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INTERIM REPORT #110 - Analysis ofFish and Clam Samples STUDY TITLE Analysis of Perfl uo ro butanesulfonate (PFBS), Perfluorohcxancsulfonatc (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 DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 STUDY DIRECTOR Jaisirnha K w ari 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 LABORATOR Y Exygen 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 : 651-733-6374 PROJETC Protocol Number P000113 1 Exygen Study Number P0001131 Total Pages : 132 p. 2 Interim R -.port #l0-Analyais of Fish and Clam Sampits Exygen Study No . : P000113 ] GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0001131, entitled "Analysis of Perfluorobutanesulfonate (PFBS), Perfluorflhexanesulfonatc (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," conducted for 3M Co;npany, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR. 792 by Exygen Research, J Fnlaher ty rincipal Inves tigator Exygen Research s'9 v6 Date IUAU' l Jaisimha 1 esari P .-, DEE Study Director Weston Solutions, Inc . Date r V d S Michael A. S ro Sponsor Repr4entative 3M Company 1L 17~i Da e Exygen Research Page 2 of 132 p. 3 Interim Report #I O-Analysis of Fish and Clam Samples. Exygen Study No . : P0001131 4U.ALITY ASSURANCE STATEMEN T Exygen Research's Quality Ass urance Unit reviewed Exygen Study Number POW] 131, entitled, "Analysis of Perfluorobutanesulfonate (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 Earygen Research's Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported to the Exygen P rincipal Investigator and Management and to the Study Director . hm IS . Raw Data Review and Interim Analytical Report Review 26. Raw Data Revie w and Interim Analytical Report Review Date Reported to Date Reported to Date Principal Exygen Date Reported, Insnected Investigator Management to Study Director 08/01 -05105 09/20/05 09/21/05 09/21/05 05/03/06 05/08/06 05/09/06 05/09/06 . Ly haffer Tec cal Lead, Quality ce Unit d'Sd9~L Dat e '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 . : POOQ1131 CERTIFICATION OF AUTHENTICIT Y This interim report, for Exygen Study Number P0001131, is a true and complete representation of the raw data. Submitted by. Exygea Research 3058 Research Drive State College, PA 16801 (814) 272-1039 Principal Investigator, Exygen : hn Flaherty Vice President Exygen Research Date Exygen Research Facility Management : Richard A . President Exygen Research uu 'l-44lN- 7466 Date Study Direc r, Weston Solutions, Inc . Jaisimha esari P.E., Weston Solutions, Inc. DEE J Date Sponsor Representative, 3M Company- Michael A. Sat/bro Director of R gulatory Affairs 6-11 O~, DatAe , I Exygen Research Page 4 of 132 p. 5 Interim Report #10-Analysis offish and Clam Samples Exygen Study No .: P0001131 STUDY IDENTIFICATION Analysis of Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Per#luorooctanesulfonate (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 TBST SUBSTANCE : Perfluorobutanesulfonate (PFBS), Peifluorohexancsulfonate (PFHS), and Perfluorooctanesulfonate (PFOS ) SPONSOR: 3M Company 3M Building 0236-0 1-B10 St. Paul, MN 55I44 STUDY DIRECTOR: Jaisimba 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 .port #l0-Analysis of Fish and Clam Samples Exygen Study No .: l'000I 131 PROJECT PERSONNE L 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 : Nigne ~ John Flaherty Vice President Karen Risha Laboratory Supervisor Paul Connolly Technical Lead-LC1MS Amy Sheehan Associate Scientist 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 Ammerman Sample Custodian Eric Edwards Sample Custodian Edward Cams Sample Custodia n Exygen Resemh Page 6 of 132 p. 7 Interim Report #10-Analysis of Fish ard 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 AtTfHENTICTTY . . . .. . . . . . . . . . . . .. . . . . . . . . . . . . . . . . .. . . . . . . . . . .. . . .. . . . . . . . . . . . . . . . . ... . .. .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 Fortification Solutions . . . . . . . . . . . . . . . . . .. . . .. . . . . . . . . . . . . .. . . . . . . . . . .16 6.3 Chromatography . . . . . .. . .. . . . . . . . ... . .. . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . . . ..17 6 .4 Instrument Sensitivity .. . . . . . . . . . . . .. . . . . . . . . . . . .. . .. . . . . . . . . .. . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . .. . . .. . . . . . . . ...17 6 .5 Description of LC/MS/MS Instrument and Operating Conditions . . . . . . . . . . . .. . . . . . . . . . . . .. .17 6 .6 Quantitation and Example Calculation . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1 8 7.0 EXPERIMENTAL DESIGN .. . . . . . . . .. . . . . . . . . . . . .. . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . .20 8.0 RESULTS . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . ... . . . . . .. . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . ... . .. . .20 9 .0 CONCLUSIONS . . . . . . . .. . . .. . . . . . . . . . . . .. . . . . . . . . . . .. . . . . . . . . .. . .. . . . . . . . . . . . . .. . .... . . . . . . . . . .. . . . . . . . . . .. . . . . . . . . . . .. .2 1 10.0 RETENTION OF DATA AND SAMPLES . .. ... . ...... . ... ....... ... . .. . . ... . ... .... .... . . ..... ... ....21 Exygen Research Page 7 of 132 p. 8 Interim Report #10-A,nalysis of Fish and Clam Samples Exygen Study No . : P800113 t LIST OF TABLES ba Table L Summary of PFBS, PFHS and PFOS in Fish Samples ............ .... .... ................. ..23 Table II. Summary of PFOS in Re-extracted Fish Samples ................... ... .............. .... ......30 Table M. Summary of PFBS, PFHS an d 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 VI. Matrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples . ......... . .... .. .49 Exygm Research Page 8 of 132 p. 9 Interim Report #l0-Analysis of Fish and Clam Samples Exygen Study No. : POOO 1131 LIST OF FIGURES Figure 1. Page Typical Calibration Curve for PFBS in Methanol ......... ... .... . ............... .. ........51 Figure 2. Non-Extracted Standards of PFBS in Methanol, 0.0005 glmL and 0.001 g/ml, Respectively... ............. ............ .......... ......... ... .... .......................52 Figure 3. PFBS in Control Fish Blank, 0.00625 }iglmL Fortified Control Fish Spk A, and 0.025 ghnI, Fortified Control Fish Spk B, Respec tively . .... .... ............. . .......53 Figure 4. Ch romatogram Rep resenting a Fish Sample Analyzed for PFB S (Exygen ID: C0049478, Data Set:061605E) . .................. ........... ....................54 Figure 5. Typical Calibration Curve for PFHS in Met3wol....... ....... ........ .... ....... ...... ...55 Figure 6. Non-Extracted Standards of PFHS in Methanol, 0 .0005 g/mL and 0.001 glml, Respectively ............................ .. ... ...... ...... ................ ..............56 Figure 7. PFHS in Control Fish Blank, 0.00625 g/mL Fortified Control Fish Spk A, and 0.025 gJmL 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-Extracied Standards of PFOS in Methanol, 0 .0005 g/mL and 0.001 g1mL, Respe c tively . . . . . . . . . . . .. . .. . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . .. . . . . . . . .60 Figure 11 . PFOS in Contro l Fish Blank, 0 .00625 gJmL Fortified Contro l Fish Spk A, and 0.025 g/mL Fortified Control Fish Spk B, Respectively ................... ...........61 Figure 12. Chrvrnatogram 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 PW Appendix A Study Protocol P0001 131(Exygen Study No . P0001131) with Analytical Method V00U1783 : "Method of Analysis for the Determination ofPerfluorooctanoic Acid (PFOA) in Fish and Clams by LChV1S/MS", Protocol Amendments I and 2, and Deviations 2 an d 3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .63 Exygcn Research Pap 10 of 132 P . 11 Interim Report #1 0-Analysis of Fish and Clam Samples Exygen Study No . : P04(?1131 1 .0 SUMMARY Exygen Research extracted and analyzed fish and clam samples for the determination of perfluorobutanesulfonate (PFBS), perfluorohsxanesulfonate (PFHS), and perf]uorooctanesulfonate (PFOS) according to Exygen Method V0001 783 (Appendix A). The limit 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-one 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 11 and V . Analytical results and assessed accuracies for the analysis of PFBS, PFHS and PFOS found in fish samples are summarized in Table I. Analytical results and assessed accuracies for the analysis of PFOS found in the rrtextracted 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 Tsble III. Laboratory matrix spikes that were in the appropriate concentration range (primauy concentration less than three times the spiking level) were used to calculate the assessed accuracies . The average percent recoveries standard deviations for PFBS. PFEiS, PFOS in fish samples were 79% t 13%, 94% 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 ro-extracted fish samples was 109'/o 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% t 10%, 93% t 13%, and 73% t I6%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI . The sample IDs assigned by the client 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 DLl - Downstream Fox Creek mouth LOI sampling location LOC-1 DBC = Bakers Creek mouth DOU = Cove at 3M WWTP outfal l 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 st ring defines the general category of the biota sample and the sampling round where : ECl = Fish sample first round 101 = 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 catfish (Ictalurus punctatus) MS = largemouth bass (Microp#erus salmoides) CF = Asiatic clam (Corbiculafluminea) F = Filet tissue sample W = Whole body sampl e 001 through 005 = ample number within the sampling area and sample type The fourth string (single character) additionally defines the sample type where : 0 = Primary field ample 1 = Field duplicate sampl e 2= Equipment rinseate blank sample The fifth string defines the sample preparation date in YYMMDD fornnat . Examples of this sample ID system are: Sample DBC-FOI-a'F004-0-041021 is the filet tissue sample prepared on October 21, 2004 from the fourth channel cat fish collected at the Bakers Creek mouth sampling location. Sample DLI-F0I-MSW002-0-041104 is the whole body sample prepared on November 4, 2004 from the second largcmouth bass collected at the Fox Creek mouth sampling location . 2.0 Q ~ The objective of the analytical part of this study was to determine levels of perEluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) in fish and clams according to Protocol P0001131 (Appendix A) . Exygen Research Page 12 of 132 p. 13 Interim Report #10-Analysis of Fish and Clsm Samples Exygen Study No . : P0001131 3.0 INTRQDUCTI0N This report details the results of the analysis for the determination of PFBS, PFHS, and PFOS in fish and clam using the analytical metho4k,entitled, "VOQ01783 : Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by LCIMS/MS." The study was initiated on November 05, 20}4, when the study director signed protocol number P0001131 . The analytical start date for this interi-in report was December 27, 20D4, and the analytical termination date for this interim report was April 17, 2006 . 4.0 ANALYTICAL TEST SAMPLES Forty fish samples (Exygen ID C0048126-C048165) 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, Inc . Twenty-six fish samples (Exygen ID C0056354-C0056479) were received on dry ice on January 1 3, 2005 from Tim Frinak at Weston Solutions, Inc . Six clam samples, consisting of whole clams from each sample site (Exygen ID C00564$0-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 C 0054391) . 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 ?AATERIAL 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 Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 rn und Exygrn Inventory No . j~t Pu rity 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 10/31/0 7 The molecular structures of PFBS, PFHS and PFOS are given below : PFBS Chemical Name: Perfluorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (C4F9SO3-K) Transitions Monitored: 299 -~ 99 Structure: 03 F F F PFHS Chemical Name: Perfluomhexanesulfonate Molecular Weight: 438 supplied as the potassium salt (C6Ft3SOsK+) Transitions Monitored: 399 -* 80 Structure : F F F F F 1? F- 03 F4 F F F PFOS Chemical Name: Perfluorooetancsulfonate Molecular Weight: 538 supplied as the potassium salt (CeF l7SO3R ) Transitions Monitored: 499 a 80 Structure : F F 1~ F 03- F F F F F F Exygen Research Page 14 of 132 p . 