Document zQ9v3bBX3b0n5bB4mrErr0w97

p. 1 a a6_ 36g~ INTERIM REPORT # 10 - Analysis of Fish and Clam Sample s STUDY TITLE Analysis of Perfl uorobutancaulfonate (PFBS), Perfluorohexanesulfonatc (PFHS), and Pexfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program DATA REOUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 SJUY DIRECTOR Jaisirnha Kesari P.E ., DEE Weston Solutions, Inc . 1400 Weston Way West Chester, PA 19380 Phone : 610-701-376 1 INTERIM REPORT COMPLETION DATE May 09, 2006 PERFORMING LABORATORY Exygan Research 3058 Research Drive State College, PA 1680 1 Phone : 814-272-1039 STUDY SPONSOR 3M Company 3M Building 0236-01-B-10 St . Paul, MN 55144 Phone : 651-733-637 4 PROJECT Pr otocol Number. P0001131 Exygen Study Number: P000113 1 Total Pages : 132 p. 2 Inte:r,m Report #10-Analyais of Fish and Clam Samples Exygen Study No . : P000113 1 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0001131, entitled "Analysis of Perfluorobutanesulfonate (PFBS), Perfl uorohexaneaulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Scrum Using LC/MS/MS for the 3M Decatur Monitoring Program," conducted for 3M Company, is being performed in compli ance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by Exygen Research . I Flaherty rincipal Investigator Exygen Research Jaisimha L,DEE Study Director Weston Solutions, Inc. .r9o6 Dat e Date Michael A ro Da e Sponsor Repr6entative 3M Company Exygen Research Page 2 of 132 } p . 3 Interim Report t# 10-Analysis of Fish and Clam Samples Exygcn Study No . : PM P000113 1 Q ALITY ASSURANCE STATEMENT Exygen Research's Quality Assurance Unit reviewed Exygen Study Number POOOI 131, entitled, "Analysis of Perfl uorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program" . All reviewed phases' were inspected for conduct according to Exygen Research's Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice ' Standards. All findings were reported to the Exygen Principal Investigator and Management and to the Study Director. EhA gg Date Reported to Date Reported to Date Principal Exygen Date Reported In.d Investigator Management to ~i y Director 18 . Raw Data Review and Interim Analytical Report Review 26 . Raw Data Review and Interim Analytical Report Review 08101 -05/05 05/03/06 09/20/05 05/08/06 09/21/05 05/09 106 09/21105 05/09/06 ~ ~5d9UG L haffer Date Tec 'cal I.ead, Quality ISLce Uni t 'Note: All in-lab inspections will be documented 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. Exygen Research Page 3 of 132 p. 4 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : POOO113 1 CERTIFICATION OFAUTHENTICTTY This interim report, for Exygen Study Number P00p1131, is a true and complete representation of the raw data. Submitted by. Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-103 9 Principal Investigator, Exygen : -~ S90 hn Flaherty Date Vice President Exygen Research Exygen Research Facility Management : Richard A . President ini Exygen Research 1- 4401-2c6 Date Study Direc r, Weston Solutions, Inc. Jaisimha esari P.E., DEE Date Weston Solutions, Inc . Sponsor Representative, 3M Company: At;", .4 14a Michael A ro Director of R Sulatory Affairs 6 Date Exygen Research Page 4 of 132 p. 5 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 STUDY IDENTIFICATION Analysis of Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Scrum Using LC/MS/MS for the 3M Decatur Monitoring Progra m PROTOCOL NUMBER : P0001131 EXYGEN STUDY NUMBER: P0001131 TYPE OF STUDY: Residue SAMPLE MATRIX : Fish and Clam s TEST SUBSTANCE : Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and PerEuorooetanesulfonate (PFOS) SPONSOR: 3M Company 3M Building 0236-01-B-10 St . Paul, MN 55144 STUDY DIRECTOR: 7aisimha Kesari P .E., DEE Weston Solutions, Inc . 1400 Weston Way West Chester, PA 19380 STUDY MONITOR: Michael A . Santoro 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 PERFORMING LABORATORY : Exygen Research 3058 Research Drive State College, PA 1680 1 ANALYTICAL PHASE Study Initiation Date: 11/05/04 TIMETABLE : Interim Analytical Start Date : 12/27/04 Interim Analytical Termination Date : 04/17/06 Interim Report Completion Date : 05/09/06 Exygen Research Page 5 of 132 p. 6 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : PU00113 1 PROJECT PERSONNEL The Study Director for this project is Jaisimha Kesari at Weston Solutions, inc . The following personnel from Exygen Research were associated with various phases of this interim portion of the study: Name IAk John Flaherty Vice President Karen Risha Laboratory Supervisor Paul Connolly Technical Lead-LC/MS Amy Sheehan Associate Scientis t Christine Edwards Technician Brittany Kravets Technician Mindy Cressley Technician Krista Gallant Technician Scott Crain Technician Eric Hoover Technician Carlyle Horrell Intern Technician Shawn Robb Technical Lead - Facilities Mark Ammennan Sample Custodian Eric Edwards Sample Custodian Edward Cams Sample Custodia n Exygen Resemh Page 6 of 132 p. 7 Interim Report i#10-Analysis of Fish and Clam Samples ~ Exygen Study No . : P0001131 TABLE OF CONTENTS Page TITLE PAGE .. . . . . . . . .. . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . .. . . . . . . . .. . . .. . . . . . . . .. . . . . . . .. . . . . .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 . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . .. . . . . . . . .. . . . . . . . .. . . . . . . . .. . . . . . . . . . . . .. . . . . . . ... . . . .8 LIST OF FIGURES . . . . . . .. . . . . . . .. . . . . . . . .. . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . .. . . . . . . . .. . . . . . . . .. . . .. . . . .. . . .. . . . . . . . . . . . . . . . .. . . . ..9 LIST OF APPENDICES . . . . . . . . . . . . .. . .. . . . . . . . . . .. . . . .. . . . . . . .. . . . . . . . . . . . . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . .10 1 .0 SUMMARY . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . .. . . . .. . .. . . . ... . . . . . ... . . . . . . .. . . . . . . . . . . . .. . . . . . . . . . . . . . . . . .. . . . . . . .. . . .11 2 .0 OBJECTIVE . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . .. . . . . .. . . . .. . .. . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .12 3 .0 INTRODUCTION. . . . .. . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . .13 4.0 ANALYTICAL TEST SAMPLES . . . . . . .. . . . . . . . .. . . . .. . . . . . . . . . . . . . . . . . . .. . . . . . . . . .. . .. . . . . . . . . . . . . .. . . . . . .13 5 .0 REFERENCE MATERIAL . . . . . . .. . . . .. . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . .. . . . . . ... . . . . . . .. . .. . . . . . . . . . . . . . . . . .. . .13 6.0 DESCRIPTION OF ANALYTICAL METHOD . . . . . . . . . . . . . .. . . . . . . . .. . . . . . . . .. . .. . . . . . . . .. . . . . . . ... . .1 5 6.1 Extraction Procedure . .. . . . .. . . . . . . .. . . . . .. .. . . . .. . . . . . . . .. . . . . . . .. . . . . . . . .. . . . . . . . .. . . . . . . . . . . .. . . . . . . . .. . . . . . . ... . .15 6 .1 .1 Sample Preparation . . .. . . . . . . . . . . . .. . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ... . .15 6 .1 . 2 Glassware Preparation . . . . . .. . . . . . . . . . . . . .. . . . . . . ... . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .15 6 .1 .3 Column Preparation . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .15 6 .1 .4 Sample Extraction . . . . . . . .. . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .. ..1 5 6 .2 Preparation of Standards and Fo rti fication Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .16 6.3 Chrornatography . . .. . .. . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . ... . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..17 6.4 Instrument Sensitivity . . . . . .. . . . .. . . . . . . . . . . . . . . . . . . .. . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . ..17 6.5 Description of LClMSlMS Instrument and Operating Conditions . . .. . . . . . . . .. . . . . . . .. . . . . . .17 6.6 Qaantitation and Example Calcula ti on .. . . .. . . . . . . . . .. . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . .1 8 7.0 EXPERIMENTAL DESIGN . .. . . . . . . . . . . . . . . . . . . . . . . . .. . . . .. . .. . . . . . . . .. . . . . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . .20 8 .0 RESULTS .. . . . . . . .. . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . . . . . . . ... . . . . . . .. . . ... .20 9,0 CONCLUSIONS . . . . .. . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . .. . . . . . . . .. . . . .. . .. . . . .. . . . . . . . .. . . . . . . . .. . ... . . . . . . . . . . . . . . . .. . . . .. . 21 10.0 RETENTION OF DATA AND SAMPLES . .. . . . .. . .. . . . . . . .. . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . .. . . . . . .21 Exygen Research Page 7 of 132 p. 8 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 LIST OF TABLES PM Table I. Summary of PFBS, PFHS and PFOS in Fish Samples .... ................................ ...23 Table II . Summary of PFOS in Re-extracted Fish Samples . ... ....... ........ ....... ............ ........30 Table III. Summary of PFBS, PFHS and PFOS in Clam Samples . .. . . . . . .. . . . . . . . . . . .. . . . . . . . . . . . . . 32 Table IV . Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples . . . . . . . .. . . . . . . . . . .33 Table V . Matrix Spike Recovery of PFOS in Re-extracted Fish Samples . . . . . . . . . . . . . . . . . . . . . . . .46 Table VL Matrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples . . . . . . . . . . . . . .. . . .49 Exygen Research Page 8 of 132 p. 9 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Figure 1 . LIST OF FIGURES PM Typical Calibration Curve for PFBS in Methanol . . . . . . . . . . .. . . . . . . . . . . . ... . . . .. . . . . . . ... . .51 Figure 2. Non-Extracted Standards of PFBS in Methanol, 0.0005 }Ag/mL and 0.001 gJml, Respectively . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . .. . . . .. . . .. . . . .. . .52 Figure 3 . PFBS in Control Fish Blank, 0.00625 ug/rnL Fortified Control Fish Spk A, and 0.025 pg/mL Fortified Control Fish Spk B, Respectively . . . . . . .. . . . . . . . . . . . . . . . . . . .. . .53 Figure 4 . Chromatogram Representing a Fish Sample Analyzed for PFB S (Exygen ID : C0049478, Data Set:061605E) . ..... ... ............ .... ..... .... ................54 Figure 5 . Typical Calibration Curve for PFHS in Methanol .................. ................. ..... ..55 Figure 6. Non-Extracted Standards of PFHS in Methanol, 0 .0005 g/mL and 0 .001 pg/ml,, Respectively . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .. . ..56 Figure 7. PFHS in Control Fish Blank, 0 .00625 g/mL Fortified Control Fish Spk A, and 0.025 g/mL Fortified Control Fish Spk B, Respectively ......... .....................57 Figure 8. Chromatogram Representing a Fish Sample Analyzed for PFHS (Exygen ID : C0049478, Data Set: 061605E) . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . ... . . . . . . .. . . . .. . . .58 Figure 9 . Typical Calibration Curve for PFOS in Methanol . . . . . . .. . . . . . . . . . . .. . . . . .. . . . . . . . . . . . . . . . .59 Figure 10 . Non-Extracted Standards of PFOS in Methanol, 0 .0005 g/mL and 0.001 }tg/mL, Respectively . . . . . . . . . . . .. . . . . . . .. . . . . . .. . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . .60 Figure 11 . PFOS in Control Fish Blank, 0 .00625 g/ML Fortified Control Fish Spk A, and 0 .025 }Lg/mL Fortified Control Fish Spk B, Respectively . .. . . . . . . . . . . . . . . . . . . . . . . . . . . .61 Figure 12 . Chromatogram Representing a Fish Sample Analyzed for PFO S (Exygen ID : C0049478, Data Set :061605E) ........... ........................... .. ... ..... ..62 Exygen Research Page 9 of 132 P . 10 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 LIST OF APPENDICES an Appendix A Study Protocol P0001131 (Exygen Study No. P0001131) with Analytical Method V0001783 : "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS", Protocol Amendments I an d 2, and Deviations 2 and 3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .63 Exygcn Research Page 10 of 132 P . 11 Intetim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 1 .0 SUMMARY Exygen Research extracted and analyzed fish and clam samples for the determination of perfluorobutanesulfonete (PFBS), perfluorohexanesulfonate (PFHS), and per fluorooctanesulfonate (PFOS) according to Exygen Method V0001783 (Appendix A) . The Emit of quantitation (LOQ) for PFBS, PFHS, and PFOS in fish and clams was 0 .2 ng/g. For one sample (C0048133) only one gram of fish was used for extraction, so the limit of quantitation for PFBS, PFHS, and PFOS in this fish sample was 1 .0 ng/g. The initial analytical results associated with fifty-onc fish samples are not reported (NR) in Table I because the endogenous levels of PFOS were too high to calculate accurate matrix spike recoveries. These samples were re-extracted and the results of the reanalyses are summarized in Tables H and V . Analytical results and assessed accuracies for the analysis of PFBS, PFHS and PFOS found in fish samples are summarized in Table L Analytical results and assessed accuracies for the analysis of PFOS found in the re -extracted fish samples are summarized in Table IL Analytical results and assessed accuracies for the analysis of PFBS, PFHS and PFOS found in clam samples are summarized in Table III . Laboratory matrix spikes that were in the appropriate concentration range (primary concentration less than three times the spiking level) were used to calculate the assessed accuracies. The average percent recoveries standard deviations for PFBS, PFHS, PFOS in fish samples were 79% t 13%, 94% 12%, and 85% 20%, respectively . Fortification recoveries for PFBS, PFHS, and PFOS in fi sh samples are summarized in Table IV. The average percent recovery standard deviation for PFOS in the to -extracted fish samples was 109% 20%. Fortification recoveries for PFOS in the re-extracted fish samples are summarized in Table V . The average percent recoveries standard deviations for PFBS, PFHS, PFOS in clam samples were 84% 10%, 93% 13%, and 73/. 16%, respectively. Fortification recoveri es for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI. The sample IDs assigned by the c lient follow this formula: Dxx-x0l-xxxxxx-x-04xxxx. The first string begins with D for Decatur, Alabama and the xx defines the sampling area within the Wheeler Reservoir of the Tennessee River where : DL3 = Up river Letter of Intent (LOI) sampling location LOC-3 DL2 = Cross river LOI sampling location LOC-2 DLI - Downstream Fox Creek mouth LOI sampling loca tion LOC-1 DBC = Bakers Creek mouth DOU = Cove at 3M WWTP outfall DMC = Downstream Mallard Creek mouth Exygen Research Page 11 of 132 p . 12 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 The second string defines the general category of the biota sample and the sampling round where : F01 = Fish sample first round I01 = Invertebrate sample first round The third string defines the species (first two characters), the sample type (third character), and the sample number (last three characters) within that sampling area and type of sample where: IP = channel cadish (Ictalsu= punctatus) MS = largemouth bass (Micropieru.s salmoides) CF = Asiatic clam (Corbicula fluminea) F - Filet tissue sample W = Whole body sample 001 through 005 = sample number within the sampling area and sample type The fourth string (single character) additionally defines the sample type where: 0 - Primary field sample I = Field duplicate sampl e 2= Equipment rinseate blank sample The fifth string defines the sample preparation date in YYMMDD format . Examples of this sample ID system are : Sample DBC F01-IPF0040-041021 is the filet tissue sample prepared on October 21, 2004 from the fourth channel catfish collected at the Bakers Creek mouth sampling location. Sample DLl-F01-MSW002-0-041104 is the whole body sample prepared on November 4, 2004 from the second largemouth bass collected at the Fox Creek mouth sampling location . 2.0 oB.> EcrivE The objective of the analytical part of this study was to determine levels of perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) in fish and clams according to Protocol P0001131 (Appendix A) . ExySen Research Page 12 of 132 p . 13 Interim Report #10-Analysis of Fish and Clan Samples Exygen Study No . : P000113 1 3.0 INTRODUCTIUN This report details the results of the analysis for the determination of PFBS, PFHS, and PFOS in fish and clam using the analytical methods- entitled, "V0001783 : Method of Analysis for the Determination of PerEluorooctanoic Acid (PFOA) in Fish and Clams by LCJMS/MS .,, The study was initiated on November 05, 2004, when the study director signed protocol number P0001131 . The analytical start date for this interim report was December 27, 2004, and the analytical termination date for this interim report was April 17, 2006 . 4.0 ANALYTICAL TEST SAMPLES Forty fish samples (Exygen ID C0048126-C0048165) were received on dry ice on October 23, 2004 from Tim Frinak at Weston Solutions, Inc . Fifty-six fish samples (Exygen ID C0049450-C0049505) were received on dry ice on November 6, 2004 from Charles Young at Weston Solutions, Ine . Twenty-six fish samples (Exygen ID C0056354C0056479) were received on dry ice on January 13, 2005 from Tim Frinak at Weston Solutions, Inc. Six clam samples, consisting of whole clams from each sample site (Exygen ID C0056480-C0056485) were received on dry ice on January 13, 2005 from Tim Frinak at Weston Solutions, Inc . A whole Whiting (Family: Gadidae) was purchased from a local grocer by Ed Cams on December 20, 2004 and was used as the control fish (Exygen ID C0054391) . The samples were logged in by Exygen personnel and placed in frozen storage . Sample login and chain of custody information is located in the raw data package associated with this interim report. Storage records will be kept at Exygen Research . 5.0 REFERENCE 1+iATERiAL The analytical standards, PFBS and PFHS, were supplied by 3M . PFBS was received from 3M at Exygen on July 6, 2000, and May, 13, 2005 . PFHS was received from 3M at Exygen on January, 20, 2003 . PFOS was purchased from Fluka Corporation and was received at Exygen on April, 23, 2003 . The available information for the reference materials is listed below . PFBS and PFHS were stored frozen and PFOS was stored refrigerated. Exygen Research Page 13 of 132 p . 14 Interim Repoi4. #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 CoMM,md l :xygan Inventory No . I&,t~ Purity (%) Expiration Date PFBS SP0000252 101 96.7 12/04/06 PFBS SP0005726 10 1 96.7 12/04/06 PFHS SP0002401 SE036 98.6 10/18/06 PFOS SP0002694 430180-1 101 .2 10/31/07 The molecular structures of PFBS, PFHS and PFOS are given below : PFBS Chemical Name : Perfluorobutanesulfonate Molecular Weight : 338 supplied as the potassium salt (C 4 F9SO3K') Transitions Monitored : 299 -> 99 Structure: F 03 . F F 4-' F F PFHS Chemical Name: Perfluorohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (C6F13SO3K ) Transitions Monitored : 399 - ), 80 Structure : F F F F 4 F, F -- F F F F 503- PFOS Chemical Name : Perfluorooctanesulfonate Molecular Weight 538 supplied as the potassium salt (CaF 1 7SO3K) Transitions Monitored: 499 -). 80 Structure: F F _ 03 F F F F F F F F Exygen Research Page 14 of 132 p . 15 Interim Rcport #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 6.0 DESCRIPTION OF ANALYTICAL METHOD The analytical method "V0001783 : Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS" was used for the fish and clam samples in this study . 6.1 Extraction Procedure 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. 6.1 .2 Glassware Preparation The 125 mL pear-shaped flasks were silanized by first rinsing the flask with 30% dimethyldichlorosilane in toluene solution . The flasks were rinsed once with toluene followed by three rinses with methanol . The flasks were allowed to air dry before use . 6.1 .3 Column Preparation The 20 mL columns were packed at Exygen in sequence with 2 grams florisil, 2 grams silica gel, 2 grams of carbon, and I gram LC-NH2 . The columns were conditioned on the day of extraction with 20 mL of methanol followed by 20 mL of acetonitrile . All washes were discarded. These clew-up columns were used to remove matrix interference and not to retain PFBS, PFHS, and PFOS. Additional details about the column packing materials can be found in the raw data package associated with this report. 6.1.4 Sample Extraction A 5-gram* portion of fish or clam sample was weighed into a fiftymilliliter centrifuge tube for the extraction . After fortification of appropriate samples, 30 mL of acetonitrile was added to the samples. The samples were allowed to shake on a wrist action shaker for -15 minutes . The samples were placed into a freezer for -1 hour. Freezing of the Exyg" Research Page 15 of 132 p . 16 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 samples allowed the fats and proteins to precipitate . The samples were centrifuged for - 10 minutes at -2000 rpm. The supernatant was then loaded onto the conditioned clean-up column fitted inside the silanized pear shaped flask. The eluate was collected in the silanized pear-shaped flask. This process removed the fats and proteins from the extract . Ten milliliters of acetonitrile was added to the samples left in the centrifuge tube. The remaining sample in the tube was homogenized using a tissumizer for -30 seconds . The tissumuzer was rinsed with ten milliliters of acetonitrile . The rinse was added to the sample tube. The samples were allowed to shake on a wrist action shaker for another 10 minutes. The samples were placed into a freezer for - 1 hour. The samples were centrifuged again for - 10 minutes at -2000 rpm . The supernatant was then loaded onto the same clean-up column . The cluate was collected into the same pear-shaped flask. The column was washed with 20 mL of acetonitrile, collecting the wash in the pear-shaped flask . Approximately 3 or 4 drops of 1-octanol was added to the extracts in the flasks . The samples were evaporated using a rotary evaporator at reduced pressure . The 1-octanol held the analytes in the pear-shaped flask while the solvent evaporated . Two milliliters of 2% ascorbic acid in methanol was added to the flasks to make final volume . The flask was swirled to dissolve and mix the sample. The sarnple was transferred to a HPLC vial using a disposable pipet. Each sample was analyzed by LC/MS/MS electrospray. *Due to lack of sample, a one-grarn portion of sample C0048133 (DMC-FOI-MSW0010-041216) was used. All other samples were weighed out in S-grarn portions . 