Document M48NOrYyDng12zD3y91YLr5bM

p. 1 A R 2 a 6 - .~~72 9 INTERIM REPORT # 10 - Analysis of Fish and Clam Samples STUDY TITLE 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 DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 STUDY DIRECTOR Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380 Phone: 610-701-3761 INTERIM REPORT COMPLETION DATE May 09, 2006 PERFORMING LABORATORY Exygen Research r_, 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 STUDY SPONSOR 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 t.1 Phone: 651-733-6374 PROJECT Protocol Number: P0001131 Exygen Study Number: P4001131 Total Pages: 132 BEST COPY AVAILABLE [wAole, Docwvnimf] 000244 Interim Report #10-Analysis of Fish and Clam SamVies Exygen Study No.: POQ01131 GOODLABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0001131, entitled "Analysis of perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Sennn Using LC/MS/MS for the 3M Decatur Monitoring Program," conducted for 3M Coxnpany, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by Exygen Research. Flaherty rincipal Investigator Exygen Research )sisimha lee'sari P.E., DEB Study Director Weston Solutions, Inc . " ,, Michael A. S Sponsor R 3M Company Exygen Research syv6 Date Date s// L1D 6 Dafe / Page 2 of 132 000245 Interim Report #10-Analysis of Fish and Clam Samplea ~ ~ Exygett Study No.: P0001131 Q_1AL,ITY ASSU RANCETATE__1ViENT Exygen Research's Quality Assurance Unit reviewed Exygett Study Numbeii' P0001131, entitled, "Analysis of Pertluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program" . All reviewed phases' were inspected for conduct according to Exygen Research's Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported to the Exygen Principal Investigator and Management and to the Study Director. PhaAe 18. Raw Data Review and Interim Analytical Report Review 26. Raw Data Review and Interim Analytical Report Review Date InsQgoted Date Reported to Date Reported to Principal Exygen Investistatar Management Date Reported to Studv Director 08101-05I05 09120105 09121105 09J21105 05103106 05108J06 05109106 05109106 ~0, f14 Date '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 ooo24s Interim Report #10-Analysis of Fish sind Clam Samples Exygen Study No. : P0041131 CERTIFICATION OF AUDIENTICITY This interim report, for Exygen Study Number P0001131, is a true and complete representation of the raw data. Submitted by: Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-1039 Principal Investigator, Exygen: -,GZ.- - ' - bn Flaherty Date Vice President Exygen Researoh Exygen Research Facility Management : Richard A. Gra~ni ~ President Exygen Research ,f-44V- ?4o6 Date Jaisimha'kesari P.E., DEE Weston Solutions, Inc. Sponsor Representative, 3M Company: Michael A. Sai oro Director ofRAgulatory Affairs Exygen Research ~/-/O/O~ Date Date Page 4 of 132 000247 Interim Report #10-Analysis of fish and Clam Samples Exygen Study No.: P0001131 STUDY IDENTIFICATION Analysis of Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFiS), 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 - PROTOCOL NUMBER: EXYGEN STUDY NUMBER : P0001131 P0001131 TYPE OF STUDY: SAMPLE MATRIX : TEST SUBSTANCE: SPONSOR: STUDY DIRECTOR: Residue Fish and Clams Perfluorobutanesuifonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooatanesulfonate (PFOS) 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55 144 Jaisimha Kesari P.E., DEE Weston Solutions, inc. 1400 Weston Way West Chester, PA 19380 STUDY MONITOR: PERFORMING LABORATORY: Michael A. Santoro 3M Company 3M Building 0236-O1-B-10 St. Paul, MN 5 S1.44 Exygen Research 3058 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: 11105104 Interim Analytical Start Date: 12127104 interim Analytical Termination Date: 04117J06 Interim Report Completion Date: OSI09106 Exygen Research Page 5 of 132 000248 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 PROJECT PERSONNEL The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc. The following personnel from Exygen Research were associated with various phases of this interim portion of the study: Name John Flaherty Karen Risha Paul Connolly Amy Sheeh,an Christine Edwards Brittany