15 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001 131 6.0 DESCRIPTION OF ANALYTICAL METMOD The analytical method "V0001783 : Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clam 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 scaled 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 ailanized by first rinsing the flask with 30lo dimethy1dichlorosilane 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 grains silica gel, 2 grains 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 clean 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 Ekouction 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 Exygen 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 pmcipitate. The samples were centrifuged for - 10 minutes at -2000 rpm. The supernatant was then loaded onto the conditioned clean-up column fitted inside the silanizod pear shaped flask. The eluate was collected in the silanized peat-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 tissumizer 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 - l hour. The samples were centrifuged again for -10 minutes at -2000 rpm . The supernatant was then loaded onto the same clean-up column . The eluate 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 sample 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-gram portion of sample C0048133 (DMC-FOI-MSW0010-041216) was used. All other samples were weighed out in 5-gram 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 V0001 783 . The stock standard solutions were prepared at a concentration of 100 g/mL by dissolving 1 0 mg of each of the standards (corrected for purity and salt content) in methanol. From these solutions, mixed 1 .0 ghnL 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 1 0 mL of the mixed 1 .0 g/mL fortification standard and bringing the volume up to 100 mL with methanol, a mixed 0.1 gfmL fortification standard 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 g/mL by dissolving 100 mg of each of the standards (corrected for purity and salt content, if necessary) in methanol . From this solution, a 100 g/mL fortification standard solution was prepared by taking 10 mI. of the stock and bringing the volume up to 1.00 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 glmL fortification standard was prepared . By taking 10 mI, of the 10 g/mL fortification standard and bringing the volume up to 100 mL with Exygcn Research Page 16 of 132 p . 17 Interim Report #10Analysis of Fish and Clam Samples Exygen Study No . : P0001 131 methanol, a 1 .0 g/nzL fortification standard were prepared . By taking 10 n1L of the 1 .0 g/mL fortification standard and bringing the volume up to 100 mL with methanol, a 0.1 ug/mL 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 . (ug/mI.)' (m-) (ML) BlmL) 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 i 00 0 .0025 0.01 10 100 0 .001 0.005 10 lU0 0.0005 1 of PFBS, PFHS and PFOS The stock standard solution and all fortification and calibration standard solutions were stared in a refrigerator (4 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/mI, of PFBS, PFHS and PFOS : 6 .5 Description of LGMS/MS Instrument and Operadug Conditions Instrument: API 4000 Biomolecular Mass Analyzer Interface: Turbo Ion Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 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 #l0-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 HP Column Oven HPLC Column: Thermo Fluophase RP, 50 mm x 2 .1 mm Column Temp. : - 30 C Injection Vol .: 15 L Mobile Phase (A) : 2 m .M Ammonium Acetate in water Mobile Phase (B): Methano l Time L.nl 1s.A 0.0 65 1 .0 65 8 .0 25 10 .0 25 11 .0 65 18 .0 65 Total run time : - 18 min %e 35 35 75 75 35 35 Flow Rate : 0.3 mUmin Ions monitored : A nalyt Mode PFBS negative PFHS negative PFOS negative Approximate Transition BM=ion Titno MQnitortd nun 299 -* 99 -4.7 min . 399 -+ 80 - 10 .8 min. 499-+80 - 12 .9 min. 6.6 Quandtation and Example Calculatio n Fifteen microliters of sample or calibration standard were injected into the LGMSlMS . Th e peak area was measured and the standard curve was generated (using i/x fi t weighted linear regression) by Analyst software using six concentrations of st an dards. The concentration was determined from the following equations. Equation 1 calculated the amount of anatyte found (in nghnL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software p ro 8ram - ESluation, 1 Analyte found (ng/mL, wet weight) - (Peak area, - intercent) x DF slope Where : DF = Dilution Factor, factor by which the final volume was diluted, if necessary . Exygea Research Page 18 of 132 P . 19 Interim Report # 1 0-Analysis of Fish and Clam Samples Exygen Study No,. : P()441131 Equation 2 was used to convert the amount of PFBS, PFHS and PFOS found in ng/mL to ng/g (ppb) . Equation 2 : Analyte found (ppb, wet weight) _ fAnalyte found (ng/mL) x final volume Q MU 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 (%) a ianalvte found (nQ/mL) - anaiyte in cont rol Lng/MT;)) x l 0(r/O 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 quantifi able) final volume (mL) - 2 sample weight (g) = 5 From equation 1 : Analyte found (ngJmL, wet weight) - I280750 - 30701 x 1 13100 From equation 2 : Analyte found n818 (ppb) = 21.2 ng/mL (21 .2 n I x~MW 5g = 8.48 n g/g (ppb) Exygcn Research Page 19 of 132 p . 20 Interim Report # 1 0-Analysis of Fish a nd Clam Samples Exygen Study No .: P0001131 From equation 3 : . % Recovery = i$,4$ nQlst - 0 ns*11) x 100% to ngtg = 85 lo 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 fish contained four samples, one set of fish contained seven samples, and twenty-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 contained nine samples . One set of clams 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 m,alxix . Exygen recognizes this and great care has been taken to integrate each data set consistently. Analytical results and assessed acc uracies for the analysis of PFOS found in the re-extracted fish samples are summarized in Table H . Analytical re s ults and asses sed accuracies for t he 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 fi sh samples were 79% 13%, 94% 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'/a Fortification recoveries for PFOS in the re-extracted fish samples are summarized in Table V . The average percent recoveri es standard deviations for PFBS, PFHS, PFOS in clam samples were 84% 10!0, 93% 13/., and 73% 16%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI . Exyscn Resmvh Page 20 of 132 p. 21 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P0001131 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 signcd 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 . Exygcr+ Research Page 21 of 132 p . 22 Interi m Report #10Analysis of Fish and Clam Samples Exygen Study No .: P000113 1 TABLE S Exygen Research Page 22 of 132 p . 23 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No. : P0001 13 1 Table I. Summary of PFBS, PFHS and PFOS in Fish Samples Ex JD C4 EuHonata PFEi CO suNanefr PF115 Ca iuNandM FFOi P ft womb CMbnt Foqattl Aocur my FovW Accuracy AaMYy Awsuod Fourw Jlodiracy samow !D tow wewt +J-% ,rtrt d-% wr,w. N-% CA049128 C00461 25 Rep 0 L3-F014PF001 -4041021 0.309 40 0L34901 4+F0014 .0 11021 0.318 40 No 30 5. 18 30 NO 30 3.84 30 <',0048127 0LS/014 PP002-0-041021 0.265 40 ND 30 4 .18 40 C0048127 Rap DL.3,F014 P'PD0240-01102 1' 0.38 2 40 ND 30 4.50 40 C0048128 DMC401 4PF001-0p41021 0.390 50 NO 60 7 .40 60 COMM Rep DAlGF01IPF001-0 -041021' 0.388 50 ND 60 8.9E 60 C0048129 DMC4 0 14PF00940 041021 0 .712 30 ND 30 14.1 50 G0046129 Rep 0IdC-F01-1PF002-0-041021' 0.792 90 ND 30 17 .0 50 C0048130 DA1C-F014PW00 1 41-04/021 1 .08 40 NO 30 70 .0 40 C0018130 Rap ONC-F01-IP!'V001 4 041021' 1A8 40 0.297 30 58 .4 40 C0048131 D5I 0-F01. P N0024441021 0 .968 50 ND 30 34 .4 30 C00 " 131 Rap DINC-F014PW002-04041021 1 .34 50 NO 30 34.2 30 00048192 DU C-F0I- 4SYV001 -0-04 1021 0.218 30 0.524 30 270 30 00018152 Rep DMC-F01 ~001-0-041021' 0 .202 30 0.484 30 2 90 30 00048155'' DMC401 49BM 002-0-041021 Ap" 30 ND" 30 530 30 C0046133 Rap" DiAG4 01- 48W002-0 -041021' NO` 30 N 0" 30 SIB 80 00049 134 0 0048 134 Rep 012f014PF001 -0441021 0 .860 30 ND 40 3.46 60 0l2-F01-PF001-0-041021' 1 .00 30 ND 40 2 .86 @D 000/8135 00048186 Rep 0L2-F01 4 PF002-0-041021 0.818 50 ND 40 4.72 90 0L2-F01PF002-0-041021' 0 .962 SD ND 40 5.04 50 COMM 00048138 Rep D1.2,F01 4Pf003-0-041021 0.24 7 DL2-F0 7-PF003-0-041021' 0.210 30 ND 30 2 .01 30 30 ND 30 2 .08 30 00048 137 0l24 01 4PF004-0441011 0 .310 40 ND 30 4 .52 40 C0048137 Rep Dk .2-F01-IPF0044-011021 0 .380 40 ND 30 4.12 40 00018138 QL2-F01 aPF005 -0,041021 0 .335 40 C0048138 Rep OL2-F01-PF005-0-04 1021 0.518 40 NO 30 Z 48 30 NO 30 240 30 C0(}18130 DL2-F01N'W001 -6041021 0 .528 30 ND 30 6.86 30 C00 "1 3p Rep D124014PW001-0-041021' 0 .400 30 ND 30 8.17 30 00048140 DL2-F01 4 SF001 -04041421 0.335 30 ND 30 1 7.2 30 00046140 Rep D1.2-F01-118F001 -0- 041021 0.348 30 ND 30 87.8 30 C0048141 Ol.Z-F01 4A8F00241 04102 1 0 .406 40 ND 30 84 .6 40 00046141 Rap 0l2401 4AMM-0-041021' 0.586 40 ND 30 98.4 40 C0048142 0L2f01-M6F00340-041021 0.418 40 ND 40 41 .8 40 00048142 RRap Dl2401-41SF0030 ,041 021' 0.376 40 NO 40 40.0 40 C004614 1 Ol2-F'014dSF00 4-0-041021 0.345 00048149 Rep D1,2-F01 4 18f004 4 041021 0.349 30 Na 30 no 30 30 No 30 832 30 %aaoawn owonc.t. 1 .0 p of srmpN two wor w*w0w Muwd of 6.0 a . ND a N01 dataC4W ai or a0owa Lim* 0( QuantltaNOa Mich b 0. 2 a" (wN wlpht). ND" s Not dsMO*d 61 or above tJmt of QmUNBeebn rhid+ w 1 .0 nptp (+wl wevn} NR a Not npOAW d a b qumYtr eoMrol tMUR Mm. Exygen Rcsaarch Page 23 of 132 p . 24 Interim Report #10-Analysis of Fish and Clam Satnples Exygen Study No. : P0(}0113 1 Table I. Summary of PFBS9 PFHS and PFOS In Fish Samples (continued) C4 suron,o. PM C8 suUoo .a PFNS Co swronw nrOs EXYW ID ,cw,,1 ~ '"isid ,~r A"* Avow-ow e .,D Aa"'ct' F`"'d Aoq~rapy Found Aocur .tsy m + & x +Mlt K - x ,v.l IM . (+/-%) C0C0408104448R14e4pOOL1t1-F-F001144PFF00010-01644-1002o1 41002A 13 O2 A23 8 0 300 0.251 30 33.4 40 .252 30 32e 40 C0048145 DL 34FO14 PF003fi -041021 0. 448 30 ND 30 C0048145 Rep 0t .3-F01 4PF0030-041021 0.440 155 30 30 0.226 30 3. 36 30 00018148 Ol3-f01dPFOp 4-0-041021 0.784 40 NO 30 0.382 30 C0048146 Rep DL 3-W14 PF004 -0 -041021 0.900 40 ND 30 0 2 0 30 C0048147 C0048147 Rep 013-F01-4PF005.0,041021 1 .63 80 ND 0L3-F01 4PP0030041021 1 .07 80 NO 30 5.48 40 30 3,8 4 40 C0C040084184184R8 pD8DC6-CF-F00114-UP'FF000104)1.0440140102211 11 ..3 34 8 5 60 0 0 0..86 9283 0030 NN RR NN RR 00048140 D6GPo1 4PW02-0-041021 1 .43 SO ND 30 110 30 C0448149 Rap 09C401-IPF002 4.041021 0.758 60 ND 30 109 30 00C0408013408R 16a0pD0BCBGFF0011d4PPFf0000330-40X-1004120121 00..9905 52 5 600 00.628 ./ 41 33 0 0 N NR R N NRR C0048131 DBC.F0I .PWO01-0.041021 0.864 40 2.21 30 NR NR 0 0048131 Rep D8C-F01 4P w001-0-041021 0.508 40 2.20 30 NR NR 00048182 O8G 0i-PW002.0-041021 0 .700 40 9.12 30 NR NR 00048152 Rep 08 0 GF'01-1PW002-0-041021' 0.736 40 8.95 30 NR NR C00004081186135R3ep 08CD-8FC0-F10-I1P4WPW0000334-0--004411002211' 00..773805 3300 87..4478 3 300NN RRNN RR 00048164 00048184 Rep DOU-F01- PF0014.041021 4 .88 D0U-F014 PF001 -0.041021' 4 .24 00048156 DOU-F01 4PF002.0 .041021 8.78 00 048155 Rep DOU 4 01 4PF0020,011021* 8.28 40 1 .02 30 NR NR 40 0.972 30 NR NR 40 0 .79 2 30 NR NR 40 0.720 30 NR NR C00040801413'1i656Rep DODUOUF-0F10144PPFP0000334.0440141012 10921 55 ..3 98644 0 0 11 ..0 02 2 3 30 0 N NR RNN RR 0 0C0408013478R1e5p7 DOD 0UU--FI00114-IPPFF000044--00--004411020121 50..2812 3 30022 ,33 8 0 330 0 NR NR NN RR C000048014588R1O5p8 DDO0UU--FF001144PPFF000055004-04411002211' 44 ..35 86 3 30 0 0 0..80 058 3 30 0 N NR R N NR R C00481 59 D0U-F01iP+N0014041021 2.89 C,0048189 Rep DL1U,F01-IPW001 -0-o11021' 2.81 30 0.0 0 30 NR NR 30 OA64 30 NR NR C0C040810840 8Re1p00DD004UJ --FF001141 PPWVV00002-40.004 411002211 1198 ..4 3 S 6O 0 3 8..8709 30 NR NR 30 NR NR 00018181 DL2-FD1, 481NOD1-0-041 02 1 0,03 30 NO 30 190 50 C0048161 Rep 0L2F01-MA 8W0014041021' P.O 30 NO 30 1 20 50 C0048182 012-F01.IWBw002-0.041021 NO 30 NO 00048182 Rop DL2-F01 44SW002.0-041021' NO 30 ND 30 102 30 30 100 30 nAbWWWV DUp*Atf ND = Nd deier,wd mt or above Unit of C1u &ntl18tipn rRk1+ is 0.2 nyp (wet weiqhq. NR - Nd ie0orrd due b qi ft oaWW r~wl! (iMxM. Exygen Raweh Page 24 of 132 p . 25 Interim Report #10-Analysis of Fish and Cl .am Samples Exygen Study No . : P0001131 Table I. Summary of PFBS, PFHS and PFQS In Fish Samples (continued) ExWW D CMnt D G :wtoAw 10M Ce 1Mrre+,u. rsN: cs turtnw "Do 0WfW@W*UbMft#Q0tIf Malyt4 ' Aas"W MdyY W .sW Atsfr ft" Aoownoy Fou+d lbpxrtcy Fard Aoaxltay i~ftl nr wt *6 % +ww w N- % wM ra +r.1i 00046163 DL2-FD14A8W003-0-0410i21 ND 30 NO 30 02 .4 30 C0048163 Rep Dt .2-F0145W009-0-04102/' ND 30 ND 30 91 .6 30 C0046164 0 L2-F01441W0044i-011021 NO 30 ND 80 88.0 30 C00461A4 Rsp F X240I-MSWOOi-0-041021 NO 30 ND 30 94.8 30 C0046165 0L2-F01-M8W006-0-Ot1021 NO 30 NO 30 166 30 0004816S Rp O12^1 -MSNf000-0411021' ND 30 NO 30 174 30 00049450 D8C.F01- 1014WO014-041104 0.680 30 6.32 30 NR NR C 004"W Rep D6t:F01 4A3W0014 041104 0. 462 30 8. 32 30 NR NR 000+9451 D8GF01-MSW0020441104 0.808 30 3.43 30 NR NR 000400 1 Rep OBC-F01 416W002-0-041104 0.884 30, 3.36 30 . NR NR 0004MO452 000-FQt 4M84M003-0 -041104 0.660 30 3. 62 30 NR NR 00049452Rp DBC-F01 4ABWOOS0041104 0.784 30 3.8 4 30 NR NR 00049153 D0C.IF01 44W004-0600 104 0.864 30 9.72 30 NR NR C0049433 Rep DBC.F01-118W004-0-041104 0.880 30 9.80 30 NR NR C0049451 090-4 O1 -h1.RW005 -0-041104 0.632 30 277 30 NR NR 00049454 Rep DBC-F01 MI8W005 a-641104' (LOU 30 2,86 30 NR NR 00049436 08C-FO14A8F001 -0-041101 0 .820 30 366 30 NR NR 00049138 Rep D8C4/'01-MSF001-0-041104' 0.786 30 3.48 so NR NR 00049486 D RC-0t-N8 002.4{141104 0.786 30 1 .94 30 NR NR 00049458 Rep O8GF'01 4A8F002-04341104' 0.780 30 - .1 .90 30 NR NR 00044457 D6C-F01 4P8 004-0-041104 0.604 30 0.584 30 142 30 00 049467 Rep DBC-FOtIF'F004-0-0411041 0.520 30 0.510 30 . 1 62 30 00049466 080-F01 4Pf006-0-041104 1.80 30 21 6 30 NR NR 00049458 Rep 08C-1:014'F00 5-0-041104 a .94 30 218 30 NR NR 00 049 484 OBC-F01-8'4Y004 -044 1104 0.484 30 3.28 30 NR N R 00040459 Rap D9GF014 P1N004-0-041104 0.444 30 3.21< 30 NR NR 000 49460 060401-tsWt0064i141104 0 .572 30 . 2 .10 30 NR NR C0040160 Rop D8K'.F014P4I005.O-041104' 0 .532 30 210 30 NR NR C004061 . DOU-F01 4PW003-0-041104 00049481 Rep D OUF01-pW0034041104' 3. 