6.2 Preparation of Standards and Fortification Solution s Individual stock standard solutions of PFBS, PFHS and PFOS were prepared as specified in Exygen method V0001783 . The stock standard solutions were prepared at a concentration of 100 g/mL by dissolving 10 mg of each of the standards (corrected for purity and salt content) in methanol. From these solutions, mixed 1 .0 ghmL fortification standard solutions were prepared by taking 1 mL of each of the appropriate stock solutions and bringing the volume up to 100 mL with methanol . By taking 10 mL of the mixed 1 .0 g/mL fortification standard and bringing the volume up to 100 mL with methanol, a mixed 0 .1 ghnL fortification atantiard was prepared. A mixed stock standard solution of PFBS, PFRS, and PFOS was also prepared . The stock standard solution was prepared at a concentration of 1000 ghnL by dissolving 100 mg of each of the standards (conected for purity and salt content, if necessary) in methanol . From this solution, a 100 pg/mL fortification standard solution was prepared by taking 10 mL of the stock and bringing the volume up to 100 mL with methanol . By taking 10 mL of the 100 g/mL fortification standard and bringing the volume up to 100 mL with methanol, a 10 g/mL fortification standard was prepared. By taking 10 n1L of the 10 g/mL fortification standard and bringing the volume up to 100 mL with Exygen Research Page 16 of 132 p . 17 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No .: P000113 1 methanol, a 1 .0 g/mL fortification standard were prepared . By taking 10 mL of the 1 .0 g/ml, fortification standard and bringing the volume up to 100 mL with methanol, a 0 .1 g/n1L fortification standard was prepared . A set of non-extracted standards containing PFBS, PFHS and PFOS was prepared in methanol . The following concentrations were prepared : Conc. of Fort Fort Volume of Final Conc. of Solution Volume Fortified Sample Calibration Std . s/ml..)' (PI-) (ML) (g1~) 1 .0 5 .0 100. 0 .05 1 .0 2 .5 100 0 .025 1 .0 1 .0 100 0.01 0.05 10 100 0 .005 0 .025 10 ` 100 0.0025 0.01 10 100 0 .001 0.005 10 100 0.0005 ' of PFBS, PFHS and PFOS The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator (40 2C) 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 PFBS, PFHS and PFOS was accomplished by LC/MS/MS electrospray . The retention times of PFBS, PFHS and PFOS were - 4 .7 mins, -- 10 .8 mins, and - 12 .9 mins, respectively. 6.4 Instrument Sensitivity The smallest standard amount injected during the chromatographic- run had a concentration of 0.0005 g/ml, of PFBS, PFHS and PFOS : 6.5 Description of LC/MS/MS Instrument and Operating Conditions Instrument: API 4000 Biomolecular Mass Analyzer Interface : Turbo Ion Spray Liquid Introduction Interface Computer. DELL OptiPlex GX40 0 Software: Windows NT, Analyst 1 .4. 1 HPLC : Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler Exygen Research Page 17 of 132 p . 18 Interim Report # 10-Analysis of Fish and Clam Samplrs Exygen Study No. : P000113 1 HP Column Oven HPLC Column:l bermo Fluophase RP, 50 mm x 2 .1 mm Column Temp . : -30 C Injection Vol .: 15 L Mobile Phase (A): 2 mM Ammonium Acetate in water Mobile Phase (B): Methano l Time Linin l~ A 0/0 B 0.0 65 35 1 .0 65 35 8.0 25 75 10 .0 25 75 11 .0 65 35 18 .0 65 35 Total ivn time: -18 arin Flow Rate : 0 .3 mUmin Ions monitored : Appro ximate Analyte Mode Thmition Re tion Tim e nitored PFBS negative 299 - + 99 O&J -4.7 min . PFHS negative 399 --~ 80 - 10.8 min. PFOS negative 499 --> 80 - 12 . 9 6.6 Qnantitntion and Example Calculation Fifteen microliters of sample or calibration standard were injected into the LC/MS/MS . The peak area was measured and the standard curve was generated (using 1/x fit weighted linear regression) by Analyst software using six concentrations of standards . The concentration was determined from the following equations. Equation 1 calculated the amount of analyte found (in nghmL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software Program- Eauation 1 : Analyte found (ng/mL, wet weight) _ (Peak area - intercept) x DF slope Where : DF = Dilution Factor, factor by which the final volume was diluted, if necessary . E x y g e n R e s e a r c h P a g e I S of 132 P . 19 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study Na : P0001131 Equation 2 was used to convert the amount of PFBS, PFHS and PFOS found in ng/mL to ng1g (ppb) . Equation 2: Analyte found (ppb, wet weight) fAnalvte found (n~i ~x final volume (2 mL)j sample weight (5 g) For samples fortified with known amounts of PFBS, PFHS and PFOS prior to extraction, Equation 3 was used to calculate the percent recovery . Equation 3 : Recovery (%) -1anah+te found lnQ/mLl - analyte in cont:rol (n & LI) x 100% amount added (ng/mL) Note: For the analyte recovery calculation, the "control" is the unspiked aliquot of the primary field sample . An example of a calculation using an actual sample follows (calculation is for PFBS only) : Fish sample Exygen ID: C0049478 Spk E (Set: 061605E), fortified at 10 ng/g with where: peak area - 280750 intercept = 3070 slope = 13100 dilution factor = 1 - ng/g PFBS added (fort level) = 1 0 amt in corresponding sample = NQ (not quantifiable) final volume (mL) - 2 sample weight (g) = 5 From equation 1 : Analyte found (ng/mL, wet weight) - f280750 - 30701 x 1 13100 - 21 .2 ng/mL From cquation 2 : Analytc found ng/g (ppb) = (21 .2 nlr[ ML x 2 mL) 5g = 8 .48 ng/g (ppb ) Exygen Research Page 19 of 132 p . 20 Interim Report #10-Analysis of Fish and Clam Sam ples Exygen Study No. : P0001131 F rom equation 3: % Recovery a ($ .48 na/rz- 0 neg,i x l 00/u 10 ng/g = 85 % 7.0 EXPERIMENTAL DESIGN For fish and clam samples designated as laboratory matrix spikes, PFBS, PFHS, and PFOS were added at a known concentration to the samples in the laboratory after the samples were weighed for extraction. The fish samples were extracted in thirty sets, five that were re-extraction sets . The clam samples were extracted in one set. Each fish or clam set included one control fish matrix blank and two control fish matrix blanks fortified at known concentrations. Two sets of fish contained three samples, one set of fi sh contained four samples, one set of fi sh contained seven samples, and twen ty-one sets of fish contained five samples . Three sets of re-extracted fish contained ten samples each . One set of re-extracted fish contained twelve samples . One set of re-extracted fish oontained nine samples . One set of clarns contained six samples. Accuracies were assessed for each sample by reviewing the individual QC results obtained for each sample. 8.0 RESULTS Analytical results and assessed accuracies for the analysis of PFBS, PFHS and PFOS found in fish samples are summarized in Table L Please note that the chromatography for PFBS was poor for this matrix . Exygen recognizes this and great care has been taken to integrate each data set consistently. Analytical results and assessed accuracies for the analysis of PFOS found in the re-extracted fish samples are summarized in Table H . Analytical results and assessed accuracies for the analysis of PFBS, PFHS and PFOS found in clam samples are summarized in Table M. The average percent recoveries standard deviations for PFBS, PFHS, PFOS in fish samples were 79'/ 13/., 94% t 12%, and 85% 20%, respectively . Fortification recoveries for PFBS, PFHS, and PFOS in fish samples are summarized in Table IV . The average percent recovery standard deviation for PFOS in the re-extracted fish samples was 109% 20%. Fortification recoveries for PFOS in the re-extracted fish samples are summarized in Table V. The average percent recoveries standard deviations for PFBS, PFHS, PFOS in clam samples were 84% 10%, 93% 13%, and 73% 16%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI . Exygen Resm-ch Page 20 of 132 p . 21 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 9.0 CONCLUSIONS The fish and clam samples were successfully extracted and analyzed for PFBS, PFHS and PFOS according to analytical method V0001783 . 10.0 RETENTION OF DATA AND SAMPLE S All original paper data generated by Exygen Research 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 final analytical report and all original facility-specific raw data, will be retained in the Exygen Research archives for the period of time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792 . Eaygcn Research Page 21 of 132 p . 22 Interim Report #1 0-Aealysis of Fish and Clam Samples Exygen Study No . : P000113 1 TABLE S Exygen Resmmh Page 22 of 132 p . 23 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No . : P400113 1 Table I. Summary of PFBS, PFHS and PFOS in Fish Sample s Ex"wn !D CNN gwr4ft ID C4 suHoni M "Et C8 iuQona M Pfl13 C8 iiM/on019 PFOS IWrdrrrw sb ~ Analyte Anryb Asw"a Q Found AOtncy Found Accuracy .w, .e +1- %) (A246,10 .0L (0-%) Found A=O" M+e. +/- x 00048126 D13-F014PF001-0-041021 000 18128 Rep DL.3-F014F001-0--041021 0.309 0.310 40 ND 30 5.18 3 0 40 No 30 3.64 30 00048127 DL3-F014PF002-0.041021 0.286 40 NO 30 4.18 40 C0048127 Rep Dl9-F014PF001-0-041021 0 .382 40 ND 30 4.58 4 0 00048128 DMIGF014PF001-0-041021 0 .930 60 ND 50 7 .40 60 00048128 Rap D11C-F014PF0014041021' 0.306 50 ND 50 8 .36 50 C00461 2p DMC-F01-N'F002-0-041021 0 .712 30 ND 30 14.1 50 COMM Rep DMGF0 1 .Pf002-0-041021' 0.792 30 ND 30 17.0 30 C00481]0 DMCGF014PU10014-04t021 1 .08 40 ND 30 70.0 40 00048130 Rep D1IC401-8'W001 .0441021 1 .08 40 0.297 30 55.4 40 C0046111 OIAG4 :01-PW0024041021 0A88 50 ND 30 34.4 30 0 0048131 Rap D1AC.F014PVMO0240-041021' 1 .34 So ND 30 34.2 30 00048132 054C401-083W001 .0-041021 0 .218 30 0 .524 30 270 30 00048192 Rap DAAC-F01-IN8W001-0-041021' 0 .202 30 0.484 30 290 30 00048133A 014C-F014ASW0020-041021 MD" 30 N0" 30 530 30 000481 33 Rap" 0M0 -F0 1.4 8Mf002A-041021' ND" 30 N0" 30 548 30 00048134 oL2f014PF001-0841021 0 .860 50 NO 40 3 .46 SO C0018134 Rep 0t2-F01-fW001-0-041021' 1 .00 50 NO 40 286 50 00048175 0l2-F014PF002-0-041021 0 .816 SO ND 40 4 .72 50 00048136 Rep DL24F01PF002-0-041021' 0- 962 50 ND 40 5 .04 50 00048138 0L2.P014Pf0010-041021 0.247 30 ND 30 2 .01 30 00048198 Rep Dl2-P0141Po03-0-041021` 0.219 30 ND 30 2 .08 30 00048137 0L2-F014PF00+40-041021 0.940 40 ND 30 4 .52 40 C0048137 Rep 0L24:01-PF0040-041021' 0.390 40 NO 30 4 .12 40 00018196 0L2-F014PF0060-041021 0.938 40 NO 30 2.48 30 00048186 Rep O1.2-F01PF000-041021 0 .918 40 ND 30 2.80 30 C0043130 DL24014W001-0-041021 0.328 30 ND COO"139 Rep DL2-F014P'W0014}041021' 0 .100 30 ND ( 00 48140 0l2-F014I85001-0-041021 0.391 30 ND 00018140 Rap 0L.2.F01 4A8F001-0-0 41021' 0.348 30 NO 30 5.88 30 30 e.12 3 0 30 77.2 30 30 67.6 20 00048141 el2-F01-AA6F0024k41021 0.408 40 ND 30 84.5 40 00048141 Rap D12f01 .M8F002-0-041021 0.308 40 ND 30 98.4 40 C0048142 0L24:01-M6F0030-041021 0.416 40 ND 40 41 .6 40 C000142 Rep Dl.2401-MSF003O041021' 0.370 40 ND 40 40.0 4 0 00048143 OL24014A5F004-0.041021 0.345 30 ND 30 83.8 30 00048143 Rmp 0l2-F014%F0044-041021' 0.949 30 ND 30 632 30 LbMbry Dup11eM - 10 8 of Nnp Uwd for rctictlm Mu4d d b 0 Q ND a Not dNN7W at or aboN LieR of awnCtilbn wNlfi is 0 .2 eyq (wvtwwW) ND" Not dOkGtsd at or above LYhR Of OYYMNitICn ahioh a 1 .0 rtWy (wM weVd} NR Not ~ 0 a1W dus brft aawtl IwA tMbM. Exygea Researcb Page 23 of 132 p . 24 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued) C4 3uron .o. PF 03 c6 awronab "'Ns CI suffonaft mm ~ ~ A.~...e ~ ~.~.e.o Aoanacr Found Aoaracy w ,n~ a ~ ID r!D ftv, u. I r. .F x + O .rt #. %I ftftl sw VA. - x 60018144 004101 4 FF001 -0 041021 0 .432 30 0.281 30 33.4 40 60048144 Rep 0 l1-F01-PF001 -0,041021 0 .428 30 0 252 30 32,6 40 C0018145 DW-F01-pF0034- 04102/ 0.448 30 C0048145 Rep OL3-F01 4pF007 -0-041021 0.410 30 NO 30 3.55 30 0.226 30 3.36 3 0 C0C040810446 8R1ep46DDLL33F-F001144PPFF000044--00-0044110201 011 00..9708 0 4 4040 N NO O 3 30 0 0 0..23380 2 3030 C0048147 C0048147 Rep D43-F01 4 PF0054-0410 2 1 1 .63 80 01.4F01 4P F005-0-041021 1 .07 60 NO 30 5.48 40 NO 30 5,64 40 < '004s3148 D8 GF01-PF001-0-041021 1 .34 60 0.892 30 NR NR 60048148Rep DBCrf O 1-PF001 4-041021 1 .96 60 0.860 30 NR NR C0048149 08G4 01 4 PF002-04041021 1 .43 50 NO 30 110 30 60048149 Rep 006 F01-pF002-004 1021 0.755 60 ND 30 109 30 C0048160 D81C.F01 4PP003-0.04 1021 0.966 60 0.841 30 NR N R 00046150 Rep DtaC+014QF008-0-041021 01A 52 50 0 .624 30 NR NR 00048151 D0CrF01.PN0014 4 41021 0.864 40 2 .21 60048151 Rep DBCrF01 -FW001 -0-041021 0.508 40 2 .20 30 NR NR 30 NR N R 60046152 DBCrFJ1-PW0024)6Q41021 0.700 40 9 .12 30 NR NR 60048152 Rep DHGF01 4pW002-0-041021 0.735 40 8 98 30 NR NR 6004815,1 06C-F01 4PWO0S10-0 41021 0.735 30 6.78 C000153 RV O8C-F01 4 W003. .011021 0 .700 30 7.44 30 NR NR 30 NR NR 60048164 DpU-F01 4Pf001 -0.041021 4.36 60048184 Rep DOU-F01 4PF001 -0-0410214 4.24 40 1 .02 30 NR 40 0.972 30 NR NR NR 00018156 D0U-F014 PF0020 -041021 0.78 4 0 0 .79 2 30 NR NR 600 161 56 Rep DOU-F01-pF0020-041 0210 8.28 44 0 .720 30 NR NR 60048136 DOU-F014PF0030-041021 6.88 40 1 .02 30 NR N R C0048166 Rep 0OU-F01 4 PP003 04M 1021 0 5 .96 40 1 .02 30 NR NR 60048157 DOtJ-P01 4PF0040-041021 6.12 30 2.30 30 NR MR 6000 157 Rep D0U4-01 4 PF004-0.041021' 0.28 30 2.38 30 NR NR 60048168 D0t L F01- K 005 .0-041021 4.56 30 0Aee 30 NR NR C0048158 Rap DOU.F01-1pF0064 0 41021 4.36 30 0.382 30 NR NR 60048159 DOU-F01 -IPW001 4.011021 289 30 0 .616 C0018159 Rep D0U-F01-IPIM001-0 -041021' 2. 81 30 0 .964 30 NR NR 30 NR NR 60048160 D 0U-F01 4PYU00200410 21 18.4 53 9. 69 60048160 Rep DOU-F01IPW0024"1021 19.3 50 1 .70 30 NR NR 30 NR NR C0C0408106418R16e1pD0Ll22--f020114-MMS8WW00010-01.4040140170121-0N.2D03 3 30 0 N NO D 3 30 0 11 2020 5500 60048182 D12-F01-MSW002-0041021 ND 30 ND 30 102 30 C0048162 Rep DL2-P01 -WW002-0-041021 NO 30 ND 30 100 30 9 AEms" GuP/err ND - trot delected at or above Unit of Cumtifetion wfrch it 0 .2 n01q hrd weipK NR Not rs0wld due b qud8y aaiUal rwII faMwM. F.xysCII R=mh Page 24 of 132 p . 25 Interim Report #10-Analysis of Fish and .Clam Samples Exygen Study No. : P0001131 Table I. Summary of PFBS, PFIiS and PFOS in Flsh Sample s (continued ) C4 sWfoeMb PM cd tuffona1r PiMS ea iuttaewb PFoi Exvw D Mi1y4 . Aft4tNG C1w+t Fand AoourooY . D iw #a +l- % AM" ANMNO Am~ Assis Fand lloartely F"W Amin" own)wo w N. % wr rc C0048163 C4018 163 Rep 0t24:01-M5W003-0-041021 NO 30 NO 30 92.4 30 DL2-F01.888M1003.O-041021' NO 30 NO 30 91 .e JO 00048184 C0048164 Rep 012-P01 43Y1f 004-0-041 021 0L2-F01-MSVV0044.0 41021 NO 30 ND 30 88 .0 30 NO 30 NO 30 94.8 30 00048186 0L24:01 4ABW006 0-04 1021 ND 30 NO 30 168 30 COW81E6Rop 012-f01 AISW0p5444 1021 ND 30 NO 30 174 30 C004IM50 D9C.F01-MSM9001-0-0 41104 0.86a C0049450 Rep OBGF01 4UW001 -0-041104 0.852 30 8.32 30 8.52 30 NR NR 30 NR NR C0049451 08C-F01-1 ABN1002-0-041104 O .DOC 30 8.4J 3 0 NR NR 00040461 Rep O6C-F01 4A6W002-0441104' 0 .894 80, 8.36 70 . NR NR 00040452 OBGF014 I8W003 -0-041104 0 .8e0 30 00049462 Rp D8G401 418W005.0-041101 0.734 30 362 30 NR NR 1 64 30 NR NR 00049 468 D8GF01-U8W0044 41104 0.864 30 9.72 30 MR NR C0049W R ep 000- F01-A13W004-0-04110,' 0.88 0 30 9.80 30 NR MR 00040454 D9C.F01-hISW0054-04 1104 0.832 90 277 30 NR NR C0049464 Rep DBPiF01-MBWOObO"1104 0.832 30 . 2.66 30 NR NR 00049456 06GF01-MBF001 -0 441104 0.820 COO49456 Rep DdCf01-81SF001 -0-041104 0.7W 30 366 30 NR NR 30 146 30 NR MR 00049468 E]SGi0r 868f002-044 1104 0.71,6 30 00049456 Rep DBCf01-WISF00 2-0-041104- 0.780 20 1 .96 30 NR NR . 1 .90 30 NR NR 006/9467 D6C-F014 PF004- 0-041104 0.504 30 0.584 30 142 30 C00404 67 Rep OBC-F01-PF004-0-04 1104 0.620 30 0.640 30 . 152 30 00049466 D8C-F01 4 PF0064441101 1 .e0 00049436 Rep 080-F01-PF006 4-041104- .1 .64 30 2.16 30 MR NR 30 218 30 NR NR 00049459 08 C401-PYY004-0441104 0. 484 30 5.28 30 NR MR C0049459 Rap OBC-F01-IPVY004-4441104' .0K4 30 3.28 80 NR NR 0 0049480 D8GF01-pW006-0 -041104 0.372 30 C0049460 Ray D8GF014 P1N0060011104 0.53 2 30 . 2.10 2.10 30 NR N R 30 NR NR 0004 018t . 000494 81 Rep DOU4:01 4 W003.0-041104 9.12 30 6,00 90 NR NR DOU-F01 PW0034 041104- r9 .06 30 5.92 30 MR NR 00049462 DO1 J-F01-PV40044-041104 3.46 30 7 .12 30 NR NR 00049482 Rep DOU-FOtIPW0044 0 41104' 3.11 30 8 .64 30 NR NR C0049463 DOKI-F01 4PNI006.0.041104 2 .97 30 5.12 20 NR MR C004040.1 Rep DOU 4 :01-PW0060041104- 2 .0 0 30 8.32 30 NR NR 00049 484 00049484 Rop 0t2-F01- PW002-0-0 11104 1 .01 30 NO . 30 8 .20 40 0L2-F014PW002-0-0 41104' 0.980 . 30 ND 30 8 .00 40 00040465 D0401448W001 -0041104 1 .20 30 0 .89E 30 MR NR Op04D46bRap DLi-F01 4f 8W001 -0-041104' t .21 30 0 432 30 NR NR *LAWS" p uq14Y NO s Not de bawd Nor above Lint of OuwttltWbn whkli Is 0.2 nyp two wdpF NR . Not Apa1~0 dM 10 qU4Mly oOr~YO1 w~At YiYMr . Exygen Research Page 25 of 132 p . 26 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000! 13 I Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued) Erscm 10 C4 sdMOab AFfB C! >taMw1Ma PFMi C118ulfonaft WOO rwdae ....w~a ..r asse~aea AtNS..d ~d CAW Found Aearu.y Found Aocur7ay Found Aoa,raq 8Yf11 b wtrl. N-% +_jrrt,M. N-% wMrl. H- X G0048488 0L1-P014ASW002-0-041104 1 .30 30 1.72 30 MR NR 04049486 Ro p DL1-601-11$W00243-041104' 1 .15 30 1 .84 30 NR NR C0049487 DL1-FO1-1,18W003 .0.041104 0.080 30 1 .13 30 NR MR 00049487 Rep 0l1-F014bSW0010-041104' 0.528 30 1 .14 30 MR N R 00018488 DL1-F01-AA6W004-0-041104 1 .22 30 0.908 30 161 30 C004"68 Roo 0L1-F01-M8WO01-0-041104 1 .12 30 0.880 30 188 30 C00484E0 DL1-F01a11aW008-0-041104 1 .22 30 1 .18 30 MR NR 00049460 Rap DL1-F014ASW0030041104 1 .20 30 1 .15 30 NR MR C0040470 D11 .P01-A{8F001-0-041104 NO 00046470 Rep DL1-F01-wl$F001-0-041104' NO 30 0.315 30 293 30 30 0 .20 30 307 30 C0049471 OL1f01-MSF002-0041104 ND 30 0 .024 30 MR MR 000494711LW Dl1-F0144fO0240.041104' ND 30 0.904 30 NR NR C0049472 0L1-F01-1U$F0080-041104 0 .203 30 0.652 30 MR NR 00049472 Rap OL7-FO1-A{3F00.74-041104' ND 30 0.876 30 MR MR 00049473 DL1-F014ISF004-0-041104 NO 30 0.S32 30 NR NR C0019473 Rep OLt-FOt-MaF004-0-041104' ND 30 0 iJ6 30 NR N R C0049474 Ol1-F01-M9F005-0-041104 ND 30 0.884 30 NR NR C0049474 Rep DL1f0144FOOS0-041104 ND 30 0 .844 30 MR NR 00049475 DL1-F01-4wW001-0-041104 0 .772 30 0 .666 00046475 Rep DL1-f014PW00t-0-041104 0.870 30 0 .744 C0049478 0 L1-F01-pyy002fi041104 0 .4 68 30 0.338 C0049478 Rep DL1-F014PW002-00411041 0 .472 30 0.616 30 17 .4 30 30 18 .9 30 3 0 13.7 30 30 15.8 30 00049477 DLt-F01-PW003-0-041104 ND 30 0206 30 0.38 30 00049477 Rep 0l1-F014PWOW-0d41104 ND 30 0 .247 30 9.52 30 00049478 DL7-F01-pW004 .0-041104 NO 00049178 Rep Dl.1-Po14YV004F0441104' hD 30 0.238 30 50.8 30 30 0.248 30 572 30 C0046*479 D114--01-1PF002-0-041104 NO 30 0 .222 30 11 .1 30 00049479 Rep DL1-F01-pF002 .0441104' NO 30 0.247 30 11 .2 30 00049480 DL-1f014PF0034A41104 NO 30 0 .208 30 20.9 30 C0049480 Rep Dc-14014P60034041101 No 30 0262 30 21 .4 30 00049481 D1-14 :01-UPPo04-0-041104 NO 30 NO 00040481 Pup Dl-1-F014p6004-0.041101' ND 30 ND 30 7 .00 30 30 7.36 30 C00004094498248R2epODl-l1-1f0.F10414'FpF000056..0o.0.40114 04'l10N4O NO3300 0 0..5 37 83 8 3 30 0 8 8..7 52 0 3300 00049483 D04101468W001-0-041105 ND 30 C0049483 Rep DL3-60t-WW001-0-041108' NO ND 30 30 1 39 ND 30 137 s0 30 00049484 Dl3F01449W002-0-041105 ND 30 ND 30 180 00040484 Rep DL34014A8W002-0-U11081 NO 30 NO 30 1e2 L 30 30 'Labmbry Dupkatf ND w Not drMewd at Cr Wow Li1rt of QuaMlMbn wf~lCh Is 0.2 nplp (hral weiplv~ NR - Not wpoAW dm b pualy aOnYal nwd fa4h "s, Exygen Rescarch Page 26 of 132 p . 27 Interim Report #10-Analysis .of Fish and Clam Samples Exygen Study No . : P00p113 1 Table 1. Summary of PFBS, PFHS and PFOS in Fish Samples (continued) a a~rro ..a ~ss Ce a0lro".a wxs CS awkeste twos ~ ~ Exymn ID Semyle ID wtM ~ A=--y Found AOrsy %I 6,*W .wt .l . +f Found Aouuy ..t .w +h 00019483 ot3-f01413W003- 0 441 1 06 ND 30 NO 30 146 30 00040486 R ep D1.3-F01-MSW003 4441105 ND 30 ND 30 144 30 C0044188 0L.34:01 -M SW004-0-041106 ND 30 0 .286 30 198 30 00049480 Rap DL3 W01 4i3W004 4.04 1100' ND 30 0 .282 30 199 30 C0040487 00-F01 aM3W006 -0-011105 ND 30 0.366 30 173 30 0004"87 ft 013*01 -MSVN006.0 .011106' ND 30 0.341 30 188 30 C0049186 DI.3-F01448f001 -0041106 NO 30 ND 30 11e 3 0 C0049488 Rep 01 3-F0/-MSf001-004110 6 ' NO 30 ND 30 115 30 00049 89 00040186 Rep DL3+01 -MSF0024}" 1106 ND 30 NO 30 118 90 DW401 4WF002-O-041105' NO 30 ND 30 111 30 000084004409409R0ep O01L33--FF004144AI3SfF0000"3-400441111 05 06NN DD30 30 ND ND 330 0 7 73 2.16 0 3 30 0 C0C0409049419R40e1pD0W1-3FFO01I--MiBSfF0000440-06-40114 08;11N 06 DN3 D030 ND NO 330 0 113340 3300 0004 9402 DL1F01-YSW06.0.041106 00049492 Rep 0 1-9401 4ASf0060.041 ND 30 ND 30 81 .0 30 105' NO 30 ND 30 83,0 30 000494.01 DGIGP01-IFVY008 4-0 41106 ND 30 0 M6 30 01 .2 30 C0049493 Rep DNACiF01-IPVYOp3- 0.041t05 ND 30 0.334 30 63,6 30 00049464 D MG4 01 4PNl001-0041106 0.300 30 0.388 30 88 .8 8 0 00049404 Rep DBAC-F01-PW004-04411 0a 0.345 30 0.464 30 89 e 30 000004004469S49R5SD DINOCM-CF-F0O114-PIPWW0000660.0-004 1 41110 086' N NDD3030 00.2355 70330 0 8 64 2.8 4 9 300 C0049466 13)iACrF01-81SW003-0-041106 ND 30 0-982 C0049406 Rep D MCf01 4M8W0030O41106' ND 30 0, .,~0 30 354 30 30 330 30 00040497 DMGF01 -M8W004 -0-041106 0.3t8 C0049497 RAp DMGF01 4A8W004-00 /1105 0.233 30 30 1 . 