Sep-07 0.363 DAL-GW-602L-0-070920 602L 20-Sep-07 2.75 DAL-GW -6038-0-070920 603S 20-8ep-07 1.29 DAL-GW -603L-0-070920 603L 20-Sep-07 0.346 DAL-GW 6048-0-070920 604S 20-Sep-07 l.ll DAL-GW -604L-0-070920 604L 20-8ep-07 1.30 DAL-GW -605R-0-070920

605R 20-Sep-07 0.0532

DAL-GW-605R-0-08040 1 01-Apr-08 0.105 DAL-GW -605L-0-070920

605L 20-8ep-07 31.6

DAL-GW -605L-0-08040 1 01-Apr-08 4.65

J.I3M-DECA T\FC WoO< Plan\0808 Status Report\Tables\Tabte 1 - 011-srte GW xts

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601R' I 20-Sep-07 601S' I 20-Sep-07 601L I 20-Sep-07

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Figure I

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September 211071.'\pnl 200~

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INTERIM REPORT 3 - ANALYSIS OF FISH AND CLAM SAMPLES IInterim Report #3 -Analysis of Fish and Clam...

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