12 30 6 100 30 NR NR :3.06 30 5 .92 30 NR NR 00049462 0OU *014PVV004fi-041104 3.49 30 7 .12 30 NR NR C0049462 Rep DUU-FOtIPW0040441104` 3.1 1 30 0 .84 30 NR NR 00044483 DOl/-F01 4PW006 .0-041104 2.97 30 5.12 30 NR NR 0003 0463 Rep DOl!4 01-113W006-044 11040 2.00 30 5 .32 30 NR NR 00 04994 DL2-F01-PW0024041104 1,04 30 NO . 30 8 .2U 40 00049184 Rep DI.2-f01-4 PVY0024041104' 0. 980 30 ND 3D 6 .80 40 00049465 Dl1-F01-MSW0014441104 1 .20 C0049465 Rep 0 l.i-f01-M81N001 -0-041104- 1 .24 30 0 .886 30 NR N R 30 0 .231 30 NR MR 1aUa 04ry Dupkob NO = Not 4WCMd at or above i.#nit d OuYndtaNon which is 0.2 nplp twat waigttl MR Wae vsposw On to qu aMty oaria owrt Iw~nr. Exygan Research Page 25 of 132 p . 26 Interim Report # l0-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 Table I. Summary of PFBS, PF HS and PFOS in Fish Samples (continued) CAW C4 iuMoMBb .Fp CO surbrltl. PFMa d eulro"ut. lF06 ~ n . *..aW...w A"* Aaemd *A A faW AearWy Found AodxWy Found Aoairacy $Bflt 0 hft)wa*t N- % we M 01-%) w~t w. +! % 00049488 Dt1-M14ASW002-0-0411D4 1 .30 30 1 .72 30 NR NR C0049488 Rep OL1-i01-MSW002-0-041104 1 .15 30 1 .31 30 NR NR C0049487 0L1-F01-MSNf003-0-041104 0.600 30 1 .13 30 NR MR C0049467 Rep 0t.1-F01-iY{SW00}0-241104 ' 0.528 30 1 .14 30 NR NR 00049488 DL1-M141SW004-0-041104 1 .22 30 C0049488 Rpp Dl1-F01-MSW004-0aJ41104' 1,12 30 0 .908 30 181 30 0 .880 30 188 30 C0049489 DL1F01-MBW006-0,041104 1 .22 30 1 .18 30 MR NR G0049460Rap DL1-F014ASWOO"041104' 1 .20 30 1 .18 30 NR NR C0049470 DL1-P01-M9f001-0-041104 NO 30 0 .315 30 293 30 00049470 PAP DLi-F10144P00i-0-041104 NO 30 0 .299 30 307 30 00044471 DL1-F014A8F002-0-041104 ND 30 0 .824 30 NR NR C00 4a471 Rep [X1F01d11&F002-0-041104 NO 30 0 .604 30 NR NR 0049472 061-F01-M$F003-0-041104 0 .203 30 0.552 30 NR NR C0440472 Rep OL1-f0f-M8F003-0041104' NO 30 0 .876 30 NR NR 00049473 OL1-F01805F0044041 104 NO 30 0.532 30 NR NR 00049473 Rep Ol14 :01448F004-0-041104' NO 30 0.536 30 MR NR C0048474 Ot1401BA8f005-0-041104 ND 30 0 .p84 30 NR NR C0049474 Rep DL1-F01-A1SF0054441104 NO 30 0 .844 30 NR NR C0049478 0l1401-1PW001-0-041104 0 .772 30 0.568 30 17.4 3 0 C00494718 Rap DL1-F014PW001-0d41104- 0 .870 30 0.744 30 f8.9 30 00049478 OCi-F014PW0020-041104 0 .468 30 0438 30 13.7 30 00049474 Rep 0L1-A014PW002-O-041104 0.472 30 0.616 30 16.8 30 C0019477 Ol1-F01-PW003-0-041404 ND 30 0.209 30 4 .36 30 00044177 Rep DL1-F014PW008-0-041104 NO 30 0.247 30 9.52 30 C0049478 DL7-F014PW0a4-0-041104 ND 30 0.238 30 69.6 30 C0049478 Rep DLi-01dPW004-0-041104 1vD 30 0 .248 30 57.2 30 C004C474 Dt.1-F01-1PF002-0-041104 NO 30 0 .222 30 /1 .1 30 C00e947971op DL1-f014PF002-0W41104 ND 30 0 .247 30 11 .2 3 0 C0049480 0l-1-F01-K003-0441104 NO 30 0 .265 30 20.9 30 00049480 Rep Ol-1F01-1PF009-0-041104 ND 30 0262 30 21 .4 30 04049481 DL-1*61-IPF004-0-041104 NO 30 NO 30 7 .80 30 00049481 Rep DL-1-P01-Y7f01}44-041104' NO 30 NO 30 7 .38 30 00049482 Dl-1-F01-0"V06-0-041104 ND 30 0 .373 30 8.72 30 C4049482 Rep 0L-1-F014pF00lj-0-041104 NO 30 0 .386 30 8.58 30 00049483 00-f01-44SW001-0-041105 ND 30 NO 30 139 30 C0049483 Rep 00+01d4ABW001-0-041106 ND 30 NO 30 137 30 C0049481 0I.3-F01948W002-0-041105 ND 30 ND 30 180 3 0 00049484 Rep 0L3-F01446W002-0441108 NO 30 ND 30 162 30 tab-" OuplaWs NO a Not dNecbd at or abava LimPt of QLm1lNion vAkh Is 0,2 1" (wet NR .!Nat ~porMd dw b pwNy oorWd nw~ filhras Exygen Research Page 26 of 132 p. 27 Interim Report #14-Analyais of Fish and Clam Samples Exygen Study No.: P0001131 Table X. Summary of PFBS, PFHS and PFOS in Fish Samples (continued) Exvw kJ ca &r% .arfea c8 a a oons " s ca auftw.atsoa ~ AW* AmenW Cfrtnt fand ACOixaCy FqatO AoGUYBCy FpunC Ap mn y ID &OWWW"L MA-%) WW +A. N- wt, W-141 COWM83 p1, - Of 44YY003 "Hl05 ND 30 ND 30 1 48 30 C0049496 Rep 0 l3-i01-M8W0030-041105 NO 30 NO 30 144 30 C0049+80 0L3-W1 4.48W004-0-0+1105 NO 30 0. 286 30 198 30 C0019486 Rep D13.FO1448M1+004 -044 1106' ND 30 0282 30 109 30 C0049487 01.3F01 4ASYY006-0-041105 ND 30 0.386 30 173 30 O0018487 Rep W401 44O N0 06 4-041106' NO 30 0.341 30 168 30 00046488 00-F01 148F00 1 .0 -041106 ND 30 00049488 Rop 013F0 1415F0010 -041106' ND 30 00049 " O1 3-F01-M8F002-0-041105 ND 2 0 0004 048Y Rep Dl3F01 40 F002-0-011105' ND 30 NO 30 110 30 NO 30 115 30 NO 30 118 3D NO 30 111 3 0 00040490 OL 3-F01 4I81 003-0-041106 ND 30 NO 30 7tf.8 30 00040480 Rop 013*01-M8f003 4441106P ND 30 ND 30 72.0 30 C0049491 0C3-F01 4A8F004-0-041106 ND 30 NO 30 1 30 3 0 C004 9 401 Rep d13- F01 44F0044041106' NO 30 Nb 30 134 30 0004340 2 D11F01 4iSf005 4441106 ND 30 NO 30 81 .0 30 00049432 Ro p 00 f01 415f006 4041103' ND JO NO 30 83,8 3 0 C0049493 C0049403 Rog DA4C-F0 i- 1PW0034-041106 ND 30 0.388 30 all 30 DM0-FOt-IPW003 0-041105 NO 30 0 .334 30 E3 .8 30 00049494 DiAC 4-0 14PW004-0-041106 0. 300 30 0 .308 30 88 .8 30 C0040404 Rep DIAC-FOt ~+WOO~O Ot110a 0.348 30 0A8 4 30 see 30 00 048486 DIMC-F01-1PW0084-041105 ND 30 0.270 30 C00404" Rep DMC-F01 4 PWOO"-04 110s NO 30 0 256 30 64 .4 30 42.8 30 C004 9 496 OM 0401 -#18W00 3-0 041 106 ND 30 0 .502 00049406 Rep DiriC-F01 4ASW003 4041106' NO 30 0 .3E0 30 9 64 30 30 330 30 0044 0407 OMC-F0 1 -MSW001-0-04 1106 00.318 30 1.30 30 259 30 C0049497 Rap D4 AC-F01dA8W004-0-041 106' 0.233 30 1 .88 30 269 30 00049 498 0MCGf01 448W005-0-041106 NO C00494981tep DMC-F 0I-MSW0VP4Q41106' ND 30 0.080 30 0 .06 30 NR NR 30 NR NR 00""99 OMC-FOS-UGFM-O-041 105 No 30 NO 30 HR NR C0049489 Rep OMC-MI -MSF002-0-041106' ND 30 0.307 30 NR NR 000 40800 DMC-F0I-M6 F003fi441106 NO 30 NO 30 58.8 40 00049600 Rep OM0f01 4MSFC03-0-011106' ND 30 NO 30 68 .0 40 00049501 OfiC-F01 -188f004-0-04 1105 NO 30 0.254 30 116 30 C0048501 Rep DA4Gi01 .M8F004 .04 1110 5' ND 30 0.228 30 112 JO 00040 602 OMC401 4 ASF0054-0 11106 NO 30 0.420 30 146 30 00010502 Rep OIACrF014ASF0060041105' NO 30 0 .448 30 1 47 30 C0049603 DIACf01-PP003 -0-041105 NO 30 NO 90 7.92 90 C0040603 Rep DMC-F01-1pf0 03-0441106' ND 30 ND 30 7.92 30 'tsbonrory DupAtsM ND a Not dotecbd at or above tJmk of qwntkaton wttch 6 0 .2 nyq (** wMpht}. NR a Not 0oqoryi! Oir aqiMy oaiYW rauk fWMN. Exygen Research Pap 27 of 132 p . 28 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No . : POtIO113 1 Table 1. Summary of P FBS, PFHS an d PFOS In Fish Samples (continued) C4 6Nf" .a FFp Co 6urola . "HS Cl sNlonst nFOs AN" Cient Fartd Accuracy Fpnd ACdxWy Faund Arcuncy EMN to sarNme ID vv* w H-% .~wt . N-% wlut M-% 00040604 DA4 C-W1.1PP004-0-041103 ND 30 C0049504 Rep OUIC-F0I-IPF004 0-041 106' NO 30 C00496W OMC-F0 14PF0064 .o41105 NO 30 000 49606 Rep DMC- F01- 1pF005o-041105' NO 30 NO 30 44 .0 30 NO 30 45 .6 30 ND 30 48.4 30 NO 30 46 0 30 C0056334 00058354 Rep 01.2-F0 1-M 3 f005O041210 NO 30 ND 30 45.2 30 01-2-F0t-AtHF006-0-041218' ND 30 NO 30 5 1 .6 30 C0066466 C00584 56 Rep 01.24 01- 1PW0068.041215 NO 30 ND 30 13 .2 30 D12-F014PMY003A4412/5` ND 30 ND 30 13 .3 30 00056435 DoU-F01 4i48Nf002-0 .041216 0.208 40 1 .12 30 NR NR 00056466 Rep 0 OU-F01 -AASW002-04041216' 0.227 40 1 .70 30 NR NR 00056457 DL2-F01dPIN004.0.04121 5 NO 30 NO 30 6.E0 30 00066467 Rep DL2-F014 PYV004.0.041216' ND 30 NO 30 6 .00 30 00556458 DOU-F0 1 -MSW0034-041216 PD 30 10 .4 30 NR N R 00056438 Rep D9CI4F014ASW0030-04 1218 ND 30 10.8 30 NR NR 0006e459 DI. 3-F01 4PW004.0 .041130 NO C0058450 R ep 0L3 .F014PMV004-0-04 1130' NO 30 ND 30 ND 30 7.02 30 30 7.52 30 08068480 D0U-F01 448W001 -0.041 216 7.88 30 15.4 30 NR NR 00066460 Rep D 0U-F0 1 -M3W001-0-041218' 7 .12 30 14 .2 30 NR NR 00056481 DOU-F014UW004-0-041218 C0056161 Rep DOU6F01413W00 4 0 -041216 4 .72 40 21.7 30 NR NR 4.68 40 22 .5 30 NR NR 0005 6,482 00U-F81458 W0050441216 0.364 30 04 30 MR NR 0005e462 Rep DO4J-F0 1443W005.0041216 0.36 30 1.41 30 NR NR 00066463 DOU-F01-U5F005 A).0{1218 1 .41 30 6,40 30 0 0066483 Rep 00U-F01 418F005.0-041215' 1 RR MR .45 30 6,44 30 NR MR 00066484 00066464 Rep 01.3+014 PW002-0-041130 ND 30 1D -3.F01-1PM/002-0-041130' ND 30 NO NO 00058496 DL3-F01-IpYV003 0-041130 ND 30 NO 00056466 Rep Di.3-F01 4WV003-0-041180 ND 30 NO 30 120 50 30 11 .5 50 30 6.44 40 30 5.28 40 0005 0486 DOU-F01-11A9F00.0.041216 1 .72 30 5.56 00056488 Rep DdU-F014j8F003-0-04121E' 1 33 30 6.64 30 Nit MR 30 NR NR 00056187 0BGF01-1 48F00S14141218 0.220 30 1 .79 C00"7ReQ D6C.Fp 1 -M$Fti06.1-041216' ND 30 1 .76 30 NR N R 30 NR NR COO5Q466 DBC40 1-MSFOt15-044 1216 NO 30 1 .68 30 MR NR COU6646t; Rep DBC,-R 1 4 13F0050041218' ND 30 1 .59 30 NR NR 00056 W 00 YF01 40F002-0-041216 0.6886 30 4.50 30 NR NR 0 0068460 Rep DOU-F01 4431'0024 041216 0. 672 30 4.56 30 NR NR C0056470 OL3-F01 4PNt001-0-441130 ND 3D 0.245 30 9 .04 30 00056470 Rep D13'F01-1PW001-0-041 130' ND 30 0.219 30 6 .80 30 'tAbalbry DupN ab NO v Not dsMclsd at or above L" of p,p00ite6on ,~Nth 15 0.2 nplo (wet weipAt). NR = Na reported due to qwlly oernd mult (dU,na . Exygea Research Page 28 of 132 p . 29 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : PO0113 1 Table I. Summary of P14BS, PFHS and PFOS In Fish Samples (continued) aJ C4 swf".M rFSS Cs swron .a WHs C6 swwm.e. vFOa ~..~.~. Ae....ee CMrt Fouw Aocuracy Pouw Aopsscy Found Acc ncy tD ,r .w+x~ . +,r-11 wwvt +J COO5E471 DoU-FOt.64f0021 .011216 0.61Q C006647/ Rep DOLLF014$F002-1-041216 0.880 30 4.68 30 1.72 30 MR MR 30 NR MR 00056472 DOU-F01-U6F004-0-041 219 00066472 Rep DoU-F01-MSF004-0-0412181 0.792 30 235 40 MR MR 0 .816 30 2.22 40 MR MR C0056473 DOUoF01-W0p1-0-041215 2.11 30 10 .9 C0056475 Rep D0U-F014ISi001 -0-04 1218' 2.28 30 10 .7 30 NR MR 30 MR N R 00066471 DOCF014AF00S0-041210 ND 30 2 .08 30 MR NR CC0b8471 Rep D00-FO14ASF00b-0-041216' ND 30 9 .00 30 NR NR 00066476 06G401-AASF001-06041216 ND 30 3 .87 C0p56176 Rep DOC-F01 .a`/SF004.0441216' ND 30 3 .77 30 HR N R 30 MR NR 00066476 DMCrf01-MSF001 4041 216 ND 00056476 Rop 034G401-M3F001-0-00216 ND 30 0 .420 30 MR MR 30 0 .456 30 MR NR 00056477 DLt 4!01-IP1AW06"1216 0 .268 30 0 .044 30 68.8 30 C0030477 Rep DL14:014P5M0064-041216' 0.219 30 0444 30 87.6 30 00046478 Dl2-F014P'W003-0-041201 ND 30 ND 30 7.48 40 C005647$ Rep DL2M14PW0030041201' NO 90 ND 30 7.44 40 00036479 Dl,3-F01-IPW0050-041201 ND 30 ND 30 4 .88 30 00056179 Rep DO-POI -IPYY0060-011201 ND 30 NO 20 4 .72 30 NO - Not dNea1Kd at or 8b" Lbdt of CYYnYtilioe whkh Is 0.2 nply (wet wrefpM), NR -NOt N!(JOrMO dM b qOMNVCpdi hlull (aikNM . Exygen Research Page 29 of 132 p . 30 Interim Repot #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Table H. Summary of PFOS in Re-extracted FIsh Samples Ca auuoua PFCS e CYerM Anplyb Found Asseeaetf Exyqm ID Sample 10 ~~~ .. .. Mt w.t wNdt Accuraoy t+rCOOIdt51 D9GF01-IPWOpt-"1021 2080 30 C0048152 p6+GF014PW002-0441021 3330 30 C0048153 D8GF014PYVa03-0-041021 1680 50 C0046184 00U-F0i-IPF401A-041021 596 30 C0048155 DUU-F014PF002-0 .041021 838 30 C0048158 DOU-F01-1PF005-C-041021 644 30 C0048160 Ddll-F014PW002-0-041421 1210 40 C0049450 DBC-F0I-MSWG01-0441105 940 40 C0049451 08C-F01-M6W002-0-041104 7520 30 C0049452 OBGF01-lN3W003-0-041104 12800 30 C0049153 DBC-F01-M8W904-0 .041104 3440 30 C004945-4 DBC-F01-WW0054-04110 ; 5240 30 C0049455 DBC-F0144SF001-7 .041104 3240 30 C0049456 O9C-F01-MSr"002-"1104 4780 30 C0014458 OBC-FO14PF006-5-041104 we 30 C0049459 D8C-F014PN004-0041 i 04 1230 40 C0049460 DBCrFO1-!P'WO06-'J-0411?4 2820 30 C0049461 DOLLF014PNEO$"1104 NR NR C0049482 DOU-F014OW004--3441104 1740 30 C0049463 DOU-F01-iPWC05 .404H 10t 2130 30 C0040485 DL1-F01-MS;W601-o{7411O{ on 30 C0049465 DL1-FQI-MSWt+0?-o-041104 7p8 30 C0049467 DLi-F014ASW003-0-t141104 we 30 C0049469 DL1-F01-4SWO05-0-04t104 604 30 C0049471 DL1-f01-MSi002-0-041104 we 30 C0049472 DLi-F01aM3F00340-04i104 432 30 NR No! tMoflMd is lo QuYYRy O wpf fMUk fAtluns. Exygea Research Pav 30 of 132 p . 31 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 Table II. Summary of PFOS in Re-eztracted Fish Samples (continued) Exyue + ID CS SuNowMb O PfOS --- -APOCOWAww"M* cow Anetyis FouM Samae ID [now) wr w.mn9 1 se "e" r,eauacw r+I- x ) C004a4n Ot1-F014t3F003-4-041104 740 30 C0049498 OMC-F01-M 8w00S-0-041105 580 30 C0049496 DMC-F0I-M3 F00243-041105 620 30 0 0058456 DOU-M1- 4SW002-0-041216 28200 00 00058458 QOU-F0 1-MSW003444 1218 4040 30 00056460 QflU-F014A$W001-0-041216 NR NR C0056 461 DpU-F01-MSW004-0441218 5120 30 C0056462 DOU-F01-MSW00 5 0-041216 496 30 C00564 63 000 -F01 4ASF00lf0-041216 720 30 C0096486 DOU-F01-MSF003-0-041216 848 30 C0066467 03GF01-MSF005-1-041216 NR NR C0058488 09C-F01-MSF0064-041216 8880 SO 0 0056469 DOU-F0 1 -MSF002 -0-441216 640 30 00066471 DOU-F0 1 -M8F002-1-041216 892 30 C0056472 DOU-F01-M8 F001-0-041218 1820 30 00058473 DGtf-F01-AISF001-0.441216 2070 30 C0056474 OBC-F0 1 -MSF0034-041218 4840 30 00056475 D9CrFO1-MSfO04-0-041216 9280 50 00056478 OMC-F0 1 -MSF001-0-041216 840 30 C0048148 DB0-F01-1 PF001-0-041021 384 30 C0048150 OBC-F01 4 PF0030-04 1021 293 30 C0048156 DC+U-F014 PF003-0-041021 339 30 C0048157 DOU-F014 PP004-0-04 1021 424 30 C0046139 DOU-F01-IpYU001-0-041021 387 30 C0049473 OL1-F01-MSF004-0-041104 348 30 NR = rVOt opon.a aus w quainr oonMrol rpul++ar,rse . Exygcn Research Page 31 of 132 p . 32 Interim Repoct #10-Analysis of Fish and Clam Samples Exygen Study No . : MOO 113 1 Table 111. Summary of PFBS, PFHS and PFOS in Clam Samples c4 s uffor" PFSa co >su"bna . "NS Cl sura .r rau Clint MS M AUW siiC M*M 1W Wad llnalyb As caW Found Aaunny Found Accuracy Foun d Ex Bi Samob ID +Nt wt +i % w.t wc. +l-16 .r.t M. ~)Y 00056480 0t.3-101-CFW001-4441216 NO 40 NO 40 1 .82 50 0 0056480 Rep 01 .3101-CFW00140041218' ND 40 NO 40 1 .82 50 C0086481 DMC-101CFVtl001-0-041216 C(fO5601 Rep DMGI01 CFVbt101-0 .041218 NO 30 ND 30 8.16 50 ND 30 ND 30 6.12 50 00066482 D12-101-CFVV0014-0+1216 00058482 Rap Dl2-I01-CFW001-0441218' ND 30 NO 30 1 .81 60 NO 30 ND 30 1 .77 50 00096483 0OC-101-CFWf0014441215 NO 30 NO 30 4 .48 30 00056483 Rep 090401-CFW001-0-041215- NO 30 ND 30 4 .44 3 0 00066484 D11-101-CFW0010041215 NO 30 ND 30 e.80 40 0005846 / Rep Dl1-101-CFW001-4-041218' NO 30 ND 30 8.84 40 00066485 DUU-101CFWp01-6041216 C0066485 Rep DOl}101-CF1N001-0441216' ND 30 ND 30 0.202 30 11 .4 50 0.205 30 10 .9 50 'laboastaY Duprio+w N : Not dNrcted at or abow LMJt of awnimlion wWch Is 0.2 npt9 h+et wsiph 1). Exygen Research Page 32 of 132 p . 