90 30 1 .88 30 00049498 DM4F01 448VV005-0-041106 ND 30 0,980 30 C0049 1981bep DMC-F MMSW00$4.0 41106 ND 30 0 .9 96 30 250 30 256 30 NR NR NR NR 00040499 OMC-F0I-AIBf00Z-0.041106 ND 30 NO 30 NR NR C0049499 Rep OIMCf014/8F002-0.04110 el ND 30 0.307 30 NR NR 00000409460060 0R0epDMDGIAFC-0F011 -4MAB446FF00001304-400 4 14 106110 NO6 NO 30 30NOND 3 300 5666..08 404 0 00000490460051 0f21aDp 1DNINGCP-0F10i1A-Iu38fF'800044..00.-004411110056' N NOD 330 0 0 0 .22 25 843 30 0 1 11 160 3300 00040602 OMGPo1-1/ 5F0O5.0. 41t06 NO 30 0 .420 00040502 Rep DM0-F01-MBF00&0-041105' ND 30 0 30 146 30 .448 30 147 30 00049603 Dfy1Cf014PFp0,9.0 .041103 ND 30 ND 30 7. 92 30 00048603 Rep 011tGF0t-1PF093.0 -04 f 105' ND 30 ND 30 7. 92 30 YabmW-ry DupNe" ND Not aet8.o at or above Umw of auanOmfon which is 0.2 nyo c" +wmphl). NR - Not MpOrrO Ow b "ft aonppl ream pykoy , ExYpn Rewwb Page 27 of 132 p . 28 Interim Report #1 0-Anaiysis of Fish and Clam samples Exygcn Study No . : P000113 1 Table 1. Summary of PFBS, PFHS and PFOS in Fish Samples (continued) C4 Wf"ab PFp pt syllonsw PRHS C6 W% nob PiD/ ExyW 10 -00" P M CYSN Found AmryCy Pouid AcaraW samum ID . .c a- % .o M . - x %sd Aocu~cy .r,* W- x C000049054094 6R0ep4DD11W Caf'J0114.P1f0P 04 .F 0.00410104 6 -0-0NO41103 6 0 NDN 3D 0 N3 D030445 4 ..0 6 3 30 0 00049606 DMC-F014Pf0064 .041105 ND 30 ND 30 46.4 30 C0049606 Rep DAAC*01-IPF003-0-041105' NO 30 ND 30 46 .0 30 0005 34 DL2-F01-M8Po054-041216 NO 30 NO 30 402 30 00066354ROp 012-F01-At8f006-0-041216' Na 30 ND 30 61A 3 0 00C0506045688 4R6e6p0Dt2l-2F4001t44P0W W00D05660-004411221155' NNOO 3300 NNOO 3 30 0 1 13 3..3 2 3 30 0 f 0066436 0OU-F014A8W002-0-041216 0 .206 40 1 .72 30 NR NR 00068466 Rap DOU-F01-M6YY002-0-041216 0 .227 40 1 .70 30 NR NR 00056457 Dl2-F01-pW004.0-041215 NO 30 00050467 Rep DL2R0141PyV004-0041216' ND 30 ND NO 30 6.80 30 30 6.60 30 00066458 DoU-Po14ASW003.0-041216 NO 30 10 .4 30 NR NR Q0056456 Rep DOIFF0144W003-4011216' ND 30 10.6 30 NR NR 00066459 DLS-F014PNf0044041130 NO 00066460 Rep 01.3_F01iPyV004-0.041190' NO 30 ND 30 7 .02 8 0 30 ND 30 7.52 30 00056160 DOU-F014i6W001-0-041216 7.06 30 15.4 C0066460 Rap 0Ot1F01418YY001-0-0412161 T .12 30 14.2 30 NR NR 30 HR N R C0066461 DOU-F01-M8W0044041219 4 .12 40 21 .7 30 NR NR 00056161 Rip D04J-F01443W004.0.041216 4A6 40 22 .5 30 NR NR 00056482 00U-F014156f005-0441216 0 .364 30 1 .34 00066452Rp DOLLF014t8W0064-041216' 0 .36 30 1 30 N12 NR .41 30 NR NR C0066463 D0U-F014W006-4041216 1 .41 80 6,40 30 NR NR 00056463 Rep DOU4F0I-MSF0060.041216' 1 .43 30 &44 30 NR N R 00066464 DL3F014Pyy002-0.041130 NO 30 NO C0066454 Rep 013-F014PW0 02-0-041 I W ND 30 ND C0056486 DL3fp1-py/003-0 .051130 NO C005E406 Rep DLSYF014PW0030 .041130' ND 30 NO 30 ND 30 12 .0 50 30 11 .5 50 30 6 .44 4 0 30 6.26 40 00066486 DOU-F01 418F003.0.041 216 1 .72 00056466 Rap D04J-F014A8F003-0-041214' 1 .73 00 056467 OBG-F01-M8f006.1 .041216 0.220 00056467R0p D8C.Po 14 IM06-1-04 1216 NO 30 30 30 30 6.66 30 NR NR 6.68 30 NR NR 1, 7 4 30 NR NR 1 .76 30 NR NR C0066466 OBC-01-MSF006-041,11216 NO C005MM Rap D9C-F0I4I3F0064441216 NO 30 1 .68 30 NR N R 30 1 .69 30 NR NR 00C06060456604R6e8p0D0OLLUF-F001144MA5FF000022..400-401421162'16 00..6 66 76 2 3 30 0 4 4 ..5 66 6 3 30 0 N NR RNN RR C0056470 DL3-F01-PW001-0041130 NO 30 0.246 C0056470 Rep OL3-F01-M+w001-0-041 tJ0' ND 30 0219 30 4.04 30 30 8.80 30 'LaOorbaY DvOkw NO s Not dsMdsd at or ~bow UM of QuaMOafoe ~ k 0.2 nOrO (wet wapht). NR s NM r~porled dw b qwlly mnhd ~uk fNln~. bran Research Page 28 of 132 p . 29 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No .: PM 1131 Table I. Summary of PFBS, PFHS and PFOS in Fish Sample s (continued ) C4 tuNo"M PFSi CO Sulfonats PFHS CII iiMfo"N PFOa Exvasn ~ a .... .a CMNI Found Aoeuru,y Fa~n~t!F~ ou~nb d A Aosew ~ra aoAy ID Hl NAM ftft) MI M. H- qMI WM yR. 00066471 DOll-F0Ia18F00 p 1 .041216 0 .640 C0066471 Rep ppU-F01416F002-1-011218' 0.880 30 4.68 20 MR NR 30 4.72 30 NR NR 00066472 DOU-F01-II6F0044041216 0.792 30 2.35 40 NR NR Coo66472 Rep DOUf01-bI8F004-0OA121 6 0,816 30 2.22 40 NR NR C0056473 D01J-F01i1SF001-0-04f216 2 .18 30 10 .9 30 00056473 Rep DOU4F014A8F001"1218 2 .28 30 10.7 30 NR NR NR N R 00066474 D6?GF+01448FOOS0-041216 NO 30 2-09 30 C0066474 Rep DBGF014ASFO014-041216 ND 30 2.09 30 MR NR NR NR 00066478 DBC-F01-MBF004-0-041216 ND C0036476 Rep 03C-F0143r004-0041218 ND 30 2.87 30 MR NR 30 3.77 30 NR NR 00066476 DMGF014A8FO014-041216 NO 30 OA20 30 NR NR C0066478 Rep 0AAC-F01-M9F'001-4041216 ND 30 0 .468 30 MR NR 00056477 Dl1-F01-IPIAl0064-00216 0.253 30 0 444 30 88.8 30 C0036477 Rep DL1-F014PW005 .0-041218' 0.249 30 0 .644 30 67.6 30 00066478 Dl2-F01-PIN0030441201 ND 00036478 Rep DL2fPo14PW0030041201 No 00036479 Dl .3-F014P1M006p.041201 ND C0056479 Rep 0U-F01-IPY1i0060-041201 ND 30 ND 30 30 NO 30 30 ND 30 ND 30 30 7.48 40 7.44 40 4.88 30 4 .72 30 ~ho" O~W ND - Not dstecbd at or abae Unit of fluenYWion MNidh in o.2 npfy toot we18h1~ NR - NOt MpdqA tlA b qldky cp0o1 rawt yixm. Exyga' Rescarch Page 29 of 132 p . 30 interim Repoct #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113! Table H. Summary of PFOS in Re-extracted Fish Samples Cs suronst. PFOa PWOMWOOCUOMMONON"M Client Analyts Found ExYOen ID Sa.m ~p.l.s..~ ID~(~ no .~ q) W .e WN09 Asg esae d Acxuraq (+a %) 00048151 DBGF01 4 P1N001 404 1021 2000 30 00044 182 D9GF01 4 PW002-0-041021 3330 30 00048 133 06<'.F01-IPYV003-0-041021 16E0 50 00048154 DO(1-F014 PF001-0011021 596 30 C0048155 DOt 1-F01-IPF002-0-0 41021 838 30 C0046158 OOU-F014 PF<105-C-041021 544 30 C0048160 DOl1-F01-IPVJ002 -0441021 1210 40 C0049450 DBC-F01 -MSYVG01-0041104 9480 40 C0049151 09CrF01-M6WOG2-0-041104 7520 30 00049452 D9GF01-hCs'W003-0-041104 1 36 00 30 C0049453 DBC-F01- 1615W90 4-0A41104 3440 30 00049151 DBC401-t ISWO054041144 5240 30 00049155 D8fiF01-M8F001-3-041104 5240 30 C0049466 0BC-F01-MSr~OW-" 110b 4780 30 C00444 5 E O6 C-F01 4 PF4060- 041104 808 30 C0049459 D8C-F01 4P9Y001-0 041104 1230 40 000494 60 DBC-F01-PN006-0-0411?4 2620 30 C00411t61 DOU-F01 4P'NC03-0W 104 NR NR 0 0049482 DOII-F01 4Ip1M004'0- 041104 1740 30 C0049463 DOU-F01 -IPYIIC0'.r40411 04 2130 30 C0049485 DL1-F01 4A.''W001-0C41141 989 30 C0049466 130- 1201 4ASW604~ 11 04 708 30 00049467 DL1-F01 -1d3W003-0d 4 1104 A98 30 00049469 DL1-F01-119W006-0-041104 804 30 00049471 00 -F 0 1-MSP002-0b441104 568 30 00049472 01.1-F01-M3F003.0-04,104 432 30 NR ~ Not IrpolUQ dN p quY(ily oonNOt rs= k talWrss . Exygen Research Page 30 of 132 p . 31 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 Table II . Summa ry of PFOS In Re-extracted Fish Samples (continued) c ow Exyaen ID 3smD16 ID C& swMOn aa PFOS PW&MDDCWMwbftsb And* F o .~a Aneww Mal wee MM Aea+r &yr f+r- %) C0049474 DL1-F01 4NSFOOS-0-041104 740 30 C0049490 DMC-F01 4ASW0060-041165 580 30 C0049499 DAAGF01-AA8F002-o -041105 620 30 00036 4 58 DOU-MI-ARSW002-0 -041216 28200 80 C0038458 DOU-F014ASW003-0-041218 4040 30 C0056460 DOIJ-Fp1-MSW001-0 -041218 NR NR C0056461 DO U-F01-NSW001-4041218 5120 30 00 038462 Dol1-F01-MSW005Q- 041216 498 30 00 058463 DOU-F014ASF0050.041 216 720 30 C0056486 DOU-F01 -MSF003-044 1216 848 30 00066 67 D9GF01-MSF006-1-041216 NR NR C0056468 DBC-F01MSF006 -0041216 6080 50 00056469 DOl )4 01 4ASF002-0-041216 640 30 00056471 DOt}F01-A1SF002-1 -041218 892 30 C00554 72 DOIJ-F01-M5F004-0-041218 18 20 30 C0056473 DOl)-F01-AASF001-0-0/1216 2 070 30 C0056474 DBC-F0 1-MSF003-0-041218 4840 30 00096475 D9C-F01 4A SF0040.041218 9Q90 50 C0056476 DMCrFO1-MSF O01-0-011216 8 40 C0046148 DBGF01-IPF001-0 -041021 38 4 3D 30 C0046150 DBC-FDI 4 PF003-0-041021 . 293 30 C0048156 DQU-F0114 PF0034041021 359 30 C0048157 D0U-F014 PF004.0-O41021 424 30 00048159 DOU-F01 - O VU001-0041021 387 30 00049473 DL1-F01-A16F001-0-041104 348 30 NR Not iaparNd due b querty oDnYd rpulf bIYrse . Exygen ReM=b Page 31 of 132 p . 32 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Table III . Summary of PFBS, PFHS and PFOS in Clam Samples E c t0 c4 a,,No na . rFSS a sur+m .e. " s a suren.r vr~ jk4a AD yr A...U.a An yn Ann$ a An,41. ~ ...a CIsiM Found Aaunoy Fand Aoarscy Found Accuracy Sarmle ID wt+k +/ % .w .c .t +1- % , a R. (-I.%) C0066460 OL34 01-CFVY001-0-04 1216 NO 40 ND 40 1 .11 2 50 C0056480 Rep 0L3-101 -CFW001 0-041216' ND 40 NO 40 1 .82 50 C0056461 DMG101CFW001 4-041216 NO 30 ND 30 6.16 50 C0066481 Rep 0IiAC-1014 FYM001 4441216' ND 30 ND 30 6 .12 5 0 C0066482 D12401-CF4Y00t-0-041216 NO G0056182 Rep DL2101 4FYM001 -0-041218' NO 30 ND 30 1 .81 50 30 ND 30 1 .77 50 00056189 D8C-101-CFW001 -0-041215 NO ()0066483 Rip 08G101-CFiN001-0 -041215' ND 30 ND 30 4 .48 30 30 ND 30 4 .44 30 < 0006464 D11-1014FW001 -0-041213 NO 30 NO 30 0 .6D 40 cooae464 Rep DL t4 o1 4F nro01 4.a121as ND 30 ND 30 6.84 40 G00 56485 DOU-101 4 fVV001-0A41216 NO 30 0.202 30 11 .4 50 C0066485 Rep D0W01-CFW001-0-041 216- ND 30 0 .205 30 10.9 50 'laboraWry DWllcar ND s Nat d.rcoed at d fbom LYnR af QurMtalbn which 1&0.2 nft"weight). Exygen Research Page 32 of 132 p . 33 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No. : P000113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples e.ltp4 SOW OI L 4 ~ p C &OW" ~ * A "2 N a~.~pb NroaWO N owry bly9 I @oo ,M.e R.ooYr,, N s6mp. ftaow .9d n9rowry 0(}f01d~F001-0-0~tOQ1 1000M1l~3*4 100MT 10 0.300 L66 O138014PFlDO/-043410Q 1 toqt9w 1w r sopq 100 0.309 02.4 93 62 NO ND 0.21 63 6.16 12 .6 74 712 73 6.16 76,1 73 DLyF014/POOZ'-0-01102 1 1Cmtr>A uYD. t9nq 10 0266 plyF614iF002801102 1 tCOtNU~ 80 0.ro0wp 100 O.Z66 L32 0.0 as 09 ND 1.40 ND 79A 75 6D 4 .16 10.3 61 416 s0.6 7 ONCfD1dPF00/-0441021 {10wM 6w L t0 rrM 10 0A30 4.40 42 ND OIA6i0/4PF001-0441021 IOOMMilreKtlbMy 100 0 .330 064 66 ND .5.94 52 744 73 7 .40 7 .40 91" 31 .6 26 74 DMpfD14Pf002-044102 1 q~ooqe99at4 1 1Aq 10 0.712 7 00 70 ND an 011Cf01-N10024-041021 poo 0 tb so KqDMM 100 0.712 7LO n No 960 Be 06 14 .1 29A /4 ./ 104 106 so DMC-f01 IP WODt 404102 1 {crooope9)r 0. 10 ON) oW.i014iw001a6+WQt (OUMnm90 6 1 00000 to 1 46 7.e0 e6 ND 1.64 /00 116 042 64 NO 90 0 76 700 11 .e 60 700 /31 61 DIK i01 P W 002~04/021 9+aeM/71 yaL to M01 DMGFOt IPNI00l-0M 7021 taoor 7+ 104100ty 10 0.9M 9.76 6! NO 7A6 60 /00 0.N0 6DA 00 No 74A 76 34 .4 44A 36 A 101 67 0IICF0f-616WOOtOdtt4t t p0e1M06>MLMN3 goo) ONc-FOi a18YY001-0-0t 1021 (Ea0U10 yt p .100p0 60w) 10 100 0210 9.70 0216 611 as 61 0.e24 OAI N 270 0424 932 93 270 ZIO 315 IN o1dCf 01.6671N0020041021 lGOONWUt4aMUM1 60 IO" 452 90 dlp" 06K}F01-N91V0024041021' lOOeW9ptK1o6M9MM am ND" 432 90 ND 52A 104 162 08 $30 470 330 924 79 OL3-FO7-IPF6D'1-0041011 1C~orot9*~ .wptMrl 10 0.N0 6.60 61 ND 6.e6 96 S.46 6.36 40 pL2F01~PoOtOa1021 4mt 1wyo K+00 M91051 500 0.600 40.4 46 71) 56.6 06 3 46 66.4 53 011PoF4'F00Z001102 1 lC6tMM bs0.wtpaMa! 10 0124t91-PF0Oi-04410Q1 (OOiwu~~ptt.ta9~e~p~. 100 0.814 We e.64 M 4q 6.40 54 4 .72 L60 36 64A Sf ND 761 79 4 .72 724 66 >iwyw nWr srYM qMYr M.i ~V~"M%9riktw ant+tMYnaawy rMw o~~ut Me+loiYh O tA O d w~lr wd 4~r6o~ Yr1~6 rlf R9 e . NO . Na dMfto1W d or Am tiN dOww6fYNn MYaN Y .01 ny0 bM rM1/0) NO" - h0dow0ed star NN .Natnid~MqOtu9HaaYN~~lYu~ 1dw~yW~I~w~liarnMT~OM~ . maw Shs aft prry rbN Man ro W U9 wMWh, wMwq vWr wry wy GIqlrlp 1ww so NYr bb ow raw dow, Exygen Research Pap 33 of 132 p . 34 Interim Report #10 Analysia of Fish and Clam Samples Exygen Study No . : P000113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) C4 9.WfarN PP" Mini Amt FWW b9ou9 C6 MOonsto PFI13 C6 SLMdrY PFOS &M tp9ne r~ s~ r~~ pNM !IwM >awt p'~ p..~~ ,.1 SY/4 p I~M 's.. ..~,in 4 ~--`~' A V RAM "'0M 1"4b MwL ~K ~y DL2f01aPP00a00Nl1t1 IOeMnrqtC.t6li+AiN 10 D211 Dlz4:01IrF0II30.04t021 1mUiX y0 M. 1rNesyiN 100 3247 7.00 6s 62a O ND IO 7A6 7S2 an 73 2 .01 9m 2.01 74.0 72 72 DL2491 rFOCro .ONo21 1CaoMtT7qw00.t0poi Oft) DL2 f01 4pF00*q-0N021 10 0316 6. 84 as NO 7.60 76 4 .62 113 as go" .a9Ktl04 w slM* 100 4316 67.6 67 ND 76.6 77 4.82 80.4 78 DL24Ot4PFO03441f0?t 8>w1S '>t9p6. 60 M9r.l OL,t-F014Pf006444I 07t Icw,,>fBW J.fmwb$0h" 10 0229 6 .66 66 100 0.736 66A an NO 7 .0 77 2.46 9.66 72 ND 60 .6 Bt 2 .46 620 60 DL24 014 PMI00140{1021 ICaM s M" r.m "% lp.j 10 33t6 Ol2.f 01. PW 001a0N 0~21 1 COMS = 6Mw.NONfpr) 100 0316 7 .04 67 Yp 7 .8U 76 66.0 68 /D 772 77 7.66 3.66 119 652 60 79 D124014I5F001444102 1 004" 041 6. a r0 9p.1 O1,241AOF W 1-04H 02 1 ! 0 1+0 90 4+w 004ph1 10 013, 7.36 70 I1D 620 62 7 72 76.0 100 0221 61.6 at Ib 77.8 78 777 166 61 GLM 1- W FQ720041021 IOe~n4tC.t0YV~>IO~rV 10 D .406 6 M 65 D124101-YBF002-0p4102 1 Kamewt MrM.1W0t soft) tOD CA00 61 4 61 NO 7A8 75 98 .6 101 NO 66A 66 04e 166 61 Dl2-f01-1L'lfG07-0414/0R1 f00wiaa SPt0.10M0 Mft) 10 0A16 6.62 61 MD 6.711 66 410 412 Di7 4014ASF003004100 1 =MhC9WL1C0MBoom 100 04/6 64 .6 64 NO 70A 71 41 .6 104 62 DLZF014R'F01M4~44102 1 pwhst,6 9. 1 0RtaNy 10 Dt2 fOt.qFD)6.0W041021 loowna 1M I. w0 Ppe yy 100 0.348 0 346 7 .06 67 ID 7.96 71.6 71 ND 61 :2 76 QI 67.0 912 ~L6 167 63 DLt .{-0t4PFOG100N021 91 0 014 19W.U P0906) OL14 :014PF001dO41021 10 0 .132 7 .44 70 0261 6.16 79 734 40 .0 (0NOW !M K 141p 30M) 100 OA32 672 6? 0161 78.4 711 JOA 105.0 73 DLYiD1 4PF003"102 1 BMsw d 4 k 0.,0 wb 9" DU-FDI~F00340410Q 1 ldo~na 90 L. IN ~ 17 20 66 !ID 6A6 y9y 60 1 66 WD GI A Si l66 10 .6 73 62 166 60 .0 76 7~*iM ir~ir anwM A~ pYYy Mw~ ~er~: Nw4.b r ~aawr wawy .Mn ortvY N a1aW ND ~ NoldwOrd9ta alewLY~IldOuwWWkm+IYahY02npb(retwly~ll MI WtwpY0dw10qrymNel IMr:61no iw rMrry r9M PrdllrMA M do rA YiwrMMg lP+~ In 7M1. 9. GU ShOm ONW06d nwiRr. weewy . aY. e wyr WryMyi9r 6m M mown in 9r MW NNa Exygen Research Page 34 of 132 p . 35 Interim Report #l0-Analysis of Fish and Clarp Samples Exyocn Study No . : P000113 1 Table IV. Matrix Spike RecoveryPFBS, PFHS and PFOS in Fish Samples .(continued) ADRW AWFGQrd /mant And ieuN . 14naw1 b Cwqb ROa0~w00 Rw-Y Si lOqp10 ROao - rd ROCe.O y v Aft FmWW Mmurlt b Sr * i Roca PAMMY w t .t rr _01- pf,,YOf.Pf00{P0~1021 ~ $06a . 111104,410810] 10 O.7114 O.M 91 NO i 10:! . . . 100 , 0 = 6.90 !E OL}FO1~F004-0-0i7021 poMlMltitU.110qYLW 100 0 .76) as Of NO O/A l0 . . O.W. . 81 2 91 pG1.F01-PF0W001104I IOIO.Nm71 o 0,10MMn) 10 1.53 5A4 JY N6 0.10 @ D.4s 117 82 O13P01-IPF006 0 041001 ICOww7yr6ws 00 400) 100 1.63 i0.4 60 NO 032 99 !46 e6.0 in 0lGPo1I/FU01-0OII021 00114114S00, R10p10Mr 10 1.34 024 {0 0. 002 10 2 . , .. 101 . NR 0lG01IiFD01 .0041021 _ OVw/NIM,, tOqo>yY) 100 1.34 0.0 4 00 0.442 eaa 00 NR MR NR NR NR O/f}F014iF002-0-041021 I~y/NMa .rM.lp.1 pOGF014PFp024-04191I leaww4 GO. K lamb so*) 10 1.43 S.N 100 1.43 662 44 6E NIJ No 938 ., . 1 1 110 113 041 .0 M 110 1!0 70 0lC4F014i003*4N021 Ie00aM0arlt0,nlMt/s 10 CAN 0 .72 oso.F01410100 03 4441021 IpMM7070e L toANilr1 100 0.00 6 OiO.t 67 00 0.011 10 .4 YO 0.614 66 a 00 MR MR NR NR MR MR OBC-F01-P1N001~041021 K048107 to R q N>lliN 10 OlGI0WW001-0041021 10wnHNaKMepr 4w) 100 0.884 0.094 7A! 7" 42 221 40 211 . Y .Ee 75 NR WA >lt NR MR NR MR MR OBC4014P W 001 4 0r10t I rO,NAYR54A 1Ipor~u I 09GA01.iW002O611021 iCmwfTqO~ .~MM1 10 0.100 7 .50 0 ~ 100 "0.700 O40 Oi .+.012 6. 12 14.2 N MR MR MR 00.0 6/ MR MR NR OOC4F01-P W 0004 C410QI sm"103 goal 111001106111 AG 0 .7% pOpd0 UlYV00 5 0041021 Rsasla M r. tw xo t1I.1 100 0 .7 36 . 2.32 7! 6.76 '70A 70 4.701 1" W . . NR MR MR OOA M NR NR NR OOU.F01 4PF001 .0O4i021 M OOK04 Irt ,uRAqyrl 10 4.90 10A /6 1 .02 0.41 Oi011F014 /10014041 021 9 100011111YcR = wtM s) .1100 4.!! 70A 72 142 16.0 86 NR , ,. as MR MR MR . NR NR p0I}4 :p14 pF002.6041021 K>ft1Ww VPk aw Pp O/r1 10 l.70 DCt>F014Pi002-0-041021 IOOOMItiMtl 10r P16 po.l 100 0.7E 131 a 7" as OJQ2 9.72 40 NR MR NR 0.722 l0.0 -79 MR MR MR OfMiF01 4 PF0010-041021 {OOM4tM As tG/0 NO Bpi" .. .. 10 5./0 12.0 00 1 .02 - 10.0 96 MR.. OOt14:91.1PF0030441021 Ip014t76 70RIlISMpO q 100 'J.M, l14 ' ' . . 75 :fA2 80.4 p "NR .. MR NR MR MR f . .qw mid" sMr 10 1014" iWM .4 OM M1: IIrOAn. rn GeerM nawy .~u. rawrre~ oreYre ND . NOI O~YC10 M ar MOYOLImR d Ou~f~Mdlon Wdd~ Y 0 .2 nn MM nMqp. NR1M7tINOrdA~bryr~ m~YalwwAtLMMw R ~rlyplw~lr .~~iowlbTaOMM. IYr: i~s NM Nw~11Ny IWI~ Mrw ~rb~ nwYl~ ~.wwy1N~ rJ'vrf My1Mp hww 1M rMM In h wr ~ . . Exygen Rescerch Page 35 of 132 p . 36 Interim Rcpart #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Table IV. Matrix Spike Recovery PFBS, PFUS and PFOS In Fish Samples (continued) OwyM 901nd >w.a r. P H sw~S ,~. vr ~ ~ ,, A 0M NKarrO IEs OO'wY M S6nph Racpw w ftoo.Ny ww rw wi.a r .L A ,I C* s,,1ar . v P Q%" Affewt in 6'anpN ftOO.Y60 RwaoMry VgW .Ww. j"NI.M .A o01,0 F01 .pF0040011021 91 w4w air 0. M rA 6M .1 t0 DOl F01 Wf00~OM1021 s+ta 6w 4 rw~>M~ 100 L.12 1l.t 11 2.30 11,12 764 70 2-30 12 .0 07 NR NR MR 60A 64 NR NR NR oDU401 Mf0 06 0 41/0 21 10o~NnM OR L 1opY tw) 10 4A6 DDUf QI 4/F0060041021 (Owrnaalrt,tpM9pr) 100 4 .i0 12.2 76 0.066 112 102 NR NR N11 7" 71 DAN a6A 06 NR NN NR o01F1001 4P Ai001 -0-0410 21 101100i50 6o r,rp6 80198) 10 2J0 103 73 0016 10 .7 DDLLiD1 4101AfOD1 4441021 IC~.MlfytKMDf0~616s1 100, 2 XV 72A 70 OA16 6A.6 96 83 NR NR NR NR NR NR oDUf 01 NMt00Q40N OQt 1CaM61601ra4waM7 056) DOWF0ldrq1002-044102 1 lGaN6s4k1 .ti6w6Nr) 10 16.4 100 10A 34 .4 160 0 .90 13 2 96 N11 NR NR 01 .6 76 160 062 M NR HS NR Dl .ii-01-1101N001-0-0t 1021 I C1111MM+ Sit l 16 PO 10W IO 0201 9.32 01 ND 0 .X41M6YY001~~1021 (OOMHMtaJ,lMlprMy 100 0108 761 77 NO 6.06 Q 662 as 120 126 120 1T1 97 0L2401 a4DYY0020-0i 1021 lmrna90 K a M160 rw 10 ND 9.0 IT NO 9.12 IM 102 110 D62-/' 0t IW IYV002-0-0{ t021 (0n 6 w ML+rWS 6 r 01 100 ND 664 60 NO 03 6 94 102 103 Oq DL2 -M419YY10 00-0.OH021 909 aaqr4rw6 yrp /0 No 924 92 NO 946 91 0 2A 103 D12-FQt-61{VV003 0441021 lCO Ata6He.MeMM6.) 100 NO 613 01 ND 962 96 92 .4 1 82 6D OL2F01 dIpYY00464 11021 06uw 10 L 10 w 4 w 10 NO 7 .E6 76 NO 725 73 ask 7S6 D14FOt~qYY004001102 1 t0 M+n94 6o p,1M pp 61M 100 ND 62A 02 NO 130 91 f6A 106 79 OL 3 F01-I4pA1009 444 1021 poemsl* CL 190011001 10 RD 7.1111 OD NO &0111 81 14111 136 DL2f01.16l1W006Op 10$ 1 1015404106 w,16 100 9'r1 100 ND 90.6 01 10 100 100 196 234 96 06C4D1-MOW001~06110 4 OCdMN0Nea10w 6 >wMI 10 DlC-I 0141SM1001 -0441 104 ICmw5690 R t0s 1 0 41r) 100 oA66 0.6 06 10.3 00.4 94 0 = 90 0.32 17:6 03 NR Na Na 113 106 NR NR Na '.F1*0 * nwA *Oft" * . paip ww dpr..ny6r.aa iA MOM" 000 ry ww . was adm w NO - Na 4M6CMd at v 600e liT M of 0lwM6Yi0n wAr eA is 02 " (r1 a aiqltlF Ml .Netep.rl~dOMb~r~rCOYd~wJIMrrL AWy~~mawMqMwIM TWy6 . NeYa Oliw tl~y wtirytab *am ~A~d wwi>1s, seOwry .Uuw ~y :aY ~961MpYa~s Iw ~alw~ b 6w rwr Ar1 Exygm Research Page 36 of 132 p . 37 Interim Report #10-Malysis of Fish and Clam Samples Exygen Study No . : P000113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) 8i1FM F~ ~ ~ ~ ~ ~ AmW ARC*A F PF oU w Aft wob d in 9 w9" R -wne RNowy in 8 CIS W13 4r AA os~~d Rrmwry CS AmAll i n l anW R eaowee ROOOwy AtK v w t AI.- ftww-w rt rMR wlrl D9C{01 .NSW002fi-N 1101 100041 It* LN wb Wks) 10 OAK 9A0 91 3b3 121 94 NR MR MR pgG4C0140ri00]444110{ 1000 "1yar.lw 1110 110111 100 CAN 946 99 3.43 111 110 NR NR NR OBC.M4{9MYOO 3"1105 I~JMYiifp0.101lb #Aft1 10 OAOD Y .@ OS1CiFQ14AqwOO"-O 1104 t~nOMasYKlww pw 100 OA00 e0.0 91 06 3.02 135 3.62 10 4 100 MR NR NR 100 NR NR NR O W4qOf4 1SbY001 #04110 4 ICaw+a 4* 1. >eMU1N 0i>c.Pp1 al6W 00tL-0i 110a m wMp titJ.1w 06 1111r1 IQ 100 O.ON 9.00 i1 0.72 10 .5 90 O.OM 0T.2 YO 0.72 1 24 114 NR lil MR NR NR NR p0(YFU{4A6W 006A 41110a 9201wM7IaiC 10 NP 111011111 10 0.032 620 74 2.77 102 74 NR NR NR 090iFQ1 4 16W 000-0-001104 XaMNY 40L.00060pw 100 0.012 91A i/ tn 100 106 NR NR NR OBGF01-MW-001 -0441101 fOlMwwyo KlOMy " 10 0.6Z0 0.00 D9GF0144F001-0-01/10 4 low/MltfpK+wM~4r) 100 0. 020 1M-4 00 M 3.40 11.7 1 01 3.95 /00 102 NR NR NR NR NR NR 000 I014 1WO 024 -0H 10t IO~MaMa 10R+>M~1 10 0.756 0.02 000 F01 4I4M 0020011104 100"M 40 r.5 0061110rq 100 0.100 SOB 12 1 .91 125 100 NR NR NR YO 1A4, 102 100 NR NR N11 0lGFOt-lf00400 1104 !a014Y f 4H 0.t5 00Aft 1 10 DY(rF01-411F004"110 1 tCwli w lwa Oft, rMqrl 100 0.504 42.3 100 0.601 aJ 01 0.504 11A 110 142 152 0.504 100 106 1Q 264 112 066'-i01-if 0000-0n 704 p16w1M4q .1Mrp6464 " 10 1 10 / 0,4 61 2 .16 122 101 NR NR OeGI014TO0"441 104 IO~wrwrrts.lwoNNr1 100 1A0 90A 09 2.15 105 100 NR NR Ni MR O/GtVt-pYrb0~-0a41tW (OmNMOfyk 0,10M40) 10 0 .401 9.72 92 3111 13D 0 W~ 01-IP1400b4 04/10OI IW610, S/K1 05MyoN 100 0.1W 576 aT 5 29 104 97 NR NR NR tOt Ult NR MR OBCf 01 PVY0116A81110K ICONww9otlwwO iW 000- f014p1110064441 104 Iu0w1w>M0.1w wb yr) 10 0 .572 10A 100 C.6T2 iRD 99 2.10 172 111 NR NR NR Yl 2.10 102 100 OR NR NR '~~VM wN~ roM~ Mayi4ia0 W, d .~ir~yc ae s owwo woowY veYs trrwf M oM[MwQ ND - Nol b110 dW M a OboM U~f d Ckw~lon MiaU N 0 .2 ~p QrM +M~+q. MR-Neitpi W &w b qww Omi1iM iMJ1 Uiwa R wa W y W Owebavo4m in Tame 1, NObc OMq~ W wANOWY rYb Mw~ wMid MMY,wMrry wYw ~~'rY ~MOb MN *WON M M eM 41 . . Exygen Research Page 37 of 132 p . 38 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P000113 1 Table B7. Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples (continued) 6FnOb C4 SWWW6 a PiNS rx,raw. PF" Marr M+ FGUW Ana .: Atf WAW In 8Mnp4 ROa0w60 Rey N 8 mpN Raarrtl ROpow, h 8 py ROOOwRrd ROCO.ryr rt w v~. ~t 00{Fi61 .IpW00S44t1 t01 IOrwwt,sKi4 M 6 41) 10 D0l}f 01 iP W O03 40A1 l0i tcaotwil yk L. w0 w6 aPr) 100 3.12 13.1 3.12 N.Q 100 as 8A0 18 3 6A0 107 103 f01 MR NR MR NR !R NR OOlL4 01- 00YU006-044 1101 (COMwQNtGl0oo6 so") 10 3A8 128 BJ 7.12 17 .4 103 Ni NR MR DOt1F01-iPYH004-0-64 1101 plod"a to 06 100 tp Mo1 100 3A0 BBA 86 7.12 108 tOt MR NR MR 0p{I01 4PY/000-0 04110 t t0OywMttte o04P'.1 10 2.97 00U-i01-OD W00600t1101 4CCwwaMt 11/pM 40ft1 100 2.07 10.! 