Kravets Mindy Cressley Krista Gallant Scott Crain Eric Hoover Carlyle Hoaell Shawn Robb Mark Ammerman Eric Edwards Edward Cams Title Vice President Laboratory Supervisor Technical Lead-LC/MS Associate Scientist Technician Technician Technician Technician Technician Technician Intern Technician Technical Lead - Facilities Sample Custodian Sample Custodian Sample Custodian Exygen Research Page 6 of 132 p. 7 Interim Report #10-Analysis of Fish and C1am~Sampies = . ~ Exygen Study No. : P0001131 TABLE OF CONTENTS Page TITLE PAGE ....... . ..... . .................. . .... .... .. . ... ............. .. .. .. . ..... . .............. . ...... ........ . ... . ..... .......1 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT . .... ........ .... . . . ... .......2 QUALITY ASSURANCE STATEMENT .. ............... .... . ...... .............. . . . .... ........ . ... . . . ..........3 CERTIFICATION OF AUTHENTICITY ................ .. .... .. . .... .. ........... . . . ............ ..... . . ... .......4 STUDY IDENTIFICATION..... .... . ...... .... . . . .... ............ ...... . .... .............. . . . ............ . ..... . ..........5 PROJECT PERSONNEL.......... ...... ..... .... . .. .... ............ . ..... . .... .. ...... ... ... .. . ..... ......... .... . ..........6 TABLE OF CONTENTS................ ..... .. .. .. . .... ............ . ..... . .... .. ...... . .. ..... . .............. .... . ...... ....7 LIST OF TABLES . .. . .... .................. ..... . . .. .. . .... ...... ...... . ..... . .... .. ....... .. ..... . ..... ......... .... . . .........8 I.JST OF FIGURES.. . ...................... ..... .. .... . .... ...... ............ . . . .,.. ......... ..... . ..... ......... .... . . . ........9 LIST OF APPENDICES ................. . .. .... .... . .... ...... ....... ..... . . . ............. ..... . .............. .. .. .........10 1.0 SUM112AR3C .. .... . ..... .................... .... ..... ..... ....... ...... .... . . . .............. .... . .. ............ .... ... ......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 ... . . . ............ . . ..... . ........ ..... ....... ..........15 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 ............... ..... .... . . ... . . .... .. ..... .. . .... .............. . . . ...................15 6.2 Preparation ofStandards and Fortification Solutions...... . .... . ............. . .. .... ............... 16 6.3 Chrornatography ... . ..... . ........... ................ .... . .. ... ........ . ..... . .... .. ....... ..... . . . .... ...............17 6.4 Instrument Sensitivity . . ....................... .... . ... . . . ........... ....... . ..... . ..... ...... . . . ..... ..............17 6.5 Description ofLCIMSfMS Instrument and Operating Conditions . .... .. . ...... .......... .. .17 6.6 Quantitation and Example Calculation ... . ..... . .............. .... . ...... ........ . .. .... .............. ... . .18 7.0 EXPERIMENTAL DESIGN ........... ....---.. ..... . . .............. . ... . .. .... ........ . .. ................ . . . ....20 8.0 RESULTS ...... . .... . . .... . ... ....... ............ ..... .... . .... . . .................. . ...... ............ .. . ...... ............ .20 9 .0 CONCLUSIONS. . . ....................... ..... .... . .... ............ .... . ...... ........ ...... . ...... .......... .. .21 10.0 RETENTION OF DATA AND SAMPLES . ....... ........ .... . .. .... ........ ... .... ...... ............ .21 Exygen Research Page 7 of 132 t)U()250 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 LIST OF TABLES Table I. Summary of PFBS, PFHS and PFOS in. Fish Samples....... .... .. ...... ............. .... . ..23 Table IL Summary of PFOS in Re-extracted Fish Samples..... . . ....... . .... ....... ............ . .......30 Table III. Summary ofPFBS, PFHS:and PFOS in Clam Samples . ...... . ....... .... ... ..... . .......32 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples ............ .......33 Table V. Matrix Spike Recovery of PFOS in Re-extracted Fish Samples.... ............ . .......46 Table VI. Matrix Spike Recovery PlF"BS, PFHS and PFOS in Clam Samples.......... . .......49 Exygen Research Page 8 of 132 000251 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No_ : P0001131 Figure 1 . LIST OF FIGURES Page Typical Calibration Curve for PFBS. in Methanol .. . . ........ ...... ..... ........ ..... . ... . .51 Figure 2. Non-Extracted Standards ofFFBS in Methanol, 0.0005 pglmL and 0.001 p.g/mL, Respectively ..... ... . ..... . ..... .............. .... . .............. .....:................. .52 Figure 3. PFBS in Control Fish Blank, 0.00625 pglrnL Fortified Control Fish Spk A, and 0.025 pglmL Fortified Control Fish Spk B, Respectively ...... ....... ............ .... .53 Figure 4. Chromatogram Representing a Fish Sample Analyzed for PFBS (Exygen II): C0049478, Data Set:061605E) ............. .... .. ............... . ...............54 Figure 5. Typical Calibration Curve for PFHS in Methanol..... .. .. .. . ............. . . .... ...........55 Figure 6. Non-Extracted Standards ofPFHS in Methanol, 0.0005 pglmL and 0.001 gg/rnl, Respectively ................. .... . . . .......... ...... . . . .... .............. . ...............56 Figure 7. PFHS in Control Fish Blank, 0.00625 pglniL Fortified Control Fish Spk A, and 0.025 jAglmL Fortified Control Fish Spk B, Respectively . . ............ . ..... . .... .....57 Figure 8. Chromatogram Representing a Fish Sample Analyzed for PFHS (Exygen ID: C0049478, Data Set: 061605E) . ..... ..... ......... ..... . . ............ ..... .... .58 Figure 9. Typical Calibration Curve for PFOS in Methanol ............. . .. .. .. ............ ..... .... .59 Figure 10, Non-Extracted Standards ofPFOS in Methanol, 0.0005 ~g/ML and 0.001 jsglmL, Respectively . ... . . .... . .... ............. ...... ....... .............. ................. .... .60 Figure 11 . PFOS in Control Fish Blank, 0.00625 l,tglmL Fortified Control Fish Spk A, and 0.025 uglmL Fortified Control Fish Spk B, Respectively .... .... ....... .......... . . ...61 Fig= 12. Chromatogram Representing a Fish Sample Analyzed for PFOS (Exygen II): C0049478, Data Set:061605E) .. ..... ........ . ............ ...... . .......... .....62 w ',."+~~>t Exygen Research Page 9 of 132 UUl) ;6 52 Interim Report #10-Analysis ofFish"and Clam Samples Exygen Study No. : POUQ 1131 LIST OF APPENDICES Appendix A Study Protocol PQ041131 (Exygen Study No. P0001131 ) with Analytical Method VOOa1783 : "Method ofAnalysis for the Determination of Perfluorooctanoic Acid (PFflA) in Fish and Clams by LC.IMSIMS", Protocol Amendments 1 and 2, and Deviations 2 and 3 . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .b3 Exygen Research Page 10 of 132 000253 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study.No.: P0001131 1.0 SUMMARY Exygen Research extracted and analyzed fish and clam samples for the determination of perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) according to Exygen Method V0001783 (Appendix A) . The limit of quantitation (LOQ) for PFBS, PFHS, and PFOS in fish and clams was 0.2 nglg. 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 nglg. The initial analytical results associated with fifty-one fish samples are not reported (NR) in Table 1 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 II 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 re-extracted fish samples am summarized in Table II. Analytical results and assessed accuracies for the analysis of PFBS, PFHS and PFOS found in clam samples are summarized in Table III. Laboratory matrix spikes that were in the appropriate concentration range (primary concentration less than three times the spiking level) were used to calculate the assessed accuracies. The average percent recoveries f standard deviations for PFBS, PFHS, PFOS in fish samples were 79% f 13%, 94% t 12%, and 85% f 20%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in fish samples are summarized in Table IV. The averagc percent recovery f standard deviation for PFOS in the re~-extracted fish samples was 109% t 20%. Fortification recoveries for i'FOS in the re-extracted fish samples arc summarized in Table V. The average percent recoveries f standard deviations for PFBS, PFHS, PFOS in clatn samples were 84% t 10%, 93% * 13%, and 73% t 16%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI . The sample 