33 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P000113 1 Table IV. Matrix Spike Recovery PFBS, PFUS and PFOS in Fish Samples BMrpM Dow~ VOW C43Wb49@ PiNa pOQ >~ M S-niqr IYawrnd R OMMry In LnpN IrootMN RaoDNry IM SuhpM NaoaKlW q mmy .vx IftbI.W .L w .t r~na +rna wrt DL.3 .F01 4/i001 0-0114Q 1 SOftw>t*0. urM Ol341010M1-6-041421 lwmnasslrr. sDpy 10 100 0. 300 t60 0.3p0 02 .4 03 NO 0.21 03 f.10 12 .6 74 Q NO 73,2 73 6.14 78A 73 DtJ-F01~t021 K~o~ral>11kD.14~p t0 02l6 DU-f01 4O+F002+f-0f 102 1 tCMNK+i1t 0. WO Ppi 100 0206 R52 03 00.0 00 No 7.tl 75 4 .16 10.3 Ot !b 79A 00 4 .14 l0,0 77 OibG4901-4PFq0f-044102 1 iamMM a"K torrM OLIGF01.5F0014-04102 1 40OMM26 lptN. 1pp01 It 0330 4.40 42 ND 524 62 7 40 a.80 20 100 0.3 30 06.4 06 NO 742 76 7.40 all 74 prr~I01 apF00Y-00410Q 1 0COD041S 403 G. 10901 10 0.712 7.60 MO-PO t-IPF002-0-W 102 1 RWMd 4+ . IN wel 100 0.712 75.0 70 77 ND 0.00 In 96A 06 14.1 00 14.1 20.0 156 104 Op 0AACrF01-N4N001-0-04102 1 tCDONaOtrk IX son" 10 1AO 7 .1D 06 WACf01-MryM001 -OM102 t IPD4atj 0 8 Y1, 1050M1 100 1A0 04.0 64 NO 7 .84 Ti 70D 11 .0 No 002 00 70D 131 a1 D14GF01 4RY0024-04/021 Nxa0131 yt6105p1 10 DMfi-F01 4PYYO0t-04i 1021 t000+,, " M IL M wq 1 00 0.000 6.75 0.000 00.0 60 NO 7A6 00 NO 74A 00 76 34.4 44.0 314 101 67 OAIC-F0141EIAf00f-" t021 10001117ti1ttr~rY~> OUGPo14W3W001-0411021 4CqD4It11 40 /.100pi "1 10 0210 3.70 06 0.824 OM 00 270 270 100 021e 91 2 01 0.'.R4 032 93 270 375 106 OMCri01 d/SWM02.0041021 " KWWillMc4MMMU 00 w DMC.F01 4A9W002.0441021 A toawi>Ip Kloew > pO* am NO, 432 432 00 ND" as NDA 52A 104 5w 470 4 02 08 $30 924 70 0t2401 .IPF0014-041001 tcwwnt SM p.+4wrfO&i Ol2-F01 1Vf001 OOL10Q1 lwDw+rytKtmPrepr.l 10 0.00 5.0 61 ND O.QS as 3.45 8 .30 40 t00 0.!!0 46.4 1 6 NO ~ a 3,45 $&4 53 Dt?F914W002-0441021 <Car4a4M 91 "D Ne1 Oi3 F01-PFOOi-041/021 (CaWI kkLt0we4air) to 0.010 4.01 40 100 0.1114 NA 04 ND !O 0.40 M 4 .72 0.60 31 7iA 74 4,72 72.4 Ri rwdw wcwY Or W4n01wd W Wc wMiv: fy~w r+~'wewr .dw o~+not Nore+~YYe ' 1A11 d rw* b wW 1r oRwa0o4 YWrd af l0 p. ND Not d *uMd M or atbOa tYM of Cor+rIWat wMaN Y 02 nyp {HM wMg 4t NO" ~ Nd dNKNd 4t or M~ow 61mN d OwdRwon wron 0.1A nyp (twt wqNy. NN . Na~ npxwa 4w awMM mwa wiwMtwia 16s~ww+ .~i. a. .~ .ui In t.ob t. NnIK Owa ws wwwy Yw. Mw. ~wnw4 awM.. e.wiy wi.. .4y wy ~MpM11p Inw tlr NY. . Y~ 0. a.~ s.e~ Exygen Rcscareh Pap 33 of 132 p . 34 Interim Report #10-Analysis of Fish and Clam 3ampxas Exygen Study No . ; P000113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) ~ ~ C4 Won" MM irnpl. tlyk.e In s.aw n.mr.i.d meow" Owavkn ~ . .~ .~ .WI-L M_ l)6 NS CO SuftnNs PFOS FUW4 Am MOW Affatf is Ow~pl . pm 9 WmMy we .vo. fl.OOV.r,a ,bmrxy OW .. w auF01 1 rFnc9 a0N 03~1 POOwnar c,NA1i~N d .bF'WIPF00I-0Ot1021 (f'J61itl1 bow . 1 10M4 e/ip / 0 0.217 7.00 NO 7J6 90 7A1 0]0 72 100 SZU 62.9 as MD 732 73 2.01 74 .0 72 OL2-F01 PFOM-0.041021 ICCOUw7qrtRqooitNw) 10 0.316 0L2f01 4PF001444 i021 9= rs -nwwctiaN0800 100 0-W 6.04 E6 NO 7A0 78 4 .52 11 .7 O9 67.6 07 !ID 76.0 4 .52 00.6 74 0t2 -I01-1PFO0b00i t 0?1 K+MNs>>Mtt 1orawl 10 0.339 6 .M 0W01 4Pf10064411031 iCaM4 t0 irr J . be nrlirl 100 0 .336 66A 66 HD as ME) 7 .0 60.6 77 2.4e 01 2.46 9 .69 72 112.0 60 t7t3F014PW 061ap{10z 1 teawis~r7.toMSrr~ 10 J.726 01bt01drW 0010011021 (Co Nns 6M x. to no 6M08) 100 0 33 7A4 or WO 7 .E0 76 5.06 13.9 00 66.0 as NO 772 71' $.60 962 79 L11 .2-F01M5f00144M102 1 (0owffwerto.ator BOB) 10 0!! .t Ck 7.F01.M9F0U10W10'! 1 40WWW19 t. 1010066ti! 100 02M 1]6 70 04.0 64 ND 62 0 a 772 76.0 lA 77.6 79 772 156 61 Dt2-F014A 9FOOb00410i1 tOOMN1Mi9tc.tDp lt+r) OL M1 4Ne)F002-0411021 (C.401I111 6/1N.1WpY SAM) 10 0 .408 6i R 65 MO 7A8 75 44.9 101 100 0..108 01 .6 61 NO 69.0 96 94d /66 61 01.2F01-6~+1021 (COwwar o . 1410 arw) t0 6A/6 6 .62 61 NO 9.70 is 11 .t 412 OtZf a1 IliF00iP W 102/ tO4040142 9 4 1. 14000 101 f 100 04/6 64.9 N ND 70.0 71 4 1 .6 104 62 OC2d01.UW016.0.66 102 1 R7MMtayk6 . i oNttW1 f0 0 30 7,06 67 Dt210014011F044-04102 1 1CAOM+ sl~a 1 i0o ~ N~y 100 0 .946 71.4 71 NO Hp 7A6 612 76 p.E 612 at 83.4 167 00 Cl t F01 dPf0fi1P0410Q1 Po om" 4tF.1IV6 Opel 10 0 .432 7 .44 0L 1-F01-IpF001-0.0110z1 (aO Wut !M K. to No SOW) f00 O,t32 671 70 0 .701 9.18 79 73.4 40 .0 67 0261 76.4 7!i 30.4 10d0 73 DL3-i01dPF003041102 1 tO"I"i 41410 pI6M08) 10 0448 7 20 69 QI 3-i01 4Mr00b0 44 f02 1 twate+K a~t t we M 4rM 100 0AN0 092 6D HD 6.06 61 3.66 100 73 WD BI A 8 2 i6d 00.0 70 'lw~ mm" amok to rprMp Iree WM~crdl~: M~w~4ra, M rawb we~w~y vMb erxv~l M ak+rlw no - Hal a.ucaa r ar aee .. tr~u dCu,bwan rYa~ r os nop (.~et +ryrt VHrNatwpqibOAMbWdMmrRflw~rMhMYM -wlyY/Mi{MYP~ in Twos. New: Smoak aW nYry /MIN aNwn tw~Md nsdM . Noo - y - whrwy awplUw f " 1r n1w s in ON taw d11 L Exygen Research Page 34 of 132 p . 35 Interim Report #10-Analysis of Fish and C1arn Samples Exy$en Study No . : PO40113 1 Table IV . Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples,(continned) C# &#"WNW AIRO" Mnt AmOirN ~rN7M aprr~l In l~pN ROCOwrOlf .(t0obwy CS SWkaft PF Aft FS" ,' MiaMt NO f0ux0 ,inlWrtpM RtroownG RUMMY h8rrplr Ye. wt.t +rK+t Miar M IqoewW wt R Peavy pL3R01 .0"FODM0.0 1021 IaOaM .awo.+e,,.w) 0l.7~ Ot-IP FGCF0~1102 1 Iu 0016080 .taoMaw) 10 0 .n4 100 0.7et 4 A4 s1 No to !s 00-e IS No O!A : . .1 01 ., o .M .,. e.ve se , . . 00 " . . 0 362. . 61 .2 Si 00i01-I1"F006444102 i 107MNp qR D.10 N OtY) DtSF01-pF006-001102 .qrM41tcawu7yl 0r) 10 1 .53 O.M 70 NO 100 1 .69 4Q4 00 NO 0.10 013 02 4At 11 .7 62 . 47 0.46 OOA 01 OBC F01MtFp0/4411021 Q0061" 4001" t0ip>>rri OeC f01 .WFU016M1021 IcatwtNOr J.wDpqo soft) 10 1.34 024 40 0.002 10A 101 _MR MR !Al 100 1 .34 0U 50 0.0?2 OOA , . AO MR NR MR D9C-i01-IPF002-044i02 1 IoawtNqas.w PPr+r) 10 1 .43 5 .04 DBC.FOt4PF=444I021 O~ou/MtpKlNpr~1 100 1 .43 602 44 00 NO NO 0 .70 00.0 W 110 113 00 110 100 70 pOC-I'01 dr1"OObOAi t 021 Icaauro0ttq a po apo .) 10 0. 9ie f.72 67 0,044 10 .4 .91 DlC-FO14PP0004441021 tC1oW1 U 7iPL 1tDM40or.) 100 0.>f00 00.0 00 0.044 OOA 00 . MR MR MR MR MR MR 09Oi'01.PYV001-04N1021 gOIMi10/ srC.10INltho QiDGF01-IPri001-00~102 1 40oana~nrH,tpt~ ~Mt+l 10 0.004 100 0.894 7A0 - 02 2-21 70A 10 2.21 0m 75 . MR NA K MR MR MR MR MR OBGFO14PW0PV040+<1021 RAw~taljR.0lO 06111140 l 10 OtlCF01lrYY00200A102 1 GOMwlp 1.weak god) A00 O .T00 7 .50 '0.700 00.0 so 00 ,0./2 0,12 102 .. .pf OOA A1 . MR MR MR MR MR MR ONGFOt-PW00}0-0~10Q 1 RAw'MtOM0,t0M/M14 "10 0 .7% ` 0.32 COG4101 .rW 00SD041021 IcOOtit,t4 J,tISMYO0Mt 100 0.730 . 702 ' 7e 70 0.70 16.6 0.70 OD.i "4J . . MR MR MR N - NR MR MR 00u+014PF0014WtOQt ,. (OOOMtw go P.lOpAMw) 10 k90 10.0 06 1 .02 149 a0 D01rF010f0p/444102 1 IdrltOtstbtlt 11ow0Uw) 100 4 .26 702 72 1A2 06A 06 MR . MR NR NR MR MR OOU4 ;DI4FF0004Mi1021 iOObNtesto 4uPPI, y .) 10 070 . ta/ C O .TO2 9.72 OD DOU-FO f aPF002-0-0410?1 IC066I146 >1K1100Ro Oth" 100 0.70 70A 10 0 .792 00.0 19 MR MR MR - MR MR MR D0U-F014PF003044t021 It>~1wOMCi~MM~! 10 500 OOU-F014/F0030-011021 IpOw/MfOtKta/M4~W 100 OM .. ' '. iZA . M 1 .02 10 .0 06 . !1~ 75 1AQ 804 07 MR.. MR MR MR NR MR a .pb n %M w .a.wtl. rw tp" Wot+ .anMvrr. tirweq. an e.w'wry w e be oW,irte ND Nddttrqa7NOrMaOImI dQiwrWllonrRYdtY030ptOMMwWq , NR -Mw tMO~tl Or b 4~M aanYd rMN1iMM1RMeMytil wrlr r~ tinm InTo U N . MMr: iYw~ MN N~wy M4 Mrr~ iwwiYi wwMY. t+rwYvr[M~ nrP~Y MM1 tww MvYw.le IA ~r MY . Exygcn Research Page 35 of 132 p . 36 Interim Report #10-Anatysis of Fish and Clam Samples Exygen Study No . : P400113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) ~~ ~ ~ 'rnpr lP wd Duct" -MML in 9- w M .k aw . PFM- C11 >;AW .t. WHIS ft-WW ft- y M OOmpb ft--W Ra w .4. wK w+l i A...t omy fe 3enpN %eoYrr00 Rraoiwy wlw. wN. t%j DMF0I4PF004A ON001 K+O~MO fw 0, f0t~ OrN 10 DOU-F01-IPF0091,"1021 rMMUT IM 4 wpp >101 +i 100 6.12 1l .2 It 2.30 12 .0 17 3 .12 70.4 70 2.20 OOA M MR MR MR MR MR MR OOUFtN M1~0054OI102 1 ~.t1MOise.a~sNN 00Ut01-IiF00b0041021 f0awl411 OIM J. t0a tpb99twI 1 0 4,D0 100 4.60 12.2 74 .0 70 0.ffi0 1f2 102 71 0.960 06.0 as6 MR MR MR MR MR MR D0V 4101-110 4Y00t .0-Oi 1021 lno I ewOM .u WNOrr1 10 2 .00 10.2 OOII F01APW001 " 102 1 (C0 0 410 11k X. 1w piYqi) 100 22D 72 .4 73 70 0.910 10.7 0 .910 "A 0! U MR MR MR MR NR MR 00 U-FO1 1PMOOQ404102 t KOMNq1M4 10osMq t0 DDt}1:01 dP W 00Q.0.04 t021 lC+bN~~e4ri.ta~Aprt 100 10.4 74.4 18.4 044 100 70 30 3.00 132 00 all 00 MR MR NR MR MR MR D24F01-N BW0D1-0-04 102 1 I C001H+O 1* t 00 1o544 OL2-F01-114 61040040-04 1021 avow" 10j, iN " Mq 10 '100 0 203 0.52 0.203 701 91 77 NO 0.00 p NO Od2 es 120 12S 120 177 97 0L2 *01-btri0QT0.011021 tG118"+tQ go R a M 21r1 t0 p, .M 1 .NS1tq420041021 lowMM M L 10,011rrt 100 ND NO 4A6 i7 00.4 !!0 NO 4.12 1" O 93.0 04 102 110 102 t06 03 012401 448Y1ti01340 102 1 10oraaly e6 r 101, pr.l 0 1.2-F0/ ip1M003p.0{ 1021 mat0$6K0. t56 1M900j 10 NO 924 92 100 ND 612 91 p 9 40 91 Np 962 116 04 4 02 4 103 162 50 013401 -p8 W 004044 1021 taeoMtkMR L 9 rM 40+I 10 ND 7.l9 76 Np 726 73 OOA 75.0 DlJI-F01 -OF3iN0040-0{ 10Q1 tCtbu+ K 64 .I 0 11106 400 +t 100 NO 92A 112 NO 03.9 94 OOA 100 70 013+01 M W Y 006404/02 1 (00MON001A0.1oM9MN 10 D12f01dRNY0060-04 f 00 1 1GnwrY 110 K 101100 4trW t0p NO N4 7.96 OD 00.0 91 09GF01 -M6W0p1-0.Oli t04 1Cpw000 Mac awrary 10 0E00 10 .3 OEt:4 01 -41iOMN001-4041 (04 10WOMS 01tRtw 00 so 0) 100 0.000 00 .4 Ot 90 NO 0 .00 t1 100 NO 100 100 100 136 234 96 8.72 iT .i tp 9.32 113 100 MR MR MR MR MR !1<t 9r>rN ft"ft OMO 4 to 60" Wet dp*Ar*: fta+biR i& NOU7h wG1Nq whN ar~alM eMrw NO - Not M4eMd A Cr Moao thW of G1rn006t 0 ofuch is OZ nyq (ruk urMyj, IW :NMtsmWMb * rNr *p*al mwi %MNr ly 6,@jW itsiitb 8wr'nwnlntrbN. 4mbc 9Up tlW Nrwryldi wew ianuhd w&u1b. n00wryMJaw '" col * YOMr **M ON aMwe N 90 mr M Exygen Research Page 36 of 132 p . 37 Interim Report #10-Analysis of Fish and Clam Samples Exygen Stn* No . : PM 113 1 Table IV. Matrix Spike Recovery PFBS, PFIiS and PFOS in Fish Samples (continued) BM~fiM *And M iM+yM /MeowW Rsoowy .r .t ss .a FO~ Al in Mey16 .r .e ft aownd ft--y in &m/N .rw . .ww ft oow00 R600Nry ..~ra 00Ci'O1i1SVY002-0ON 101 100wiMi 110 L M rA left] 10 0A00 9A6 OBC.01411SWO02 0-0H10 4 91 3A3 122 94 MR MR MR (ta01661io .leoM yM 100 oA00 Ot.O 96 3.03 113 110 MR MR MR Dec F01.MBW 003-0pi 110a ICM mMiOpea.l04110Y0piir) 10 0.600 9.92 91 3 112 13 .5 100 NR NR q OOGFOI+qW003~04110{ 100 0,eo .6 .0 96 s.az /a 100 MR MR MR D~C.FDt-AiS1M001-0W 11 a iCwwtea4rtwMM~> 1C 04 bi OY6P01 4Y6Wf 004-0A1110 t KM04M01M A +m Mrkti1 100 0.664 9.90 PI a72 10 .6 90 97 .2 96 9.72 124 114 MR 1R MR MR MR MR I>OCin1 414SYY006-0 W 1104 l="Uw7r KwpOprl 10 0.002 006401 4rISW006-0-W 110{ twMaMNW4+ma+spew 100 0 .032 0.20 T{ 91 .6 01 2 .TT 2J7 102 74 108 106 MR NR NR NR NR NR D@GFOt-NOF001-0-0N 101 IOWSw tI a14 III PP11 spbw~ to W C.F01M Sf001.00t1104 f=wwE so +4 "O pM IwW 100 DA20 ON 00 330 13.7 101 MR 0.020 0!A M 3.l0 100 102 MR MR MR NR MR OBGPo 1JAOF00 ~801110/ Kti0 MNIM 0. 1oAi too) 10 0.T66 4.92 @ 00GR01 Yaf002-0411 t0i I9m+MM 9010. 10 nD Mwr 100 0.760 $0.8 OD 9 .94 1 .94 126 100 MR MR MR 102 100 MM M!( MM 0lG4r01- W0040011104 lO~a~MtyrR~lM6r~+) 10 0.601 0804o1 4PcoD4o441104 / 0.9 100 0.3N 11 .0 1+0 U2 1 54 tOmlafs %a.0iawyrq 100 0.504 OW .O G 0. 591 108 106 ti2 264 112 DBC-F01.Pf 0064-0ar10 4 O:IWNYyk[,Mp68PWY 10 1 fi0 10 4 OOCF01 ~Ilroob-00~11 ot la0aOW 60F.lwoo " / 100 160 90a SO 2 116 122 101 MR e9 2.15 105 100 MR MR MR MR MR OOGf01-iP W 00~-0OM 104 (aon~alN a, to M M+.l 10 OAN 9.72 92 3.21 13D 97 MR 10t MR 09C.FL1-WM10040Qtt 10a NCa+ SM lrtKfO0MpM1 100 0.464 df,6 07 320 104 10t MR MR MR 0BC,i01 4-W OOi 0 W 110F IC.04O r4r 116pY9PW 10 0.672 10A YO G5Gfoi-M1M006 0041104 KAOIMM7MsJlteMtrr) 100 C.S72 i2.6 92 2. 10 132 111 MR 2.10 102 100 MR MR MR MR MR "r~a*~+PN1awaa~sWwwsa~~cw.riYoYN.u~npwifabGVu~.~~'ro!'o: e~+w~+Mrr0~ .uSnrMooOsrwroS nyapOwwYtn~Y.n tMrwl M a1GWbtl NR-NdnOpryaArls4~MA'raM'01qM11Mna Mi I~Mq~YwnlYNaOwwUT~YN~. 1bb: ~YIW FN w11~iY UW Nyw~ Mw1id ~MYlly wM~r vr1UM rl~N ~M~IIMyMM N~ Mp~~ Y~ rM fMM ~ . Exygen Research Page 37 of 132 p . 38 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Table 111. Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples (continued) 6n010 DwatIm C4 SJAWAft MISS a 1111011111114116 ":Is Ama.a MN I'm Mnanl MR tpluld In80mpM R~mrOnO Row" In %00* Rspdwod RooOw, hgOnpU Roe" %Kew" r~ *w .L DQU-F9bIPW0030441101 4Cr 414M00tKt00O 000w) DOtl.F01 dP W 0Q}OM1104 it:00wr0iOML100 X6 SPAN) 10 3.17 13.1 100 1.00 103 103 MR MR HR 100 3.12 00.0 85 eA0 107 101 MR MR MR DOV.OLIPY4004404110 4 f00wOMttlMcC.100o0i00r1 DOILFOt -il' W00t-0dN 10/ ICeawta 11" 0. fo0 Ms 000) 10 3AY 12 .6 93 100 3A0 0!A 06 7.12 17 4 7.12 106 103 MR MR MR 10t MR MR MR 0O1I4-0 t.li W 0004-041101 tOsr+wM Mrt+O p plOOlr) 10 2A7 t0.3 75 DW4014P1N006-044110 4 IooO"nNrf.+Oe"11Opw) too Z .DI 23A at 6.12 ti.12 1 &S too 60 NR MR NR 104 NR NR MR Dl2-PO1141Dri002-081110 4 IONINMi01t0. i0pi :.w1 10 1 .64 11421f01-IPW0024-0010 1 4C114os44 M M.100 0M so") 100 1 .04 1. 