75 5.12 13.6 M HR HR NR 83.6 61 ki.12 100 104 NR Nit MR O WO1.PN002b0 441 /03 iC10NW4k 4 * Opb4M.t 0t2-F01-IPYM00 2-0 611101 9 NtMM @Pk 4. te3wb 1900 10 100 1 .04 1 04 0.48 84 80 .0 79 HD /0A 104 (L.20 1{ 2 61 No 074 06 8.10 124 118 Ql14O1d10W0014-04110 4 /amNwrsdl.nriclWy t0 120 10 .0 otf sO1 4AMMio01d.0At16t Icau~wMtxwowM~t 100 1]p 88.0 94 80 0.808 11 3 IN 0.800 112 111 NR NR NR NR NR NR OUf01 IBW002~-ON101 p0&I0601f0liK 10M4JOY1 10 1 .30 0.7 6 88 DL 1-F01 4ISIry002-0 6t 1 t 0 1 IOMrrMt>r L troi a/ .1 100 1J0 B0 .4 79 1 .72 12.1 1 07 NR NR NR 1J2 100 OB NR NR NR OLti01 4000O61441110 4 ICODMMI7/t 4 t0 w6 N4) 10 0 400 6.92 M 1 .13 102 81 NR MR NR DU itDt dr>d1b'0010-041104 5x6WNfUa0.149 1Aeow 100 0 .500 88.2 w 1 .13 00.8 OB Wt NR MR OU -M-MlY10040- W 1164 lOOOMiM yR R 1 0 M 1M0.1 to a1 .F01~8YM0048041101 IpawNMr,toow~e~Y) 100 0.000 841 CAN 81 A 78 84 0.908 f.78 88 161 201 0.008 90O 00 /8t 280 108 OL1 f0/ 4AWNF004004 1104 M1000606110% tomb so" 1Q 1 .18 1.80 76 n1iD14 BW000dp1104 woouwycKUO poo rirl 1 00 1 .16 02 .4 at 1 .18 t0A 1 2 NR NR NR 1.16 96D 08 NR NR MR DU-FW AIBF001-0A/1104 (000W/ta OPtt.apY 0@9 H t0 No 7 .14 78 0.313 8.32 82 200 011 401 d10F001 -0 6411 a MOW" OM A aewr>IMW) 100 wo 78A 70 0.318 ODa s0 293 303 30 1 101 'M~qn r~e 610wf . M 106 9 *4M WAS +'rl' IMw4% Ensajob Marl dw iM W M0MaNwd ND ~ fVat bYCUd ~t s ala0linW 0I OuMtlYMOn dYdt fa 02 n~ {we! twldd) . NR . N01 '" b P~1' pM1Ytl Irw~k M1M. 4M1~1~ Ip111N M Yf WII Y1 T~EI~ t N4 Saw Aft fiMWAry fMl o MMw0 MWAB8 w ooft MM" wMbawq wy MIoMT MM /M nlwr M Mb rrr dob. Exygen Research Page 38 of 132 p . 39 Interim Report #10-Analysis of Fish and Clam Samples fixygen Study No . : P000113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) mNp~ OL1-F01-W00244)4110 1 09I71tMM.,OMO" 0 .1-FOI~IQF0t1i00N 10 40 41aw OMm4IOMm X CO PFtiS PFMO C5&Mo1W~ Ant t APM pMQ Aman My M ~Iw R~q wNr7b In 3nA ~ Alt eo, w~ W R,Ao~ wwTN N Jr,i~x r RO" OO~ rwOp #~a,w, M~K KlK wtK rIK KIK MtM . 10 ND BA) 00 0 .420 10A tlp MR MR MR 100 ND aa 00 OA74 96.4 00 MR MR MR OL1 401 4 1SF00 3* OH 101 AOaM OM R M~ rrwt 10 tx1f01saWDOw-04110 4 lcola77sOD.I01"byiq 100 0200 0.79 0.701 MA M 0. 802 102 04 0.002 062 as MR 66 MR MR MR MR MR 011.i01-Gap0040Ot1104 ta aw7iaK> 01+014ANI004-OM1104 1mOw 80 l.IaOM*aMr1 ,oonMN 10 ND 61! N 0 332 100 ND 00.0 A7 O.S77 t0A i0 101 100 a1-FOHI6F006-0-0N/0a (CMMWS OM 0.1 .1 O OAst 10 No S1if014AOF000A.041101 (OOO"ialrtK1O10080y 4 00 ND 0.01 !0 12.4 82 0.484 10 .1 94 0.664 91A tp NR MR MR MR MR NR MR MR MR MR MR MR OL1f04PM10014)-04110 4 lODMnOfMl10N0 too) 10 OL1.F0fpW001-044110 4 co00MN{ "k J. NO ,p Orh., 100 0 .772 0.772 a61 79 4A00 212 itt 17A 20 .4 so 64.0 tp aS60 w .0 97 17A 113 96 004014P1q10024M041 10 1 WowM7fwKUnMyrt 10 a40 an 82 OL1+014Py10o2-0-01110 1 MOOMhUk L. /COwMMON 100 0 .060 70.4 75 omti aSTO 9,16 Yf 10.7 27A 117 800 97 157 100 04 00-0014PN100540411 M l~t1MC.10w0rAM+1 10 110 Y0o DL1- N1 -PW 00,}"110a (O60Ur77 yt0.faop a t bo 100 ND 90.4 91 90 O.T00 QM 92 0200 106 106 iw70 0 .30 t0.7 109 73 100 DL1-FC14P1M004~04110 4 lO~Ow~70y e.,o~al~rt 10 ND 0 .W14PW004.0.O41104 t0~1Mltyi,l00p00Mq 100 ND 0.4e 06 71A 72 0.230 0.l0 00 0.210 bl .E Sy 60,0 72A SY,O 140 0p Ol1-t%9f~FC0?4~110/ 1010N1At1~0,tOt1001Y/ 10 ND D1,f01'MF00P00N t0s Po">"MK1MOO M"1 100 ND 6. 00 00 0r12 0,20 in 86.4 0 9 0.222 0!A 06 11,1 1 09 70 11 .1 100 97 a-/f014FOC300411 a 11NN"M l0 410 " Yy 4 10 ND Da-14101 .pFooa4.W104 Wawa 4r J.t00Mlar1 100 ND LOCI M O.ZdS 704 79 0.265 101 100 20y 30,5 of 00 4 00 205 109 00 3Mib,WOU~rcNr ow iOnObti 0 I1MC1~l. ftvbN1111 swim A111MrytWOranotMot444 0 ND - MW a0tschd at Of OpOrO tiMt d DIrYMa,,MrYI ts 02 ndq MM rr~lr~ IAI' Np ~OOIM M ID?~M E1~Y1 ~R YYa Ib7il~b wwi M Mwn M TYI~ t i MOM t"p tw OM~ Ttf6Y rft" -MbW --M% -w-y Mo- -V _y WWft Moo tfq vjW" b,M wM dN 6 Exygen Rmamh Page 39 of 132 p . 40 Interim Report #10-Analysis of fish and Clam Samples Exygen Study No . : P000113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples (condoned) BMpu pllll~ G PP96 I P Cs RNS lNiad Mroud Amt FOU+d Aftwisell 1. Faird MAWFoe H0ad l0 9Mtpl IYmMO RsowrY N160miaN RiaoNnd Reoowy in 01, 0N Rlaowe Wroqry IA[. bill ." w. wtr~. wtM. wavR .0 K Dlr t f 01-i'F00160/ 110/ t6m 10M1i/YK10M40M 10 ND BAD OD ND 9.N 96 7. 00 1!2 02 pL-1 *0t-pF0010441104 ~a sp l tao .~ frw 100 NO 644 06 ND 90.9 9o 7 .90 102 OM DL-1 f01-PFODd001110 1 IOOpp111lqMa Is 00 80" t71-1 fO1 -W F0064041101' K>tOwiMa.tGOwO aa) 10 ND 900 ND 7.44 74 044 !6 0,75 9.00 O .Yfs 96A es e.72 LSA 71 0 0.72 1 02 93 00 F0 144101N 001 4O4 1106 1ooelwo spi L wr son) DL3,i01 4 yYtl001 Q-0 11105 1dwWly r.w0 110 go") 10 ND 6.38 100 ND Ois M ND 0.20 92 139 106 all ND 1G6 100 1 39 25 E 119 DL34b1-WW00244 41105 K,mwr~rO,vMf~ 10 NO Al." 94 ND 1 92 90 100 1 50 01.3}'01 -IA8YY002-0-011106 ~MMMlMM.t00oq+N 100 N D 90A 9J No 106 100 1!0 293 IN 01.14M1 4 qW 005" 1105 ccaouMe aai a ..e or .w 10 No a9o 0a ND 9.Qe 99 t 4e 1sa DI.Sf Ot41 SYYn0&00/ t 100 low0a so A w7ArMr! 100 NO NA 9D ND 102 102 146 764 100 O0 A01 aApN0040-011106 poMrArROq Goal 01.3 F01-MBYY00 440N1os tamai ftk L trr AWL" ,0 ND e.40 93 0216 0.N 04 ,99 72 5 10o No 9sA ee 0 206 1 02 102 1oe 301 10 0 0 (34QI 1A6M10064-0 4, 1106 100400 iKC.toqr 111111110} 10 d.341014ABW0060041106 1ao.wOt M Q uo ~>wy 100 ND NO 111. 511 90 0.300 11 .1 10T 173 10 6 100 100 0.316 100 106 173 36 6 77 4. tomb paw) 01-3 F01a1lFOp 1-0G41105 IC0001 rtlo f 10 WD 9.N OS ND 11 .! 11 4 110 130 DL3F01-119F0p1-0O/510 6 1~w0 ~.~w~4~.1 100 ND Osa 9e ND 10t is* 110 234 110 DL341014AMOfaOMllos Ioaww Ots.w7NNOM 10 ND 0.l0 W No 10.t 104 119 96.9 DL 3-FO140r002-004 1 t06 taa.u.o 10 K .t.owNw 100 No 0" a0 ND t03 e03 lie 219 100 OLSF01-A AFOG5 0041106 OCmWM fpltaA01W) t0 ND 9.II Olhf01-1~FOOSOOs1106 IW~MiO J.Y>'IMSM1~) 100 ND l0.9 to /b 91 ND 11A 119 107 107 76,! 020 70.6 /90 /1A YampN Mal" Momob 1104YW'Y rwl pd.iiil4>t "dtr~ aH soOwwoMtwf rWr 1- be akUMd NO - Na dWctwl A Or own Um0 of G mMMf " dw dt Y 02 nOq ,%w oyn~ MR- No nporrd a. Is wrw ourd w .ri t.r.a te,wwNvca,. .iw an wum tirqy n. Netic Slam W .r.rr WAS Me.v iewww "sew . t - cwiryti Whrs a" rcY .Oy* M..Ou .da. te as W. Mw Exygen Remmrch Page 40 of 132 p . 41 Interim Report #10-Analysis of Fish and Clam Samples . Exygen Study Na: P000113 1 Table IN. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued ) SW MW .~ ~ ~ Ar ArM Mwet Anil Affewit tpws r+9rrq1 RAoow~0 RborrY IR 9rnpM Rt~sw~Nl fLao mY ti SovVM Rs oowmd Rrm~wy . .r ..r. . . .t. . . .t .. .t OL}FOIIqF0040W1106 . IpOwrls~aK/0a101My 10 ND Lf0 16 10 '11 .0 .. i1o d1F0111lIF000 00{110s 1000winlMt.,rNw 1114 .l 100 ND 90A YO No 104 104 130 130 /N ?30 ,00 OL}i04M'1R, 006044 7105 pmtwtsr c wq~yr) 10 No 0.!2 !0 OL3-F91 4100006-0041106 40101610111 go a 1 apM spot 100 No Sea 0! NO 10.9 103 . NO 4W 1 w all $7 2 01 .0 IV w D OW,F01 -1PW006-0 -0 111 0E 10a04011N0 It,rMMy 10 ID 0A0 VMe4*i-rww*444110 6 ~owa 00 r. 100011Pr) 100 1D ilA 83 N 0398 0 .31111 932 01 012 79A 90.6 w 913 1S6 96 OMC404RV00s-04411b5 IGanwlit0.10 Poi soft) 10 0.300 0NGF01dPMf00ldAt110 6 FwdMM pklt lawelpN 100 0.300 R01 71 90A YO 0-V! 0.796 . -9.711 104 . 00 9id 107 10 4$10 .6 low w 0MC401-IpYY00 6 0 441 10 6 l~+~MttrM~1 10 ND OAO C11040141'MI006404,1 10 I"J .100 pu6 sM6p0o~w H 100 ND 00.1 SO 0.270 0 02TO 10 .1 91 .MA 1'iA 106 106 la .a 169 a DIAL' F01 itlYV0030041/06 {OM911111 60 K 10 00 4101100 1o ND a64 pdG W1-tt6W0 W A"1106 ICMMwN* L NmwO t/W 100 NO 021 00 0.572 110 9 2 0.902 1a . 1a / 06 :W ]N 364 4M 110 Os1Cf V f a17YY001A091106 p00NM7yt0,M~~1 IO 0.319 447 9Z / .W 12 .1 102, 269 2Si O4C.F01 411 SW006 0W01I100 , . . FAM1~I ~la wolp Wt 100 0.710 02{ 02 12D 101 . as ,279 313 54 oMC4 iul -14111100060a110 5 pmr~r 80 E.1 6 M SPE.1 10 NO i10 42 0300 11A 1 00 NR NR NR DdCGi01 4A1YY00680 41106 10~~rtAf ./mOO~MU 100 NO 99.0 94 0.910 its 111 !!t NR MR OMGlOt .ipCOQOOr1/0! {OaOw.My.O,+OwrqMi 10 GMrr014W002-0 4011w R7aow 10 1tw0pe 81Orl 100 NO ND d 30 04 NO as w NO 10A 104 NR NR NR 104 , f01 lit . 11R MR DMC401 4AW003"1106 (OOOntuYOrtt IuMapp) DNCM4418F0W401 1106 001014111100 OPi110NM soft) 1 0 IID 0.20 43 ND 10A 100 !p 1 972 A ID 110 loOl 6{.9 100 . 110'' sea 104 131 'SrPr+MkM ~/M Mb ~ .~ .9~~ oftR M i0flrliM AM>MY wY~ 'be arOWYO WO . Not dft p w a w above t1M1 d OrM Mm vlnoM M 02py (wt+r+y y. t111 . Nq iard Si. to 4+l 4 asiYW wNA hMa Ib~ry~y ~Mr N M~ww In T . W I L Nabc 110 o oft w~rwr two ww" wiwr/ NwiY~ .~ewwY+wttrr my V" NO~IfM M rw . A 11,41 row 4" Eaygen Research Page 41 of 132 p . 42 Interirn Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P004113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) llMbplb AN10int Mn FMwO AmbWt And FanO AW*WA MR Ae11pA ftWa M 86i1m hmMfdO Ra'OMry in 86nON ksmmba RamMry in 9mpb RemwW Ii=Wry .a R Mt w .a ~tt +rr. 06ICf01 4fBFOM4A411 n 6 06K. 19105999) 10 ND 9.78 DMCi01410l0040-04110 6 fdMMNbal None spew) 100 NO 68 D 66 as 0154 11 .1 0.254 t07 106 116 123 101 119 226 11D pMCrF014A8P00S044i106 OswllQbyft 4w N.yr1 10 D1N.`F014ASIZ006"110 6 Icawm 1YO, tbM Mrl 100 ND no 8.52 96 0.420 122 116 U6 193 631 8/ 0 .120 110 110 146 290 14 DIIG i01-MFOOS0441 i O 6 1CWltl204,MA661Ir1 10 ND 7 .92 79 ND 501 0MGF014FF0004041 t0 6 ICmAeoe6rtl, fm J NNNO 1D0 ND 62A 67 ND 1o6 106 105 7.1 2 7.62 16D 61 101 13 nLIG-F01-IPF 001-0-04106 SOMW01 tMQ tOMM0) 10 NO 7.0e dW--FO14+F0044411106 tOmlMU 9/Kf00wh %4 100 ND 632 76 ND 10 .7 107 44A 80 NO 107 107 44A 56.2 134 90 D11Gi014PF0064ft5106 IOO0M1a6}tl loop OMU 10 ND 7.66 19 D1MC-POf aV/OG64dI i 106 1 =90a 10J.+aoorsMM1 100 ND 13A 0) 10 .3 103 404 54A 76 ND 96A 06 46.e 121 75 DL2401-4MON041210 looau br R n cr WI 10 DLbf01 iVMOCb00~121 6 tamNsws b<rf. no Or yrf 100 ND ND 6,M 04 ND 10A 100 492 $32 62 ND 102 102 462 50 2 100 142 93 151.2 F054P1MOG6.004121 6 h9fMMwC.aM~Y) 0L24014P W0064W04121 6 tcoNrrSOD. loop" Wend 10 ND 6.OD 69 100 ND MA 05 ND its 116 tl ;. 22.7 9S ND 107 1a7 132 121 too DOU-931418 W i00?044121 6 SOOOONNML1eM GPM" 10 0106 6.62 67 DOUf0144W002-0-04124 {eoab"Nbpa .S Po qb.l 100 0206 072 07 1n 10s 1 .72 on 62 MR 91 NR Na MI MR N/1 01.2*014V W 00460t 121 6 to N0476R4w 010, 1111610) DL2-F014PWOf4d4)4121 6 lOmeas7it.0100eo soft) 10 100 NO ND 6.06 61 76A 77 ND NO 10 .4 106 962 OS OAD 14A 90 6.E0 612 00 DOU40140yk00$00412/0 1006tM06McM,NIdr604 10 WD 6.12 61 10.4 19A 60 NR !R MR 0OU401 iA W M007A072M W M&Uw AO t,+ m MfMN 100 NO OOA 66 10. 4 106 95 NR NR NR 'SAqM ~~ ~4 M~MiYi0lwd bti~r: iwadm .oauM armmy rWe NmOt W oiabfr b ND NW d0ret60 al p,rea~ lJmO d OW btabm rlYkh Y .0? Opq} 0m w lyf~ NR - NCIO00i00MM1pO06R+s01MY1Fm/[yiMr 11 aiM/WAMiYL'6t'.aminTaEH L Npft 6>[a Oft WMM Fy 1 6y M11016 RYIMIp IOYr, Ii ftNIy Y7MNK SAW x/ M0W *Oi'lY Vahan in !te mar dah L Exygcn Research Page 42 of 132 p . 43 Interim Rcpowt #10-Analysis of Fish and Clam Samples Exygen Study No . : P004113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) CA Sdkrgft PM PFMS ~rw,w vFOa MO ." Om romw POW" ?r~pb 8pbAa in B, P, ROaOw~d P4 oOr+ry b~nFU RN~mA r w RAO O r w 7 wemor I n a~i0M ROpprMrO Rrow+ry 013FOtaPW0U 80N 13 0 IOOON~My- t,sONNw 10 1 MD 7 .52 OLSP01 4PYU00180 4 1130 ~OmMy~MM p .1rM % fMq 100 ND !iA 75 as MD 11 .0 1t0 NO 111 110 7 .02 7 .10 17 .3 YW 1 14 106 ppti 531 .46W00111 4412t 4 (~AeMw %PkQ.UN fAM 10 7.09 11A 76 DOV~1-0 06121 0 Ip4wpyM6 1qMb fMr1 100 7.06 AS2 76 1b4 :SI 273 122.0 1 21 MR MR MR 107 MR RR MR DOOP"46WOPI .O." 12 1 0 I= wrlMt.rw6 2M+0 10 00{J.F01 4A! W 004-804141 6 lO~oMwM P .+AMMr! 100 4.72 4.73 10A f1 21.7 2G 3 72.f M 21-7 10 4 76 42 MR MR MR MR MR MR p0Ui01ANDW 006404121 6 1OprIMR 4PYqM706 M1 10 00U>'M-AOfW 00SQ W 121 0 p~oe~WArw,wopM open) too 0 .784 7 .06 67 1 .34 0264 72.0 72 1AU 0. 5 2 87A 72 an MR MR not no MR RR OOILF01 4A8P00604112/e poaqrfqMf,Mqb yw) 10 1.41 ooLLF4t4A8Foo&o-o4i2w 1 (G+qMMwa~woiM4r1 100 1 A 1 0.00 72 6,10 17A 62 MR MR MR 7" 71 6.4 0 94A M MR MR MR O13f01-IfNM002d0411 30 10A6U WL qw6 >M * OL 3-F014PYVOOZ-0 0411 30 10~ no F. INo on tow 10 W 7.92 79 NQ 9 .04 90 12 .0 /6E 18 100 ND 0 12 61 MD 110 . 110 12 0 106 113 pL2-Po1 41Y003O4X 11 30 lowM~M>M6,wA+r1M.1 10 ND 7,l0 60 O(.3-fpt-rW0004 8111 30 KNOWN 40 MMCM+MI 100 MD MA bl Mp ND ! .N . p 8.44 12 3 107 102 6M 02 0 60 97 001YF0144F0004411716 40"19" NytR .qppiepw ppL4V14A8FOQS Qp{1216 (019"M go L 1wMN+ N 10 1 .72 4.00 73 6.54 14.3 100 1 .72 N.6 !0 6.5! 107 100 MR MR MR MR Mt MR 0eCd01 rtar0wtoN21 6 ICarw OpGpoM son) OOCi01~00it-0N31f (CN wfyi0,/op yty 10 0720 L96 D1 100 0.220 C" IS 1 .70 11 4 t .7Y 06.8 07 MR MR MR 96 MR NR MR 0e0.F01 JiiP006.0-01121e ICqMW 7O K 0004OW 10 No l.76 61 ' 1 .26 DECi~1~F006-0-011216 N1aMwLal./00M>r~U 100 NP 10.0 ' bl 1AE 11A IT . SOPS so MR IIR MR MR MR M R Sw+r4 w"As owes" so rpld~p 1wM W iy; s+w~~ rwaw waawY ~ w~~ MC~IOiYt~! NO - Md4MWt>,ONorana+WMtdCurAMtan wYahlt0,2ny0 twM waqlt ~ , NO-Met pqti0 AIM M PrM iA1r IMIA MIMR Il~~ll~ly~ ~11Y a1 ~MM~ M 7NN M . Merc a n" so MMYry 1r1 m /~pl~ AM~M 0801K NMVM7 w l m aNwYMOMr iwl M~ AN~ r w~r bY . Exygen Research rage 43 of 132 p . 44 Interim Report #10-Analysis of Fish and Clara Samples Exygen Study No . : P0001 13 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples (continued) lrnol0 C4 lhAlon" PM ~ a PMS M10JM Am Am" MI011t Aft Al" ,VNO.. #AtfowW MWR 30f,04 M!lOIr 0 1 ROOOr1n0 R1q0rwy ONNhW0 N~aowntl MOWrw>r N lOllpb Rco.dra0 Nrmwy YL R Y X K 11R 0Ot1F014170024-041216 woONw 9001.rp f1w1 OOU-9101,110OO 14-04 1910 [d~RaM OM K 100 fr01pft) 10 0.!B! 0.24 100 0Ad! 06A il 69 4 .0 14S 9i NR MR NR 4.Q13 104 90 NR NR NR OL14401-MW001 "11 30 1Ea0Mn00MalOw 4r.1 -10 No 067i01 ~WOD1-0441120 f00000 M 0 O 0.6fOMOV+I 100 NC 7A0 7e 01" GAO es 9.04 171 02 CA 82 0.246 101 101 0.04 102 99 OpU401-M170 02-1 4 01216 409"W71 so 11000 Opp 10 0.640 OOU-F 01 .OqF00Q-s d/12!1a ICOtdU71 so A IN w000b1 100 O.&0 9,0 4 2.0 04 61 4Jls 143 N MR NR NR *AO f03 P6 MR NR NR D0UF014AW606-0.00121e 0aMO 7e7tRK Mq %iy o0U-F01 J,ISPoO 6-0011210 IOpIM72qtL.f01 P00yft1 10 0.7i2 100 O.IiQ 7.76 Ilia 70 so 236 2.36 S .l0 66 NR MR NR we 63 NR NR NR GOll-F01 J 9 i001-0-01121e p00o00/n00~L10A yW DDU F01 ~if001J> 04t218 It1m 0/sfytr./wM00 .1 10 100 2.14 2 .1 9 11 .1 !D 1oA 20A M 42A 61 10.9 104 90 MR MR NP MR MR NR oW,F01418 70060-0412 1 6 (Om0ux00~0.~yrl 10 HD oeGFO1-MtWoo5 o0412 1 6 iawKxMaN,~aM~M~ 10D ND 1140 66 240 11.0 N NR NR NR 84A 64 2 40 10! f04 MR NR NR 004F01 44SF004d04121 6 IOOeMM aO lro0N9p.1 10 ND 7.72 77 08C .F0U15F000446121 9RJ.~oOR~ OM 61Matf +I 100 ND 76.0 76 327 12.9 00 NR NR NN 3 17 00.6 96 NR MR NR 04GFM-NBF001 4NN 1216 1COIIUOy0,/0~~1 10 NO 406 07 0 .620 9A9 {7 NR OAtGiDt ~qF001 ~0/12/6 Ipot.0a04t0.wOM Oyrq 100 NO rd.e 0 0 .420 102 102 OR MR NR MR NR OL1 f o+~PMl~i-0041216 lpOM/~1M lyA,fWU 10 0.263 7 .40 71 0 .eM 9.96 1 3 00.! a " DO-F01 JPW006b04/21 6 1LOGdM11tqJ100~00f0101 100 0253 72A 72 0.014 00A M 410.6 145 76 Ot?C01 .~p4V00~.a0/11~0 f IC0110o01M 1. to so 14r) CL2-F01 OW003 040412D1 IOmwMMi000t1,ISp0>y00 10 ND 7 .04 70 100 No 71A 72 HD 0.04 90 7.16 13.7 Q on 97 0 92 7 .40 61A 77 46V rya4 iOMFb No pMft MI %1 /6 fr~/OMaew001~ q00Nry VON plrrol4e ErIR4oUA rtD NOt dWCtOd Ol arNo .r lUrt dQuOnllalbl WiOh IO OS ny0 (wt+W~iy. NR-MM n Ppbd d Y0Up4My0071r01 fPMMla 00-0r1yW ftO rNd Ow 1A TdElOY. NMFlM00 tlNW wrMINMyYhY MOM* iF1N1d INWU. AOMq N41M RryYYy 0~ OMI NO r~N Y~ w ~M d110 . Exygen Research Page 44 of 132 p . 45 Interim Report #I Q-Analysis of Fish and Clam Samples Exygon Study No . : P000113 1 Table IV. Matrix Spike Recovery PFHS, PFHS and PFOS in Fish Samples (continued) ~ndY CO CO 9u<aW PF11S CO siMarb PFOs Am"" Mni Fond ArPoLO Aml Fmrtl MMut I A" aund 6pftb Jos I' WaOw~d R e ewwY in 9rrpN RrcaMr0 R-Mry , ins n , Iioowwad Ibeenry ~MK K r~frt ~1~1, Dt}/A 1PYYC 066YNI07 RANM7i W 4+e 10 Nr! 10 asso+-wY00soo.120+ por .w~r,. wMy~y loo ND a1e +o us 02 ND 0.90 90 a s No v72 97 4AW 74.0 91 { .ee 94 .4 a o M.rn.: 79 ww .w: 84 w-4.: K . Gr .drdo .Md..: is eY~enro .a .ro,, 1 2 sWdWdc.w .~ 'YrvY ~Wt MoM4 ~~Pw'9 ~ drMuiM MwdA M~oaniW MOOwf van ow~al M ala6W No s NOt M4 w 0 L or LYnt d OWrOR1Y0n Mllidl is 0.2 on (MR wOM UR ~ No1 AaYa W~ mi~M C~M01 wM~k 1M. 11wd!'M ~/Y w~ ~qwn le Trb ~. WNW am" W ww~ry Mb dor~ nw id w wW. wMMry Ww~ s1~1' Oyyl'M tr ~w~ Y On wir AMw Exygen Research Page 45 of 132 p . 46 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 Table V. Matrix Spike Recovery of PFOS in Re-extracted Fish Samples ca surom(. PFOs AnXxwk Arn( Found Anwx" S+n+vb Spicee in 3rmpM R KovMed Reeorwry DNaA ~ r ww! wl lack) wet WI. DBC-F01 4P W OD1-QO 4 1021 (Op048161 Spk C 1000 poA) 1000 2{IEO 1 8E0 08GGF014PIN0020041021 (C004 1 42 e pk 0. 6000 ove) 5000 3330 905 0 OBC-F01 4PW003.0.041021 (r.ca 1618oY E l COO 000 ) 1000 1E00 3190 DOU-F0I-IPF0p1 0641021 (Camn " $pt F. two ppe) 1000 OOE 1780 75 107 150 116 DO'J-FOWF0024M04102 1 (COON/05 dnk Q 1000 ppe) 1000 636 1740 110 DOl'-F01 4 PFO06 .0441021 (OW 61 418 Opk K 100 P0e) 1000 644 1850 111 DOU-F01 4FVV002-0441021 IC00I014 0 31* 1 . low "b) 08C-FQ 1-A fiSW001 Q-c41104 lCC UOWO U J,10p00 9 0 1 1000 1210 1 0000 9180 2610 140 23200 137 DBG-F01 -M.SYY002-0-1y{ 1104 PWOOdo t SO K 14000 DeC.w+-MSw0o3-aai l0 4 IOnaa62 ft c L ,16,000 Mb) DBC-F01 -Pt$W 004-0-041104 MMOO03 *P ` M ppb) ppu! 10000 7520 19800 10000 12e00 23200 L" 3440 8520 91 106 102 O 8C-Po t -MSW 00b0-041104 (cn0 rwu sok n.1 036 0 toe) 10000 6210 16200 100 D8GF01-U5F001-0041101 gw oMe apcG 10.000 ppD) 10000 O9GPoi-WFOfl2-O411104 !C00404" SOk 0.1q000 11pb) 10000 5240 14400 17E0 16200 02 104 D9C-F01PF00S-0411104 (C00tW00dpcl.i000iVp) 1000 law go 06C-F014 P W 004p.041104 !co"64 0 4k f, moo 11116 ) 1000 1 230 7600 196 080-F01-IP W OOS0.041104 (COoiaeoapwG.mOOPW) 5(M DOU-F01 4PW003-0 -041104 (OOWwa1 80 M 1000 ppe) 2820 a620 1000 2270 2640 7a 371 0OU4 O1 4PVY0040-041104 IOOwMeepcl, ta00qpp) 1000 1740 2 740 100 DOIJ-F01 4 PVVQ06 .0-0N 104 (00049M 30k J. OW ppb) 5000 2130 7600 10 9 OL 1 .F01-IN$W001-"J 10+ 9=4"N 3Pk K t00D ppD) 1000 p~ OL 1.F01 di91Ap p2-8Od 1104 (CM400" aK c. 1000 NO 1000 708 law as 1780 107 O1.1-F01-MSMIt7.03.0.041104 (C040 e730k 0,1o0c We) 1000 e08 1930 123 0l.1-F01 4A81M006-0-04170 4 (OOawl g ftk 8 .1o0o YvO) 1000 004 18E0 10e ?lot tsDa1W dw b qyellly OaWtl nrAl hMra . Value s sr not MeludW in IM wormy ~4ikica Exygen Research Page 46 of 132 p . 47 interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Table V. Matrix Spike Recovery of PFOS .in Re-extracted Fish Samples (continued) W-OS ce soroiwls Anw 1 AAA a.+e /t,nM M Sarnpli SpIkKA In 8KmpIK R4eou On0 R--wry +ra wL DL1f01-MBFi>a 240041104 (0404M71 apc F. toN no) 1000 666 1660 112 D L I f 01 . MF0 06.0041104 )COGYt'17101 9, 700o ppe) 1000 432 1670 124 D1.1-F01-MSFOO6 4 A41104 (ooo0474 sa K 1oDO NO) i 1000 740' 1630 /0p 0IMC-F0I 4AS W 006-P04110 5 SCOO040 :!q ) .10001q) 1000 DMIC-F014d9F002-6-041106 (CODOrW 30 J.1000 ppo) 660 1780 122 1000 820 1500 68 OOUF01 -IASW 002-0-04121 8 fOwaMMapiK 10.003500) 10000 28200 32760 16 DOl1.F01-MSVV0004D M121 6 !C~ sp' L. ep oosl 5000 4040 10200 123 DOU-FIII-MSW 601-a04/Z1 6 1000ee410 SO C, 10030 Yrp 10000 7600 25000 174' DOU-F0I-NBW bo4-Q6041218 lCmas01 !ot D. am ios) 5000 5120 9660 96 DOU-P01-M9NM06-0041210 98854W 6o E. Iwo Mal 1000 466 1760 128 DUU-F01-14 SF005.681121 6 80000 O 30 F . ION CDb) 1000 720 1820 110 OOU-F0,-1ASF009 4-04121 6 (COMM so a m0o 06C-F01-4t5F006-1 -04121 6 Icaoee-tKpcK I oooo, W wM 1000 s46 10000 9so 1720 3 24OO 81 23D' DBGF01 -AA9F606.4W 121 e (000"W301. IMIM Wb) 10000 8980 24100 151 DOU-FOi-IASF0024 041216 (C0066 81so J . 1000 ppp) 1000 bq 1720 108 DOU-F0I-AISF002-1-04121 6 O04065471 fp K, 1000 ppp) 1000 892 0O0J -F01 419F004-0-04121 6 (ooocenz 90 4100o ppb) 1000 1820 1960 2700 126 S6 000- F01- M8F001-0-04121 6 (0~473 90 0. GM ope) 5000 2070 7960 118 OaC-F01 i13Fp0i0 -0r 1216 tc00e54r4 D, uwo ppq 10000 4640 I %w 109 DBCf01 -i1SF004-6p4121 6 XCOw?5ftk K mn OW 1 0000 9280 24500 152 OMC-F01 4 tSF001-o041216 (COOMM 81* F. WN oos) 1000 6/0 20W 120 08GF01 a PF001-o-0410Q1 9=4"" BO 3.10001Ve) 1000 364 1360 97 08 0-F01 a PF00,1 -0-0 41021 (0064I15130 fl 1800 PO) 1000 203 1340 106 DOU-F01 4PF0034.0 11021 (Obe+ 86 3pW 1. MW 06) 1000 36 9 1400 104 'Not r 40oM0 Ow t o WoRY oonYd r wi faiusa VKMw an not IntliW W b ft urwwry W~fies. Exygen Research Page 47 of 132 p . 48 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Table VI. Matrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples Sonpho Mal 6pW CA &W&VW PW ouq AnoA Md U Ornpl . F9uoy..6 ibawwy In so" .rr r r .. M M Fwro AnOUII Npo1wW RACaMY he P, Woo M d PAW" . rw. wmu vi . 10uoM-qlp~FwrM) 10 NO 0,90 00 ND ate Q 1.92 0.99 46 D13161-C/WE0140a1216 IOO~9D IM 4+~1oel 100 NO 026 62 IO 96 3 96 1.92 662 63 pNfyq ICPrv001oON21 6 tO mm, so E. Who OMC.IDt 40Fw00 WD4 IIt s poos~ntor.w~ 10 100 p 0.01 NO as 90 as NO i.M M ats 11A 61 MD 00.0 OY aie We 67 01.2101-C W001401121 4 IWU1asr14M~y 10 42461 2;1MM8 "Tri 6 O" Rtmlpj 100 ND 726 73 No 7.64 70 t61 7.62 67 No 836 94 ND 101 101 1,61 0 .4 ST OOGq1 - CJVr001-G-"1t16 po0M/eNrl16rM1 10 DSGqL4 ;TW001-0 M1216 Ipee~wy h ,,taeqq 100 NO PD 103 103 MD 646 64 NO 10 .6 100 072 97 444 4.45 130 IAs 6E4 52 0L1~01CrW0014N1R1 6 1CaONd"rwKaplr 10 NO a1 401 -CPNaD14 .61Tlr6 10044w~ 1o 1. laOwN 100 PO 6.06 YO NO a02 03 6.00 16.6 IR 85,2 86 ND 103 103 8.00 9 5 0 60 oo1F I .Crw001 4 061416 ICaarr6fY K* wq 1D IO 6.+6 DOIf p1171M0014A4t216 {mbtilpN.le0ipl tm No Ma 86 ss 0.202 0702 4,32 6f 11.4 960 90 1 1 .4 172 9e.0 6o 47 M~Yc M 4rwc 03 Mn w 73 > ION" pN/s 10 I bndwd Owtwlaa 1 8 Mrw VO O " MS /6 P.O - Nae diaY091 a ~bnM LAM d OirrliDn wNtll Y 02 Vp MMI w$lyMt Me1~ iw MIt w~nT 004AO .ia pMidM M.IY, werY ~~ wMMI' ~pl~/ Yaw M wMr M M rrr M K Bxygon Research Page 49 of 132 p . 49 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000 113 I FIGURE S F.xygcn Research Page 50 of 132 p . 50 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 FIgure 1 . Typical Calibration Curve for PFBS in Methano l ~ OO+a0s0 nr. .N (rr Mk ~:n.~r R.N .r . s ell 1W .wWoAII.aT V . 1 .s1. .m4 , . fm ..ooo (, . o.aoaq e.i . e s.a.a 0.o.e a.ea aoa aa.s ~ aa.e a-0 .e Y .6.0 ZA66 1a .0 t .o.6 0-0M 2 9 0 0 10 f2 M /0 1 8 20 22 2~ 20 ji ap ,17 aq 3 6 A b Q M 4C ~ ap CowMMNti n0~1 Exygen Research Page 51 of 132 p . 51 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P000113 1 Figure 2. Non-Extracted Standards of PFBS In Methanol, 0 .0005 g/rnL and 0.001 g/mL, Respectively , 1lTOe-I!rl~ ~IeMuY)2lR~7R1 av~wINfN nkw Ktieif~ as .: sea.. ..r, farua ar. cr. fer. asst .ra o .a aoo w 20 a ,QD teD , .b "0 = .r a,e4 s .~ s s a s s 7 0 10 riw4 . OY , prim P ee CSIM4iQ 1W bMA a4w ~6 2 W N Nin eH000{wi4 Aft u 7e0S! 48u 4& "96k Vol . MO R7:0-418 .0% 42 12 tiJtr ,4 .e0 Mae texr 41 n rJ +4 ,a +s n em 70D eee ON 400 - }m 4# a.,a, es~ aa ~om .+o.