1Ds assigned by the client follow this formula: Dxx-x0l-xxxxxx-xr04xxxx . The first string begins with D for Decatur, Alabama and the xx defines the sampling area within the Wheeler Reservoir ofthe 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 LOT sampling location LOC-1 DBC = Bakers Creek mouth DOU = Cove at 3M VWVTP outfall DMC = Downstream Mallard Creek mouth Exygen Research Page 11 of 132 000254 Interim Report #10-Analysis of Fish and Clam Sunpies Exygen Study No.: P0001131 The second string defines the general category of the biota sample and the sampling round where: FO 1 =Fish sample first round I01= Invertebrate sample first round The third string defines the species (first two characters), the sample type (third character), and the sample number (last three characters) within that sampling area and type of sample where : >P = channel catfish (Ictalurus puncrarers) MS = largemouth bass (Micropterus salmoides) CF = Asiatic clam (Corbecula fluminea) F a Filet tissue sample W = Whole body sample 001 through 005 = sample"number within the sampling area and sample type The fourth string (single character) additionally defines the sample type where: 0 - Primary field sample 1 = Field duplicate sample 2 = Equipment rinseate blank sample The fifth string defines the sample preparation date in Yy1Vi1bII7D format . Examples of this sample 1D system are: Sample DBC-F0I-IPF004-0-041021 is the filet tissue sample prepared on October 21, 2004 from the fourth channel catfish collected at the Bakers Creek mouth sampling location . Sample DL1-FOl-MSW002-0-041104 is the whole body sample prepared on November 4, 2004 from the second largemouth bass collected at the Fox Creek mouth sampling location. 2.0 OBJECTIVE The objective of the analytical part of this study was to determine levels of perfluorobutanesulfonate (PFBS), pertluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFQS) in fish and clams according to Protocol P0001131 (Appendix A). Exygen Research Page 12 of 132 000255 Interim Report #10-Analysis ofFish end Clam Samples Xxygen Study No.: P0001131 3.0 INTRODUCTION This report details the results of the analysis for the, determination of PFBS, PFHS, and PFOS in fish and clams using the analytical methtid~ ~ entitled; "V0001783: Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS ." ' ' The study was initiated on November 05, 2004, when the 5tiidy director signed protocol number P0001131 . The analytical start date -for this interiin report was December 27, 2004, and the analytical termination date for this~interim reportwas April 17, 2006 . 4.0 ANALYTICAL TEST SAMPLES Forty fish samples (Exygen ID C0048126-C0048165) were received on dry ice on October 23, 2004 from Tim Frinak at Weston Solutions, Inc . Fifty-six fish samples (Exygen ID C0049450-C0049505) were received on dry ice on November 6, 2004 from Charles Young at Weston Solutions, Inc . Twenty-six fish samples (Exygen 1D C0056354-C0056479) were received on dry ice on January 13, 2005 from Tim Frinak at Weston Solutions, Inc . Six clam samples, consisting of whole clams from each sample sits (Exygen II) C0056480-C0056485) were received on dry ice on January 13, 2005 fmm Tim Frinak at Weston Solutions, Inc . A whole Whiting (Family: Gadidae) was purchased from a local grocer by Ed Carns on December 20, 2004 and was used as the control fish (Exygen ID C(1054391). 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 MATERIAL 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 000256 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0041131 PFBS PFBS PFHS PFOS Ex~aIennvSntory No. SP0000252 SPO005726 SP0002401 SP0002694 I&I 101 101 SE036 430180-1 Purit " 96 .7 96 .7 98 .6 101 .2 EUir_ation Date 12104/06 12104106 10118106 10131107 The molecular structures of PFBS, PFHS and PFOS are given below: PFBS Chemical Name: Perfluorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (C4F4SO3X~ Transitions Monitored: 299 -* 99 Structure: F F F FIFI F F PFHS Chemical Name : Perfluorohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (C6Fl3S03'K+) Tratzsitions Monitored: 399 -3 80 Structure : PFOS Chemical Name : Perfluorooctanesulfonate Molecular Weight: 538 supplied as the potassium salt (CgFSO3"K+) Transitions Monitored: 499 -> 80 Structure : Exygen Researeh Page 14 of 132 00025'7 Interim Report #l0-Analysis of Fish,and Clam Samples " Exygen Study No.: P0001131 6.0 DESCRIPTION OF ANALYTICAL METHOD The analytical method "V0001783 : Method of Analysis for the Determination of Pertiuorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS" was used for the fish and clam samples in this study. 