40 04 ND 10A 104 l.2q 14d 41 80A 70 ND 874 46 0 .20 124 1/6 D L 1401 .AI SM W 01-0-04110a (006041030 6tOMb4111101 10 120 10 .4 94 01.1,F01 .11131011061-0441101 IcoolaMOKa100MOMe) 100 1 .20 16.e 00 0.111011 113 IN MR MR MR oAi! 112 111 MR MR MR Dlt 4011ABNr002041/101 lOtIMMMSMcKtO1MJ100W 10 1 .30 0.76 AS 1 .72 OL 14101 iaW OOQ4Wt 10a pMM00ftkL100wiJpd 100 140 10.3 79 1 .72 12.4 107 MR 100 96 NR MR MR MR /1R DL 1 .F01-YOIM003.0-01110 4 iCe~ so F 101N SOW) 10 0,580 Dl l i;MA16M100y0.ON 104 R70wa0rMa0.100iAU0W 100 0.500 0.02 AO 1 .13 102 91 Mt MR MR 00.2 as 1 .13 9" ts MR MR MR Dli -P01 460bYY004044110 1 KftiMOMOO.aN.YrY 1o am 0.62 76 0jw 9.76 !Y 1u1 201 OL1.iM449*1048.O41101 pasw sow F. lop W 0 Mr) 100 O .COa 84A 64 0.00! 904 so Its 260 Ice OLif01-MpMlO0b0-W 1104 losatMlOk'Rto1M4v*1 10 1 .16 0.00 TL 1 .15 Dl1 f07.M!'iW W000{1101 Kawww010t00t+M4061 100 1 .18 qA at 1 .16 10A ti2 MR p6a 80 MR MR MR MR NR D0-f01 4t8F0D14pW1 t04 {0104 0pOfpktMp00p.) t0 ND 7 .70 7tl 0.315 am yS 293 303 . 004'01,4131`001404110 4 ICOMMw OrtJ. IN M so") 100 MD 76A 70 0.316 BOA L+0 21 3 3" 101 >t+ .wi. nru~ . . .o~.o~ Me w+q N .~I .~pWwnry. Ow.a~ .e+ea..r w~wrr .+w ama awaMtW NO Nd dOYdOd at s ibw0 limil of QwMiYYbn wi0d) tt 0.1 n00 W ws**. NR . M01 npnYd As to p~Mllr aonitl MW t iMMr1. Rw PItow wri tw ua.w ki TAE* l NrY: >Ilwafa tllN NMN1Yy bl" MMwlt IMf W O MOMbu ~Ie01ry vM~N Ifry vl1T MOM~p Aaell M qIN~ 1~ M tM ~AI. Exygen Research Page 38 of 132 p . 39 Interim Report #14-Analysis of Fish and Clam Samples Exygen Study No . : P0001 1 3 1 Table IV . Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples (continued) 5stp0 AW*UM AM a Won" "ss M~wn( Aft ane a cs>~a,~ " 9yk W In 3 +04 R"aw" Rem"" in JrtVk lptowW Ram" .. . . .>k ,c .MM. .N .6 in* Il .Nk ftoOwrd ilratwy .K .G 1 Dl1 FOi .M8F002Q-04110/ (t:asM7tlMK.ti0M4Mi+1 10 ND DL14FOt-W002 0-04110 4 IblM"ntfN410tn690+1 100 no too of 0.624 10A 04a 06 OA24 964 IS MR MR MR go MR MR NR DL1401-MdF00",04110 4 (Olarh7N to R r tW NM) 10 0900 L70 DL1 f 01 .FqFOO7.0-041104 {EGOMptytRtO~MYyiy 100 0 .7A1 64 .4 as 04 0.002 102 OS MR 0.042 Ob.Y 06 MR pt 10:t MR MR 01.1 401 41lf 004.&04110 t 9 Oh6r 78 OKE.woP 1100M 10 i o 400 00 0 .512 10.4 91 MR MR MR DL/401-YOF004-004110 1 AmtwaM . tMMarM .F 100 ND 06.0 e7 0.l3~ 101 100 MR MR MR a1+01-i1DF000A-04110 4 (wwRb4 aa P* 4Y) t0 No 0.81 00 0.001 10 1 t11401.1A5F0066C4110 4 (0004wr4 twKtm PP6 fwp 100 ND 22.4 82 0.004 YiA 94 MR MR MR 83 MR MR MR Ol1 f01 .1P W 001 Opt1101 IDaotMtf to ~ N M ON) DL101-IP1M00 (-0041104 (00ww/sr J,lroeMStr.) 10 0.7T2 O.M 100 0272 04 .0 79 OJ 9A66 11.72 i 17A 0660 97 .! 9T 17A 20A 11s 00 00 Dt. i-F01 dpfy002-0Ai110 4 (o004M10 400 .u MP eMr) 10 DL1.F01-p W pOZ.0-MI0 4 (OOak7S 1101 . + 0D N yry 10D 0.400 a00 02 0.460 70.4 76 0 .636 US N 10.1 17 4 0.510 46_0 07 1i7 100 117 St OCt-s01.itIN003-8041 104 R1WtM71'ttt C.10tMJM"1 a14101-PN(003-004/101 0 C04xs71 so 0. MONO $$04) 10 100 no 2 06 41 0206 a.44 92 t0.7 73 ND 00.4 00 0300 106 106 S.20 100 100 0040VI'W0644441104 (ao4wss ftk e.to,)r 4 rw) 10 11 401457W004.0041104 I~tKqqtf,foop fyr) 100 NO NO 4as es 71 .0 72 0.2M am am so 01 .0 as s" 72.0 ~ eid 140 00 Dt1iD1~MF002-0.D/t 1t 4 (O~o4Mlsyt~0,10s~Otrt) 10 NO 0.00 00 Dlt -fpt 4PF00M0F1104 10001104iK/MUo Or4 100 NO 00.4 06 0.?2? 028 0.2t2 010A 111 111 102 96 11 .1 100 70 91 Ol.-1 f01-pF0p0.00t110 4 I~~N 4t4w4+t) f0 ND !.!0 M 0.?16 102 103 202 30,5 00 OLt 4P01 -V Fti094401110a 0ow~d4M~ 1aot~fM~) 100 ND 78.0 70 0a5 90 4 00 20.p 100 as 'SaM10N(OWN ONtNr IMlow4 (M 2* Illq W. MtMMV6 InaoLtilmtrfeomry MW Crnot M ralaiM ND , ft Olbcat Of 40040 Unit Of CuMY00an Mittt h 02 FM/0 (twlwqil . NR~llutepaM/MbWtlMcsiwal M" 1wa Irrrllw.nwian~wwtM7AW ./. NOIC Siwq MM iM.~Nf YbY aM~w~ IMwdr eMyM~ .1~OwA/Y 11~kN A17 w7 eoMoY *so** NhIM to ft am dMW Exygen Research Page 39 of 132 p . 40 Interim Rcpurt #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 Table IV . Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples (continued) N PM A"" Aft ftM m BMwpie BDxOd MBhnwlt RSanland R Wmay Nw .e Ovww**t r%j ~~ ~ ~ ~ + ~ >e eft Not in>l&?Y* RiaotwW tboaA ty bBnipN PNoavM Wtowry v* r. Mtrt ~wvt +~t~e Dl-1 Po1-pf00f-"1104 (CmMnytKtvM0 1p 1 q 10 ND 0.00 DC-1 -F01-pF00i-001110{ 1CatMnlqR4NDn 1Yry 100 ND 641 00 ND 1 .46 110 t.00 16l 06 ND 90.9 90 740 102 62 04 q.-1-P01 4PFZ10i-0441101 pCONMw 40 C. t0 M M* 10 NO 7.44 74 oa73 9100 as e.7Z 15.9 74 DL-1 f01-F'FOOi60A41104 ic0ow1a01~D.lalwOrrl 100 ND 04.9 as 0.373 OOA 90 0.72 102 93 Dl300 141PO001404 1 f 05 0e400 fiu.NrwOp.r 10 ND 0.36 M DlSi01 44W001 Q-0/ N05 4060"M NO 9. 40 W* IMP") 1100 WD 05.6 as ND 9.20 ND gas 02 IOD 130 139 t06 256 lit DL1i1D1 4 9W 002-0441106 I 304106116lYw 0. w MOMM 10 /tD O.N s/ NO am 9Y t00 100 Dl SF04 MBIM002-0-0i110 s 1CacNM/MN.tWwriMW 100 ND 90A /q No 106 100 t00 10 :1 no D W 401 IASWOOS0411105 ice 040401104 l 000411100r1 10 NO O.Ip Ob ND 9 .30 00 1" 154 D41F0/i1$M0030-00100 laNMMiy".+Mwe w+i 100 NO OOA as NO 1 02 tog 1 46 264 toe oL3-F01-NiYV004-0 .Oi1106 toam"NltR.rN 00.1 01.34 014 SY11004-0-041105 (000M4M 04& 1t00peY 1 r10 DL3 F0 I-A/O+ry00 5446 /106 10w~wtD0~.0ropprOw .l DWF01-MiW0064-0t1106 KNOW 80 0 4 10 we sake) 10 NO 100 ND 0.49 06 0.216 9.010 5.64 OB 0296 102 94 /90 7Z3 102 190 301 1 03 10 ND 9.00 56 0.300 1 1 .1 107 173 103 100 ND 100 100 0.369 10$ 105 170 ylE 70 OLiF01-1A9F>70{4041106 IcOw~wOMO te~r9pir~ t0 ND 9 .10 D43F01dOBFO0U000110 5 RMw>~~.+~M>r+r) 100 1) 04.8 06 ND 11 .4 96 NO 10! 11 4 100 110 110 1 34 2 11 11 6 Ol3 W t-N01'003OOt 1106 40aww 40 0.191M01aN 10 ND 0 .00 9 ND 1" 104 lie 1619 00-F01dMB1'002O4f t 100 (OIOaw 9M IS, a01~ i~w t00 NO 0" 00 RD 103 f02 116 218 100 U W -i01-109F0040-04110 6 tCnu 66M ya1,1epbi Ow 10 ND GL 3.F01-M8F003 4HOa110S K7om$rMiMr .+toMOoou 100 WD 9 .32 9" trf ND 11A 110 01 ND 107 107 759 020 70.0 /00 11i 'O+iro NOW" riowis to "prit0 WM wqwwwy. tlwMra M W0 4%w Mmwv "Am arnd be wk~ ND Not dai wW M or 000 th+0 of ousWlMfw wfyrA r 02 no Sw` wMgh l~ !N1 NO IpOfl sd dn 00 qMiM1I0aM011Mwf MAv& Nl~MI~ nwY iIrA117~ bTMN N. NaMC ONw . Oft w. .rr bw Mowr rowww w .Mr, *MOON wW.s .a~y+X.v ~i11Ah tnr O. ..Ia. ti Ow 1. . ir. Exygen Research Page 40 of 132 p . 41 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P400113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS In Fish Samples (continued) ,rpY if*" CO C" Mo wna&" M Y+9rtq1. Rroowoll ft oswrY i11Wnp. fEroWA od ftaamy . K mawlpl. m Roaowod IMN)WOWL Arcawy D13.F0!#FaF004D041,0 5 KOOI NMtMtK100Ni W 1o ND 0.90 90 ND 11A .: 110 130 Dt.3f014Abfti04-0-04 1106 -, qOatrN Ilot 0u 11 M M" 100 NO 90A 00 NO 104 104 .130 1" 2 10 100 Du~ot w~0as0 .an0s I00+Mltor0.to mrow.) 10 No 0.l4 00 ND 10a 100- Ol}i01.N$FOOi-0441106 , KaMrartM.0uoMMb ) 100 ND OS{ 96 ND 094 , pf 4 1 .0 912 six ttt 9{ DNGi01-IW40004-* 11106 I01101660 1 0 Gr 00 tMrq t0 NO R90 Our i0wYV003 .0-011100 tOODUwalOr.irooMM~N 100 ND NA 83 0.300 9.Q $1 612 764 84 0.3R 90.8 a 912 130 16 OMICripldPlYD0 W -01110 5 If%GMNMsR IOA >trrw } 10 0.700 011C,f 01dP1Ar001b0/1106 1COIMIN 411L IIOAY 7rM1 100 0.700 9.04 004 77 0 .30E 00 0.306 . - 9.70 a 9iD 104 104 AR6 107 ' /65 SO 1JINGf01-IP W 006004110b PUMM A I,+ 6 M411614 DMK F01 M~1hf006-0 W1106 qOPtra trA<J . 140 r" p"1 10 100 NO ND 9.0! 00 0270 . 10.1 90 . IM.4 !/.4 M 0.Zf0 106 106 i4A 75.9 1lY3 N DNGF0140WO0S0 0/110 6 IOONUwio KwrNyMrl 10 ND 9.94 DMGF01-ME 010003.0 W 1106 4C=MMwNt L. VmwO fMM 100 N0 92 A YO 0.60tt 110 112 0.'J 07 10{ .10 4 106 a64 364 30 454 110 OIICf01 .fA3VY00 W 011106 . {C06WTpiC,t0MM~1 10 0.310 9,aZ 42 1 .90 12 .1 , .102 . 23i jyp D11C.FpLMSw004OAY110 A+wqMt4N0 O lM0iC rl 100 0.310 924 02 1 .90 101 . 96 . 256 313 94 0I00GFOt.MSriI0066UM1t 10 0 0004"M so 1, to Ppe SOW 10 ND ale 92 kw If* 100 NR NR MR DNC.i'O t. W YM000.0Ot110 6 IOwiMMMr.tooowlMq t00 NO 03:0 91 0.900 110 /17 NR NR MR O OAG4014ASV002444 110 0 t0oowMM 0.1o1MNb 10 ND d76 04 ND 10A 101 DMGiq1-NyPoOl-p-041106 , Icnow 1111 aptn6 t10wr4w1 100 ND 97.0 f! M 104 , 101 Nlt NR NR MR NR NR DMCrFQ1i~i00if0-0N 106 IOOOwooqwtiu loualwr) 10 ND s20 42 No 10.4 104 $4 .9 DAIC.i04 4ABf000-0-011106 dca~ MttmlMMw! 100 ND ; 07 .2 67 IO 110 110' . 911A 101 104 /N , rivw MMw a.ww srWrq M .r pier+y' rrMWR aa+Mw wew~y ww urwl a oraMNs NO NoS dNOdod at Cr aboN tY+W of GwnOMlon wMOh l0 0.2 ny' {+wt ~y1M . . wt-Nat /OtIWMt~WrMyOaN01w~AMra 14r bA~M~M~MMrwInT~YM i NoM: iMa Nr wwiwy WO rlNra w bb/ waft. weMryawArr ftw viry oN#* 11sw be rw n w 1M raw 40L Exygen Research Page 41 of 132 p . 42 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : PM 113 1 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) ARMUM Aft F aM AMW A" r.~ !M*OM 60rer0 1t18wro16 RsooWN6 R6catiry NBrrIpN ~N, .1. 11t. mo M1010A AM Rrad R~ry lein I Y Rid lls,ca)wry IRM. Wtit AfR. DUCf01 AIBF0040-0/1105 1C56OM01061L1000111r,q 10 ND 6.76 56 0154 11 .1 DNGF011 -1 t111Q04.0.041106 1dN10616O t.ms 4b Irw) 100 ND 6!JO as 0204 107 10e 116 123 107 11E 226 1t0 0MG444A6fCOb044110 6 Ow"w>tM4torVt>a.1 10 DI M.FD/ 4A6i0060.041106 R~+~ qO, ta~o 6~r~1 100 ND 0.52 95 NO 038 04 0 .420 122 116 /46 1l11 0 .420 110 110 146 200 114 L1MCM4Pf0030441106 pone so 6.140064w) 10 ND 7 24 D11CFOtdf0034041106 (Omtmc640P. tm o arrrl t00 ND 02A 12 12 ND 104 106 7,02 1611 61 MD 10/ 106 7.12 101 13 DMGF014PF0040Ai110 5 1aMMtotaNQlOpYfpA) 10 ND 7.62 7Y 0MGF01 dPRD0440N /05 lOOOIMGr1Mnw6M"M 100 ND 832 93 No NO 10 .7 10T 107 107 44A 552 44.0 134 00 OJ GFD1 4pf 00d-0Wo61106 /DOerMab 4t L 101Mr 01ft) 10 ND 7.46 T! D1NGt01-iVW644t110 6 Mwes" 4t1 quow Iolr.) 100 HD 75.A rb NO ND 10.2 103 48 .1 06 .4 00 40A 54 .4 121 75 Dt2-F01-iAW0064.41210 (oae M%6 [.1iw +l0 .1 10 D12*01 4W Of b-Op{ 121 5 taoo~a. t~r r . m Nr yr) NO 6.44 84 ND 10A 100 100 NO 132 tq NO 102 102 492 $9,2 100 40.2 142 91 DL2F01 .Ip W OL6A.Ot121 5 f~+MWraiMGqa~lpr/ 10 ND 6AD 60 ND 11b 11s 01.24014PUI005.0.04121 5 IcoKrriwO,~a~p6r~y 100 ND 64A OS NO 107 107 13, : 132 72.7 as 121 106 00U491 4149YN002-044121 6 0011"I6>Arl aM Ww3 DOU-M-AI$Np02-044121 t 10 0.706 502 67 in 104 03 NR N+1 NN K~w4adtar~ry.l 100 0100 079 67 1 .72 021 01 NR MR NR OL2,iO14PWOP44d41t/ 0 IDOm06N3^4wpMpq 10 ND l06 67 ND 10A tOr p1.2-R11 iYMp[4.O W /21a (Oml"si2/qbDOMsoft) 100 ND 75 .0 77 ND 062 OS ~ 6.A0 14.6 p 6 .60 1'12 00 DO U401 -618VYU0340t1210 10e0"406 10 K nMfMN DOU4:01 JUaW00D4W 1210 lcanea~r IM~+r~wfW1 100 10 ND 1.19 111 10.4 ND 6!A Ol 10.4 10A YO 105 96 Not MR NR MR NR NR '9~ro1. r.rir. . .cwr ND . Not dw1c160 N I6. pliho wal .aWe~~:6~,rbt.~ a~earw t1mM d Oi.r+6tNat w6O~ .n .oettu . ~m~cv ~r r 0.', np0 (uM widM]. C~Ma a aawra NR s Nu nrawo 4~w baYflb 4aNa nwAlYUqs . 1ban~lq4 wwir e+er.ax, ln tYlb : Sb" IMri ww~wY MaM M)ar4 nIWrMl~MM. Mara" rMqc ss/ arlM6inMLt1a ka+ 4 rw~ In 1M ar Wn Exygcn Rcscarch Pap 42 of 132 p . 43 Interim Report #l fl-Analysis of Fish and Clam Samples Exygen Study No . : P004113 1 Table W. Matrix Spike Recovery PF'BS, PFHS and PFQS in Fish Samples (continued) CA Sugorg" PM M~pirk NM rand MNwrt AnN FpurM rryiN llOw d U 8Mpb R907-ad R60w wy M>!npl & OMEWOO =L Mlrt wftt (ftw .*w_ PF+IS a~,Cw S PFOs MP .11 Mil RroowNl Rwonry IN ir1rONl$ Re00+rM'M) R*op-y ww wt wlwl s0 .6 OIA-FOt4*ri0i041}01113 0 ioopN4piwt 1~M ~1 10 NO 7 .b 75 NO 11 .0 110 7.02 17.3 61 Di:J.F01-IPYY00~.0W 11l0 tpmlwp9rt~.>vMMrl 100 ND !8A as ND !19 116 7 .92 114 406 DOLL~U1~W001 .0.0N21 9 (CWAOW ftMt160M Soso to TOIL 14A 75 DOU40149*W 001-0 44121 9 lC60rrplr MNOIM SOW) 100 7.00 832 76 18,4 71 3 121 NR NR NR :A4 122A 107 MR NR NI! DO{J,f0140W 006-001124 6 ICNO s/pO.aMr too) 10 DOU .F01 Miv00640N 21 i ~ M t .+eo fM>M~1 100 4 .71 4 .12 101 72.9 R1 21 .t 20.3 M 21.7 104 T6 MR 92 NR NR MR NR NR DpU .F01i4NY/006A941214 (OpOMMt 40 4 911 7068016" 000.l01.AA6YU006404121 6 R' oarwArM memo 6yr) 10 0.304 7.06 67 10o 0.964 T2.0 77 1 .24 6.52 1.34 67A 72 06 MR NR NR NR NR NR DOlIF0, 448f006" /21 e lOoOMW IMGIOrMMM+) DDU-F014dMD060-04120 Kamm qrqwo 0" l1var) 10 1 .41 100 1 .41 6.00 72 72A 71 4.40 174 6.40 94A 02 IN MR NR NR MR MR NR 11 7-F01-I P W o0Q4M 11 Jo KarwM so 6.prM>M**) 10 DL:%F01.W /Q6jy1fi11120 Iau"M 4"/ . 1U pO >tW) 100 i10 7A2 ND 61 .2 76 111 ND 9 .0r 96 12A ND 110 110 124 160 46 106 92 t743f01 4 1M00344X11 3D IeuNwlyr9,~o~r>yr) 10 ND 7 .96 EO Olif01-M'VY0000041120 KMnuiMN,rohrlW" 100 ND 61A M NO RD 9 .M 1 02 . as 8.44 12 3 0 102 6,44 92 .0 67 DO{}Fp14A6FOQ340N216 IOMww" 9M K.10 ph ape" 10 1 .72 9.00 73 DOl}F01 -MISF000{F0 1216 1010144011104. 1q 4 tMMI 100 1 .72 90.6 66 6.90 14.3 77 NR 6.50 107 100 IIt MR NR MR 1K DOCf91 11lY0001-041210 KNOW pk C, to pi soft) 10 0220 9 .36 0lCi01446F00L1~N /21r fCw~/M6 NaNryrl 100 0?20 9 3.6 Et 07 1 .79 11 .5 1 .79 96.0 _ 47 96 MR MR MR NR NR NR vec-F01 1AiF00s0041Z1 e ICNMiM7O K 11000110ftf 10 ND a .76 64 0ECi01 At6F006 "1216 lG1o~wla1Mt410QM7lM# 100 ND 9DA .111 1 .66 1 .01 114 96A 97 so an NR NR NR MR NR dww;r wraN ne4 ) n. .Ws~ r.d .qM .~..yc ~..~w ..+oo.r. na~r ww .at a e~ar.e NO ~ NaldM6c>td4tara0awUnitdOunwtWOnWrohlsA2n4OirM~At} . /U +Nat rpalq OA1 040ft wymt on" /Mrwr . 11wNOW wo M wm drr.n Si Tom* M. Na1K AMp LY fMMMf 1M0 ihO+M mNwMI N~~AR MMAryM6r~ M ry1M6My ~w111M wM~ U 9M ~r d1r . Exygen Rewmh Page 43 of 132 p . 44 Interim Report #10-Analysis of Fish aud Clam Samples Fz}+gen Study No. : P000113 1 . Matrix Spike Recovery PFBS, PFHS and PFOS In Fis h1TableIV Samples (continued) Ar^ON Dow~ C4 OUNOrd" MN a*mnt A" FwW *, w,, 00 = pMsd h arnpl0 R~W ROOOrMy N ',wrol0 NOnOrOrOd ROOOyOry N 3rnp0 ~00 MoaneY 'r K Mi- 'x Mr r~R 00U-F01Mlf00 2-0-Wi 2N{ KbMOwf 041.+owta# .) 10 DDU.iOi.NIiF0Q24.611216 (eOOlOMOM N.tnw %ft) 100 0.600 0.81 M 4,E6 14S O.OA6 !!6 03 4,,SC 101 9P NR 0 MR NR NR NR NR DL'1i01 JPW001-0-00 f 130 iDMM~rO0NC/OMOM+1 DO -F01 -FIM10D1 G001120 1 0 ND 7.00 76 02 44 am 00 0 .04 17A ~ (OOOt0a001r0.1M 06 0pw) 100 ND 62A 12 0.340 101 101 0.04 102 43 DOU+b14 4lFa0 0-1-041 216 Ie010Mhytl 4 OqiOw) 10 0.6 0 9A0 64 tAE 14.6 00 MR 000 sot-A4ti002.i d/2f 0 te~nMSi'101~Ai0ew~1^r) 100 0.6C a4.0 61 4.6! 