+z ~x +e ~ , : a s s s T s a +, n +a ,4 +s ,s n tw.. .r Exygen RcBearch Page 52 of 132 p . 52 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 Figure 3. PFBS in Control Fish Blank, 0 .00625 pWmL Fortified Control Fish Spk A, and 0.025 g/mL Fortified Control Fish Spk B, Respectivel y , /U~! 1~...,bIIMR. .. . ~.. .l~ .a7~,i.. N!rQER OftWaft"Ma ,. 0 .47.0.7 i.0 470 A70 60 7'm` 1. 2.i0 1020 .=. a ,4p M.OJ 634 17 .43 1 7 7 4 0 1 . O 10 , Tw rm . ~W . MN .N Ik A q{1pC) 300 .OipD r.u wwN 10 039 . m OOt000E .s ilf Aew:744f4 N . .Y XM.M! t1O. .ps RT: ~A2 nb 11 12 ti 14 10 ~ q 4AR ax 1A7 A y ~ 2 3 4 7 0 0 7D 14 ..nM , Ms.M. P f (PCY ) 7RO .ODD D Mu uyT f. 11 W N NM r 06/MEAN AM: 37p0 o.Mb RMQt, .Qaq. y IfT :0M7 in 12 13 14 M 10 17 1A M 0. . y. 1.O M 7y 0000.0 C 0.0 4w4 7 i 7 0 10 TWA. M e 1f ,2 q 14 p IS 17 Exygcn Rcsearch Page 53 of 132 p . 53 Intcrim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 Tigure 4. Chromatogram Representing a Fish Sample Analyzed fo r PFBS (Exygen ID : C0049478, Data Set :061605E) , CNA " ilf/f OlfNw) USMMO fr -rMl 7 0 N71A^N Mtio lfwrll Mfa Q9w * IrlOQ Moe Rk afOI w M ro M ao b m ti ~ p 35 ~ - ]0 26 m 18 10 1 4 9 4 0 7 i 0 10 11 12 49 M IS 10 q TIn6 Inia Exygen Research Page 54 of 132 p . 54 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : PM 113 1 Figure 5. Typical Calibration Curve for PFHS in Methanol W ON0066 i'oh .94b (iN O 'NnW 646xrM e . el1/d wWOMl %O Y - 2.M. .00sx # 7.W..002(r.OD091~ 1Dd 1.M0 7 .2.0 12tl 1 .1.0 1.0 .0 0.0 M ~ ODtl r 7Di tC OD.O OD46 4.046 aD.O 2o.e OA 2 4 0 0 10 12 14 10 14 n 22 24 20 X 30 22 N 70 20 40 it 44 N 4@ so C .ne.ft0NA qM~ Exygen Research Page 55 of 132 p . 55 Interim Repoct #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Figure 6. Non-Extracted Standards of PFHS In Methanol, 0 .0005 WmL and 0 .001 g/ml.., Respectively , sn77s .rAOprwfrpvNaveew-/INrMZa~afi ..ulwae,.~ &-w rsrrwwr #"ee rwl p. Mr ru .r. +o .72 ao o am am vav. +ao : a o e s o ++ TYw. Mn , e 021e PFFNC9ba irp M D+ReA sw+- mm N.9 441ebmee1e06i .iN Aw.:971w ewti N .1{Ut I=. IN RT: 10 J .In te,3 170D 500D TS, O w eeD 10 0 +a +o +e +e +T 700 vAV, +,.,o ia 0 2 a a s e ~ e v io 1 + u +s +4 1e +e +t TYnti nM Exygen Rcscarch Page 56 of 132 p . 56 Interim Report #l0-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Figure 7. PFHS In Control Fish Blank, 0 .00625 g/mL Fortified Control Fish Spk A, and 0 .025 g/mL Fortified Control Fish Spk B, Respectively , F.qMt u1M! MVi f.. .) ~ea~... - . .qrA s .. ]e Ih .. neltffis1A ones rt Ma.q /tat M m /am ~ 0 11 .47 AGAS 1 Ix 0 AG 4 :aae e~e. ~ an a.14 . 1 a a 4 e e a 0 t0 It t= a 14 TY...'Mn , MN~M OIY A KMS 0O0 >D0 .0M 0 a.w . sample 10 Mal fwn001o06E ..M Peas : 1e0711 N1M0 1 4hN 17900. pr 11T: tOJ MIS /3 .ee INa 4 .ts, tsao ts ts 17 1 .00 e4 ion 0000i00 iJ7 0.00 I a ! 4 6 7 i t0 TMM. M , Re N eMt0 0 - iMjOQ 300 0Ap 4 MI . asny1Mt1 Nal1nm 0 9 1Off .mM Mw 7=W1 ..r .r INIgl c 30100. am IIT: 10.4 min 11 t] a 14 M t0 n ap4 1035 s~o M 11or OA SAM 1 t i 4 0 --4 - - s a e o 10 1 1 /= 1 14 10 is 17 TIM, M1. Exygen Research Page 57 of 132 p . 57 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Figure 3 . Chromatogram Representing a Fish Sample Analyzed for PFHS (Exygen ID : C0049478, Data Set : 061605E) , prAp~ PAS (eAd ....)LRNU . .. -...~rN yr~ rw . Idnse.Ar ArMr 2lM -...s IAh~ l10A $M ll7 . N ,,m ,ooo 000 "o 70O ~ aoo ,oo wo aoo ,oo 2 3 4 b 0 7 11 i q 11 12 13 14 16 /M 17 Thw. mM Exygen Research Page 58 of 132 p . 58 Interim Report #10-Analysis of Fish and .Clam Samples Exygen Study No. : P00p113 1 Figure 9. Typical Calibration Curve for PFOS In Methanol ~ m~msf w.~a(noT'~n . .~~.rw. .~~r,r ..qwu.~~-t .~s.+aax .9.9 .+003(~-oLae) 6~d Gies 60.6 4a@6 1,0.6 MAOS r ~ ~Dd z.e.s sc .s I ~ e 70 1 2 14 1e 10 31 22 20 m 39 310 32 94 90 A 40 Q 44 40 41 00 c.. .~e .w.. ..kpL ~ Exygen Research Page 59 of 132 p . 59 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Figure 10. Non-Extracted Standards of PFOS In Methanol, 0 .0005 glmL and 0.001 pg/mL, Respectively , ,l~df .~i sE....M w.a~a. . .. -. ...b ! d]~ .u. .N.lOE.Il. ti .. aa....a M+wNe aa ~r. xr. rss .t. ,o o 'e ~ aQ +oo ,2 .b n +2a~aaT a o rims . .,I. , fiT- rroN (NlaMard),1ppA4 OA uw-rwyl .t .laf hw.061 8 06isi0 MR + 4167 . .1MN Height ppp y . RT: 128 wl. +o w +e +e n 70 4 }g OOe .Y . 000 4w 700 2M ' 700 O IG + a ~ a a r ~ a +o r.ne Nu 72 .45 tt .A2 ARA + +~ n ea w +o +e +~ Exygen Rcs=h Page 60 of 132 p . 60 Intcrim Rcport #10-Analysis of Fish and Clam Samples Exygtn Study No . : P000113 1 Figure 11 . PFOS In Control Fish Blank, 0.00625 glmL Fortified Control Fish Spk A, and 0.025 g/mL Fortified Control Fish Spk B, Respectively ' Aw~t C~Ifwl P~Oi RAwfaM!)I 9"ftd /N IwyA /d A Mo /(7NWmAI AN: A~ iw~b Mi/Ot l41sM RI R! 1/i 12D0 4D- 20- vas ts+ too a.4+ 4.49 ta.+o "M e.~ A ~ 7ao .a o~ op ttm te .oo nyo. nat 7 2 i 4 6 7 0 10 tt 1 2 is 1 4 10 10 17 Tlr . iY % , RrM atirYA PfOt (10C) A O.OM D 8wrfwiyI4,0AlOIwo001006fW0 Awc 71000 ~. * 1Not MM. on OT : 174 w~ 4000 12.i t2A4. 0 1 2 a 4 5 O 7 0 10 17 12 t i 14 76 10 47 Tlwb w M , Ilw .etiMi fo!(OL)i00+000 aw e .~yM11NM M8 w001lDOLwO N.: 787M1 oe w Yt MNMt 10000. w XT : I2A min t. . 4 Z tDM eooo.o oa 12.40 t x a + e e 7 o to tt u ,a ts n a n TNw, nIM Exygen Rcsearch Pagc 61 of 132 p . 61 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Figure 12. Chromatogram Representing a Fish Sample Analyzed for PFOS (Exygen ID : C0049478, Data Set:061605E ) ~ COMM .,, M ~..~.~....... ...~. >.u,". "MM.M ~ .7lt ,2 .6 , ., .0 ,Ad ..0.4 .C a. ~ .o.. ~ OAM ODM A.~ l.OM 24M 140 OA CAP t= 1 Y i 4 6 0 7 ~ 0 t0 IT n IJ ,. b /0 a TYw . ~~. Exygen Research Page 62 of 132 p . 62 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 APPENDIX A Study Protocol P0001131 (Exygen Study No . P0001131) with Analytical Method, Protocol Amendments 1 and 2 and Deviations 2 and 3 Exygen Re-search Page 63 of 132 p . 63 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001 l3 1 8uypa haoeol Nwaba: P0001131 STUDY PROTOCOL Study Title : Analysis of Per floorobutane salfoaate (PFBS), Perflaoro hezanaul[enate (PFHS ), and PerQaorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fiah, Clams, Vegetatloa, Small Mammal Liver and Smal l Mammal Serum Usin g LC/MS/MS for the 3M Decatur Monitoring Program Exygen Protocol Number-. P0001 13t B~cYB .n Ra.e.ea~ Miah.e l A. s.uu.e 3058 Research Drive Dirocoar of Regulatory Affam Swa ColiaBe, PA 16801 3M Building 0236-01-8-10 Phone : (814) 2724039 St PAul, MN SS14 4 Phone: (01) 733-6374 Par I'd 6 s Exygen Research Page 64 of 132 p . 64 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Stady No. : P000113 1 e.xysen i,aocd NW%*cr. rooo i i3 i DiSTRIHO'17ON : 1) Miimlu ICari. Smdy D'aa,tar, waloa Solutim 2) John M . PWbaty. Prinoipv fnve@ iSMM. MIySn ROSS-h 3) Mid4el A. Saotao. Sponsor Rap"aaitl&*. 3M. CvmpMY 4) Exnm Rnereh QwlityAum=caUmt P~1af63 Exygcn Rcscsrch Pagv 65 of 132 p . 65 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Bxyps Pwtocd <Jmber. P000 1 131 ?01' PROTOCOL APPROVAL StWy T1tk : Aaalyiia of PwfluooobudmwdftMe (PFBSJ, Partluoao4aunaul6onwe (P nIS). AM Patkw oocaonwUonaoe (PF06) in WSW., Soil, Sedimeitt, Eid , Clamra, VeceWon, Small Mvnmt+! Livan md Sau11 Mammral Sacum Using LCJMSlMS 1br the 3M Deeaw Moaftoeift Pmtnm Exyypn P rctoool Numbar: P0001 1 31 APPROV Jaiimht we 9ooe sotatim Michael A. oru, Sponsor RaPwwilalire 3M C rI5o ftM ~eanch _ s~-G~'1-kvr' Richatd A. (3 mi. dew. Facility Mra`anaR Dda Exy=ea lkamko~ 4L- --aAg/k aRer, Teehai d. Qaality Aseorma Unit Ua maveh PsV J o/ 6S Exygon Research Page 66 of 132 p . 66 Interim Report #10-Analysis of Fish and Clam Samples . Exygen Study No. : P000113 1 Buyp a hdaol Nrabet: P0001171 TABLE OF CONTENTS TITLE PAGE .-___. _ __ - ____ ._ ..__ _ _ _-- __ .._. ._ .._ .._. . . 1 p141R~(T110N.. .. ... ..... .__.. ._._.-_.. ..__ .._ .~~.. .... ._ .,_.._ .. ..__~_ .... .. ........ ._ .. ._ .. ._.-. . .. .. ..__.T IROR0Gi0LAP4iDVAL_ ._ __ .. _-__._.... .. ... .. .. . ... .. _-----__ ._... .. .._ ... ._ .. :... . .. . .. .. .. .. .__ .l TA8L8oPCOIrI'8N18 ._.. . . ... ._._----__ . _ ..~_ _.__. .. ._ .. .. . .. ._ ._ ~ .. .. . .. .. .. .. . .. . .. ..... TEST MATERIALS M __ ..~_... . ._ .. ~. .. _ _~ ., . ._ ._..._.. ---------- - -------- - . ....... ..--_ .5 o8JC71VE_ . ._-__ .______. .__.__ _ _ . . .._ .- . ..---_- .. .._ .- ._. ..__... .. . .. .. ....__~ .._. ._---. .. . . .._ ._ . .__ .6 IERT1Pt0FACQdTY.__ . . . . . _ . __~. .._---- . . .. .._ .__. .._. .. ..___. . ..__ .___. ..._. ..__. ._--- .b slONSORRElRE88NfAT1VE ._ ._. .-. .._- ---------- 7 P110pQdED 6? pEa11BNPAL START AND TBRLIWATION DATBS _ .__-_---._. .. ,,_.._____...7 IDENTIFICATION AND NSTIlICATIDN OP T8L T839" JYSii'M . .. ..______ . _. .., .. . .. .. ._.. .. ._ .. .._ .. . .. ..a SAW" PRt1Cl RE A1aIT. RBCH VT AND RETENTION . .. ..9 SMQl.E ANALYTICALPROCBDUaE3UA MARY ._____ .__ . . . ~ .. .,.,._ _ . _ _ .__ . . .9 VERI} ICATIONOPANALY[g'.ALPROt1RE .-_ _- .._ ..... ___ .__ __ .______ ._.... . .. .9 IETBODiOROONCR+OLOPBIAS- 8 PA'R8TICAL .... . . _ . ... . .. . 11 Q .lsTATLM8RI'_.... .. ... .. ___ SAFE'CY AND HEALTH _. .,__ _ . . . _~._ . ~ ,- . .. .. ..__..........__. .. ----- - ------- . . . ..__. . .. . ._1f . .. .. .. . .-_. .,,_ .. . ...... .. .. . . ._.. . ... .. .. .. _ ..-_ .. .II ..._ __. ..~- ~_ _~ . .. .. .._ .,, _ . ....., ., . ..,_. . ._. . . .. --. .. 12 AMP.NDM8NISTO PROTOCOL .. .. .. . .. .. .. . ... .._ ._-..---__. ..15 DATA RECORD XtEPMO _____ _ _ . . . . .. . ..~ ..... __ .__ .___ . .., . 13 QOAISCY ASSURANCE . .. ._. ~ .__. . .. .._ .. .. . ._-__ .. ._. .._ ., . ._ .. __ ..____.-_ ... .._ ._ .. .. .. . .... .. . 14 RL'W IiON Of DATA AND AWUVINO . . .. ._ ... ~_.. ..__. _.__ ..---- . .. .. .. . .. .. . .. .. .._ _ ..__..__. .. ..le APlIWDi?IL ANALYTICAL ME~IODS . ... , ., .- . . . .... .. .__ ., . . .... .. ._ .. ..,. ____ ..__. . ._ . .IS r+' Pep1of63 Exygcn Rescarch Page 67 of 132 p . 67 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001 13 1 Bayp" Piolocol Nip6 r. P0001111 ~ ~MUCTlQN Tbc purpose of We study is to p a0orm caelyaie fm pa:$uorobutwesulfot Aue (PPBS), PaJltlorodexwaWfomtc (PFfIS) a d yerQuoroodanaulfonwe (PPM ia water, toil, seditamt. !lelb dr[u, ve gaudon, small mammal livea aid awll mammal aRmn us" I.GMSIMS ior the 3M Decam Monitoring 1 roormw 71u audy will be atuhted kr camplitten with EPA TSCA Good Lt.Doruaty Pcaetice Staad st4 40 CPR 792 by 8ro Quality Assurance Unit of Exygen Rae:sh TBST MATERIALS The tea m>turialt< we parAaorobeamawltoaue (PFBS). Oboe" (PM) am (PFOS) &W we all aWlied by 31#4 PM Cbamicai tJ+ma P Molecular WeiSilt : 338 auppUed a the potassium salt (C4f401'K) Lol Number. 101 Pa~ity : 96.'"d. Tnaatiaos Maoitoaed: 299 -a 99 Elructu~e: F F 4 F _ f~ ~~SO3 P1RH S Q+otnlal Na m Molecular 11VeijtC 134 wpp6ed as ILe pWauium all (Wi)9O~7C) Lot Numbar: SBA96 Paity: 98 .6lL Tmudaoi Moaitocod: 399 - 80 Stntcaue: FFF F f F i ~ S0 .;- P".s afQs Exygcn Rcscarch Pagr 68 of 132 p . 68 interim Report #10-Armtysis of Fish and Clam Samples Exygen Study No . : P0001131 Exypo Pfaoow) \4r*. . : rooo 113 1 r. . PF+06 Choi" NaW PerAomoocbcrwl6oame INolsaaLr Wdjht: 338 supplied as the pawilun u[t (CsF,4O3R) Lot Nmnbet 717 Auiqr. 86.91L ?Iauiliont MaubmW: 449 -t 99 $fuAVZC: F F F F F F SOl' F OBJECTIVE The puqroto of this Mudy is to yufam mlywo for c (PFBS). (PFAS) and pafluaeoocdnesulftauc (PFOS) in wqa, wil, modbwnt. WN4 than. raRtrtioq imaU mammal liven md sm&11 muonW taefn for the 3M Deca4u Monitoring PmVam using the aurmt rariom of ft 1bGovm& Ezypn snFytical methods ; V000178D; ' Method of Aodytin for the DMeminolioo of PerAuomoetacwic Acid (R70A) in Wao by LCIMSIMS " V0001761 : "Melbod of AnVys6 for the Ddomiimdon of Pa4uomoeurroic Acid (PFOA) In Soli by LL'JMIS/b1S" V0001782: "Method of Aadyais for the Daleeminatian of PixAuorooewwic Acid (PFOA) iu Sefimeat by I.CJM .SlblS" V0001783: "Method of Amlymis for the Dalernoiation of PecAuacooctemic Acid (tFOA) in Pub end Clma by LC/AO/M8 " V0001784: "Method of Anmlyaa for the Delemiratioa of PoAuocooctmmic Mid (PPOA) in Vept .tion by I.GMS/MS" V0001783; "Method of Analysis for the Delermio don of Perfluoroowwic Acid (PPOA) in Smell Mammal Liver by LGMS/M5" V0001786: "Method of Mdysk for the Dowmiemtioa of Peefluoroocarwi c Acid (PPOA) in Small Mammrl8etum by GClM.SlMS" TESMG li'ACOJTY Pxy Sao AaOcairh aase Ra .e.erb .Arive i-+ Swe Co~ PA 1680 1 Phon: (814) 272-1099 Pop 6 4f 65 Exnm Research Page 69 of 132 p . 69 Interim RepGrt #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 ~ STUDY DrUC'1'OR lawnshs Kwui P.R . DEE Wawa So1000 , iec. 1400 Weslon Way Wed Qmwr, PA 19380 Phone : (610) 70t-3761 Few (610) 701-7401 j .kaw4we gm olntioet .wm &cyaa Psaa+ooi Number : NMI 13 r SPONSOR REPRESENTATIVE R[ishad A. 3-ukwv 3M Compmay Director ofA@Vfaloey Aftirs 3M tiuildiog 0236a1-8-10 St. Pnd, MN 35144 Pbono: (6$1) 733-6374 PRINCIPAL INVESTIGATOR Joha M. Phbaty lsxyRtn Reftoa b 3058 Rawerch Drive StI60 Colbge, PA 16801 Phonw (E14)172-1t1'39 j~~7~kxYYea.oon PROPOSED E7PERIN1BNTAL START AM TERMINATION DATES It 1 s pecpoasd that the imalydod pomas of this saidy be condneted hom October 0 1 , 2004 to Doe=her It . 2005. The actual expetimmtal etan and Nenidnatioa aaw will be included i 1ma Goal Tepact ~-- Pq~ 7of6J Exyg+en Research Page 70 of 132 p . 70 Interim Report #10-Analysis of Fish and Cllun Samples Exygcn Study . No. : P0001131 Rary ro ?AOtocol Neoiar. h00111 1 IDENTQtICAnON AND JUSTIFICATION OF THE TEST SYSTEM The Wowing we the last syet.ms toe ibis shay : wftar (pomtdweW end surface w.tar) .son sadfinW t Fid . Cl.m. . vagdld= is 310 .0 Mammal Lim . surd Mammal sam m The aropla wUl be oollectad by Warooo Solutioa .. The omaeo! wepes wiU be porchssed and prsysled by tko testing itwkcy. erseh.ro snd processing dedils Ar the woaol ssmp ke will be included in the final report .t.ociued with d" study. The taq syst ems we cJSoean to socaa die eavhoolneaW impact of PFBS, PFHS d PFOS In the Droaatua . Alsbsms was. SAMPLE PROCURItiMI'NT, RZCXEff AND RETENTIO N wd,er. wU, wdsla.w, Sse, clm. vem amAa ., mw msmma! hver sod ,mail mammal savul samples will be tooaived at Paryfa, daetly from Weston suhtiao. . The derdl . of .mnte prooosme for mis study at outlined in the 3M werk on mtiBN "lhsss 2 Wait TNn for Sampling Endroemaeta! bteda" '!bs wader sod types of ampbs collected wilt very dqmndmg availability In the Sold. The total moubar of s mpta received aod analyzed !br each noauac will be doaaaenced in the Anal repovt unciatod with this nud y wala. soil, and .edunmt samples wilt be used as received without llutha processing at Exyp t. These samples will be ttcrad tefHpnrod at 2C. -M. Fish, dsu4 "getstioa sod wly]I mssnalsl liyw rnnpla will be processed according to the appmpri.ee adlytial method (ses Appendix (). Then rmpLs will bo seared hmm at 6la'C. Small msmsrl whole blood samples will be eaauitil{ad in the Acid at the time of wllectiao and the serum fraction will be used In the nudy. Small nosmmd so= will be stored 4a= st S -10'C. The receipt and processing of 1M samples will be doarnrnssd in the final ... report and mw dm associated with the rKudy. -~+ PIK. aOras Exygen Rescarch Page 71 of 132 p . 71 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 sx".e rm Md tr~ roooi u i SAMPLE mENTi F3CATIOH Prior to analysis, each nonpb will be aeigeod e lehorstory s .mplc rafuencc nanba. The reBereooe number will be mdqae eod win dislinguiih each l,bantory omple tlrt is prvoeaed throu Oaut the an alylial proeaduce . CtroonatoYripbie 4ets will be idantiGad by the Laboratory sample tefeca" muobee. Sun* storage omditiorn wed locadaae will be documented t}mughout the swdy. AANALYTICAL PROCEDUM SUMMARY Rnfe:.aea: 'Jq001780 : "AdedbM of Analysis for the Del+m daadaa of Patduorooccuwic Acid {PFOAy in Wow by I,GItiS/b!3" V000 :781 : Method of Analysis for the Detarmrimtion of Patluoeooclanoic Acid (PPOA) In SoU by I.('JNS/b!S" V0001752 : "dtotbod of Analysis for tba Datermiae<ion of Paifyuozvoctanoic 00.,, Acid (PBAA) in Sediment by IJClMSlM .S" V0001783 : 'Modlod of Analysis for the Datwniostioa of PerAuorooctanoic Acid (PFOA) tn Fieh rd Clame `y LCIMSIM3" VtYM017114: "hSellod ofAnalysis for the Detamiaatioo of Perfluozooesanoic Acid (PFOA) in Veptodoo by I.CJbISJW VOOO1783 : "Afelbod of Analysis for The Determination of Perilticrooctanoic Acid tTFOA) in SmwSI Ltam cel Liver by LCIMS1MS 1000 3 736 : "btdAod of Aodyeie for the Ddamioetion of Paftuorooctanwic Acid (PPOA) in small Minimal Sam by LC/MS/MS" The obuve mactwde as analytical aoo&doas capable of separating ft isomaes of PFBS, FfH8 and PFOS . The boal report will include the women armned into total PFSS, total PFF[S, and total PFOS fouad. VBiMCATION OF ANALYTICAL PROCEDURE A laboratory oonhol simple Will be need for the prepentioo of fortified omp+ol etooplas. The tat tnbetanoe will be made aw solutions as per the ar:thod . aod added to Ow tartrlcee via a niimupipetta ~ For water aempliet=, Exygae will ewly one bottle per ample collected. The bottle@ will be 500 mL preckrmd SeUSbee Premier wide mouth IiDPS bottlds. These boeWa have bow routinely wed br fluonwimunical sample Post 4 af aS Exygen Research Page 72 of 132 p . 72 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 Farypn 1rotuool Nwnba: P0001 13t collection at llw tertlal facility aed have beta dmmn 10 be D" of ?F%, PFHS and PPOS. Samples will be added to aeb oocMainer to a volamstric fill !'wa at 100 aL A Said daptiate . a low field VO a and a hiSb Sold *&c of sect ample will be collected. The low and high field *p** boulm will contain PFBS, PFRS and PFQS ae well as pRfluorooctmoic acid (PFOA) wd 1 .2-13C pa9 wooctanoic aefd (uC PFOA). PFOA and "C PFOA we ioctaded in the aoMiane used to spike the samples. The results for PFOA and uC PFOA will not be npoeted in Ibis Kudy. Exygen wi ll supply on field btrpk (control Water) and two Add bLak spikes (aoaaot water fortified with PFBS, PFH3 and PF03 at a tow and high level) fcr every twenty Vies oolteotad. Al the UMinj fieitity, each wow sample (excludws field duplicates and dold qfta) will be extracled in duplicate and wilt also bt fati8ed at a low and WO ooocaetratian with PF'BS. "HS and PFOS and prooewod through the described ptocedure to detamine method accuracy and to cbeck for bins. ~.. For soil, sediment. olamu, and vaselatioa. BzySea will wpyiy onc 500 mL pept:kaoed SeUSpee Pannier wide mouth HDPE botle per ample collected or a zip-ntl bag. Al] ooon nwnlbey used for sample collection win be shipped to the sample boadoa. Smpiea will be added to each ooaaiaer or bag in. the 6etd. At the lasting 9cUity, each ample will be e=acmd in duplicate wW will also be fiortibad at a known coacentratioo with PFBS, PTHS and PFQS at both a low and lo* krd md processed through the dambed procedure to determine raelhod accuracy and to eLack for bias. For =all mumW liver. Exy`m will supply a 50 mL polypropylene ceeaitln'e aibe: For =a11 mamaa; oaum, ExYOen will supply a collection kit for auk ample coolaaurtq mum aepastor takes (red lop), vacutwiers. needle holders sad needles, umsfer IdPa~. and PafPwpylena tubm. At the teaaft bciBtl, each liver and serum ample win be mctiaried in duplicate and will also be Wiled at a known concentration with PPB3, PFHS and PF05 at both it low and hiab level and processed tiaon;k the dcacnibed procedure to determine awOW accuracy and to check for bum Low and ' qy*ma 'nz lav~di for each matrix am defined below: twia Law Leqel K Leve1 Water 500 USIL 5000 L Soil 4 awl 40 W/j sea :n.~c a MWA 40 n 10 Awg 100 cum 10 IWE 1lootlys y"Ptation 10 AWS 100 rwa small Mammal Lirec 103WX too Ught Small Mammri sawn 10 mt. 100 n L Fr`.loof u Exygen Research Page 73 of 132 p . 73 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 8a"ao Pmteeol Nuna: t000113 1 A +% Raavacia are u/icipted to be b et rest 70 % and 130% of dw fortified kvelr bovaver. the exact p>ecam and aoaeuy wiU be detavniood by the analyaia of the quality eomrol umpla tlaalbed above. Aatemait of wnracy will be twAaded in do &W report MrrBOL FOR CON'i1lOL OF HIA S Cooa'oJ of biar will be adAraaed by taking roprpaeadve sub-wepl a from a boom,oaam mixtimv of each mhfx km un4natod control wapke, and by analyzing at least two levels of LmdBatiom. STATI8IICAL 11STSO1)S Statistics will be limited to lbws apeeitled in the wbjed method s and to the oalaalaBoo of avera;e teeovrriaa, as appli mle. Gil STATEMENT 001. All a p*cb of this study iMil be per6ocmod and reported in compliance with fiPA TSCA Good LSo7mory Prsr.tioe Standads 40 CFR M. The find report or data package (wppliod to the Sponsor) d" contain a statement that the study > W owatmeted in compliance with cvn eau and applicabla GLP s cmdank and will outline any 3eviatioce in to study Dow dioaa standaMa . Th:a aMa,anatt w il l be aped by The Study Director and Sponsor kq eavaatativa. MErORT A Sal report will be ptopwed by the prhmc pai lavouiptor or t4dr daipa at the cooclmioo of the study. The report will incUtde, but will not be limited to. the follorrinv The naaAe and addra+u of d a Study Dimaoc, Sponsor Pipesmsfive, and of the trliaa Ao mty. A scatemeot of Cid? oompitaooe lauy reiatod docuanrntation. auch as d aia-a-onrody ieoada, mug be in the study rocor&). Pey~. it q/1 Exygen Research Page 74 of 132 p . 