103 p! MR NR MR NR MR OOUF01 40 f0044 01121 6 IC=Ma Y2 i k K+01 010al 10 0.702 7.74 70 2 35 1.00 66 NR NR MR 0 00-F01418F00604012 16 IG4N7lOpLtM P06 low) 100 a702 91 .2 60 7 .36 86.6 0.3 MR NR MR DOUP014Ali001044i216 40oo01w 14 bk L 10 M>MM) 10 2.16 11 .1 60 0A 20A 90 NR MR NR QOU4F0111iF001A441$1 6 iooo~st' fp R u0'M OMr.) f00 2.10 02A Ot 10.0 104 92 NR NR MR 0DC4*01-#18F0030H 4/216 tooNS~sa0r~4wM 4r) DBC- f01-Mlf00"-04121 ! IC" MSa so", IOO M GO") 10 100 NO ND t40 06 2 .0 9 i4.0 04 740 11A N 100 104 MR NR MR MR MR MR 06C401 44F001-0 041216 IOOO0N70yt410rMOMft) 10 O9GF01 -MSi004-0-0/121 6 lasateOMJ. Ia PAiOr) 10D No NO 7.72 77 76A 70 3Ai 12.0 90 3 A7 00 .0 96 NR MR NR NR NR MR DNC-F0I-MB F001 -0-0412fi ICOOUtMape4 4OM ap") 10 NO 0M CFT1 NIlF001-0-Ot 121 s R on M70Na0.wo ab 00Y) 100 ND 0.06 91 !0.0 16 0.410 0 .42 0 9 .00 102 17 102 NR MR MR NR NR MR OL1014PWODi-0Ai 124N OWW7 Si A N IM Op" DL 1 F0 I4PVY0068041216 4O 00 Ow71y,J.100M0/44) 10 0.257 7.40 100 0253 72A 71 72 0.644 0 .6" Ot2f 01 dPW0p}O.p1 120 f KO.OOt10 7M K 10 p *rr) C13F01dP4Y003o.04120 1 10 ND 7.04 70 NO 0 .l6 93 OOA 6A2 66.5 06 405 145 76 9.0 90 7.46 0.7 42 Icr W70 ftk 4 100600y) 100 NO 7/A 12 No 92.0 92 7.40 64.0 77 '6~'~OM hbd1I~MMIW1l1~ pY~lf IwM 0 . 1/1., f~fY~.In w111W IpMy YMM "MIN M dIq1~1 ~ ND ~ Nm dONd00 M r OOow LNrt dQuOrrlsYOn wh)aA 10 03 ~fyy 1w01,wWpy) NR .NN^wyyMrMqYrlyeaWOlwMO k.W NatryWwrMrwMa .~InT16NM. 1101~c l1~0f Pds wn~wry IbY MMa~ N~r4A wOrM~.,Oaw~ry M lliw ~Mwif M/MrM~M Yn v~r~ i~ Ylr hMr rI L ExYgm Rcsmch Page 44 of 132 p . 45 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 (continued) BrnplN U CS BuMatift PFHS C! & uon~Y Amok" Aft F&AW AinowR MM iaab Awaum SO" w l n 0N ftosww Rw Wy M 8urob RR0*00-W 4K rl . ~wt ft--Y Am t In 9 1y ll~aow~d Rua~r .~l A DW"1-rYM0068W1201 l6MM79pttit0mp NM> 10 ND R70 92 ND {.9p 90 4.00 14.0 01 Ot3i01-IPN~170 1 ICaoewn 1 J. IN 00 now 100 No N2 as Np 972 97 4 .40 94 .4 90 A.WMN 'n ,w.w 64 13 MWrw OdW, 12 's..w ~ ra~a rNrunow.i+M k++~ N ..~r~ r~ ~earw wa0wy nw aree be arow ND w Not OM/d00 M Or ODp7i tJnM CI CWnqdYen Mlkt~ Y 0 .1 an t" WMM MR-ho rNOrIWiNbpMV ivK01MUR*MM. R~Nylt~~/Yan~iwnM7KM~ . NNW 916" Ow Avon"; so DOWWOM Exygen Research Page 45 of 132 p . 46 Interim Report #10-Analysis of Fish and Clam Samples Exygan Study No. : P04d 1131 Table V. Matrix Spike Recovery of PFOS In Re-extracted Fish Samples AmmjMS= pb $piksd Dsrce DBGF014PW00/-004102 1 (=alai spcC, uquppb) I ca s~ron. ~os in Sol"* wet wk. ` tnWo~ lo0Ol wne~ d Pecawry 1000 2090 2860 ~ D8CrF01-IPW002404102 1 (C004e142 00 D. e000 avb) 5000 3330 DBC .FQ14PW003.o.04102 1 IcDOref[q 8 0 E. (aoo cob) 1000 1EE0 DOU-ia014PF0p14)-04/02 1 (oooater apt f, 1000 oro) 1000 e6e 8080 107 3180 130 1790 11 a DO'J-Ffl14PF002-0.041021 (C"Ia680 0 1000 Plow 1000 038 1740 114 0OU-F01-IPF005044102 1 9=4198 Opk KIND Prb) 1000 644 1650 111 DOJ *01-IPNf002-0-041Q2 1 1C0001 00 Spk 1,1000 00 b) 1000 1210 2810 140 DBGF01-M6W0o1 O{341104 foop$RJ,ttlAOOwM 1d006 9480 23200 137 t79t'.FO t 4ASW po2-ol)4110 1 9 OD 00481 30k K 10,000 ppb) 10000 7520 19e00 01 DBC4:01-M51M003 .o.041104 400 sws2 MW I- ION ppb) 10000 12E00 232D0 106 DBGf 01 4ASW 004-0-041104 (CDOOOOl SO M lOOOPPb) b000 3440 8520 102 D9C-F014MSW0o54)44110 4 t00o40is4 3o+<I+.to.aao PPb) 1 0000 D84F01-A18F001-0-04110 4 9II (14401l6 epc C. 1ROOD lyb) 1oDOS 5M 16200 100 3210 14400 pq DBGF01-hiSF002-0-04110 4 P 0404608pc 0. 1G000ppb) 10000 4700 15200 104 D9C-F31 IPF00b.o.041104 (cttawae 30 E. I000 ppb) 1000 AQE 1600 pp D6C-F01-I P W 0 W-0-041104 t =60+a0 4k R. too0 PO) 1p00 i336 2600 130 DBGi-01-IPYVOD6 .O441104 (caaaaDeo aa00U 110 ) 5000 2820 6520 79 DOU-F01-IPW003-0fi41104 EDOO404819pk K f000 OOb) 1000 2270 2640 3r OOU-FQ1 rFW0044.pf 110 4 9 OO+aie28nk), IoooroW 1000 1740 2740 100 DOU-F01 4PN1U0641b4110 4 (COD4a00 7 Sqc J. 3000 PDb) 5000 2130 7000 109 Dl t-FO 1-Af 8M10p 14-041104 (01114O4 6 aik K 1000 ppb) 1000 O11 .F01.0i$ Wpp2.6Q41104 R MMM 8 o C. f000 00b) 1000 ON law as 700 1740 107 Dli-F014d$1AK1034.041/04 (C00404610qc D, INC yob) 1000 A6ll 1 930 1 23 Dt t -Fd 1-AiSW006-0441104 tooaaieo So e, tooo oob) 1o00 e04 1800 104 'TiOt 10pbt1M) AN b ay~y OonY01 itMd( hNlfM . VMIM ilr nol YIduOW YI aM MAqlfr t~4411~C4 Exygen Research Page 46 of 132 p . 47 Interim Report #I O-Analysis of Fish and Clam SatWles Exygen Study No. : P000113 1 Table V. Matrix Spike Recovery of PFOS .in Re-extracted Fish Samples (continued) C4 suron.rn wos sA~np~. BpYkW D O-F01-M8F002-0- 04110 1 (04016411 sfpa F, 10N op0) 1000 in s.mp . n.l wl R.cw .no R.oo" ry (noolwal wt. x 6E0 1060 112 DLt-P01 4A3 F0064041104 MOO6w74 ayk 8,1000 ppb) 1000 432 1670 12 4 004:01-MSF0064A11104 4O004 004 ta H. 1000 WD) 10( 0 740' 1090 109 DMGF01 4 ABWOOS4 -041105 11 M4900 30 1,10001q) 1000 S00 1780 122 DMC-F01-iN9F0020-04110 6 (pecNwG apr J.1000 Opb ) 1000 820 1500 88 DOll-FO1 dM8W002-0 fi4121 0 {OD0004M 39 tK .1.0WOp01 10000 26200 52700 45 DO U-F01 MS W 002-0 -04121b (COOe4~es Spk L. eolo PPbl 5000 40 40 10200 123 OOU-F'01-MSW 001-0441214 (COOMNO fpk C, too00 qb) 10000 7800 2~',~000 174 DOU-F01-WW 0044}G41210 (c OmaMt aot 0. am ps) 5000 5120 9880 96 DOU-FOLIASW0064-04121 0 tC oaeeaMQ so E, mw on] 1000 466 1 T00 128 DOLL-F Ot -1ASF003A04 121 8 (CGCECtlf'JpY F. ION ppbt 1000 720 1A20 110 OOU-F01-M5F0030d1121e (000w " so q IM pps) 1000 048 177D DOG F-01-IASFDOd-1-04121 E lCaoro"7l0 l+,tooooprM 10000 9020 32 4 00 09C-FOt iA8PoDb0-04121 8 (04000104 5r1F.10000 Poo) 10000 6 900 24100 or 237 151 DO (J-F01 4ASf002-0-041216 (C006UMi so A /000 ppb) 1000 MO 1720 106 DOU-F01-MSF40 2-1 -04121 8 10406e471 so K, 1000 pb) DOU-F01 4ISF00446.6t 121 8 (0000e+7 2 lpt t, 1000 000) DO LLF01-NISf001 fi-04121 0 ICooeN 9pk C, lDOO ppe! low 49 2 1960 126 1000 1820 2700 58 5NO 2070 7980 110 08C-FO t -6ASF002.0.041210 lC00e6/74 34* D, uoo0 ppq 10000 4640 15500 109 DBC-FC/aASF004 4). 04121 0 400060470 3465,10006 111104 10000 9200 24500 152 DMC-FDt 4MSF001-0-041218 (Ca06eae 9pA c,10oo Pob) 1000 810 2040 120 D6C.F01 a PF001 -0-041 M (0004 N40 Op 0. WW pb 4 1000 364 1350 97 D8GP01 a PFOW-0 -0t1021 ( cooul6o soM H.10oo ppe) 1000 203 1 340 106 DOU-F0I-IPF003-0-04102 1 fC~o~e~esav . tmo ppy 1000 359 14D0 104 'I~ot r1KwiM0 tlw barly cmYOl n~ /aaNaa. VaM~ Kn OatNCbO~tl in M>Nr~rrwy WYfes . Exygen Research Page 47 of 132 p . 48 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001 13 1 Table VI. Matrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples dripb ~ 91311" ~ 04 SuArao ~ ~ ~ Aft ftr4 I MS n+FN R6cv40M R-owry b36 s0M RpPwW Poem" kin ;* RroOwtl Iboowry nltwa . ~1. MIMI M'~4 tlwM. 1~iM. {Or101M0iMCMwY M NC O.a D13101 -CPW0014041210 IOuM~Itt>~4~wiP1 t00 No K4 00 02 No NO e10 02 1.02 0:3 2 OdA f0 1 .62 06.2 u 63 OW-401-CP1V001-0ON2t6 (P2uwat M k swM 10 NO 0L04 DMK'i1D1 -CFlNbCbP4t17/6 IQas",,apM .NaqN lOD NO i2.0 90 NO 63 Ni? SAM 04 0.10 11A 61 01A w ate W- B 07 C1.3401#MtOD14041216 IOOO~MIIQ so qNMy 10 NO Ol2-tO14FM1001-041tT11 6 9010W 10 4tmlibl 100 ND 720 43 0 77 M NO ND 7.l4 101 76 tat 7 .52 67 101 1 .61 a0t 4" DBGq 1 iDMM0tl1 4W1216 tCe0MOt o N} 70 DOG01 CE NM001-0041213 {OOOr~Yal ~,~oopCl 100 NO NO 107 100 64.1 6 4 NO NO 10A t06 PT2 IT 4. 16 l46 06. 4 42 DL 1 d01-CM1Y0014ott21 6 00006 MK+erM/ 10 NO DL i.q4.CFWOD1-004 Q16 iC07E~M1iM41LOW> 100 ND 8.90 60 NO R 3 2 1] l.iq ta .0 02 86 2 06 NO 103 103 OAO 000 00 00" 1-C/MJO0U006131s PKAW tM tA 10qq 10 NO 064 0 86 0202 432 at 11.4 173 41 OpU.q1.OFW001 4146 1216 00t ilpYK t OUpp) 100 ND Ma M 0 2M 118 0 of 11.1 96.0 OT +brq~e M p Mwwe 73 iw6r~0~~Ml~c 10 7M~r60~Mwfae 16 6y .~r6p,M~ M NO Na "babO at or iliwe lMM of arM6MOn wood ~ Y 021b0 (ww wo IaM} Iler<>Mp Nr PAM" YEb IMWAia Ww~ MUM. POWMY vMYr rYV" W'r/ faM W NMw M Mr Mr 6M a Exygen Research Page 49 of 132 p . 49 interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P4001131 FIG URXE. S Exygen Research Page 50 of 132 p . 50 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 Figure 1 . T)picat Calibration Curve for PFBS In Methanol n 00/Q064YM.~(riNjlin.af'MM~~~~/~vN11MIMOTT-1 .l1~q04t .YO7M000(r .0.i0YQ) WOW e.i . e e.o.a 0405- 5044 {940 4A~0 9-0 .4 2bd 2G .6 13d 1.046 0-0W 2 4 E ~ 10 12 4 10 M 20 22 24 20 M YD 32 74 ~0 ft ~0 12 M 46 O6 CoMmYri~n. epy Exygen Research Pap 51 of 132 p . 51 Intcrim Report #10-Analysis of Fish and Clara Samples Exygen Study No .: F'Q00113 1 Figure 2 . Non-Extracted Standards of PFBS in Methanol, 0 .0005 g1mL and 0 .001 g/mL, Respectively ,!lfV0 - Pm A-4-0 ""Us Ahr OW-aft 1itMQ ?!'R c+s or 4 Sf2 ml0 0.6 1 3 00 210 ~ 2w ~ 100 tOD .41 4 2 .40 3& 10.42 1212 13,42 MAO n - All ' 1 Z a s s s 7 10 11 n u 14 10 t0 n Tle . Ob ~ ilT2~Y~K6fCUMOMQ200AW0A we rrtN 0 2 1 30 +tim00/eO6l.wiA Arfx 16T puMr INIqt 70l . M M : 031d wl ~ 002 T0 0 E06 g 7DD Oh:A !00 4" 1 .22 1.!!.. .'A 0.10 10m .104t 121 4 + : ~ r s a f 10 I 'l t= ta 16 !0 n tr, w. Exygen Research Patge 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 g/mi, Fortified Control Fish Spk A, and 0.025 g/mL Fortified Control Fish Spk B, Respectively , ! ~at fi~qi~Wa~1Y0 A~aww,2M,Mp~ .aara .wapp .N~Ma NJ~d6BwM g ii` 4o aM ,ap 1/ 3.01 47a 3.79 a.41 7'~" GAS 1020 ,.m a.u , 12.2. '403 -"34 17.13 2 s 4 a s ~ a T.M. M+, , R n wN SO A Raf (OQ 200.009 awr sample 0 d31 bw 00100QE.da 74174 w .r4 IMt1At 1100 . .1 . RT : 4A2 WAS 10 tl tt 10 14 10 16 17 4012 `~ 104C Ow . 2 .52,,i~t 0J01.67 !~ 1 2 3 4 4 a 7 a i 1D it T MO.. AM , RYaM/apl P Fia1q2Y.OOAu .u . uap 1.t1 .11aMO00100faw11 ArN:2,t0 o.wHt Wyit: . *I UT :OA27 e h 12 13 1ve 1a IS 11 1aM OA 1 .0M 'yl 40CJ0 .0 4A4 a 0.0 2 J 4 f 0 7 0 a /0 11 13 t~ 14 1D p 17 Time . tin ExyVn Research Page 53 of 132 p. 53 Interim Report #i0-Analysis of Fish and Clam Sampks Exygen Study No.: P0001 131 Figure 4 . Chromatogram Representing a Fish Sample Analyzed for PFBS (Exygen ID: C0049478, Data Set :061605E) ~l~yR+Mwqt1ltMlllrwa+ MVh21N71RM~Mlillf.rA Mw a7~ ..~..r /i~~r wu a'. Atr aw.h ~o a ao es ao +e - ~o ia w + : a s e 7 Y o +o +1 14 17 M 1s !a n Time. milk Exygen Rescamh Page 54 of 132 p. 54 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P0001 131 Figure 5. Typical Calibration Curve for PFUS In Methano l ~ ON006iFYA.M (~FN~q.ht.arPyi4. .('1l~wr101Wy~Y.Z .M.~OD4K~7AMi000(r~0A001) tA.O 1 .4.Q t3.e 1.2.Q 1 .1.1t 1.0.0 ao.s saa ~ soa c e.o .e aoa +.o.a 2Do 6 iD b OD Z 4 0 0 10 12 11 10 10 70 12 24 20 it 90 $2 04 36 86 40 42 ,11 40 C.nqMUW R ~1~ ~ Exnm Reseuch Page 55 of 132 p . 55 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : POOQ 113 1 Flgrare 6. Non-Extracted Standards of PFHS In Methanol, 0 .0005 WmL and 0.001 g/mlL, Respectively =,13 ."M , PkMlueQ 7ltMt! art MM m / e/7M1Mw M1MaEw/ Arw 1H]rwwY !A1/ft 74A we RT. 11-I wM 10.7Q 700 OOD 300 Ya. - 9qp 1OD C t t a 4 o e 1 ~ 0 10 11 ~4 p 14 18 +e 1 1 TN~, n~M ~ tp21/ .KNi(ll"iarp90CDAOA sw . .maple I ,,>*.OE1l06i M Mar3S1n Mwf M~~{ht ~0 . o0s Rt: /0~ Ne 1033 aa o ~oc a 200 p ~ ,, .,o 1373 t 2 3 a 0 e s t v f0 t1 12 ta 14 Ii te 11 Time. nin Exygen Rcscarch . Page 56 of 132 p . 56 Interim Report #I0-Analysis of Fish and Clam Samples Exygen Study No . : P40U113 1 Figure 7. PFBS In Control Fish BIBnk, 0.00625 g/wI, Fortified Control Fish Spk A, and 0 .025 WmL Fortified Control Fish Spk B, Respectively , Af/~Mt G~NII M7A ~M~I~MMJ~lIwM~f~f NMMA 941F3111 R7! Ml MtZ 1N rmmu t1D1 WA6 1 :.a 10 +so ~ .,.a. soz o ua 0 +~" .ax e 7 s~s o .+a . ,~ase em 1 s a a if s 1o e1 1= u 14 ra 1s n 7w* . ** , 40844F ts 0 A WHO (OC) 3 GY.OrOD am ""Is 10 N7N Mm 001N0/i.rM 7NY : ,l0711 SOWN 1NMN' 12M. OW PT: 193 IMS 1 .OON 1 t0as Oo00 O b _ YJ7 ODD + : s a d s 7 a o if 1~ a w 1a n ~ Tr.R WAR Ne aO .M 009 rF N! jOQ 7Y0 .pA0A asw -="16 11 N]I t.n 001000EwN !4K 777p~ .w~Y N~Mt 7W00. aK NT:10.a ml~ 7r0 " 10 .i0 2A" , O~ 3 + e 0 7 s o 1 0 1 1 n ,s 14 10 is 17 TY", ~I Exygen Research Page 57 of 132 p . 57 Literim. Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P'004113 1 Figure 8. Chromatogram Representing a Fish Sample Analyzed for PFIIS (Exygen ID : C0049478, Data Set : 061605E) , OIFHIT~ MR RAr~wnr~) HR~ ~ss~o -an W N ~IK~ i w Klf~fE~NI ArMa 2Nf1 cIwY ft/Oft 1= ow RT_ M w/i +ooo 000 too ~an wo 4W 300 Ma i0o '1 t 0 4 s o r s i 10 11 1: ti ts is /0 n TM., Nn Exygen Research Page 58 of 132 p . 58 Interim Report #10-Analysis of Fish and Clam Samples Exygan Study No ., P0001131 Figure 9 . Typical Calibration Curve for PFOS In Methano l ~ OlMD6EFirwrN MCI* 'Un. . f 11./wr" C~ ~r wliMkMY Y- 1 .16N0d1x .3Sl .MD3boAY00) 61 d Ob 46 OAwi 4L .6 oa .s aaa 2L.6 iD .6 6.OM 2 4 0 tD 12 14 15 tY 70 2Z 44 10 2i 76 22 34 iq 30 40 40 M 40 r p CwwM .M.. .N64 Exy$e' Reacamh - Pagc 59 of 132 p . 59 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: PU04113 1 Figure 10. Non-Extracted Standards of PFOS In Methanol, 0.0005 g/mL and 0 .001 pglmL, Respectively -PPM , if9a! pbManQ IlLNL O am rwA I Mi ~ epMOR+rw Amt- sxfswMt Jhro a *I** xrs 13 3 .r. 14 .,e .oo 'oo 1Z ~ 1 : a e e 7 o to 11 u u 1~ 1f ie n $V77 - Oral AUMw.94 pp DqQC uw *ryl . 2 Ow hw. at W6EsiM Arl' 1~!!T Mvwk Ndk ppp ya RT: 1~d wl~ I ~ 11i7 ~1Llt 1 : ~ 1 e e 7 to It n 4 14 te 1e 17 Tem . . whi Exygen Rcscarch Page 60 of 132 p . 60 Inbcrim Report #10-Analysis of Fisb and Clam Samples Exygen Study No. : P0001 13 1 Figure 11 . PFUS In Control Fish Blank, 0.00625 glmL Fortified Control Fish Spk A, and 0.025 gimL Fortified Control Fish Spk B, Respectively ~ Jt.ry..t C*.a.r .prostMh...1 4MNU ... ..rw O .I 7/n., . M'lMWaaw Arp.: 27r ee..e. lAi.rr stlDr xr. ln.l .a M p "no y 12 .10~ C CA 121 1YY ~ 4.48 1 2 41 64F, .a 770 t.1 020 D,q 14AD .1D N3T 16A0 {IpD= 0 y 4 t 9 7 0 0 40 H M 14 14 16 M 1 7 Tl.~., nJ . , II..NntipkAtf0ll'~hi1DD.MODiew-,.e,,~1C~faIwM00100QEWY Mc ~1DDD ea.At lMyAC QOq, ~M NT: 1Z3 wir 49,00 . 12.4i 2D00 ! D 4 s 1 0 to 41 TNM. m w p .auAiDMY/rof (D C)4DDAAOD, .a .swpN14q7qinm m/eoeCalR N~c 2T141 ew.Y NNplit 10D00 . Mt RT: YiA nie 42 1a 14 16 1p t7 12.40 1o . a O tt oa 2 i 4 0 0 J D /0 11 it la 14 1A 10 1? TYm,n M Farygen Res=h Page 61 of 132 p . 61 Interim k" #10-Analysis of Fish and Clam Samplcs Exygea Study No. : P000113 1 Figure 12. Chromatogram Representing a Fish Sample Analyzed for PFOS (Exygen ID : C0049478, Data Set:061603E) , COMM PFOd w++M+) 46 MA se w mMph 21 07 0 If 60 IifiMl.w/ AW~ 1Q/lNCwtr iwl~Itr fJOrKpoe RT:72l oO 1 fM 1'1~6 1a~e O.o.~ an .s 4DN ~ .OM 7A~4 1'a'~ tt OA 1 2 3 4 0 0 7 0 0 t0 i 1 t2 ra 14 10 4 p Una, mi n Exygm Research Page 62 of 132 p . 62 Interim Report #1 b-Analysis of Fish and Clam Samples Fxygen Study No . : P000113 1 APPENDIX A Study Protocol P0001131 (Exygen Study No. P000 1 131) with Analytical Method, Protocol Amendments 1 and 2 and Deviations 2 and 3 Exygen Research Page 63 of 132 p . 63 Interim Report #20-Analysis of Fish and Clam Samples Fxygcn Study No . : P0t1Q113 1 PxyFa homcol Numb4 c P000 1131 STUDY PROTOCOL Study Tide: Analysis of Ferenorobutanerulfoiute (PFBS), Perttaorobe=anesulfonate (PFHS ) , and Pertluoroortanesulfonste (PFOS) In Water, Soil, Sediment, Fbh, Claws, Vegetation, S>nall Mammal Liver and Saull Mammal Serum Using LC/MS/MS for t h e 3M Decatu r Monitoring Program .- Exy g en Protocol Number. P0001131 Bxyp a RastacL sea= RtwffA&wM- MkMael A. S.ntao 3058 Reuwc h Drive Dimccar of Regulatory AtFam Sate CoUeee, PA 16801 3M Building 0236-01-8-10 Phone : (814) 272.1039 St Pwl, MN S5144 Phone ; (651) 733-6374 oo- Pve f 14 6j Exygen Research Page 64 of 132 p . 64 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 e"M MWd NUMber roool 131 DI5TRtHU"t ION : 1 13aiwmlu Kan, Study DQacW, WeMoa Solu6ow 2) John M. Pl.haty. Prineip .l inwatipnor. ExyIPe* Anseseeh 3) Michaai A. Saotm. Sponsor RquwwvtWva 3M Company 4) Exygan Raevch Qudity /wuance Unit per 605 Exygcn Rcscarch Pagc 65 of 132 p . 65 Interim R,cport #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001 13 1 R ry80 Prototvl Nmber POAO I 131 e "` PROTOCOL APPROVA L 3tady Titir. AnNysis of Puftavbnanarlfonwe (PFBS). Perttuonoheuoml6aute (PFFIS). and PerfiuotooctweaWfonate (P F Ofi) in WaW. Sa1, Sediment, Fish. Cfana, Veptefion, Small Mammal Livon and Snan Mammal Sam Using LC/MS/MS !or the 3M Decatur Moakain; PAro gmm Hxygp+ Protoool Numba : P0001131 APPROVAI S ! .tom4l, gsim West= SoIntims r~sv Michuel A. tom 3paror Rapisenw ive o 3M Canpn deulllM. FwNaaty, a{pd Invea6sa t" ExySen Re semh ~ -` Doe Richard A. GqOW. EXAM dam . Facility Ma ngema l ccT'- ke) W/ Date L StwtTer, Tao4t " Exymm Rmmz eh Qouity Msurms Unit D&W r~ Peyr ) e/'6S Exygcn Rcmmh Page 66 of 132 p . 66 Interim Report #10-Analysis of Fish and Clam Samples . Exygen Study Na. : POOb1131 SsYaea Protacol Nrmbci : r000113 1 r+ TABLE OF CONTENTS ... ... .. . .... . -I DL4I7tAiV1lON .._.... ._..~_. ._. ....._ .._ .... .......,. ._ .._.~.... . .... . ...._ .-_ . ._..._.. .. . .... . .. .! PA01~[ OLAPPRDYAL_ . __ .. .. .. ... .. . .. .. . .. _-.. ... ... . . . .. .. :_ ., . ._. . .. . .. .. ... ._ TAM .............. . ...._....._ .. ... .. .. . .. . .. ..... .. ..! . . ... ._....._. . . ... .. . .. . - --_- . . .. .__.~ OS/BCRVE _ .._ ___..__.. . . _ __ ._ . . ... _ . .____ ... . . .._.. . .. . .. .. . .. . .. .. ... ....-_. _-_ . ._.. ...._ ._.. .. .. .6 S'BSTWOFACQ,(TY._ . ........ . . .__ ._. ~___ ..... ._ . . .. . ... .. . . _ . .. ._ .... _. .__ . .. . .. .._. ------ 6 SFVDY AOlHCtbR.---~.. . .. .._____ ... .___.... ... .. . .. . .... ... .. ...M .. .... .. . ....._ .. .. .__ .__ ..... . .__- .. .7 rRII~ICJPALQIVYSTIWTOR ._~ . __ .__ .______ . .__ _~ PROrOSBD 6XrEAt)rtENfA18TAltT AND TORMP7AIION .- ________. . .7 IDENTirICATlON AND 7[1STflRCA?10N OF T11E'CSaT EY81T'M .. ._ ... . .,... . . .. .. .. .. . .. ... .. . ..... . ..a SAMPLE rROCtAr&d47+1T . tBCB WT AND RETENTION ~ ., SAMPLE . .. ..... . ... ... 9 ANALYTlCAI.TROfMDIlitESGatARY... ..... ...... . .. . . .,., . _ . VER3}7CA.T10N OF ANALY17f'.AL . ... ,4 10 P7AOD FOR COM'tOL OF BIAS _-_-_.~ BTATfTtCALafBlHODS . _ . .. . .. .. . .. ..... . ._ . . . ., . ..I I d1 .P STATL~1l~Ni .., . . . . . . . ..,.,.._.... ..__ . .. ..... . .. .... . .... .._. . .. .. .. ..1 1 REPORT _._ . ._^__ _ .~ _ .., ... . .__. . .. .. ... . .. ... .. . .. .. .. . .. .. ... . . .. .. __ .. ... .. ..._ .. . I I SAFETY AND .. . ..12 AMENDMENTS TO rAC1800L _ _ ., .. .. .__ .... ..__ . _ . .. .. . .. . .. . .. .. . ._ ._ .. _ _ . .. .13 DATA RECORD 1CEEPIIiQ ....... ... .. ... ._.. ..._ ... . . .. .__ __ .._ ..,,_ . ..13 QUALT[Y ,... ._ . .._ ...- ., ., . .__ __ ._. ... .. . __.. .. .. . .. . .. . . t4 APtFNlION OF DATA AND ARt7WRW ._ ... ... .,., . . . ._... ._ ..... .. .. . ..... .. . ... ._ ..__..__ ... .. .. It APr6NDiXLANALYt1CALMSt7i0CS .... .. .W ,. ,. ,, . . .. .. .. .. .. ., . .. .. . ..... .. Fwfof63 Exygcn Research Pagc 67 of 132 p . 67 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : Pa00113 1 hype Phwaeot Nu *wr: POOO 1131 01' INTRODUCTION The parpae of this uudy Is to perfam wratyeit for perQwombuteneaulfonete (PPBS), parlluoroboacueMdtonata (PFFtS) and 1xrAuoccoctanaolfo rfl te (1'FOS) in water. soil, sediment, !l3h, clwms, vegetation, small mwnnul liven and small mu=el sw= mung LCJMSMIS for the 3M taecatMr Monitorisjg Prop- Tb3 study will be "led for tompliaece with EPA TSCA Good Ldwswry Practice Standards 40 CPR 792 by the Quality Assurance Unit of Exygen Ressamh. TEST MATERIALS The cm materials are paclbcxotrmr netulfoaate (PFBS) . pcrQuaoh~ocaneeul Ixnete (PFfIS) and pafluotooetanesulfio,ute (PFOS) and we all lied by WE PM Chemial Natoc P Molecular Weig x : 338 xtpptied as the potanium salt (GFSOs'K') T.ot NwnbW. 10 1 Purity 96."MA Tmdtions Monitored: 299 -e 99 Srrttcst~r~e: -~Spj- PFHS Qieedal NAM Motecahr wa ialx : 438 supplied as the potassium salt (ciFi3sa,'?C') Lot Numbar. S603 6 putty. 98.6l6 399 0 T1i011tlota Mt701tUrtid: t Sa1X ttfe: ~ 8 ;- F F F F F i t so Pap i aj6,f Exygen Rcscarch Page 68 of 132 p . 68 Interim Report # 10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 >an.4 Pwsoml wmnu ..: P000113 1 ,... Prns Chemiwcal Name Pflworooct inrwl Foo ste Molea Lr We[itX: 538 supplied - the potasaitnu satt (CsFij3t)sTC) Lot Number. 7 1 7 PurIrY 8 6.9lt rtonsiaoo. a ostiootsa: 494 -4 99 swuca.m- f F F P FF F Spy- F OBJECIM The Pupoto of this study is to pCrfo M amlyAu for p wftuorabu>uiaulfonatc (PFBS3. (PFf1S) and Pafluotooctanesulfaoace (PFC1S)1n wow. on. "&aadt, l4k a1mN, vertabaa. stowl mammal liven Pod email mammal maan (b; the 3M Decatur Monitoring Prognm uw g it, ,~ catrent voices of tho following ExyBw w vjtiul metlwds : V0001780: '7wletfiod of Analysis for the DNoma~rtion of 1'etfluoraoctxioic Add (rFOA) in Wow by LCiMSfiW V0001781 : "Mathod of Andysis Sor the DolwmioYion of Pxfluoroocunoic Acid (PFOA) is Soil by LCUSIMS" V0001782: "Method of Analysis for 11r Ddprmiostian of Pafluorooctanoic Acid (PFOA) in Sodimeat by LCtMS/1NS^ V0001783 : "Method of Analysis 6or on DeMenpimti w of Padluocoocnnoic Acid (PFOA) in Irish and C1aM by I.CMS/MS"' V040 t 784: "MoWod of Analysis for the I?ak+eudevtion of PorBnocooctmpic Acid (PPOA) in Vessl .tioe by LC/MS/MS" V0001785: 'R4tathod of Analysis for the Dqermtoution of Pertloo:oocunoic Acid (PPOA) in Small Mammal Liror by LCiMS/MS" V0001786: '2iEthod of AndyYi for the DMOnniaation of PMharooat~wic Acid (PPOA) in Small Mammal Sarum by L GM W&S" TESTING FACII.IT Y Exysm Research 3059 Reseath Drive Sirce Collem PA 16801 Phonr. (814) 272-1039 Poe. d afa s Exygen Research Page 69 of 132 p . 69 Inter.m Report #10-Analysis of Fish and Clam Samples Exygen Study No . : PW 1131 ~-- STUDY ]DIRECTOR Jaisirwha Keuri P.E., DES Waloa Soluliau, lue . 1400 Wepon Way West Chewr, PA 19380 Pbonr: (610) 701-3761 Fa: (610) 701-7401 j .ke~ri(~wa~towotationi.caw SPONSOR REPRESENTATiVE Michsel A. Santoro 3M Compayn Director of ReB,utdory AJWn 3M BuiMing 0236-01-810 St. Pad, MN $5 144 Phono;(6Si) 7334374 ikYIAa ProsmW Number POW 13 1 PRINCIPAL mrsnGATOR Jotw M. FWaiy lsxpgn R,awaocH 1058 Rereercb Drive Staie Colkge, PA 16801 Phone: (814) 272-10'39 jolr.saha RyaKygca .oom PROPOSED R"ERVaNTAL START AMID TERMINATION DATES U Is Proposed lbat the m.lyttua po,moa of this sWy be coaducted &nm Oclobex 01, 2004 to Daoturher 31, 2005 . The actual e:paimaitd stan and 1rp inatkoa dafM will be included ip the Eae1 tep oct, ~. . Payr 7af6! Exygen Research Page 70 of 132 p . 70 Interim Report #10-Analysis of Fish and Clam Samples. . Exygen Study No . . P0001131 EayVro i4otawl Number. e00I i) 1 r- IDENT[FiCA1TON AND JUSTMCATYON OF THE TEST SYSTEM The ibUovi+ias ar. the tog system for this *Sdy .' Water (p utdwtter end set thoo wttr) Soi1 Sadimm l FM . Came Vegaldoa Small Mammal GivR Sma mammal UP= The raaopla wi11 be oollected by Watton Solntione. The oontrol samples will be pn~had md PtePued by tto testing fiic+'ifty. Pusvbaee and processing details Ax the control samples will be included in the baal report associated with tN widy. The WO systems were chosen to access the mviroomeoht impact of PFBS . PFHS and PPO S in the Decaqu. Alabama p sea. ~" SAMPLE PROCUREMENT, RECEIPT AND RETENTION Wdr~ soil. udimep% $elt, olaq vqlaFatiaa. small memmJ fiver end mull memmol awa rmplor will be received at Euygen directly from Weston SoMiws. The detaib of sample pioawmmt for this study am outlined in the 3M west On endued '?hue 2 Work Plan for sampling Environmental Medis." The wtnber and typK of aan or collected will vary depending Rvail.bility In the Hdd. The WW number of samples received and analyzed kw each matrix will be documented in the Rnat report ueociatod with this study. Water, wil, sad edicaenl samples will be used as received without fiuthw Processin g at Exypa. These samples will be stored rettiga rsted at 2 0 C-E'C. . Ftb, de;: . YmfsAon and m ll mtnasal liver samples will be processed GCOW641 to the +Pp OP riste analytical method (we Appendix i) . That wnpi.s will be smrod harm at s 10'C. SmsA mw=nW whole blood amptee will be ee90i2iiied In the held at Ow time ofsollaKioa and the wnm fraction will be used for the .ady. Small mmaw sstugo will be gored IIvzen st S -10'C. The rexaipt od processing of the samples will be documented in th e fwa! .~ report and raw data associated with the study. ~ Ae~edaf63 Exygen Research Page 71 of 132 p . 71 Interim Report #1 0-Analysis of Fish and Clam Samples Exygen Study No .: P4001131 Bnyra Ptoeoed NrtT* er. pOOp f 13 1 SAMPLE I]DENTMCAITOX Prior to aoatysie6 cub sample ..i{1 be aeignod t laboratory sample ref=rnce mmbar. The trferoece number will be sudque aid will distinguish each laboratory ample that Is processed ehtoughots the analytical procedure . Ciromrtovaphic data will be idaititied by the laboratory sample reference nrmba. Sample storage oeoditrona ad bcatiam will be documented UYVUghout the auay. ANAI .Y71G1L PROCEDURE SUNIMARY aefecaooa: 'OOOI 780: lathed of Analysis for the Detaem{nuioo of Pa aroroowaoic Acid (PFOA) in Water by LC/MS&W V0001181 : 'Moqmd of Analysis for the Datamimtioa of Pafbiocooctanoic Aoid (PFO1.) in Soil by T.GALSIbIS" V00017a2 : "Mp1ad of Aualyw for.the Drt4cminstioa of Porfluoarooctacaic , . . Acid (PPOA) In Sedfioent by IrdMSr1KS" V0001783 : "Modad of Analysis for the Detaetoisafion of Pecflua+ooe:anoic Acid (PFOA) in F'ieh and Clams by LCJMS/MS " VM01764 : "IrSotlwd of Analysis for the Daqa issfioa of Aatuocooctaao ic Acid (PFOA) in Vegetation by U`,lMS W V0001783 : "Mahod of Analysis for the Determination of Pertlucxooctuwic Acid (PFOA) in Small MAnwrl Liver by LCtMSJMS" t'000 :786: "MpAod of Analysis for the pdaasiastion of Perfluocooctaao;c Acid {PFOA) in Small IMu nmoai Serum by LClMSiMS" ~e a>>wro me'.iwJs we analytical madiious capable of separating th e isomers of PIFBS, PFHS sad PFOS. The $qd report will include the isomers auAwd into tow PFSS. tow PFFiS, ad total PFOS fou nd . VERIFICATION OF ANALYTICAL PROMU M A laboratory control sample will be usad for the prepanti on of fortified Cawotnhtxr4olanrmd apdlade. dTtohethteonmraetbrieotaanvoiea awmililorboepimpuetltee.inw solutions as per the For water atmplia8, pxygon will supply tine bottle per sample collected. The bottles will be 300 mi, prackmed Soilgpec Pr=ior wide mouth IiDPS bottla. Thae bottles have been routinely used ft Auo roehamical sample PW 94foS Exygen Research Page 72 of 132 p . 