74 Interim Report #10-Analysis of Fish and Clam Samples Exygtn Study No . : P0001131 Ex" r Ptotoool NnnEea: P0001 13 I . The signed ad dated mksnait .by tbe Exyiea Raeareh Qudity Aaaraaoa Unit rcpPdins dates of mdy iapociioa and data brediegs wave mporlad to tbe Smdy DirecW and Mapaperoent. A description of dye exact aaalydcal condition, employed in to smdy. It the subject method waa lbUowed auctly. it it aecatuy to ioolud oely a copy of ON walytied nlofhod. Any modiBWiau to this method will be inoaponted MW the sepolt. If OW 10a4 bod is photo-redueed, the ptojeel number and PV om abar must be included on ach page. Dw uiption of the imawneabtian used and operating cooditiorr. AD raniq from all sib aadyzed. Coorto! and fortified samples will be idomiSod and the data tablo will inckde ample number ad fortificuion WWI. Repraomative chcOmttoRnqa for each aoa yte in cacti matrix, Including dm=WVNM of it a ndard ad a control ample. and a ohromatogram at a fottiBctioa level The location of the analyte peaks will be clerly idanti8ed in all ~. AU cRU>metwet that may have aPlaoted the quality of intao ty of the data will be doeumaitod in the repoil. Locations wham aw data and the fmal npott use to be urhived . Additioaa or oanotioor to 4w 5aal "part Shall be in tlu btm of an am-dm" a load by the Study Dlroctor. The ampfd M qt " clearly identify that pat of the report that I. being altered and to tarona for the altuatiaos . The wwaft ent will be tir ed and dated by the Study Director sod the Sponsor R Weeotaava All applieabb nqnaameots for capoitio S of tWy rasulu as par 40 CFR 792 .1D.S . SAFZlY AND HEALTH 1.bantory personnel will practice pod snitauon sod hoMh ha6ita. Evay rwaousbl pneaodun shall be tai[w to prevent {naAvsAem axpaun of pnoemsl and the eovummmt to at mess or reference ubNmae(al Part (1 of 6J Exygea Research Page 75 of 132 p . 75 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No . : PM 113 1 A~ r. exYp n ttotoool Nuoubtr : roaut 1 31 AMENDMENTS TO PROTOCOL All ar iIIaat changes to the aHytical ptpocol outlined here will be azpimtied in wrift signed and dated by the Study Director and Sponsor RepraawttaHve. Amx>d>ettta usually will be isued prim to initiation of s tudy plan ehaSe. HowNevef, who a change is required withoat suM ciau time for the iau of is written ampodmatt, that change may be effected verbaay with wpportiob doamrteotatioa signed ard dated by the Study Director and followed with a written anadmwt ar man as poapble. In this aae, the effective dat+e of the written amendment will be the dte of the documented oha 8e. Copies of the 61113ed ammdmeots Will be appended to aA distributed study pha copies . The odPmt amendment wi ll be maintained with the oriain d tAdy ybrc Any &% iaticra bam 6 study plan or from the analytical method aR provided will be doeurnmoed and mnocted puqoptly to the Spon sor R . DATA RECORD KEEPING Records to be mai> u iaed ioclude the following (as qvroprisfty &avVu eradoni dool(y Sample ruaipt rmxda. Amp hiatacy, and chains ofcustody Hiamry, ad preparation of itutdard, (s;ock, lorti8ation, calibration) Description of auy modifieatioua to tbe method 5taotta+ax eon abeeia, baxbahed.s or logs Aolytioal dis tables Ap dwortuacgrephic and iustrunbsoW condition Sample ettaiaatfoa and aotalyiis dam A complete lift o[+ttady p ansomsel. tA paqsa and iaitiab Any ot6a~doa~mqmpoa neocefssa~ry fom r th~e re~co~nst~ ruction of tlro study Cb,rt+matoVxat- All aluoooaoo~,uos will cant= the fouowing: Sample Idenfl ftttlott.lyoUiou date, arrow or other indication of the area of adeont, and injection ptmbee eotievpndkil to the run. Additioaapy. SoRiQoaeooa will iocitda the amount of analyta added and the sample amber ofthe simple that was 6ortiQod. Analytical ahndard chramatogrtaro, w ill additionally include The concentration (e.g . B(rN-) pate 1i of 6j EXYM Resemh Page 76 of 132 p . 76 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 uy~+r~ .aoot rw .rx.~ roooi ts i ~-- . At pat of ft doaraiartauio4 the following ahem will be included in each xcalyaical ow a tan sheet listing to amp1M to be tun in the ^ mad an kwom au oooaiom skeet describing the instrument type and oparatiny calwition. QUALITY ASSURANCE no QA Unit of Bxy g m Research will Inspect the iady at intervals ridoquato to aaut+e compliance with GLPa. md will report the 3tdho~a of audits to the Study nuueeor. Ety@m M.n.Remea; wad the Sponsor aepraeaaMive . RETENTION OF DATA AND ARCHIVING . . . All hard copy taw data, indudiuQ, but not b=led lo, the ariginal dwomsormis, ao*a6eeti6 ooaeapondaao % and results " be included with t6e dati pacia~ts waMaittod oo Aa $Ndy Dirocooc. These will bo uchivod with the odsteal $tu8y plm, anoaodn>asti, lfaal repor.t and all pertinent iato:mdioa Som ~e Sponwr. The tarring facility "l keep all elecboeie raw dm eed any ieccumeaa , aqe34nnwat, sod stoup logs for the paled of time specified in 40 CFR 792.193 . An eo w copy of the mat@Nh anbmitoed to the study director will also be kept it 1lx7pA Aaaudt. E;y=m will obtain patmsion from the Mrdy director beforo discarding or ~ Pqt/YoJ AS Exygen Research Page 77 of 132 p . 77 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 BspW PrWOOOI Na whar: POO6l 1] 1 APPENDIX I ANALYTICAL METHODS V0001710: 'Method of Analysis for the DqermiAa tioa of PerNuorooctuwic Add (PFQA) in Water by LGMS&tS" V0001781 : '1lethad of Arulysi . for the Determination of Pertluoroodnwic Acid (PFOA) in Soil by I .CIMSlM" V000176Y : "Method of Analysis for the Detaernination of Perfluocooctanoic Acid (PFOA) in Sedimeal by LGMS/MS " V00017a3: "Method o(Aral)Ws ft the Daaminufan of Perflumoouanoic Acid (PFOA) in Fish and Clams by LG44SlMS" VU0o1784: "bidhod of Analysis for the Determination of Pmfhorooctanoic Acid MOA) in Vayetation by LC/MSlMS" V0001785: "Method of A ndym fs hr the Ddamkwti on of Pa4hwrooG woic Acid (PFOA) in Small Mammal Liver by LGMSlMS" V0001786: 'Meabod of Analysis for the Ddamicaion of Portlaocooctanoic Acid (PFOA) in Small Mammal Sam by LC/MSIMS, , Pnp is aJ6J Exy8en Rewarch Page 78 of 132 p . 78 Interim Report #10-Analysis of Fish and Clam Samples Exygtn Study No . : P000113 1 ExY/w Pwacd [V=dm: R0061 131 Ap~ ANALY7IG1l. NEnB00 MW/N. . bw. vWnp i[W1 rtAMMON M Me Yowr 0YWa'a R~rL~~y 4d1 {RIOA) Y Wow AnyYal7~NaRRwallpc kMM R~yw.A wOf RwY Dri.. ~r1r CL~y~ PA I mt IMroad WA ^'w_a .), cr ~~,r . i p y ~o H .. r Tow" tad., ua,s, b,7..~..~.~. TwJR~w 7 - Poe 1s yfas Exygen Rxsearch Page 79 of 132 p . 79 Interim Report. #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 Exf{w Pfolwal t+ w bw: P0001 01 ~ oar ~.rr+ rM. i w i. v1041 r ANALt71C61 . Maiilps "'"' ~ i rely itnwts lA l.y . 11Y rr bob Y. ovbr 1 ir a. irYdr ri qariris ef ~m~r~t b Hkh I F~,rw WdA (Wu r . vMw mqPld r . w d.a M. !/MOrM~1o --M) W, nr 2A So" Ll Alwqsi~wtlYw.l~l prde a U irrrslriWMrpeowriry )A tr"l . RNYnnot 7.1 AtLfprL .flw MVlll r 17 l101YyM/~01.i~{I{~rUl~rrrt ..y11.. 3 .3 >rl . + N 00 6iprd +..Y 4 Wowed e .t4l4w w~w 7 .t AOrplwrrtMrwyr~YLL~.~weMq .ep.a(o.~.p~ 3a Amy INW IW -MW y lr+lr ae.Y r esnk W w-xoo rye for -s rYrw rd M wfa.ld w/ At as Mowies. 3.6 UWb atiai= /w .irr wM b q .Nl L IN aoplig pin IN A;. P1 A 4 0 A. owm rl md" 41 wow - Mu o.r a: MWh. .l-rLC P.r U Asrerow AMr.-ACJ, ~aqw O.Os aA Frrwe.l brAsi- WA rAYlert fA h~ wl spi^r 11 A io P .A ~ lyil itA. o .owL eyil . K Prep" Y 40 2 W.r. .~ .~.1 wis . wqM. ~el~ .t s .qr ewY" of iq" fJ00 /L~wld r ~ W~ Wr i'UMr .Yr (Y,fJM~71 , 32 AM+ iw OwOK ~d lYif p. .hYr opMf.nrNimWkri. , L3 qirtYO~rqohY Mmw y ft 6000N & 1 4 Md./lYibYll~7W DWAMr EL i sSA ~M~r~~i~f7alOC~L10910~L~. 1 7 qlaLLC/iaww~bMDia f.t 1rLdr1OLC v .Itk !.f p*.rM~a 3. 30 Awy .~.claowadwlo-rMrta .r~~:~e.rwly. IM wWn1)7* wfRp{11Gt~!laWy rqrlr ~-Pn<olas Exygoa Research Page 80 of 132 p . 80 Interim Report #10-Analysis of Fish and Clam Samples Earygea .Study No . : P000113 1 PAqnm Ptolocd Nwber. POOOI 1] 1 OY~~~rrM MiY~ I4~w V101~7N mwPow w LC#Af00 )w wow !.12 O! srIUL S.i3 C.AWYW a POYb dpmYf 00 aL yd}poqlwa wr t 30G0 qa w pwr~+8 Ik p.w al A.r3daire>twqMwRrOCqw.4l .i .w.AS 1 .w . So x ..sy (Ink u> a4auo! f t T~rc ]0"C 47 MLr1VrW : aru/Ir.r:me.wr.taW.rr M lId1Ylfw A) : >tYrAri M 0. .7 Gnli~ttwpc 7M~ R~M MOL(MI) IA 2A {bLlmO 0.0 N 3f L3 ed ff 7f 07 LO ta 7s 0.7 3110 23 73 0.3 2iA 63 33 0.3 L1 i~eWaY~Yre aSr3 .parYOwwilsrrrcAr70Nl .), 4.7 Qi-- 1 OYC Am -ftid dmdad a lb r = onm [I dTire - 73 r1Mra no iw" as"= M YrMO 0a iM a/ may be rrwm a oft b dp iLir r 1Ql.C ffM~ a 7.0 1RLA *pde 7.1 Wdt 3an011 1 M1/Wfl/vlaolr,awyrdy 41 3 , 3N OZ. 710 rtw -ft- - bwtlW r a rW WA OW be CMrLd m nod r 4iYe M maeqrri. Ryr~iat amYUr Ll 1Mii1Wr L 1.1 : siI ~rrl~r rMp I~ wrL ~ iaird tiy Wk.O 0. i3~ y er rraiir MOM r 1000 wL drMw. AIIrtm vM~ ay be qrL Pw if qJdJ Exygen Research Page 81 of 132 p . 81 interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 BxyMw Aromcol Nwubsr : P000113 ! r~.>trr+ wwr..IM.vaar Kw.fnct~L tltnro ~ A~d h~ M~iw~ Awd QIOA) i r y LC 14CAq R6 R'r~Ahw~~ t .t a~Mi~ ArilMM~is bY~1 w f.t .t iwwaawtWriwd-100~uLaflfOAyralpaa~tawa ataertytlu[ mnld ~w~aW Nr ~~/ d~Ya r Ip/ wL .iM reA! a 13id. L0771Wa 9.1.2 At tt~~. MiYiaa rMI1fOn d?!Oh is pwgalal by kYriae IV MIL Nia 100 MAef. ~eldw la a frt wlw of 100 via wr.r ratbeLl~MMM ! 1 .3 A 1 .#M /AL ~diqyN M1riY1 af rJOA i ppand y lnip 4 In *1. dY 1a v#ML rYdwo Y . f W~aho[ a( t0a r+6 -a r d ir a171 E1. U f6W0 9.L1 A4 l'/%LIr11WnWnNaaff10AfS pwYadrPMa4 nl to OIL Of So IA a OYir r a>rrl vaYr a(100 vM% rYr d is 4126d. Yai4. 9.1 3 A oIl r qM%i . wwsria awaw, of T!'oA it rra yY~qia~ 16 AI. of M .0l fr1eL nlrm m a And veima of I00 wM rr" aa 1!f aI.Idll6di4. !.!i lY/r* ,r/ hWdfgMfi= raYaraaMMMaNM nM*wwmar Iy IC W M MM fpt a arci~ rma of mayr Om wrlw a[lwwwim .2 R~Y6Cai1wUal~lri w fll Lowufi wliwWa aw lydl rr pnpw/ 4!lrl.C .ww. 17R MY~II~ wwri w Aawwd 1- $1 w awsiw v~dw. soo n !22 r lCfwtY~Iat wid 09000ft WMfd awc Mu Ww rY Ioa >wpMUiaaudaL GtiaMENNOW MONSOON v41101104f CS wW ead AthrKeu MANOR" vr m 1 " C4 rM DOMINION, fiWaDI p iC~ A !tt J(C~Yy~l p d NC %C~tr) no w o in xcw .r*A,4 uc >Ir o r~o tx.rwrrs ~o w o na xtrrew~ to WI d" rwarMlwdMwM~rioe Me Ord is apW M P wa wiMl w~+wMirt Iris bariAM dlr riAdrd & ry iA uasdan (trE1. 70!' -~ulr MOueao WooOra fyt r4 r- Axr !9 ayf6J Exygen Research Page 82 of 132 p . 82 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : PU001131 s~~ r~a~aot rt~~: rooonl r bl'Falrr~ YA~~M~, ANALy'nCA1. Mp0! L(7MMs VCbl~b in WNW IV - . .. t127 A sa atr/~/ rlrib (wyrd two MMS,y,MWJMW 6 w.h . rtNaftl~iatd~wi . . , !3A 810040 ago" 91104011m MYrYin 13-bLrlyMay3m-- at" a TCbN.a,btwwrh . !2.! MNM M qlw mw aalOu wOriwr a(atmmMma m q br lwMnd ar aw~d l0A 1woltawU . :IG1 No lw* of WON aomw0 (pVO N710 Of )M) afY/ Y k* M MY1 w a wyrR out* *NOW Ya,k wha IDU am) wd we yer immommY 1ti1Yd a 7 aOA MlO~t1001 ctf~ MM1W yit~, to ~ N pwwa.r m. ..y Ar to t,ra &Vf M 1.07 lY A- Me NY awi tiwloey ra+ r qO wi0 4 yww rw~rY~ai....li .f.abry.r< 1u tiqbt3zv.o0~e 11 .1 bln rrrOrlLNqYralwdwNwu 4fiMWr ,O~Liroro ~O so v' 17WWA- -ihp a la (lslHy awOK e~lw i/ WA It .l Comas" i Cr we afslM it L 0 My Yy 0 mbg 10 rt . r.ahr~ NtM~OYrf sLd1RirCwrr(-tbMYR) DarntxwMwrvadrT U .i (wdar~iaaaMiwOCrA~tweiyr. tliwrial~rr UA >Wr VOL d w1. 1 0M M+wd t.'dMA s ML N Nrb 1~ .I.pyp~. earle~ w . te .N .orr - ~ . u 113 Awl++Os wias~ettAlswi is Srl`M.i its pwrr51 y Ml iilwt b~taa+aN~i~trMla .PbwOfblNw saawkisaOr NOlOR#~{ ff M~ n A oNMrM w~Md ww rvU aM AUew W IT3 l~rNiattt+pArqailurLrtlaar~wra,ean~.rsbwl~ awab iA W ti~a~qMw~ a li 3 As ado wl of aswd aMhotlr fstlrrN wr 1r txbNO w Ae Utiq a+1 d tts n1 N S wFla r iaawsd wriai wM w iMwrw brrab war SYIe -rlW. M as sammexxv. a rw r a 2010ow orMAw wilh am P. fyawN at r4 b0N4! at a aw lirN by w~oM M~tlM saw" Y "MaN qt+y 3. 10 appw (r baMd It rl W Ibi ad No bW/ ftmdsaM1 ~ a11Mr NM, pYYW , wliwlia+a~i~a~tlr 66 PAR a,i 1ri tljacrn ts a irq4 r. U.a WE Yrr Wri abw 4 wdMha. LYr MstM am r~rOrb,niyrblfa.r~a,lasss vs ~ s(~wt w Ib,fM ~ Paw JO y( 6S Exygtn Rescmh Page 83 of 132 p . 83 Interim Report #10-Analysis of Fish and Clam Samples Farygea Study No . : P0001131 Exyps hoeecet Nutber. Pooot 13 s uhriw .r Mw.nrrvooonw ~ ~ ~Ai~a rIW~My ILY11 lM +n~r at~1 w a m& / aowwin aft 3Ma+L3m 3.3 for ~Wv~Jw1 w~+wrtpr ~ W 5MM OWN" *MW 1W wrMi Ariw rwqor- A47 +raila iYy ~a~n~ld Iw(tr~r 4a11 i+ ttinYr4lMrM W w.rlpwi. u.a x.qr...G1owlY 1 .1.3 CYnarq m wina Pwtia6r&V iwa3Ner6aasaewti 1413 awa 7 1* 413 w)ral wm pwi p M POA -ion -b% Ox waatfas Wa Ma1 M~~ala M W dca~w fodK 133 li4r11 WiR ar/ M aw RQA a wvai 6rw1 N Mft Ow I.CQ. If . htt eatYla7 N17d11 bwh Varu i w !0 a47 .ln v ~ Mrt w v4 sly M AalLd AWIYr a>" ra ~ 66 w 4awttri 133 MwbNwdWpyrafool[ ar atasfw MMa.ww 701I M K Iw1~avMr. Yaarwl 4irfrarreo -wqmlMwab.ae ~af ~t Nfaaylw IMW M aswealMa . A" wa rfr vu OrIM 70 1l4M idl be gab=al br 63 mobs tv d ~ it w4woaim u a+upA dwL 13A AW alt ~ MOW 4a+4 N M a OWN" 01" W/ N&A do MW iw 7rr m ar be ala6N faf M wtaioea of 66 aYiNaNa auw . Mwwr. b WA saYft of saw" NNatiNa arM * Yn awlG be wylrlaMit am so ssw/ 30K or a0 wal a wiw of snmN prir4 ILt iL eowY1 MM W ra0~it~.r~lIlMliinMn fWft ft awh U. tb.s . *al wiwpia* wr sum be a+lw at 441* 64UNFAK ad *4 dmfti afaa d1Y'tf M 4900MMIIOIIY to , . 13.6 14N Wa da MrvM al6r k ad wa,Iw Owl nol triR non dm l411 w6Ya1taaly "~L 9(81lMwds &illwwwAilinI1 -iM a urlltlo~l >tr 61r dw as awn w w~liwi . lsA CatNlri . 1 4L 1 UrYMr oks arAlwrwNdAbMafard/i+QA Lna1r'1, lad 4e " k arr) rM4 r Mr1aM a A%* Arrn c.Pd ww VW-) rrma0by M Nra Lv a aatiaw IwIm %V6 hod AiU QWIcIILL:iala9G o1 a OF $180 OF bin b"" r JIM nAr w ilwa{ IAwewury. Page 21 atti s Exygen Research Page 84 of 132 p . 84 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 Exyvu Prolocvl Numbu : P000113 1 rN.w. . .a wrr ~r. w~rna x u M+eia SrftU ? Adl awwrYy U'4*60 lai F& rwPia WMI wa Is~wa aaas d MA riw to i xwm a, we *I!- iMIdwMwMr rlwW 6sr.M ww.q. wnwMy tKJ lwlM*riw 66vd~GYd6.60WLI too Patr 22 of 6! Eaygen Research Page 85 of 132 p . 85 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No : POOOL 13 1 EsWea tromcM Iarnbar; t0001 131 00~ ANM .YnCA41riTiOD 1Yd1Mrr v0001751 Me*" dAd7'+*r Of DwrY ahn A hrONMUMr14 AW MCA) 6b SW by LGfiW A+tlfNOYTmW{HaiWr RyvetrrA ]C!l1NN.akDAw lYyCo k#% PA i31P1 MM-n+ W. C-LL t9lulo4 1d Qri!/ pn T.r.w i ..r, LC-Ma. .r" >r.NF+ .,(,~, tYfrt- D~w~[ ~iwlni0w~ Arrlar. d7w~>tw~t Tod hem 7 Pa~t S) qf63 ExYSm Reseamh Page 86 of 132 p . 86 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 Exlsem TeO looalNwaH w POOOI () r ~+ u os.~+~. w.rwr.vrwri n .o. 4 .A rr ft trao~ws -a(towl wsaley {. ~ri0dilrMq4AlfrMfeWsdwr~ef~wwRwk by ID~~~,y' *mow * ue6~w MW 7.A as" . al Al.a eYr pA l,ww~eraMw. t2 ~~~wIM iC ban ~ wOY d 4irr M^ep.r afay )A ir4a~/~ir~a~ 70 Marlsftrrql.r .w.o.. 7.1 Y .nirrrri ..Ala 7.7 lirN~ se~ M qw IOaw be a/~wa a~fu6r. a a. . >A Mr+YuaMM jj yaWbRwl wft rwWlMloraa+uf~. 1.f iw Mw Inua ON"" w1 N " iOd 0 Ir a wviy }M fu +i *O& a0 byr~M/~rrariA u t.r.-1wCpr at Uwa .f-MetCr~ A.r.raa. .a-was.>ryra.~ M M.^wwr-4 AeW - V1p ..11d 6 so l.w.. .~wr~.r abaNNOWWk wVdA pwW" a# s l wbi i~ rra .rYW wls iywr~ ~ r s.]u~ rL wrwdr ~ riNr l4r Mro~ws ~lqA~. s.2 wlwl.aw~wa.w>irrwrw~w.~~u~rw-. u ArqfalMlrra*rl~rww~r *.aeoot ~ s.r foiu . &Vwi+ b p+rlWsrr ft w hw vAw. ss w .l.yn+>,rrrwl+rr w+rw wr. s~.t tis .t~ls~L ~~wY I~~ir..~~ 4 s.r 3" .w<tmcnu>t sr ct~r.r.~.w s.u Mrps+rpalooorl.wlo-uo .u,riaawaww~. . 7.11 ~Mriat~AhVw& w(1y1L71 9lartlyn f .12 Y{~ww1 Wd/" 3.12 li mmis brk 1wlw ~ Awe 24 4(,U Exygen Research Page 87 of 132 p . 87 interim Report #I O-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 6aygas P:otoeol Num6r: p00011 3 1 k, ..f .r~ MMwtU--) n rtr , rariarr Aaa (PPOAJ . -; LflMttlMi s .: 'R.i...ia.rrn.. ils Crtllwap"4(tli*ftxv 6plpaPyNrrbarfoOC~ya. Id G~y~Ya &y NN SJ Aa~eied0l~ iMqYw ~i (Xa~eea ~elfao6e1 .21 a~ a!0 ~v~. Sr , 4TM: tbrOR1JO) i3 T~o~ 7P~ Cf )MIIMlMw(A) : 3rKAr,wleortorrauwiyr ld NAWlfw(n t NMMn( u a~..w.sar nod" As ao u ta e Lo ss ua u 33 raw w . t.~a .w oa Lj U 10A ]S f3 Ls nj v b Lf lf 1ow YrYitlF If~t .(raNftrar.t>oaririOwL} 1.1 QaMrMa'lrtAlr-rYrdrdrdaaM.+waa~a W 7laT(~uf -sl~lerw ~.. ~ aa~ Iwaw+ iYrldra/iYrdssy6arAylia oft to TV ALSO NPOM 7.1 IYft Umwp llap ir Mlp[ooia reitsit 413 - 709 iM: far HOA .wraa laaa 9M showemYlNa aw f WYMM a pi la rd my be drw/ in wow r WO M Lo w I renerk r u Pus LL) 2 aM rrwirr ac~r la rw L}wpad fy aOW~/ 0 . t ta ~ a! awwonm mom a t0oe rd. Kas. A.'doY w~w~aprYa/wpwL M w roie ss ye s Exygen Research Page 88 of 132 p . 88 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 exnennaood N4 : raoo1 u1 r,. .>+.~ masw . Awnr3A)i. a ~rrrw~ .nr.. bq rss . at nr+r. .r-100 .ll.r. atl'POA b ~~s le ~, ~~I W w+d ku.wri 1a ~1 r ea.r r 1ao .LL rirol r a 13t-UL I MIM M ft 0.14 A10MIdOetWlWrMr M or ITOA is by Moo", 10 be w .L I ORti .w. . !.1! AIA~GfwifNtlwMMMiM~flPOAbP~+df'M~Tf1Y 0LdY30{ OrL 901MIiwr S IMIMYrrdIOY .lyrawm .lu .a,l wr. Anl pAoOLMlwllfArtlsrYod!lOAYp I dey4soks 10 . aLM~lA!/1~LwIr1~r~M .M..dl00rial.ar.~ls ' s I3SwLU7/l~rl1. l1 .f A GM P /YILrl111WrrirdfFOAiw pw wl ya w4we 10 d of *a !.1 pS1rL n1tWm r & 6d aMu ol 1W I.AI rirdY & 130 rl.[al6bnb l.l.i ZYrNtM bWwloOrMrwnrNwartOi~niywrar go wI~YyPC o/ w ~ for a wRimlr pried er6 amp" . /rYrof~rW a u !33 w.1.wc1M~r.arw . I.Gi W rlYrlw raWY n p pM M 146C .au its Pa~rd *Ono am arn+o . Rw.a... ih .. w its Tbr a.+s` erid+u wrlr MY'frl .a-w4W.n. nry i e a..snuin r.A/.r. r.Y. .of a.+n . .ww c11e,~ /tia%on Vr IrWC1rYf.l~ lI ~ ID It" le r N iM N if R61o w0y.1 N i11 O M q/hy-2 to M r 10~ IGCWMN py.) IM IM 10 770 ip i! 41 IN .~ Ir ~ 10l0 %LtisAMw~ 7Y rrMld w~orsrY~ofi~wiYrllll~ii is qi r M ir ir41 wrer~IM ~ar tw erwraYr dMM %Jwd iitfYe a+ww~e (![,. snood odbmdw on" Pate 76 of 61 Exygen Research Page 89 of 132 p . 89 Inocrim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 r- 010- Exygm r0609a Number : r0001 131 m..r.. .w~sr>zrc.c MOM* a...rr. Aw aroAi a sw a n 0.2.1 A aa7a ailld OWN (aaOK 6I1<1 9@LbLOiaW M wrh USONONINNin Wool " 1~J.{ !ra MR s~awrl alae 4wda in 1Sat. pobV ap A. uiaa a rCMPC,+MIw *otf 92.5 AYa7aawYew artYalarafafeYrdaoaY spyrW u ON" 1Qf ~aoklatlh 101 Yq MIM of W. Ia mw (qpkak It R me) ant +n<hY r MaK O 1pd Mat ( ba ai t+& GM S =t of aAeQ l M nyua aYaN ii6 is bow rwew.rLr AW o.aa Wikd 1a wey PoMallNM ar brat bwL IO.S Maya,n fa 6a11 BW 1 olaf iOkalr 6 wow sill N RaCi14Q is v qWr a ww"w Oba L aia ro}x Ili I . GeaMie 11 .1 we* ! I of aw Y YY 10 iL'al plop, lati atltl6 P 00 (ImYfy a t~;Ftl~aa 1~ a'1 a~ ~t~ 11S AMSd.dnatrd dlakaaa ad.adiabrAr - t7 jglnw 113 7L new b Oiaa b a dbwab tu6 l modem he -1$ Wevies. 11A ~ea6 fa wl~a y r 40 MI. .~M~ .w in do f6 aL p1~rqNar ~s 18106 It .! t7wMOmp k-10ayaNaa-)OSD IPIL t i s Ca dkir do C. srs mifttra (t & 6 al,) by paarg 10 at. s.rma YYwl1~ 7 ai dIQLC aMar F i borh~el Da ~at M ao0s~ s by It.? 1+" (yaW L wow" v IM asd 6 a6 CE A@ oroily. Diwad +r Ill llar *Y d nl. I06l1 aa*aL CaWu I ml . G( dire tas Vaeard lf et.rappaqt .riya 10. plow wt... - s ni.l 1lJ A . Mkg a WM*W ttJilflMf . ISA CYwa.+~o~id lil i+wl ea a~aa aaar ~IM aa+6aa at.4r ! MifM arp~ m 1191"(S Own. A O1gtyal alnrd aaa 1 WAO d 1,7Msr OIW adAd+1 tst ~ia[w6A ..a,~.ri~rMtua 11"O xaawaaM.Owww. 0b ~r.lrwiart~1 .n It.f ~a ~riw aa et aaarat .rMrn airra awr re reAw~e r we b4ow+.e e s do r ar a r ivts is uae.d aor" .r ea Yiaa,~a~i baaw w7~ 3 l0 aaAl As= IrIfw. am aa of Sd 1 PW 17 of 6 f Exygen Research page 90 of 132 P . 90 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P000] 13 1 EKM- r.nw.d Naber, rooo1 t 31 ~ s--+ INw 14i. ..M17N An .~rncAria,yon r~s w=~rs=s ~Mr~aR ~ AtaO (}FOA) ia Sal by 6CKf~Mf 49suft man" A0606 =or be WMW a an boom" of a w~ lNw6 by w~iY1 "mown M nirb hawpou *m .l0rnVlr *rrriiraarWrldrlrW MI~YY} Yd.uwrrlw, wnwd rliswM .YYr a rt be Y dR W Wf Yljrll~ r a r~l . ML I1+1 tlw yrr a w ir one Itir ^Wrao~ Liyw ~ waYa GWrvw K w~iWi.rlwM~rarayir.r~ .'~m. ~'w d~ +yt !~w aj`Wi,~ J~d (e.rMrdk. ~ .ls~ou 117 iMM is *PA ri MOW padd MWOM n. ANY awqw Y rrlrrrw wpm= YII M W 6hdst r1 me.11n L 1~0 AaoMwM~Y 1s.1 Clwrrpw wsalow al dlafa dwsuir ieaY]Nar/m . Maw d 4131 Oft 7r 413 mit pim: ao elpma w Y!!OA eaa nhue IN rMM~ IN OA M I YSMw M M Iw rh whw IIsi4. 1 11 lYY/ 1W art rl arrb!!OA at Iwi Y. M tAQ. U . lYi arir I~OA s Iwi ~MYa !0 ri. fYa ~ ro hlr~c wry~. . r~r r irir W Ya~lw rt ~ Iw saasy , Is~ 6wwY~afwlal~i~~dr.Wa~7nertwYr*roAt)ONof Ylr lo m TUw. Yaao rd 9" m saw* 6o r .wIWr tlds. j . NOW w drwVY *Add M aawGsi Any atria *ft woa 74 ]JIM alwi/ M adlo 6 by Y arl>r r rrme if nar". I. 17A Api wMW m WY/ t W r b a q101tld *Who y niy 9r HIP am tw. OW b arW 6ra Y rakalniw Of of Wq ~ mrvi . rnwwr. Y YW aaMw of wnMM eirlm 1rYi an mom M oi~srr~w ~t .r r..6 70% dw .w eu~Er d .ouW .r.qw, t1.f 116 It rs drlr MAw 44 In w4Ltlr awvn rnnrl WW ev iQf10 so man If rrinrd YnaY YI Waft am W.W. i!a QPa W IMP IMI Ya oiw 064W lawae.r wwom. ..d +. wY~rW. .r. ... .rd~w irwwwWyna bwrlw `r rwwua ~Y/ri W w~MM. swl aw !M aw. d~.n ! a% WOO MW Mr >r Mwrrlw *r wxl w...6 u. irie .ft. =moo" mom Y waaw a rw ..bd ~ .r Pw it 4,65 Exygen Research Page 91 of 132 P . 91 Interim Report #1 O-Analysis of Fish and Clam Samples Exygen Study No .: P0001131 BtyVm Probeol Nrma: P0001 13 1 `ts~ IIw.4 rww A.M .TTIC+Y. *(Awfff~ ~ LC%Imn n ..rr v~ri~~ AaN(PPOA mfmly UA Cddrb r I l l 1JM r liw~ b riwYft 2 . Mar[ ~f lfOA 4~l (w ,y/L YWd M/~ te*wlbttia~ 1,y~c rt~wr.~~ Oft bad py't) M .t .e.. . :...en a OR CF-br.y.fii-hlw sr .r~ .. mhmKa.~.. .s. Kl !M IWOM riW rib la"m dMrr dllOu pir a swew1 w . of brwr( O"wn r w hdm a poem ewer". swwa>'(%) . t W .l ..~h..df-tdQ ywo- m.~+a.rrw..~.....uwlal . (eo 143 ~~ Ytiw 4 - ~w1 IM M ar or "OA 6d 'o~ yL o ~ PPOA b~1(A)mrsk -OWA (S 10 lu ur r 800. r .r dft w. r+.w ar Prow tw is pb w mbwdoL Moy AurUpb)eY -W& MCA rr (pM)peonrwr rw4tyl r~.w~ A.s. " alas Exygen Resemh page 92 of 132 p . 92 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001 131 r~cr~t,oaoott~ rooo~u~ Awu.rncAt. rsrHOn H.edlMii~c v00o1 7 YMM6 d A~y~Y MM OMr~YYw ~fM~wrwuwir Add i MA) Is wrw4~cw~a~~ 3M Rnmwb ou.. 6rr C164% FA 16101 rwe...: w . /vV.T~~ aO. .bn.~ir. .... A" "' ToYI hfc , paw JOaj6 f Exygen Research Page 93 of 132 p . 93 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 EM" Perbcd Nr ahes P000 1131 ~.. s a qrNaf w 14 :x7aw{ti7far aS'wnAi~w7ipYi7s- _, VFCA) is [1iW~LS 'ma[ y 73io mood b is be a4Uryad ir 4. boWlor a+i ~is~ioa af p~0~arooa~wc W b Wo hA~ Lil il Qara f a mod= Mw 4ia~a n~r~ (117bHA M b rYe~l .W 2G !~ 11 y~~t ~ 2.7 ~~+~l~TiplOmiMAwYrlrynya4arw1fr3wp~~y 1u Jaw~iaR.~6wttat 7. 1 AlYas30~dMMnrybRrwewl~a N. .~~P~~a{fa~ilAraMYaaflna~M~ . 