72 Interim Report #1U-Analysis of Fish and Clam Samples Exygen Study No . : POU(11131 F-YRa+ hognol Nmuba : P04D113 1 oolleetiou It the tadaS kidiHty aid have been >Ihow+a to be fte of PFBS, PFHS and PFO3 . &mpla will be added to each ootttdaor to a volumetric fill Me at 200 mL A 6eld dtqliate, a low lSdd Vat ad a Stigb }Itd qa7cc of each ample will be oolleetod. The low and ho field spike bottles will contain PFBS, P6'HS and PFQS at well as pafluaoooGwoio acid (PFOA) aad 1 .2-13C pa8tronOodtwoic acid ft PFOA). PFOA and 'rC PFOA are included in the solutions used to spike the wmplet . The results for PFOA and "C PFOA will not be ripened in this .Wdy. RxyVa will supply one new blmlt (owtrol water) and two field bLdc spikes (coatrol water testified with PFBS, PFHS and PFOS at a low and hith level) for every trveacy samples ooflaotad . At OW testing faoility, sub wauc sample (exobidias Held dapHcates and IIs1d pltos) will be extracted in duplicate and will also be fortified At a low and WO ooocantr'Atian wfqt PFHS . "HS WO PFOS and roomed tluvuib the described procedure, to determine method accuracy and to check for bias . For aoil, aedinoaat, olAIms, WA veSDatica, EttyYaa will supply ona $00 mL Pock=ed Se3/Spoc Premier w6ie mouth HDPE bottle per sample collected or arip-sea bO& All wWamWtmt8a no for sample collection will be chipped to the simple location. Smplea will be added to each container or bag in the Geld. At the Seating llcUity, aaeh sample will be extracted in duplicate and will aLto be 60rfi6ad at s known ooocattrstioo with PFBS, PFHS aid PFOS a t rbolh a low and high level and processed ffirotiSi, the described procedure to detarmine method accuracy rid to check for biat. For small mammd }iver. ExySW wili R*ply a 30 mL polypropylene tanutthp tube., Par waall tnlanma! lerum. FTyVu will apply a collection kit for each armpb oorftnung Our= sepantar tubes (red bp), rawtaiaara, needle holdara and a>Mdln, trtaatar prpcltoa. Mad Pd>Propylens ttibn, At ft tastiIIS beiety. each Sh at and serum umpb win be extracted in duplicate and will *be be fortlded at a lcuorwa ooeemhatioa with PFBS, PFHS and PFOS at both a low and high level and processed through the d~ procedure to determine -dkiod accuracy and to check the bias . Low and high i' }eveL for each aartrix aro dcfined below : >~taMs Low Lere! H Level Waller 500 m/L 5M nj& Soil 4 a sed~.x 4 10 ;p ryll 40 n lpp cum usla 10DOWIZ 3ulI= 10 null 100 AW R Lfi'et !b 100 FIFIR Smdl 1ulamma) Senuu 10 ml. 100 L Parr /a 0/45 Exygen Research Page 73 of 132 p . 73 [ntaim Rrpoit #10-Analysis of Fish and Clam Samples Exygen Study No . : POOU213 1 Union PMecal Number: P000 1131 Raavcria are anticipated to be botwoen 70% and 130% of Me fonirced levelr, Doaevetr. t!e exact proaaioR and accuracy will be determined by the mal* of fte quality control Wmplw described obove . A wtement of accuracy will be inoladed in the 6a d mpos. MRi'ROL FOR CONT'kOL OF BL1 S Control of biw will be addruaed by tating repoe jenuavt pdr "Mpky from a hoewgaaooua matatm of rich aatrix from untreated control eampta, and by anal 0114 at least two kvelt of fatolHcatione . STATISTICAL M21MOUS 344tio ia will be limited to Slam rpeoilied in the "Jed rtxtlrode and to the caloutatioo aS:ventge tecovak% aR appUr ibie. GLP STATEMENT All ttpeob of dd study tball be performed and reported in compliance with EPA TSCA Good Labaatoty Ptrtiee Sdmdardt 40 CF'R 792 . The 6nel report or data package (attppliod to the 3pomeor) rJwtl contain a etNC nent that cbe tidy was conducted in =opUMaee with COMM and applioabla GLP standards and +viU outline any devifdons to the study lEvas those sorndude. Th:e elaranau will be eiprod by the Study Director and Sponsor ic:apeveeaistive. REPORT' A flail report WW be pnparod by the pelneipd inveatpior or their daigtxe at tiu oonohtsioa of the etudy. The tropoR rviU inchtda but wil) not be limited to, the folioW4 The nape and eddoen of tAe Stady Diter.tor, Sponsor Represeotadve, no of the testing thtU'ity. . A uatemem of GLP eompYmoe (aay related doeumentacion, such ~ dAiawf-au kody reeerda, mud be in the study recotde) . ACre !1 af~ Exygen Research Page 74 of 132 p . 74 Interim Report #10-Analysis offish and Clam Samples Exygen Study No . : P0001131 Ex"- Ptmteoot M rnhp: P0001 1 3 1 .- The OVed and dwd dalanoat .sy the Parylen Research Quality Assurance Unit reiadios dala of study inspections atd dates 6ndiRgs ware reported to the Study Director and Man s gamat. A deacriplioa of the exact analytical conditions employed in the study . If the subject method ans followed exactly. it is necessary to include only a copy of the analytical ate(Lod, Any modifications to this method will be inootponted u' tto ON repozt. If the method is pltoto-reduaod, the project camber wd prrC auoatber mud be included on each pap. Dwaipsoo ottbe imtrnanaKStion used and opaafiaQ conditiorK. AO monks lkst all site aadynd. Control and fccood &"I= will be idenfi6od and the data table will include sample rwmber ard tixtificuion level. Raproaantuive chtomODS= e for each analyze in each mmin, including cbomwgwm ofh standard and a control auaple, and a ohoomaorarn at fortification tarel. The location, of the atslyte peaks will be clarly Identified in all chrorestorwo. AU oircumtmca that m ay have Affected the quality or imell ity or the data will be documented in the ripest Locations; where raw data and the f" ripest a m to be atehived. Additions; or corrections to be l6rAl report ahall be in tiu form of a nnencluman isnod by the Study Dirvcloe. The amendment shall clearly Identify that part of the report t4w is being Altered and the reasons &n the sltastioeit. The xnandoneot will be signed utd dazed by the study Director and the Spons or Repeaept~ave~ All applicable nqauamems for reporting of rtndy raaln asper 40 CFR 792 .185. SAFETY AND MALTR 1.aboeteory personnel wiU practice food swaitatioa and hMNh h&bit a Er=7 twooablr pncae>tiw+ shall be taken to pravant inadvsrtent ntpoaur of personnel and the envuoonrari to the test or refineacc snbMto>oa(A) . Pruy tl 61 Exygen Research Page 75 of 132 p . 75 ~.~.,,...,_.~ ..> Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 e~n r~orooo Hurratr: eooot ~ a, AMNIDWIM TO PROTOCOL All sip isant changes to the analytical protocol outlined ham will be expressed in wtidetS, dgtod and doted by the Study Director and Sponsor Reprose ttative. AmandnwMt usually will be issued prior to initiation of study plan eA>tnWL Hae19vae, who t change is toquirod without sufficient time for The issue of a written ameadmaty that change may be effecced rqbnily with rsPFo1648 datmtta g ion sped and dated by the Study Director and Mowed with a writtdn ae =dMW rttr t om as poaibk. In this ase, the effective data of the written anoea4nwnt will be the data of the dooumpKed ch1109e . Copies of tba signed ameqdmmts will be appended to all distributed study plan eapx+ . The MQinat amandetatt will be maintained with the or Miad study Pb r- Any davirbi= Soru the study plan or frees the analytical method as provided will be doeunneas d mod reported ptomptly to the Sponsor Raptesattadve . DATA RECORD KEEPING Records to be maintained include the folbw~ (as appropriata): Sample tracking titam(a) ' Sample rW* r W xd* atotssa hiotay, and chains of custody History and preparation of 4-dorda (4s00A. fmctfiaKioa. caU'Destion) ~ Deaaiptioa of any modiftcatloo s to the method LiaWm aat run Woo* baxb-shws or bp Analytical data tables Ap chraaaooVaphic and jewumeoW condition Saa*1v wmya0latt a+rd avalyri s dota A mnpteoe haling o[atqdy p moarnt, apaturea and initials C]tto11olo40cal presentation af W study oo reepoadmce Any other douenwlation necessary for the m pons3tvation of tho study C11rOtaetOQ'aII1ti- AU oinoma0ogann will oaotain the followiag : Sastpfe idaatillculoq Injection Oue, trtow or otLm Indication of the arcs of iniav4 and injection number eotrpponding to the nat. Additiooatly. fati130+1tioo+ will include the amount of anatyte added sad the ampie mm nba of the am* that wn 6ortiQpl. ~ Analytical Standard dheomatoganns will additionally include the 0o roeatcatioo (e.g.. ghal .). PLyt Ij oJ 4U Exym Research Page 76 of 132 p . 76 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 liyIes P[otol NwNUr 1`000113 1 .... . As praR offt doauuNmtNioo the folbwict: eheeb Witt be includod in each amlytiaal set a run a6oet hating the sfmplK to be nm in the so, md an iawuu att ooad idoeu sheet de.en'bin to iaskwnent type end opentiaa aaditiata. QUALITY ASSURANCE The QA Unit of Exygm ReeaMb will impeat the >audy at fate;veb adequate to mom complieacs with GLP ". and will report the 3dit~ of audits to the Study Dircea. ExAat Ma ayemmt, end the Spoueor Rpr.waative. RETENTION OF DATA AND ARCHiM G . , , .~ All bent copy mw data, taeludirg. but not timieed to. the aigfnal dwvra0109=ns, wozk"eu. ooeeapoadaooa mid rewib shalt be included with the data pedcW ta*mittod to the Study'Dimaar . These will be archived with the odihisr! Nndy Plen, uxedmmtg, lttrl tepcxr. and r17 pertinent Information from the Spoowr. The tasting fliotlity shall keep ill aleetroaic raw data and any insavment. e4WFom& and amp lop`fa the period of time spociGed in 40 CFR 792.193. An act copy of the materials w6mitted to the study dirator will also be kept it ftygaa Rawarck Erysm will obtm permiuioa from the study director batore ditacsdin= or ~t "nP ;OL nqt Ie of d3 Exygen Research Page 77 of 132 p . 77 Interim Report #LO-Analysis of Fish and Clam Samples Exygen Study No . : P000113 1 KxYPx roweot tsmber rooa< <3 1 . .. APPENDIX I ANALYTICAL METHODS V000178p: "Method of Aoatyde for the Determ13u4oa of Perfloorooctuwic Acid (PFOA) in Wata by LGMSdMS" V0001781 : "Metbod of Amlyw fa the DetarWt ndion of Perfluaooctuwic Acid (PFOA) In Soil by I,CJAdSlM" V0001782 : "Method of Analysis for the Ddanninwtion of PerAuaooctruwio Acid (PFQA) in S .ditaml by I.GMS/MS " VOOO1783: "INednd of Akill 46 ft the Detam ination of Perfluomoctanoic Acid (PFOA) in Pisb aod Clams by LC/MS/MS" VU0Q17E t: '4rl4od of Analysis for the Dotacminstion of Parfluorpoccprwic Acid MM) in Yeyetatioa by WM.4IMS" V0001785 : '1lfethod o( Analysis for the Deteeminapon of Pafluorooqwoie Acid (PFOA) in Small Mammal lirar by LC/MSlMS" V00017E6 : "Ma6od of Analysis for she DetsnWnsNon of Porflooroocqnoic Acid (PPOA) in Swc Mammd Sam by GCIMS/MS, Aop 1SaJ'6l Fxygen Research Page 78 of 132 p . 78 Interim Report #10-Arnlysis of Fish and Clam Samples Exygen Study No . : P0001131 Bxyaen RoWAol Wumbm: Pt100I 13 1 AKAI.YTICAL METHOD, 1(MW thY~ YMOI~p by Lc4a" . 4.I,w aroAl r w.., ~+yNM~ r.r1o~ r.alq t. I ,N bnrd, s07f w ...d, o em 3w caaw P.4 Ifni Aff""Wiliv ., tv41 Flow 1 Php /6 q/6 S Exygen Research Page *79 of 132 p . 79 Interim Report #14-Analysis of Fish and Clam Samples Exygen Study No . : POpO 1131 ~1N~ ~~ T+m+ber : P0001 t3 l iyp/rr+ yAdN AS/ALtTMA111gTR00 MOW OfAftb4s hrOWDOOMM"m Om ttnrnta ' Wa17U r rw tA twp tlb Mae" Y r be amp" rrfs WL6r MA4uowmaa afOWfMqOWNWaie MW b WO J I rr Npi1 Ol rrft W W1Mrd e~ t~n M. lo Y a ie Druhs(bCAN/ is wow. tA St of 2.1 AtwA s~iww~lY6wtywt~r~x 34 ~ I Yr 100t, ~~lw lw~qc rrq~nie~f ir papr ~dky )A DrMbROpM&.[ it AtYrIq~I dWt~ylersYwwle~ 31,2 tt~ berlrtMwrr~yYt, anva wAlAwui dm" N W..wd r aqwtbew r is+w 7 .4 At1rOOIwtritMMwyiytWN Wiwb ft wffWMdfur WAWuW 7s A~~r~ItseWdqlrW~~mlltrlOlA~yM-DGOGIrni~t-s aiMr a1 69 + vaa wnt wi hr *A asraioo. ] f Olt- MlLaiw PGOWWs WW b ** dEd in Oe apliis via ir dii . iA {rr m a/ vr(" 41 OslttIOLC OsY 41 Mrlomm - IMt.C rW A twwAUaaO~w~Ad1 Cl~AWW 5 .0 hw" W lkbpw" 11 AV*, I , t{"m ,r.mqnM .4+6y K p.eP q to la 2 ",w4 r Ndj* .ir . .sMw. qlw 4w. OWWAO of kw" S-ia rL . . ..w+r, omi. .1(, . SnwmrNRA'JAb$qAn $ 7 A ~nt~ r wllni wn ils 6t /rt tf~rbe OW prM:vOos. !.7 ArllYwtidr .~~iUMw~IY~UQOOON~, f.s M~ KrwiNpblwtrytsrNrly~tibw st Oly~i~l~+lr~rpa100~L1Ot,~IaR~ it itlattAlias~.. .ser wr 3.t tit.~rrIVLC.wtlt s .t DIVOR641 paw = xn FA Vn f t~tq~iCtt~ d~M4q,, wA H ., : PAW 17 oJ63 F"Y8"' Research Page 80 of 132 p . 80 Interim Report #10-Analysis of Fish and Clam Samples Trarygcn . Study Na : p0001131 8s7fa~ iyvbwi Nwibar p00p117 1 Y~M~A YMN tlr~ vlilUY MUM" )Y aw iu ! fnarYSl~iYL 7.13 Cwultp a*AiM dw*Mi{ !0 aL Pshrmlo n 4MO Y a00D qa ~ a a 11" 117Y. . 4- 1 AYiridtl~>fl.o~rY.llt(t.r,wlewwf,J.l .r. .w .rL ~r vm a~osaszl>q rs 3rc u Yow.)rY~iY~ : ~.7 aw1i.YHqra c =k,(A'Y'11 AwrwbwYr 11nla w %e 20 (NUMI to 41 is oa SA ~ n w. to u n w 70.o s1 75 0.3 7~>t 45 sf 0. 3 1~ IyYtlrMlY~c iSM~p~biia~r~ibra~rliY701~1 a7 a+.rtrta: Tw~cN..- .uww.a .a .r6wra .an. u 1110s IYK -v .rwr I^` A!~! YrIf~Y! M YYMA Y 4p!n.+{.Y rl{mf Y .c l3I .o.7 ~~J' w AYyM M Yrlf I O 7.0 lprwlS.r 1.t idt lM - a 0 nMMrMIiW a0de,nr~wY(t~~n-r JOfYK. UM !bw Y11MYW !Y j0Y11 o Y! rN Yla amp be tAMp/ 0 S.M. N Oi waft w" +f aw IA AiyrtifadalbrlYr L1 1NYM MOO l l.1 : ntt l~YnhY !rm w wrr Y pq~n1 lrf''Mni o . 1 3 4 f of anYaiir wYr to tooo wl K.,rr. NbYrw w1Ylas my be pmpmt ... pow to ya.t Exygen Research Page 81 of 132 p . 81 Interim Report # t0-Analysis of Fish and Ciam Samples Exygen Study No. : P000113 1 Gx7san PhoroCal Naobtr : P0001 131 ~~ Ma.l n .r ww~)w ANALt'ifC.Y >IlefllO ~ ~'w~i~ tls LCIMMs AddQOAIi~ Wally f.9 itr0W twwlir tt lnildleiYlwlMwlisbYOw ,1 .1 fnon ~~Mtl[WWw4f-IOOIy+~LstIfOAYyvr~lfhpyl0 w% ef~r1l~ Mnld Owwoui 6r Nl M/ dtlw No Ip1 ML al ~~ellll - 171 ~. LD!'i lei a 913 At6yS%L S 111w" iYflDd} rQA 4 p IMIMIYytsri4iy IN ~1. M 6r 1C0 yMeL WM{r M t iul wW~r af 100 ~ ewMw b~tlsN,1L!lIoM R !13 A1 .ff4LAdM~NMwArIM~f9f0Aipe'r~d)rMlnpMla l. dllr ]O 1~aL rlwW r a irl ~ahre of I40 rir avurrl iw t 1!! r61p!ltuMk f.!,4 ARl1yhlLAIIIWM1eMIM0f9F0AYI1~4rMYyYM enlIG d.dYL4 pd%t, Irirtta6YraYMol400vft owned w a ttW ML iJ1!lMl 9.1.5 A am POe l . bdIldwiw Mialr sr pp" i t }Arl by MuqiaK N wL of M 00.1 WOR Mhaeo d a lid Wool of 100 wrn nobodies 135mILEMbodr, *.IA lL ft Rtlh nlfnli w w>rYom we is be Onto is smih- 41 VC AM 4m sell Or { suioNw poll ori mal l l~s~ IIMdfA~~ 4.f lWid CAiWbrlOrfe~a 921 LG1 IM wllrwqM lMdmdl w ppr~l is 147,C wow. Ttic sun"* o o w ...w .t ~ayr w,. .wrs.. nwe .Va . YrMtw ra mpla f2J 71r M1w4 s Y l llYirl aMir dNWol rax w mcor my be fl~rM r~i/. wool c. ..:. lYw: sw . vM.r d C.iw .o . .t owrM .rftrrr . vw.e o .+wcw m Models &VAN I D 41 h" ft"611Y xitm w la 41 7f f0e sol a )a w ~ xC,r,~yr) IC 4E4 M NO XC too )M q 3" XC~r~Mp~M IN M tl !10 )GCarryy.s to on d 1o04 M YIYwa Thf wiMM16 agam IMIM eI*1411N 1YiP7 MMYe6 is 4qW/ p I. ill in" 4lwwMi *. +rw rewlrwiiw~ db Ilu b d iriry 66 uY~ctian (SlEi. 7fC - donrlLLil blwar wool hp4 r - ,p". 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