3.3 ~pal ayynW radd be tlbwl ro pMl1MaN W mm lS a~nk~ lm a1pNf W peoMas ~ 7 a ANi ~ YA 6r ameian. SM Ptiat pin for ft. . t i Wrr-IKCiaY 4.2 wand -lLC p d. u n.rbAA l-AaSw Vay ... A.,a.ia.rla..r-A .Cl.l.rwa.w 4.a .aw~a .~.i.Mr- SomArd+ s4 Mm rad Xmkma.t u ~ Apm ~~batP~~7 s e3 ~aw{ raafa4wMm/pllafmr ld~yan~a6}.100 72 AMfa+r swig*anrNla~1/rt Wip1Rw qrwiu4pa . S-3 rrbWWd'a1a,r~i6~fwa~qMaA000~ S. oil 1 111 Mmudhp ubdL Si iut y fJ la~t.aYalOLCrYl4k IN oiyaa "* a-L O.w AMAlywa (NbipO PL wi lOda'U. Mr OI*aaMN ya s.l] qfwwy~ akVasf~(ItlC11>f[~m1~ , f.12 lLweaaa.adRN, M2d7 PaK 3f qf6J Exygen Research Page 94 of 132 p . 94 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 Bann Pmrcd tNOOObcr ?00011) 1 ~~ y.wl.r.vw~nr lb,. ~aan~l~ s.n w .. .. s , : w,l..w. .r.. . . . 5.17 ,'CrY14wr1ba(~t>nrL~sl~anrlrpbar 3000 q a ro c, . --+6pu ** m 62 Tearoom 3rc iA lfilil t!M OI ~ u auwJnA, NA~a~~ Acw~ r Xlur .Yfr ZMLOIit w For. Rw MA X1 lalaiu u u a~ la ~s U 25 yA ts it.i u 3s 73 73 33 0.3 oa 0j oJ 'f.i '11irIM.Vo1~ lily(~d4rrr/rra.~r sop" 7 Q.rYY W . : Ink Ma -rd mom" a.ghwaie . wna 7b bw r~Ofllw w Yr~d a s fli rd oAw dqd i . wer a MIYi .rr IR[,C ry.r4 7.1 mom MM6mwyM+r9nla lQr.M, w.rli~ 4 17~7Nrft ir 7V irw rrtler w inrd r a~Nl r0 aqM olre'd'a Mda a .gumirO.WlQlllleia LO h.~rnen df.ri=r LI 1MiM If.r h.1 t d! wrdw rwr L wrR 11 PrMa~1 ly ddirg 0. 154 * of w.l oh. .ndol.a1oo 9 rl.d..lr. Iyr1M r Pop 91ofe1 Exygen Research Page 95 of 132 p . 95 Interim Report # 1 4-Analysis of Fish and Clam Samples Exygen Study No_ : POOO 1131 Ex)'YeII Pmlocol Number . P0001 13 1 ellln r~r arra wrrv~l m AtUL1ftWAL ORTBOI) ir - A1 u Otllmcn tty . I.CitAL1/3 u enar.~wl.. W IM~rii~+~i .~e~ .dbytlCNtlOsL~lacricaWa 1000 rl. ohw~ AtlrrMrlwrnqha~rL !A OlrOrll~sda 1.1 7orYil I~Ib1Y~ plrlr 1.1 .1 IfMa a rolk aMYa d-10011/'~1. o[ VFWI Yr rw~l~ 10 ati dwaiwl aWrO (Nwiwt Ml+029 ~ Ow r 100 aL . i M~d ~ a 17f~t.Ldf ioM. f.12 A 10//ML Yllydr rr100 d "QA N pwprd y MYlpry lo i af Y IOO IIOYL wYin r .5W .dmr af 100 .! a .u . .ul Ya11frLLW/iw4 Iii A1A'rldilYRwW iMriiJAlOAb ' bybi " to a1.tYN~I.wMMraArlwtrrd100WO,~~a a 173aL1p{M14 1.I.s A0.10/tiL,l111/winrM~ra/1)OALpIprNeyY~i~ly~NN a4ef1M 10 ~OhIL Wlos r~ Yu tMwr af l Ot1MU rr w u a rif aLi O!! IMY a Al.! A 001 WM[, f~Aiil~r w4eea dl11W Y ~rai by wimp" 10 UL at do 0. 2 rlrMa w a Arl ~a6w~ d IOtt wiY wAWi Y a in si. ( M brl L O.li iLNelt~/rAOwOwrWaanaMalr~tioanM g rnr ~rY~ fS ~l w r1YU R[ ~ min~ Nr~ d6 IIIOaIhI 1sY`dp~ai a 92 v"OftorYali at 1JJ 4CAMAiW rYm I mYw N p ant m a .E w tl .u s4rea m0.1 WsL YWO0 wYew f11 71r 68504 Y a DOW amok. tle+arl aomo orariw any br --Z r~irMir ~trY"r vab~ nlrw crrrrr 1{ N 10 IM ! lE0 f ~ to 2 Im i N N IQ) 1 .4 f N 10~ 0.3 7 N Id 0.2 Pajr 3.i qr61 Exygen Research Page 96 of 132 p . 96 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : POQ01131 ZxMw hwtow WsdPer Pool 13 1 ~ ^ .t~~&a .r ~aa 1,, caMMo P].1 IS A N/Mr o soft* b Ii!aL tDi6 wlv.ra" 00lY w r YC w I'C, ~ ratr+rAr f]A AWrY/w0~~ Mdawt+alNuaf MMrda my be I ' as aa4t. taa Ar~>wt1! 1S7 1rL tf " it anon am" ~lltla~ !o R MQ ma MrLIs Y Mr wa wrwri and w-i me Oaw/ Mu/ob h niNd a mo~ rrwr~lsprl1 lOMwllj~r~r1l nowqRr o ehtt 1~2 4i~O lrl~Y W Wo>WrM~Mrwi 4006"s .itl be ~oaaMi blb~Wlq ~a~ AtY1 /asj K 11. 0 Iripts>Ot;oa ~ 11.1 i~ f ~ d~b l1M >0 ~i Iab1AJW N~f~a ~bw Ifiraiy a+ aw1~~lrl~a ~ ~d 10itt ~a ~ 112 A01 H M . af Ni arU WK e* "NO r6 rhq aa a adw aosa WO 11 .7 Qwl~~ati~a{+~Otlfi~fR+~aii1~IML 11A Q~iM tla cw IN awldt# (l i 6 SO by Mwy l0 sl. r M- t YqrY y70aLMID{C ww (-2 &VIr4 Dawlp a+lwea6y Ili lod fWne to IIqU a *a "Yo=! Cr !17 Saa14R. D1wC dM&L UA AY !tl rl. d am Ymml D to wim 4 4 in r rM1oo of tlr 10 nl "wow tai* C* vow wd Ad* a i s,AR moon A tr IN -Io air r 11 .1 QitYr~tlltlR~oid010qts~dpWra llJ Dwwrr~ArAaflrvwplo~rl~l ~~sMdr * IlA Wall 6P G WMt# 4 MI afwemai LO M do attwenta4lir ft aMbra~irM711J. a .1o C~Ira~+WCrt~a/1AIpP6f~LJb~wle~lo~f.afW .w MiwY 71d.aflQ'LCr w 1-2Mow c1. D a" 1atWh rom ft 11 .11 AN M tr6w14 -00 i of vow ad lw a Ow mood eoWdv-d itwnMip 11 .1 2 ilti Mr -f M1. 100 otitWlt CtiOra f OI. of sba w iao WnEwo 11 .1s s at . r ')'Pr) i L. a,rr~/.Nn (6d ..1. - s,q.> rv ~ PqrJlqfaf Exygen Rescarch Page 97 of 132 p . 97 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 8xysm holocd Number PDOO 113 1 1141f><. .r r...N.r.wmm : . .: : Am4ft :i IMDW w~~io.KF:rr...~+ . A.. f-wV M s.s ..n by l.uwan.s lso vw.ro/.~ 11I i~w~aiaadniaYdsd.~4a.i~dlYlasyMiwelM 1(y~ 4~Ya A arWfra Yfa~l mom pra0e aa4 YIY .~ an I31 :23 1 3L t 121 ~fr~k ! W ri Nl POA weawwftM R last Al. .. am ooaew4 W aa kwM a,owMiwYfrY~a+rpaYis Al a1w aw of arwd i~tla nr1a~Y was M islrM r *a O~M{ af/ it Al Old Of 900b ra >waiAY nr[ I. Yrwwad lw at oway 7-10 ryAl.s Al a slfaawlw. w main wit of emawaina s+dolb +r' be Wow Y Al aw dks of a go "Wow by "Allow am"* Yr g wd w M iN amw ia7 (Y ne~ Al a am" w oi ~inM~ 4 dYe ar~, adWa~n na1nYs was M iM his aN hit yr~Ma la ax 1Ywa Urn New r1r1nC oanw Al fam IayYa LYw Kataau cvw ac Parra/ferdatibrbPlYartan+ Yhra~i{*rook ara wim will wda M w aal arwrrlw as* 1twL7~ 7.I Y* a~a~~Mnl ~eRaattfbamk YrWY ""now *Add r1 arrd 006" wywM Amy "mph" dw wwHrrlrAqr~r rW M faAn Alyd all rrsYqaL W Mq1e.wOWa 11.1 Oor/M qr ior 4 pwt MaM daw, Alit 70 aim am a Palm 04l) asa 1% fl5 was pwal wqaaA M M/PGA riaq s4k 4e Yyrefr A~~wM~w~1 Y.Mr MateNierLr. W MAN Wall! s nt arb /POY1 IN Ywb /ar *AM Al IAQ. 1( 8 Irat mau l70A at 11"Y Polar Own 00.I aoh&4 dot a is. bWi Y aopY astr r M Wm1 ad Iw w/w as a~e Mx.m wra/. 11] Raawds doom" AV m ls,ria7am, 00 be bo-aft 7011M% V( Yi da vaM W 7a 406M oft YY a#Y Al Movable babis, the Mike M a[ ampYa raM M wawrr. Aq orN 9ta ern r is. 170 Mall M awYa41 by Al awyw it 4wrun If ~ftaceioa in 4aaaalal 17A h/ 011110110, 0010I1 71 !i r M a iMOWwl wtlhr by Wing go KWO >t m 7h4 off be aaYMW law do minimal Q( its wltY"oa a.K Bwwt,. Al "Id tieh w at rrmM rMnriw Mad" *0 Mww I .. SrYrM 0001 is OWN 7m of at W aoIMEN of asrwW Ke4A+ I" ~rlea aMfaraw QI Aff WiYnMa qeval 1Masr~p WAS be 1!ho PI' wm l 1f wtYwa .awn hn www arw qeww it. MOMWYr wM am M aiaa Y 46R Yarawwt Nwria . aM I. AVM" a trdwer r duOCYf daY I. saYywl Nwad i Pap 31 y/6) Exygen Research Page 98 of 132 p . 98 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Exypa rmWa Haft6a- roooI 131 AnAl. crAMMI 13A XOMM NOW Weal s 4 M %Wa .~Iwl~a YwrlrtirMa now& OialiwwwM M.i iJwMitUr .yqrW~rrlwYrfi~~catrlOA~f:~~Y.L. Met a Pot (Ye w n PwM. rr.ewr+~ . ~~rr~s~llrr[~aeirw~ro~r : 140~l~1(MAr WW ~ D7 DF - rarlywfddfW vMYrwdra, Vnwrry, 1u P. Aiw OWAM d* Men rrr er wqA '1.r r .Oramoa .o be OP f+4- ~. I wrweA.i~i a.ri.l - .wr/oe f~o.r .rdWs1.1 ~ ~ao . a~bu .+l~a4r.y 1l3 ~~~owr~,~ru .,rw~iY.anr .twwboe :~ .c naAhwd(w)- = 0 *t% a HA Ur 6o YYrL~ @"we Mr) r arcii4 N. arrt of rfO k 0 .1 : qr t.web wi*L w~OA Ilw M) dr~i~ ~ q~oY fe~r/ (p) .(tao% ~ ~ew w~yk~~ rr,ia~ /" PqV % qlbi Exygen Research Page 99 of 132 P . 99 Interim Report #10-Analysis of Fish and Clam Samplec Exygen Study No . : P000113 1 Sryyai Proaool NWcber : PooOt 131 ANAL mcu kdffwn IUed ..rr. vM 70 MtiM OTAOwrYi 4 M Dwf UYrwO dRMrwwft wY Add (PP pA) I. sfO rd a..m y wWal wt A-Ay "Tadft?wft. bowman" 3= 4 0 eAONN LWCdf~.M~dpt M+w W rs CAL !d GYTalqr TUWiri 1Wdr. LC40.1a)v Reno" MAW DW t~0 Vi~sla~tlK OP-dess. OE7irRaw#^ -Ae" Dow WId Pao- i Pare 37 of 63 Exygen Research Page 100 of 132 p . 100 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No . ; P000113 1 axyv n z~onod r+ w .nbm aoool M 10- 4M~ ~~ .arrao C1m b LC/WMt iW~N~Ye Y00~17C w no IA rTwN ' lti wdr0 Y r M~.1 Ir i~ Ydrfw ~1 ~rYrtlw ~l~wlva~nwic mm by Wall lY~rs~s~ Lip" IN sm*W a As. t~rrrMAa Dtlmr QlAtlALA w 6i r0 ~Ya a t1 t~M7 TJ A bsN shi n'w a h WMwf'Iria a 92 0111101"!~Yr IaD! be" Vdw my ebmad ir pql sal C` 02 11 N bill 70/d IM m1pU hr mWOs 72 lryw. ww be } IwU w ..ni . sw ON lr. rqr r . br p.. mer .y i. ..d.d. .lr ra v. rb . + . ..o . u..... .IYw. vu rf..Ml ...r0k bdo .rwra.NwY. wl MA w/ /Yu M wl i Moiimiii aIwOt w07 i" .r ..boll. u l "Y midr } es/ = r10 M WwYbO In ft ftvpig Ow Mr aw ~, . . a0 b~.~~Mr~s 4.1 WOW-JR4C/Mr AfrYOi-IaLC Owi 42 aIIIIa(17 A lla ir 4A IU4W -1!l.Cpb as aw~~11a~+W->Y+s+d 44 llwl+a IMsil->Rwrwr u ~~~~ ~ s >t,~l~s. .rr-thy.+p+r u0 nY~rl~a.i ..-!J.^spw pub 44-1113 = 1i A+= ~iAuI lw-A.Cl.R1"1rOiW 4.13 helwe W iAl tlqri 10 limrrmispipffr1 7.1 A YWL P~M~oO im 4-ml" i4sbk of /rNiy of q : IM! !"11! Ilia 0 w1A4 trie0 && U MMhb ml 5-20u yI.OrMIniM alA1~ ylrr>T~~r(LL7YL114 !2 AOMr~ai~t~wrWfrl~ir~~lfrriqrre : 7J A~II~dN Y~YiwqiNdwdY~/!o t00001 s M1~rt ^ Par JA o/ OS Exygen ReScarch Page 101 of 132 p . 101 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 s><, V. Awooa r ambc.: eaooi ui mm=wrz MMLT,w. rsTxou Q.u 1uMt+itl la ra x. A.iq -..+ .. x3 flrrWL u iss .c sro< .1 So MLA"" [i ~s .c~..wrbvlrrr~~w~ ~.s c~..w~..w~rpoiaor, wa~ooua s.to OW.ID!l~~~yoaw, f.ll :MLqKFPLCnWIdt s.t7 cl~wir~i~rl a 5.3 Air~i'r.(toIOOONL.w l bwoYlJ, .o 69e 806 q0.. ili p YY- p0M14 (lWw al. m k0.r719r) , l. t7 wide r1ot * 11M L 516 Crifyr NP*Y 0* W 1SlO OI. M41/77t . ulr a 2000 ~pe aa al~csn . . 6J ewy lulceM.ilwqr.pR. M.wldwleatLl,wawm . l, pRr1821e54eu 3% 62 7400mftu rrC Si wrb rlM(A)i Z .N A...:= Jlaw. iat w.wr as IY.1dIPyMp4 : hyswe ! cs onrM rs~s 10- SOLlrYl SA u row am as if 0.1 1A p 3f U +o ss n u ~ as rr u 32.s 45 is & s U WIWO V*hwe 1f(a0*loomrrwsouUwloyL1 cr Q.r,l.: r.tn,.-ow.i . w u A..r.K -ssa:iu. r1w Al m ew /mYas in IM m0o6 r a Mi& r/ ry be e6~ . Mikr W rHwlw M Is~l rywa 7 W J N! PaplV y/6J Exygen Research Page 102 of 132 p . 102 Interim Report #10-Analysis of Fish and Clam Sarrq)les Exygen Study No . : P000113 1 Hxyyea lsbeol Aioe~er. P000 t o L *a .s .w.. r ....>t...wlNxt AWALMCA L CLd * [.blA&Ads ~ FMII sM to lii*4 so= 7.I ~Is/ rA nws~sy NYi++MWA wda aioeiwiqals ,1N rri Ar 'As Nwso~iis w rrW/ r tlq~iM W Yay ~e Arq .a is aas n ~isili00q~e L0 IY Varir {Sshmbr LI IbbOG Thw LI.1 3 aM rrldm ssYr Y rra ~!~w y ~ 00.1 Fa , ef w Wwiw sMwY 1000 wi .dwu. U rmw.. ~ .riw ul A1~aYYYilYai~dt,~rs/~yMO1~7~alYmAic rYr IroLrwYrrl Li3 3" OisA~Ywrlrs in et,w Y I~Ma by M $ir~ 7 ML dM EM449SWsrilm Is a ttisl vapow st10 1. -ft qL,er. M srwiw osyM I -. ~ fa an" P"P"M 0.1 Adsd Wb7 YtlEwin brtf~ ' f .l.l Oqw a m& Yrrw d-NO WeL sf ROA by wf/AY 10 sY ~~W W~ Nrwts~ ~ DsTi1y1 W~M~Y 4 106 ~d. rN YMh1ul in s 13i+1. U R WAS. 9.11 A 1 .6 wY6 fNYsMb MAN" al yfW1 y MIYy by riwn , d. db ]p phi wWw in s fta n0es et IOO .YU ssM.m Ys W a1.1 M MY. AI3 A O.t Ii/'rLwYtls o wsslWssafNOAttARrMbppss I . alL slYS 11 NIYLrWefs m s W qlssr of I00 w fs aA.w ia s1tlsd{OfR b/ a 1.1A A LOI a06sl, iAf OMM a.kd- of "OA Is p~rr 'my Myrq 10 al. a/ aw 011 wd . a.l W rs M a Oal rsl~ of 100 rN rr/ Ya 1 79 P{.IDIi ys10s l.LS Asw~Wf~YSwMtls~wYMtlwslbsnMtewrr OMVYW! I'C r w rrHY hr s ardssro Y+riN of 6 snap iw b Ystp~rla r+a~rl i" Pap l0ofd J Exygen Rcscmb Page 103 of 132 p . 103 Interim Report #10-Analyais of Fish and Clam Samples Exygen Study No .: P000113 1 r'- firyjea Praoed Nrmbu: P0001 1 31 ~~~ rrr>w~neo~w us" w , V! A .WiIlI11L.LL f MtoD ChrlSrllJNtl10 1~ " WA ~'s.! MJ1WnalMlf .s~iitM/.r .~iao~ii .dri.~o n ddr I A PWAt.lAlV.l. Wkdd r1.1 I~ND ~+6 b~id W~le .Ylsra aunrn.m may be 4C F&MMrM vir Ard a Lh~f~lw{ L du IN tw~w~ew I I r 1a Y6 lDl;! ~l0~l V W u too GA17 u la 0.91 100 SAW tIoS 100 oAqS N IOO 0AIII 1 1i1 !Yw LISaL M nraarilwlN 9 21CYMCMI 93A AMoomw+" I owaN eroNN lfom *land" wy NpmprN a MI tOL 1~A ~uAfstl~ lSl 4i lmb N~1w YrYi (O~IMOy m er Yw) ~ wt feeWM a~ Wr ~ I COMMA 4Oqwwraeftw mwrr7lr *A b~ ra. 107 hr so to WrYwr "M"M d *am .{(1 tt sped" 11A tuipUR~erf~ J U !1.3 1A 1!S lilt R f g of f~ ~Y Yla $0 MI, pl)pyylwr ortri~ wra ~ n Pbft Mr i wll. Aii70~L~farridM L AI Yr A wWrYM afrer-11auiw. qNwi 1 YM Y 0 6MI rh - 1 Yrc ~..t~rWw~AS~ =iBduM. prerytlDrka ?a* r]0r1.lirrlN n Aetrlal[Oddl=i alga got, 2X sir ad I f W-141t On YYw, 11n wow. MO 20 wL ei wwlrw. *IM 70 M44 Of no oilY . DYrd i wWa Do w Ww be w.M a 9% /11 r:'s go 17! d -- 0 01do by Arw" rwk Ih . 70% a -- - " i wMrr Nil" !Lm an INC vilk Uh- us., IMM e by aYw Cheu lrs). Dey rr Iyla ewteelr MUSS we. IhI rb A 7M1 a w/r a watu af oweovo. wRf~(11 /lk Iq`r(laf6J Exygen Research Page 104 of 132 p . 104 Interim Report #10-Analysis of Fish and Clam. Samples Exygen Study No . : P0001131 e .~na~.iah.~ rooo1131 ~.l.r~ >r~~ w.rr vw~m Cho oUt.XT1CAt MiT710 a ~a CMy~sa/s At n nM .e .11 .1 Ort1w Or 70 vof . pl)rw/yl~ w" mio" waqM r -4o00 +~m AN -W 111111001, I1J tiMUlbwwMw r .-dYwd/ IIalr/IriuibMe"Waf ir tr.'+lW Alm COO ft 40Mw in w ne ra. .t.w ra. ifty. SUL ti.f AN 11 ai. or Mty nAir r to m,b 1. th % wL ariMf ub. 1.~wY .bltw.it/r .rnMSWd .R~r-tt0 O.a-ft .in. . r~r~Y swir-i~~t.~t~+.rr~wr/r.wN. .i 1 .1o 4hldMl 010,14tritt-1Nr11rYW .oYDMd M Irhf. 1N1 .137 Flow 4rNrYsBomw Air -tYrw mom CreilYI w!D ml. } pbpopyYw wio oeriig anrk s -20W Min >r-*,doo m MIA Doom ft ~ Mr Soo ia ttl!! wlma CdM go rw i.s. M wr our-MW Ovok w~ ovewhe s w i is A~r ho I. oufM ~IAOII M , i1J~ Yr7Y~LdrAwhlY4p~~rITRwl~a~ia.eYn4r~Mns o irr ~~d Orc 11aJ IIY~ wLw1 &W of I7MMr1 D L INM to 60 pwrjlpl i /tnk ad tus rtl. iw w~ .~Miy i .inx ~r.w~w.m.w . Ilar SLO iYaoMrM IQ'I,C didyAwnrbbrM It lu S Asa pwwrta~~.atrnCv%n. lu a~a.r.~y . 121 1?3 123 W rim+. .~. . .rrJ aniM .+d ..oN .rA .iba,.q4 aw+ 6dMH0 q*w w ..rwi.a MOW Ms rrw ad lavw so owelywr+%bl Ruilmill drlOASM oVrMyrft Wool lwo s oag wmw uria4.d4 aMMirwrYMrYy " M, As r1iuM ofNIi1YwMWnY nor[ M * . ad of a r'M wl b MwA vow M iswN W YwwM rwy S 10 4MO 1\ AS U I 11~11/i UNA M o f OilA1rIM NMadwa my br IyMd' at So byi naing of a OK AIIwN by ptlhnion preaNt Lr+ww/rweyf~qrn4irp~reee[tY~rwiOMKarndrOU . Y iMw aW 91I1moot6w dwiM a- s be do IIM M IW byutw in a M p Vi !MI SOW Moo r wim Sir piMUm Lmot aooOro eunw M ~w~ilr~~ .i4 r by Moor w~Miir wwt Inc rwrwy dpwk wa tiws .ii . do" .WAN w~{ M Ow,,. A7 pr .a.rN.RI oR.~ piVIAL vw- Gift Aqr 41 qf6 1 Exygea Research Page 105 of 132 p . 105 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Fsyro Ploloea xumbw- P000113 1 A.~... Mrr t..woo~+o nMcxncx MCIVAO a.rrrs~nona A T;r .w 1:! M* Mlrw iaiY w ard rob! 169w" Mp Naylw / A sar .rr .6 mV Ys +ere I. IWw. Waa rd roaryi. . 1ID A~t~QYY 1:.1 awrsrm ~ssr~Mws~rkdsY.~risr)ilrwAsws'rw O" D as To du ~ p~ rrsysa as b flpA Seim as at &yrw WOO Mw vwm~ IM MwdAa Ywiea (!s NrtirlVi .s .rtp .r'rrPQA rww rSrvYabtAQ. 1 . 111 ir!!OA r Iwi pmrrdm 0.7 wl. r s am iYi nnpl. ~trslrYMr/Yrersf wNA 4rrra~a.A I>tJ RrUreft Of /W yiA at YOht O iw moo M MpNK 7*.1]01 d ~i'>wr ~~s, Ys N!d ~Ur W wu4r ~M aeeA4W A~iu. srr ads M1wyb YW M~rM~r1 . 11,t Aa~ ~tlrMw laid Arl M b s Mrlrsr wdf~ by aft eke Ns twr Tw% aq' Y rrViY !M Is riYYon 1 d s MYl.stiw enn lisrwv. Ow IMl rrlr of dWriw on"* ir aesW be mckdd ~rrrt~r/'10M df~ rrl airrMaaYri iysr L 0 3 7Ss weMrMa wegis W he rlrriw mom /oArd isre r am (Rl i0lrl3 It r1Y W40 @ss" Y ssrr f.r llswr. Uw OPM dM rr YM M MW f~t boar" wriw, .1 Is rir w~ a6wsr ~r d~lw rrdi M w~rll~S L U6 !<wriw ir boom rtsd06 ad is MW M all MM iw s~NaiiWrsr>rws . Yn~rYsiirbillrcawdrNiliwr~.i~r :~ . arbYcM .. rr a. rt a.rb ~ .syre. 1 4.1 UbfIDY~~MUMMIwY~M~rafflW)t~tl<r~eLL . Y~d m ~s! rw} ~Iss Y Yisd ons !~ ~O+ss 1r<w~ewu ~rsM b Y Mrs L1rt+lAssw ~/~: Mq~MW 1y1~i1~Iia~LJ~aYU ~ 1N1 UY~rilY.rK~rtiwbiwweli~~srt~l~lOARWfeNb~u ~+i bl~ lfOiA4>./ lq}Y1 rrur+WM W De -Ira..9y .Wt r. w .d. . . .. diMra, t .~wwy . Yt7Mi /WV 43 cq/6 S Exygen Resemh Page 106 of 132 p . 106 interim Report #10-Analysis of Fish and Clam Samples Exygea Study .No . : P000113 1 b yW Mend Number roont t] I J, Wind X-6. VMM iku MAW ,w Ax,.c .Yricu . arsTaM s or so w e~iowi'tia's Agw y rm~~a j t bmbt c NNts tw Fr a *n kAUWe ds tawe ae r or 1 FDA Miw o aruiwa, w bMM~'fo{qrlMl~wMfW Or'r~r wcw~b ~SAH ~ [~yla~y~11t.11~b ~~s~Mb~arlN~~ r10~ . ~ryrrYr(+~{1 Exygen Research Mr1A s Pup K vfkU Page 107 of 132 p . 107 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 6,cygm rnaooot cs . alw : pWc 131 uw .nscAt. MeM oa . lww ?M w vm61,M M~a dY~4'd~ ~r r~ A1Mfrr+M~Mt Aslf I~/OA11~ YMiM~ bI.CJW+N~ AMrMitwty ..iwr : Orr cN 4w, PA 1p01 Am-Ad Dr. cpJcaday ~ wYiM Lolbwr L0.q.&rt+ 1. ~ Dr:~~ V~eA~.re O~. .r .Rndw~r.e~ ~ ~ TaWIqW 7 - PqQs I5 of 6J Exygen Research Page 108 of 132 p . 108 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 EcYFm PPaocd Numlcr. POODI 13 1 lqr+tw..a ~wh.rr v~W irw A?Q4.L%i1WAL ~ ~ MV Y IA >Ir~ 1Fb aid i, 11403 MO"W iR bt wrtla0 d Wsur" d W6= oowac a+li by wo Neb- Ui 3PN-IIUYM D- I5.1'JIASM i ~~4 .w46d M a Madan mo& 20 softy 11 AMpsiwnrAMwwsyMwd~~. u flu 100>t Mfiw A~iiK my d~MO fu 9~ap r VMW 3A 6000l. R l b- 1.1 NMrtl g dYt ~ Of wiMfw 7 7 ~wrsd! r rrew~/ I~w ~noin !rw MM !s0 UMPN W a W/w~.r d M~wiw .iR M W Nw M OIqW ta wo rm ~f Yw0 I~w Y>lu~ ~r wMVM 0 AN" kr n{YM iuaia. ~i4dr 4Y wl PAM M IN i n h~ rea~ uW this of 17 t mob MONMa www ~ A be p Ddlld is to w Wry pla, OF 4+ lRqi- a 0 1wM r0 ilrri 41 MMr->'ICpr 42 -twr p d. U C~Ia(qNo r ft -byrl.Y 40 MslrM-10'LClW 4S 566w Pt/M~7o0rtl-11N MU I10 44 Ilri/pWl00WQ- VA rtpN 47 IlW iwllw [GIG6 - logo ratf y I-0~ -1?LC/96 40 L~IwwObW-Ilw~~pi tq WM~MeaYwM~r-1~t sea 471 T~II~r-lf~~~pr 412 Ar. .i.n.w-~lcs.lAwreaw 4 3 h~wrrM~iAdr- W*NKVd" s.o iiw~~d30}.. r 1.1 podm of e w ~ ~ - ry~~ ~W .~f~f.~ . ~~i }1w r1.aomrowiwardn Wx /pr owwrQ.pY+1/y !s AJwiwMair rwiYtir7 mkiWRw w ApwMaa 53 Aw1wY t1h~ A*h 4(aa.0 b4aoNt a tirt~~ PtWr6 qf61 Eaygen Research Page 109 of 132 p . 109 Interim Report #I O-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 mr:aeeoi xu.e: roool 131 ~.>r~ Itdel A yM rar M rr vwi ~w AJUL NMI" ~0 ratnsyroie AAW 4 n "1rwa+ by LCMSflIS !.{ ~on4' wiw~r f.f Ifsd. ~wr~~ h ~ SA s9r1 .Y~~WY~liwariti0i0reNs $.1 11 rt.i4eWUpt1}r0~e~rd~ Ww Y.1 p1~r/rrYrOf/~pM00+1 .106J00W,} f! lI7sLlaRr#w~~rlruMa 5.10 3rLdrrlVLC Vlild. s.n olp ..rw*r . 5.1 3 ArsO}rr p0xa OI. .r 0aao rll. O riwa.w wL f.17 !l~rAr~QOi~A~~aur.lwm77. wesra~~rlr. s.ls d~y~rOdMel wirk0flrtO Wayylw4Na r 30o0qa /"` L~ll~) Lt Ar1~1idd1~rlVe~W~v(K~nset4n01k1,x .t~w+tsOrr.fN ?ft w"soaaol u s.y .+.M we 6 3 MaNr / V w N1 : f w Aredrr M . in wrs LA MANN=($) : Memo ~1 Oi~el~ Maw am !LA ~ hYbii~l Ol is 33 W 1 .0 BA i" tt.s 63 33 0.3 ss 75 0s a ts oa e ss oa LA yer Wh~c IS pL $M tw Yowm O r . rr6 rr s0 fL} cl Q..Orirr t,re A.u- .r .r .r.er0 .rw.6. . rv.. u II~TIrr -ss~~ra SrMwraYfeww~rrra/MNd~ywewre~eArr qirir i4 tRSC ryrr 7.3 r1fQNOl~t~ 7.1 11ere ~ M~dq I~l/ OOY. ~o~Yr1e{ 411 -~ ]f0 aft fa "OA. Pqs17 oJ6S Exygen Research Page 110 of 132 p . 110 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 F.xryjea PIoMOOt IVWn6a: p000I131 ~a~a~~~ 16arlNa~r\Meo~7M ANA L aaios ~ A~/ A u V by u7~alAY ~~ Sb aYna MOM" Yoao"o a FMa rd ayf' MaMwO A wWr o a p1Wa Y)mf{ alwia ~a fa~alfa~d~aillra Ll 1rYY AM 1.1 .1 2 vi asiraaMso wa M in ever In pnwal y MiWug 0.1 34 1 of ^riw ~w~ r 1000 .1. at~Mw. {2 6errrWrY ~ 1!.2.1 2%mOAb YY Y~~N itF~~ bdMaHrt = t olaoo~0~r ai/IMt06aLKWi a12 IO% DimakyUlalt.w/1M Y MAra is w~M by 1nP 3 .il. of ~law r a drl .a1a.a d I O .C .f 6 wMs Abame Maew>wqMtwpoi f.O wens hq at11W !.I ~idSraia~mdYrlo~iNOb a 1.1.1 lwOn a not siMn OF-100 rWOl. of flpA by sryliq 10 nyl of arlJa~l nil *wd ad Go ph ad OihY M 100 ml wA atirrrl Y l 116aL f M0 MaN. 9.13 A 1.0 P!AmL 6 Il Iwdw aiOa d!lOA . Impaei by YriapaS I iJr1 40 M4LaaWa.aaVlw ho ad100 wiMwMhrw mim 127 wilAilMlL P.13 Aa1pVL4Wadias minim 1 FF" ia I dryLi0i10 at1 .dM 1 .6 M d. nvf = a a Mod w1~ ar 100 Wfi rafaad in .12s mf.60HlaAa. VIA A OA1 whaL YMlewlr rY:ae of Il+OA is papor by br,MK to i N>r 0.1 M1L rlWOa to a MOM wmr of 100 vfw embodies 121 r1.1I7li 1Ms. V .S 1ba~a ad6rYrtl0~lYnleranuMw~w~ianll~aae at #T am M a" M a wxiw }dN K{ naJt 111 Irbi C . 1i1{w a f21 1OAlOM/ a~rlw atwYda w Asd fa an8aml rb M1~wn stab 1 .0 WYL Yd6rOw NMNa rw~W' Plq* .e Oft" Exygen Researoh Page 111 of 132 p . 111 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 s~ . n~~l r~l rcoo t i i I "" ~r.es~..e.t~ aT ~,. ..rrw .r w~ ta~.~, by LCiM1tiM! !:: Tls Mrrly M f, ONMI sU'lPlc WO iwl Mwnrior ery be Popw/rrW L Common oClu wlb.rr voL. oiWr Or.wue . LO It IN I.t iS IM M33 1.0 1 4 IM ~1 am N NI G,MS O.Yf p 101 tm! ~.1 10 IM epi W~r1Y ~r~narbWr i TCr R.'.+b ~l r011M~. 1i4 A4wr w- r d~dob ryr 6* CP r IN" 10.t iM ul`J! 10.1 R~i lrr ~f I~ylr ~d (~ISYy 10 at 1~) w~t irJ,W s Ir~ rr ~YwM/ wr'Y W we Wwrt Ili RA9N s I~wn ~wr~rl~ (lir erwl splaob ~Ify PM i011111~- s Ar~M iwe0 1.01 lV~Ifl~r-k Lil in/ W wY 441M+q1 W q+Ln rtlt Ir #dfim ~,.~ i w qrFMy ~rr .r~llr ~r Y~ ~yrc 11.0 ~1 . Rrrliu 11.1 17d!} !/ at L on rmp Y no f0 N. !ep}eiy)~w euuffl,p rMt (1Nba rwK svios W mink wd". 11.Z AM I0 rLdmribrirlsa~~ .dMrw7wrYk~M~1lrwM .7 QYIAr r 711 rL /M)ip/IM~ 01w aewle! root r -2000 ep b -44 eWrL 11 4 ?eekWrW~Y!ltMrWi,irdeMr`~4~llWta 11? Pink M70M.Mrfr in owpr..wrY2l6eioL2liir pt 2 *AML sill l! LC-W4 OadW o 4. rY ..r dA 30 rI. of s .rrel SIR 3 0 r1. drwoi ift Dud i wba D~ a rkw rs ~oN~s ,r *06 I 114 i1 W1 10 w lb r[. PW& i+M Orb by nra! wi4 On 1uK lre~WY~o4Y~ JO rMon rMYr Biw w W vW rWr N . Ww/ y rdWM 10Yw eN14 DP 66 AMr mqlrMY be b w aw. 4ww b i 4f~sor rY a s e mm deryr lL7 DwrtVa,ritwra~7RWWIIWIrMlyww r ON 1oodloloill Yt C1FYa b N oM d Ow l25 rL 4Ynri /wnNrpe OWL M.fw' A . 49 of6J F--xygen Rxsftmh Page 112 of 132 p . 112 Interim Report #10-Analysis of Fish and Clam SarT1ts Exygen Study No. : P000113 1 exYps r,oaed Nwaeec roool u 1 w. . .. . .+ . w., .~....~~.. AAwLI'TICAi %tY7110O .. . 1 w epftia b LZMMU 91l AY 30 idrrdYlb rON .ybob 30qta .etp p {r Il! Now 60 ^4qwYM-I 0 MWOww a wiwarirrWor. 11 .1 Coorwils SCOWL AM PO 4-4ira .. 11 .111 D aIt >r now ar Y ra~ !i'i 6OL~ CJIIr t!~ Yr! AM IN wr. ~+iM~d e~t so wwOw .YO *s * w MrM 0s wUN rawir 11 .It Rap" r"@ 1 U 6 A 11.11 "IY t1 .IV AN 34 i W of t+r od is *0 MOM Am an pow-iyad Mt d "wr r iMrr P ~ oft a wwT OwM- (M <M'Ci al ." ttAE Go 6W "1"S b MOMM 2 ML at 2% Mil" aer is rwtr.a n ~as~ir~wrrrwWaa - 1LU 71~frWnYrffiLCd.Yaiafvembw POOL 11 .10 Asbrrr+Iwifir~~S16CAaMt. as ta IJ.i INr~rr~rMrd~arWiard~~LrM1d~rOiiusre LOIOA O AAVA& A WiWdr MAW Wr NMeft a/ AM. Jl . 131 .>Arirb dN'OA wrwA.lit r M M.it !w v.r. www.r.. Mw1Y rwM iri/N inr wlliwt UL tj.7 A p al W al N =ON" nYe/Mr r odrp Mart N WAWd r CM Mgglooft =l d W r d a wrY ac BXWMW mod" am Nor Yr~aY Yw~ wey i10 ~la M~ MnMba a rqtw r~ H W rd Ml VAis a ON6 rM b Ydwr r as Iwor+{ N~~r 1Vw" aN Yr d uiasia swills irArwr "rP 3 - 10 ropM (ase r" tk .rr/ NMMriYrW wrii} 1rOrt~wrsW Ali~\wlri arMlw am w16* idsam YI . r+Y IN . 1tA IIN Nam rr M t wrr for Ossakrl m {Yw mo&M owns at piw~d t rrryMOYtYrrer~rlr ay Uf WW o Yj Mr/* w un lil nlyd1111 ME" orteMoOs oft HNrl.yr 1 3 (N Arakri ~Mrw 4rs ti.f tr+Y n lleoft iwdl .r G wi am" nw~ A" "now dw v .d rrrrr p rr rtwll.O &r ilu W .4' 0.0 ~nigesmi dYds I7d Qw~re~ w~ ~Yw ~ N~ ~f. M~W fw r KO im ior m prm of 413 rR The 117 prrr s=Mp=ft 1 r !OA Wiaq .Mi k M rqYrr W(N/ rr4l~r+r w Ir ~f wrAi~alM. a~ Y ~~ Pq~~ SD o/6J Exygen Research Pagc 113 of 132 p . 113 Ir.terim Report P 10-Anatysis of Fish and Clam Samples Exygen Study No . : P000113 1 H ne. rraoeol Number. Poonl II I ^ ~w> bl.~a !.7 Irrl~1~4 wt rw ..+l.!!p~ 1.MI . ~ ..r w.a i. WQ. 1r . YWt ariullOA e Week IUM So 0.31PR m n a w bleak awpy IS] RO Mr" .f r.YM P . and w Ma vAm d be Y .t.aaa 7130% of r: a...u r . .r..l 7a. . .e. a. ui. rl. re .t .rpW rd/ 1.u+.Y .rw. 13A Aq 0010 fr wr d M 6 Y M . fulfNM autYr by aNe% tee !Mr rar T1R ap M adii !o~ r wbi d o da. qYtrrio ona "MW. to am rIt d . Mimfn vIMM"* Ow a" be "Wed ~.R rI .U WA NY WW arr . ( .rii *" I3! T~. .WwIM. ...iair w at .Yv.1. s w..e rri .r . lam a' :aNn. If wM rl. "err am vrws ru Une .. .. IFINOPIble be e airi r~wl.NSr td~ w~l ~s ~~ie:M~jn~ d w 136 R+rJ .e rM rwur Mari WA aPw wir we QriO a .w M t4 %wiii.M ad ri see. 1fwla.Crtir.blwaY riatiwYwhY. an .+.b" an so io in e.Rwwrlysl. MA G1+Yir r 143 UM IM 18-44 qwl. . I. .YNIMI. r .r.IN d rlOA rd Q. aWM. tow M P@* ry =y r YAYj !n7 Ob.Y M$Meeim ~/tIM~U p, .alAbp In Ws Lp a . .%w ograrn . rlaA r,/ (76 a0 - MNL r m ., ..r:.t dim" KS ~ r aptl~p~ewrtM~wsdi'POAbr~rer~ .l.w 110A bmd(M)~ ~ ~~~ (f1 DI - rw br Mfat r 6W vaime, w 4W, ita.ewary. 11.1 Per asp4 ha LL Ms MM Owi Y of FlOA rwr to .xt.qiaa, aw t. 60. .i.6 ."Wi. to ads" r r.. .t wawy. 1--Y(%) . 1.1r .rw ...el WO - .dw h udi.raL.wi .100 W1aa17 .~ (~~ /r i .t ; Pa~r~/ .f61 Exygen Research Page 114 of 132 p . 114 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Haypa hmocd Num6tr. p00p l I)1 /' ft ANALYTICAL MHINOD www MOW. vaoata MEOW tAWNY IR w **WON" d I'r1 * wwWM Alll a'pA) b MM lf+~~ IIm y 1.c r M Arl 'l~Wi~dsfri00a Aryy~Wrr . , f1~RrWDA~ JwCNYw PA lM 1 Mr-~ + Dr. ~ ~-~ ~8{tr.lo~f Dr. TrYiiW 1 oMt.1C W mt~ vreb ~WV DW qwA:aa 4~+~ ~os~~ ~rw~a Arlr"s 7 PtrpJ2o(EJ Exygen Rescarch Page 115 of 132 p . 115 Interim Report #10-Analysis of Fish and Clam San. pies Exygen Study No . : P000113 1 PA" Probed Nmnber. P000 113 1 ~~-+ ~. . . ...r .~.,~+ A&%ALVTWALfttfMW awb aaiw .riri, w 2d uwrwialry~7MwoarAwMi~iN M~~I [J w b7 [.W WS 10 ~~ c '.!i rA60d 18 r ti M*IAy tw er WNW 06 prNrtw orp~hoeeeum,e U l! by NO Irw~ { krd a I Y oviw a s lydw M. s~r~oe~i~ nwa~rQ,ClIYA~ i~ r .i .r~J ~wr. 1A ~y 2v. 3 ~ w,arorypreWn ^ 3.! Mr.~ssdrA~l.s.d.ria. SS 7.7 i"W emu M P wrd Mb /Nrdr NOW !Y i~ sor*le 1m s iwt s~.e ~~ r1 Yrm ~es wi66y ha Kw* !hr aepla a cwrat r1 Mw . w Y *MM MWw "now r tliw. A. w b e eiw,w 860MrLa %i ad 1bN M wAlw M 8e m ar ap ow Nw d a!~dpis If fw Y r hwfLfrt rmrtef rqV (AM UM . 6M s is w~Yll~di r46o~Y~~1rs.~li~d Si o o~wl-jsow~~ w to w ..akr w rof this I4 Rwgar r>e~IrY 41 Mwc- aLC ~ ~r.~_c`. + L7 AWYIY-lOLCSI16 lA A1 AuOM- A.Ci LMn Owia ~ ~s~wer~YAd/- 5pwAWA sa ~rarr r1 ~~.~.w 3.1 A Y!A p.hrrn. so" .r.wr"k .4"W of /rw% to M 2 Wj* loft 5.201 41rMM1 r 1 1r1 E MW ws~RnC1MbM~1. f 51 Alwiwrwle . 4ftbrNkirWWw =9 qbwAwv4a f .] ArlNirl 1 rr~~lb dmiftA Ya000Dt 8 . JA LdYywlb~rorMl4~rY~ !! UaLY~ w~NNI~~~rMl~~w, 3. 117 itMlLl M WOOL S.~ 7~f.~Nll.Cd~llt hld' Pow S! 0/63 Exygen Research Page 116 of 132 p . 116 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 E xnan Platoccl Nvmbri . P00011 3 l F1~r11~1~r~ IMbi 1r.rrt0lMlp _ A7iAY 1/!Llw00 wiiow w i1, R ' Mil ialw! IRdM1Mrl lbne1W IClM l " 7.0 01~Yrtrr l.10 AM~Orwlwpv10i0p.rl01/OOL).~Ofqar0leYp . l.11 'V1Npl~/lliVr{r(1l,C10lflsrri~r . f.st q'~~wMUawrllll !.1! 1SIMI~YR. Y1M+Ww/iir. US C~l~a'ii~ot~wi~ilsf.ye/~JIw~wYrM)OODys { .0 Giloir~/qttit>t)wr l( ArOhU CUlot PrMNr lv W1r.m >fmr81q.11 no x s0 oi sM (tA I-ION007110 p iJ TMVrrM f0'f. to M""=W : 7 rU J1traJr, Arr w Wow 6" MdOmPOMM : Nohow [S G" rlwPM 1br Raw nMLLoid %A fi~ fal~i~ a cs u a 1. s ~s a i.~ t! 7S .3 AD 73 7! 0.1 .~, a! t! !f w {4 iljwFaY~Yra 1l01 (awrsirr~rYterrdrl0~. V Qrrunm Irt+Yr-aWWrWrAa4Uaoaaaa~s. 0.f ArTIc - 2l 01YWt 71M iwwrWM w YrNO r 9 Oft r/ oWM sirpl 0 040 e q uw4o r I</LC OMr 7.0 1Mqi0Mfou 7.1 Yali fY b"I q WpMLSY roft oonAmiM O1.1-# lN Ns hr !!CA 1T. 1Mw ewWba we how" r a'fY so se be awOM in sr. M 9~iiAtA 1[!1(1 q~Ja ArJN Pap Jf ofo J Exygen Research Page 117 of 132 p . 117 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 r r ExYr'd > rOOMd Nm*t: P0001131 ~~r 6w+rr.r . .wwm AV,ti7 y~}pp 0 . _ Ani+& ft 6 6y~1~Y w~ Aaii OW-M) is SnMI by ae ~o.wJa~a ti U~ial~Ewa 1.4i tdta~..lwwrrla .rrYAr.ey .Muaetsaaar a~sa,laa~rw U 1DOpwC ~f.va~. Abram alr,w aq be pAw6 90 anAd N a1 l~.1.~7bd~a~la7.haaa ~.I .1 !1*rr a r& =lain d-1e0 WaL af /F0A by waiyeat 10 q sf rlYW rrrd 4~.'~a~ .6 er pow rY raa. is log r. rnIh aatilla a "'Sol [blEtoa4. 43 .3 A1bwr1.lrNiwda.Yiatwdl/QA1Lr~wlNlnqral sL . 6f Oa 14D rMw. YMalr r dad vMrw or leo wY rwrw laat]!aLlDf{lwtl a M-3 A.01~wl.ANta~Yw&41ftfPP'oAiybyWlyiKID rt.aHr tA rw1 asWr Y a WI wlwa M 100 .ri~ .~.w n a 17SaLL1>!lYada 41a SbAtarMAAiMaolrY~wabawwlfaaw nip wrY ic 424Tddik ir a ra~ pnioi d 6 wattl. ! :t sw6nrt11lrada,laid.r 4.7d L.rcsJM. am1 .aawYYtYMwIw/O.a1M11i. iwiiAYswp*.ai to w.aiwd v eYaio. W Tr 111bar/ s a MAIM waww: 609pwrl a,sWWIaa ~aar a rtd r owii df.~l/Vr iafY b hr6 rieCMd UMVIAN 1-11 W IM 3A lM Za IM ID 16e la JA to We N 16 te uc aa 1 .6 1 t ILI M/a nOrF Ow RlotlY OotMw t 7'C M 6'C ~ 42A ANnaaY r+laww rd ceaawdtlaY of Manluda way 6e prepn! Me" raite ss oleJ Exygen Research Page 118 of 132 p . 118 ~ - - - interim Report #10-Analysis of Fish and Cam Samples Exygen Study No . : POOO1131 sJI) en rMaool ra.e.e roool 13 1 .a~.a... I,aLTfCA6 werfloo 1 Mwn~ 1 wtlp LGIffllft w.+H~wr. vbw~u A) ie 11A " ir.k Lttlp 1.0) 1a& rr A Ka M b wmww (p *Wy 70 w Mw) was ucYrs r k" r rMadYi rd Mi We award aweY IMi41 r lao+ ea.n+rrr(wawrol spin) `"wfb~r ~+osrr rr wM wek . d IOA .i iapen~ ir so asd M.-f /pi w. ~t ~drw rlu b 01 a rt. v .~ .w.r. i1 .1 "wiyljdriMalre .l0allp W wmi 1w Maflonlyr 00164 WOW U at orawlp. low 68 4lrirrwifrdfiwrnqe dwaaiotwqr Mop ralraroab brrs. ralwi 11 .7 AYwurw NEON 6ra bd rMafadl0a$. 11 3 A~aiaaasa~rrlq llrrrlrr4-1dauM PA 7Yaa~r ~ do -ok wing a awwi>t 1}rw dro a lf *1. ' Ili AY6a+Lalrlririaali .kalr-JOaar.a.avdwuuo. *Aim 11.6 co -in 40WROM Dwaf M a Pra M rM s X ni, M #aMr oarAp OW ad ya 7 5 . . , rLat Y lld Gdpor M Gw !a'E arafM (t L f rN by pod" to oL raOMrwl 11.0 1+ Ss ~ouvt+a+aeriYw~ 'Ulm 'Is Dwgwd*mm IJI arr Nr .T i.t of rYrK CMia Z rl. Of *AM ra a paraaa - If*b~/11ra .~Yratta(bralra~r~Sa~y. . 11.11 Aat~a~la+arryAwaw~wt WM80i. 12~ Ci+.r/qp If.1 ij.RlVra*ata,tafai .Wri mirk w10 "at . op4iaw dW LOU" arhm A r3ilYea Ihrrd atMt pew* at ham N a Molr l wYrd!lGAarwwdft aftLaa/wwawwaetr~Mbalmlt aralarNNdruaMrlatrt ItS Aaw~ r1dw11rlinrrabirwtMrerWatM bqpo ry oir da ad ds =Wk M. QiY am M iraapa0 rnw m wq 5.19 arsb a M a alMnrtl % as on" rw of arirpaa ar6w ru> br NJ"" / Oa rWMia{ Of a aR lWrrait y pMMY~aa a~0ad~ l~aatYwql-loa~baaa~l~rawaafdrwafwWwl a iY aaS cJWrl " Mrlai oft be M Kt W hr "~Aw. n~ at Or+M. 17.1 W Sam ww dr6 wawa rr lwwdslfa lirr sfafwi arv . n lnrrM brU a,lMa b War>t/orn oft !k w* ae6 af )aak ww rw s r , Payr id o%6S Exygen Research Pagc 119 of 132 p . 119 Interim Report #90-Analysia of Fish and Clam Samples Exygen Study No . : PQ00113 1 4syj.n Proool Nurba: PM t31 .w.u+ vc&L Nslsoir rr.M.rciMbLOtts w Add **Oj-Qf. JwA Gi a 6a mohd wmwmrWa 1M 4 3 MjLy= 1.) (or ap~iWlW t .~... "I"M 133 faoM AWsr iNi0 so =NW wwOd wtbara Any ua~ls Ur .wr ioN f.a ayW r 69daa 4u Mry .d ...atr..d. UA IYr~~w6YtY 13.1 CWWOMPOG wrt rN a me a(& UMIr we M MP MW Aew a PM a 4(413 OR 1M 413 Ma plrt aellymY r dO RGA rift MrM ile 4w*w Ym Pw on" PIPM80 bIM daAr IlaaiY. ri3 MIA" blob t1!1 Mrir ~lOA rl Wi ~MI~ IW Ni WQ. if 0 11A IC a Yls 0lOA a(waY wr~ t~ 10 y+~ V a asr Mwk a~a~1e ~rt Md W/~1 M~Iw ar ~e M aHOn W . U3 1rwnds rf . "M Oft aY RAW Von eat be iwww 7&t3^ at Vt b /w TAM If a NMer q Iw Wk wYiib A. rw"b *Aft Na arYa at af 40 A rtl he atasrri A+Y MWM 0" so* 70. 13IK /iwU M walwr by M rryn r IirsYa It ft wrsfw r +wr t 13A AW aMtMm Wobd r w i M b tt a~Mteal arYr y oft Ni MrOr wr T . Ow be M-iY/ r Ni aYiY w oriN wlihu sa aeve bw..c Ni WW ..r& arawW. . .rri to MW eo seNdad MW a.ta wrl ll%dvwt at1w NMMNt+ ilaML W 2M w/mWo M Aiw a) Na aYWa atwr gnr%Mi rrc M MM Oe &MM At alidlr n w 1r MI on" OW liwidt am appwp Mr rM r be wa ty .Ow Yakwt qnrhw ad Ni ~rdr r tY wYirtnt e1~I~ iwUMwr~lyr L 134 IIMkWa Ni. Mlwt, tfUrY r wMW v M IN *it u tMr 3s%rilYfrrwlNodai NiwiairiiRas awir~Yww .iqi n wllYrl ar Mr r r art Mw~ed~rL 14.0 QiaNm lt,f UM rAiwi/~rinaalw`wtlraNSaftlAAb~wi(nynnL Ywl so Pak +01 ak i Na MrMA as w (tMr "was" Pw%wtww 0>MW b ft Nr Lya M Oa/as : !lY,U Irl(>,IaJ~-~~~ I Dt : aY.pr how dw Q- OrurY7 qAlA ixwMl ~Mrr w CiYrL ifaswry. A14M SOW- 10 .~art P~rJ7 ofQJ Exygen Research page 120 of 132 p . 120 lnterim Report # 10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Fxyrn ho~ooot )Vumber. P0061171 ZZOIWAL mat" YrrOl~..r ylG~tsAs I~a 1rr .wb +YNIw .*r ~..w s ..r. ot!!OA rl. . q aa.~vaa re r rb,l .~ .Mrr.r wn+..s.r~ ~r t.+..rcx1 [w .~.era.rara ~ ~.wr rm..auu~1 ,iw ..~+..r.e~~ t<t 1!w i Rrl q Wr b u=wn ir wwiM d T[OA 6 .d i. qn .L u #" 60} "OA Rri( O)~ ~4 ww~ld hold? I"1 Pop SQofQS Exygen Research Page 121 of 132 p . 121 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No . : P000113 1 e:y~a rrooea Numbv Pooo ~ u I AMLYTWAL METHOD wisN L"., vreoj fl c KWwf AAr4* M v awri~IW dhrONfMM~r~ MY fROA la f aNt IYrWd tww b Le M{NO A.rr+ .r r..4 .ft- a.ri. .a .rs ~~Do " AIM Qww, PA 16 01 M/ew~ ~ t- t-I S.Ap~ ~alu/w fw :ard r nw lob" LwbK 3,G4 q.lc ww buNw i ~I~w7 Dow vr~.~a.~ ~+ Ws .a...a twtp.os 7 Post S o/E3 Exygcn Rcsoarch Page 122 of 132 p . 122 tntcrim Rcpoct #10-Analysis of Fiah and Clam Samples Exygcn Study No. : P0001131 ex"ea r Ioroea Nwonw. 8000 1 13 1 s.. .r ~w+.urr. aro~") . ~...r~. .b~.o~ra U sup TW aWd is r M r pioN brM WNW r1 rtriw N~Almnonrok ~ii_ ~l 18~ lrlrr~ LWI p/MP "wow a a trar Mr. qwNwr DM~A~rtLClOAtq;onrll rorr rAe. u w~ Lr AMra~lrn~~W~+yprloa Lt Ow~YM~~rrilWwAnY~aMY~Vdr~itrb~WRwKUy A~wWe K 7* lM MbAdobsu d 1.! Mlr~l~{ .~(rrt~ilr~YMLa u w+w4Mvwo.ft rawrw or r ... w .. a....wse .m .rM. r~is ~ r~rra~~w~rar r wrr*srwkr.. ~. X3 &Mb 1WA"ft i OO.~w .a be wOd 1i* r Y. WAPhe oft a Wj 11 Pd44 e.r.rrrmr d.r 4.1 VOW -tV&CSdM 4-2 we.d- SIM 1 46 43 abriw-1lw +mb IA AsriaArrr-X" %OWN an* 43 MrrrrieAW-lfpWAlrfr SA iw MMr M il"vMM S.1 A Y* pm&mrw bpd dw orqM syiY of pumiq q a J oAwY wA" wrr Ir1wM ow" J mum" fN* rL wrwl r~ tw~ Wrilr+e+r (I CMNtt} . 73 A &wl.rwraMrrrtr p t 7J Arb~tli~wwwi Gfyoft aoOM ~ . 7w 59 M[. Wq a rWr MbW V7i.rwrril~.rM. '.! urLwewYpy~ .pl.. .rAlyMw . 5. 6 ar~w~ .+a~i~r.Uuwo.L maa .c> 17 12WILLM boom 311 JdNrlll.CrfiYL Po" LA ie~ O+s oo.iuD p. .riawKtwrdrp.rietiPL 6.I1 Mrll 3o )tva l ft QU a 6er~k^ Un na~awws l u v. N"s ~si .r. Pop AO ayQ.t Exygcn Research Page 123 of 132 p . 12 3 . L. . . . . . -- - s ~---lntcrim Report # 10-Analysis of Fish and Clar_ Sampks Exygen Study No . : P0001 13 1 Eay~ Pmbcd N~sMer }p00i 13t !_a~~_~~~ [ ~ ~~Ahn"rlT1C.LMiT110 0 16 On 3twMd lrM byiC4A6 M! W~ M~i~ 1AN~N~ Ad 1 w saw 1 14 3.13 tMtl~~Mibd4iwir I! ~al . NI~yLw w M M 3000 p~ 40 C`ra~r~W ~ S ; Ar131fyCtlrello/wY([yMr~lei~rYfey,2f~nsSO~r .fM ~!:! p706~fft30) S : Tqmvw~ !0'C fs1 lI UYl = W : 3 w1lAswww A ~ a Wrr rd lkriYNwp? : MrYr l 33 6W~hyre !Mw 4r S1YJoW YA 7V ~il~Yl or s is 013 la 63 7S aj !:0 33 73 0.3 3 .0 ri 7s 0.3 nj u 23 w ywlr YY we li wt . (sm be iww/ a a wreY r 34 M" al p~Mds lwkAiw-~s~i~IdaMwia~wrw AA x..r.ft -nw .n . To Mw mwidm we Ymid a & V* rd my be dry/ ia wrw a "rim 61 IQIG vioa 7.1 )0s ic IWMsm atli*piw W3t W5, wiedy 4 17 ~ 1N Yn hr 1P" Tim dbwr awMirs m wrii r a MW MY MW I. sirird m adr w ipin frUiW OM m !.0 hl mtMl l{m P.O MAN Ph = R61 3~Il Miw~wa nw~ i rMr 4 / wryM y dllK 0.q4 ~ e( rrls Mrs r t0o0 ~I .d .w. ~~rar~ ~wrwtr7M p~n0. wr l J ' Pap6/cf6S Exygen Research Page 124 of 132 p . 124 Interim Rtport #10-Analysis of Fish and Clam Samples Exygen Study .No: ; P000I 13 1 Hmat Iroeoool Nombu : P0001111 Fa,~. .WAt .Yl7cA6>~JYOD 1V~~1~ 1'LON911Lt r... .wr~aota. "IQ M" M Saw All ' >111ab0lI~M/Ot 'RI lt~iri~Vdlk~Nrd~>tWlr f.t.1 Tl~raiMLWltiw~i+1001rIbLaf!lG ~ .~ytlual0 .r drlow -BMW (aOwul Arr/ief) wW /iw o t70 nl -b , ., rafrrlfaaTll~LIDr[MNa (Si A1A pay aL h iWwasMMdPrOAIs I ~rNyYril" r i .t . dds 100 p01rL "Mfr r a!{ wl m Of too .011 MOAMM r . w .l. L ra b. bL A1.7 A41Mw1.lNOMf~wAthadfPOAis - tiyaia0ia01 . . a1d~ 11~L ulrhn M i 6M ~da~ard100 air arMae~ in s lt! ~I.1D/~ Y~M MA lh *AI/ MnNOWr/iA w M M ia owed ma Ole a ~lay~p MC M w tiYh r1 afrcaa~apriod af s axrt1~ M 0r 4a d~qrla f.t 7~rd~ICii~Ar6r f],1 ICIOAA ~~ ~i ra~p~/ ia srerN ~a Mtiw 917 000 "n~ly r a O~Md ~wMK d Wnat eo~iar roN a . . /Im MYanYI OWAONVAM Orirlr Grw+Wa O Iw N L u ta u u u in to too sa lu 1 .0 ni ~7I N too 0. 1 L l i ai ~a 00111110 30 iiSwi. twiwW rylA aal" i='Cti/Cw I 4i MIra f7A MYM tM dr~ d a7wYWr ef dmwmdm OW M pqrN as arYA It0 / md " q lop la~ W d a~lr ~Y~Id dp~fe~' f0 r Ny rw Ydur a Na r aWa W MOal Will M BOrN O11 MOL OIwfM s 4Yrn Nwwaiw(Y mod qi)11 vqdly pNeAwd nmmr re, OM awM 10J 1 .thi MMIM *r ILM allberYe 4tiafts w! MpiM rilt hr wsilird a YW qrlq as PIN 6r 41. paOo. hw+ . Pqi 02 of 0$ Bxygcn Research Page 125 of 132 p . 125 Interim Report #10-Analysis of Fish and Clam Sa:nples Farygen Study No . : PUOU113 1 "a,, Sane Peoeocal Number. P00011 3 1 fqrtlrr~ Nd.t Il.w. NM11N ANAL MC[H01 GM tt M IWlr ~ As{d(Z'FOA)i MasrLL tors by LOOaOa 11 4 M11 4 11+wdi o I l.7 Ilwra 1 aL d=npy i ft a!0 sl. /el'wi7traeseiOMqbw Uwtih a asft wpbr t0 aa1 sk adp. ?M tiM sMwawr vatatw of mr. GW M Stww" dong" am On srVMiaarapWaOn m. 1 .2 AM 10W JYampUratidwMSa(3OA2. C.yy{1tlY 1 03 VaUaA r 4 MiaK ttA Ttsrre t .c of &. .yr oft a OSpa.qY pip .w hag . Is aL 114 Atl3 wLat mosial" 4W lhtaar .l0iubw as w ayalo .Yria. 1id ClwtltlMrttMM 1100tpRAr-3ai OMu 11 .7 Lem" d- tr owwA iw t f0 aL iqu .6k wri6 o6e srt .N ) 3 aLM+4f. 1 12 Qoi1r rt CR f!! rsY~ (1 10 aLt b 1 wift VO ML =wow ~1YrMys~t .K1111,Cw!(~21qiYr} DsaelNtMtrn~dry it-0 (,ct4M~Ua~Yiart:rl/lcwuiyt DYerrir.. :1 .11 !t+ vfO f wt. of s iri Allan 2 nl . d Mrte sq s pduMf 13 W. I 4M* go'M MIN110P aM (!W wlass - 2 fat.). It .tl P.rysa W iydae~ayt CAAAil. Ilk tN ot6s awa rrOdui i mod" OW4 ka0tbtf6d "sob irw/r LO1690 aAra A WbMPoM M adr/ MW panda aU wdaw at Ust1 MOVIE& 1I .3 MI" d!lRQAwrs PO tlKteltYiwLvaataaaaeaeatierioa kwsM rtM irtaYl w~ ~.tltl.t r. 11) Ai a An at drMerir owwwa wrt to 4eWM s M Mrani 0 rAe d W sea UryN R friii saw tw LiMnNwa1 Meraw a~T S-w uw# la As a 1Yrv% a) so** M K Wbntlr strOrY sry M W aA/ a Or t 10illi Y0 at 0 sR 613010111 by MYMMdu Mrdsnq Mqwsi Mry ilO r~i~ (bsr~1 ~r a asmd aK dardrOt) k Ytiw a>aA ONrsWa at s"ft am M on ds d be 64M." in a sr01s st 1 : .5 :SL 6 or dYeid wrwi hr qua1MwNL LiMIt MaAYd ewva re VEM rt *r b M b Ita aia eNlw son tA wrrlyNwk rM "trs 01111*010 it su wCWas asriltirt .yati 3 .3 (K ywal,rl uR~aa)MSa IL SMMb aIMPww *Add nl ON" MWid Aqorr. AMy sry1R tl~.c ~MrsYS/rd I~MII~ rwN L~ ~tlyditMd Yr ~ly~d y,S .Ii Page QJ Q/'6.! Exygen Research Page 126 of 132 p . 126 interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 r- exyps rmlsea Nmba : voool 1 3 1 &" alfwrA 11AW 11rrwY4 117" AK4LLVtWAL MM!> m memo 3a~w by u fwl 17 .0 A~LrwOGri tit ~l~rywsrMwF" d.*raMw bnr Mom fWnapan.K d417 w. The 415 wr prM wWwOw k 0 So 0/ON VA" .d# WC M~l~ irOM ar, ~7~ ~ Ir dwiYw forW ~ 172 JfM00.11mb aw wt orYb MA at LwA pow am do LOQ. U a IWt awrtr MA at 1-NA Vwe am 10 I. Am a ~ 6 m4 ~ MW M 6Mm W M Or<wlpw. wrl fawwwd 17.) lrnwi~lwwal~irt~rfaw~i~~ rb sw~7p.1 WA of iti twiw " Mrr. [ a ewod Oft ii .d id* OW w 1 11 W.N. WA or "now dwY 4 waw"wi Np Is q q wai& 70. Li0li tlr~M M wWw1 Yr fr wYrw M Mwiw It w.wwi ft is w>ML L7A hr ah/s7Yw O rai bad b w * wised wir yy aft on Uuw bw 2w4 ay to maw" bw M w sYabm of do o000oa ana w r .rs. ft l .w arin d .lwfu w.arr ON ON" be wcwwo awd rswa " 70Kd4w walwdrMrr WNW . L)! 7% wriew MWilir !4 M w1Mwio w .w am be am R' awl g w mYa wws rr mom am w.u uw WWAI wp WO Y Who 46 84M b n M wl "Waft anE dc s/wti ar0w Wwwl Y4 Kw+lr MU Mw~WlaN . DA ltwdss lVw Iwww w1N& wl U000 sur .n dill non aft, 34~iIVY~rrbMd~ ffwi~AlMLMrOrilaewYwhewwrlwa ~ wlfilw~ WA M IN r arc M ~wdyW . {M ISIaWiw 14.1 LMl~YM~I~qrWYWrYw6rwwwdTlOAtwOtW .e~a1, Owd w pd* am* w4 Or wdd is Pow n/wla ~wrswM wwrd Mlrw r.{wwl/MM !!oA Awt!Ohi1 IhIt~L .yYmwfl a DF a afipa Yl.mr Dr krrly wWY M trl alum aw dWiM4llOwarwry. AiFPal Irir' 20 W F. w Rdw 4NIW sM bow* ww wo d ZPOA pow I s aauum is w M~Lr N~RY arWYa1M ~wi~ IMORy. Rsw~llly~ [Yiiwil~riw/bl~T~-~A~irdinWR~l(I~a~1 .)) 100 /{) 1el 6! q/63 Exygen Research Page 127 of 132 p . 12 7 . ._- ..~, x. ~~. .~~. Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000123 1 8 "es PMWeol Nw*w.. Fowl 131 rfarA ..~r rM.iwrrvwnr AK~~ hwW +Z AROPW Or*ii .~,:r.~h~r wa ~aa 1 . a M. w i $~ bt.G&Ia la.] III M OONwis r eowwl r rwM*f "pA Me6 r ymL a nv+11wM (Ar1- now ,. .M ..r..(W ` 1~1 .t Per (3 of 65 Exygen Research Page 128 of 132 p . 128 Interim Report #10-Analysis of Fish and Clam Samplcs Ecygen, Study No . : POQ01131 B RESEARC H 3oSe Ra wd, urlw Pt~. 911-m-1as9 SUM COUeRe. PA 16101 Fix b+231-ISM AlrlepolDOr1t N UQbM :_L tr.cow ow ojnao s Eqpen 9bad~r riln+b~r Fooo1 i31 aMm ft* wrr+e.c P~prlof4 bon. 1) AnfAAical Pro=&" SunxrMry 1fW01 7ft Sec9on 9.1 2) VNMcmft n dMWyfatt Pioo odws Ailmw= 1) Add b 8@ ctx1 a) , BaCtlon 9.1 .Q, A*1nMk vwfO lk d afanA~rd~ mry bs uNd a P~Pa Ill 'ON FRAM Ask- d Mock aoMiftm as nsosewy. Atwm O Mvels d fm elcMon .oka" m" rro b. php .na. 2) lmw .+a I~f,p1dp kwk a fi. an .lylw tor ..ch nnabc nry tw Wa r.d d.p.narp pn~~ awY.bM to uaDrsaaor~ ~ b ao~ arWyb oa,oN+YallanR srpeefsd in to 11 1 RATMOU 1) HpFwr oonomhrmn d tdnd n i need b be pnp.r.d In ordv b so* IM wmpN OattlM at hiplrrkvi . 2) ~1r wrt~ st~ r~Nek tor s~~ru a+Rnrn~l !wr ana wnm vh . a++~ IMn spabd. BPMdrq d ft p dRMm*W kv* h M Probcd Puts to WlkSd oon~nMon bwa 1tin IhN dercaon iadt ANo. b wnyk wvrk b tl Qround wv Y r Mnpkr we * apscbd b wN1y uo .d to W.4 MMmird spidnp +w ob wad h the p+aboa. wWnn tw M A S rM /hw srffOn qwtly @aa sd ft pRrh M+wk, @n scaxw* V WA for Now in to bol~ ~ ~ i~.ab ~ o b Its ~r~ IMPACr ON The LOO k 100 npfp fOr all p tarpk d tmd n~rrnd Mr OW M SC00 npk& for a 0.01 mL On d smd n* nrrt son= . d spidr~gIbraMv swtqmpl~srrd M Ow Mrtmar QC waowry dRh a~in be used. OWW w b~ I"M-Ugt 0- .&V !Ulgr R 1 eqq~n cAU i~a~w ~~u ae .l., Ir . ~: . LMPArtr oe WM2 ea= ; . . - ' ,u~n+esrw~n~ ta a. ,~.... .~ Exygcn Research Page 129 of 132 p . 129 Interim Rqwi #l0-Analysis of Fish and Clam Sarnpics Exygen Study No .: P000113 1 RESEARC H 3051 p4m"rdh tkt.e Phow. a14-Y72-1039 Statis CoUe~!, FA 16601 Fac Rt~-i31 156D PROTOCOL AMENDMENT Amendment Number _ 2 E1fiCWe D6W 03I0TId6 ExMn SAsdy Number P0001131 QI M 8tudy Number. p+"1411 None 1) Ropwk pop 110(05 2) Tast AAa0M1rt, pqw 6 d 66: PFOS rwwitlon etonhorrd 499 -:P, 9o. 1) U*wd d arr ieW rpat IrMsrke t "rorls v A ba isswd. 2) PFOS Mansam monNonO may siW ba 499 .a 6Q Elsa 1) Ow 10 to mau6:tie ttas d fis d i i M11~ YMer1m npwl~ wi1 be itRURQ b Mow to eiM~l b no" dah In a rmMrrlNaM mw~~ ~+br 4 tK 2) ihw AM 4000 LCJMSYW syawms datwi to 190 ,a AA PFfis irwvdlor wkh gar swNMV tan the !N a M trrw6a -3b aO - 0, t 1) Th~ eM~nt w~ b~ ~bM b balYr~~d i mon q~fddy . 2) The 480 onbR dRMeMd wlb paMK NnoMIrNr 6mwar. yAM~p lo M W . ~ .s ow If ap~tr~ Deb aoo. .s f -wMw- Of ~y ~aat u.. Ex~n C!W 1~w4r w~ ~ La1WeY vaGOt7Ri ; ACMNWMTNE FORM Exygen Research Page 130 of 132 p . 130 Interim Report #]0-Aaalysis of Fish and Clam Samples Exygan Study No, : P000113 1 ~i-i0-tlli it :11Sv~ Fro~-IFSTON fOWi1dK t T-IN P .OW/101 F-pT RESEARC H 3055 Research DrAR rhofu: 814-272-1034 State Cobgr, PA 16601 Fn: 51+h231-15M DEVIATION FORM X ProJad 1lpedla Comm ____ realty m MaOm Dale d O"men" mm MyW woled s : IM!"t owwron ~ : M can Prod 11 : y m u b o ft a d v e n. aMP I OLP Oar ~~ wk R.F.nncr* : g M d d m O w k d f M T V r m.ftft and s .,~,,~ Pro~oe.l ~r+oa r O; w Nckeaek kpw cm- NA 0877124 INA SOP WOW LA264AA29M Carerkw* : Rgo le IM taco : PIA _ . piolow se.w o,at mntW and forWMd cool WnpMOf&mchrm*kwMlwwWpmAhwww. 0011b01 dam wK not O bb Ym tl. PNI{ vm(Jte l M Uw 001*0110 {}1? iflNpb01 I1/.0 !Ec Cbm 4uw: P4np.ra0on No ~ .p.trh kRpsot on 11w Msyab kw"~ CNent Piqued X O!!w IWhon ia~~.d j MM 1 ~+EP'~s rw~.M~Mor R~q~.n .ie Dlt~ or ~ lhA~+' GUOVAnUMCt .b 8paror caw uaa spornorMWolp.tnK ow Exygen Research Page 131 of 132 p . 131 Interim Report #10-Pnalyeis of Fish and Clam Samples Exygen Study No . : P000113 1 ee-ie-2eMJ 12 :34pa iror*sTql fOURIolls + r-314 r .014/ea4 h437 - ~a 3056 Aeaea idh Drive Phone: 814.272-1039 Ste" WW", PA 16Q01 Fa= 514-231-1580 RESEARC H DEVU1llON FORM gem* X Pr~ apaalie OwjiNbn FaeA qr Dariatlon 1 f Dew of Ooauno a ; 1 Tro4 Exypan Project * : P7i01p1131 DwiMlonY : 313 Clentp"Odo : MA Remo it : OP-Mt 4/,.W n 9lNO ft Md O m P Ptomoot Wqiod X OLF cow US: 2M .20 Saclbn d.2.3 Ndaboak wfihnor NA x SOP Loghw' : NA Can4einer 0 : ~, NA latt : NA 114 (30li ~ a kl TOkw) w w epw11 tl1f eqiritl0n dil+e d QZM 3106, but RE544 (TaM~) uMd b malor'1.T114 ~hd a+ 4?/N104, iLZ114 was u~d to a~an0ond pauwal+a prapNsd for 11m Mh ak c9on from 11/ZrN4 dMbaph 01A07A5. cause: _ Ptipuatlon _ Maysis _ IrntrLma,c ,,_,_ Cpset R44LV a JL otl,er nogatlva iepact am ft s0idy. Toluene was used a4 a a solvent tor to piassw i ra praparMta+. OUnatl Wkiaroshna, which is the cmbq ayant rran not aW rod. 0w+00m lesuwd . E aypwi .nt Dab M ~y~Y ..~.~~C ~.r~a ..n ~ cim ' Spoftw ~f ~ cow oiainyAaunne. Dab Sponsor AlruManm Otf Exygcn Research Page 132 of 132