6.1 Extraction Procedure 6.1.1 Sample Preparation Before the samples could be weighed for the extraction, they had to be processed. To process, the frozen samples were placed into a food processor and homogenized with dry ice. The samples were transferred to one-gallon Ziploc bags and placed in frozen storage with bag left open to allow the dry ice to sublime. After sublimation, the sample bags were sealed and remained in frozen storage until time of analysis . Sample processing records are located in the Sample Information section of the raw data package. 6.1.2 Glassware Preparation The 125 mL pear-shaped flasks were silanized by first rinsing the flask with 30% dimethyidichlorosilane 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 mI. columns were packed at Exygen in sequence with 2 grams florisil, 2 grams silica gel, 2 grams of carbon, and 1 gram LC-NHZ. 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 Extraction A 5-gram* portion of fish or clam sample was weighed into a fifty- milliliter 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 OOC1258 p. 16 Interitri Report #10-Analysis of Fish and Clam Santples Exygen Study No :, P0001131 samples allowed the fats and proteins to precipitate . The samples were centrifuged for -10 minutes at 2000 ~rprn. The supernatant was then loaded onto the conditioned clean-up column fitted inside the silanized pear shaped flask. The eluate was collected in the silanized pear-shaped flask. This process removed the fats and proteins from the extract. Ten milliliters of acetonitrile was added to the samples left in the centrifuge tube. The remaining sample in the tube was homogenized using a tissumizer for -30 seconds. The 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 -1 hour. The samples were centrifuged again for -10 minutes at -2000 rpm. The supernatant was then loaded onto the same clean-up column. The 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 Solutions Individual stock standard solutions of PFBS, PFHS and PFCS were prepared as specified in Exygen method V0041783 . The stock standard solutions were prepared at a concentration of 100 pglmL by dissolving 10 mg of each of the standards (conected for purity and salt content) in methanol, From these solutions, mixed 1 .0 AghmL fortification standard solutions were prepared by taking 1 mL of each of the appropriate stock solutions and bringing the volume up to 100 mL with methanol . By taking 10 mL of the mixed 1 .0 KgImL fortification standard and bringing the volume up to 100 mL with methanol, a mixed 0.1 p.gJmL fortification standard was prepared. A mixed stock standard solution of PFBS, PFHS, and PFOS was also prepared. The stock standard solution was prepared at a concentration of 1000 uglnrnL by dissolving 100 mg of each of the standards (corrected for purity and salt content, if necessary) in methanol. From this solution, a 100 wglmL fortification standard solution was prepared by taking 10 mL of the stock and bringing the volume up to 100 mL with methanol. By taking 10 mL of the 100 ug/mL fortification standard and bringing the volume up to 100 mL with methanol, a 10 pglmL fortification standard was prepared. By taking 10 mL of the 10 pg/mL fortification standard and bringing the volume up to 100 mL with Exygen Research . Page 16 of 132 00O259 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P0001131 methanol, a 1 .0 ggIn1L fortification standard were prepared. By taking 10 mL of the 1 .0 uglmL fortification standard and bringing the-volume up to 100 mL with methanol, a 0.1 pglniL 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 Solution Fort . Volume (~~JmL}' (ML) 1 .0 5.0 1 .0 2.5 1.0 1 .0 0.05 10 0.025 10 0.01 10 0.005 10 ' of PFBS, PFHS and PFOS Volume of Fortified Sample, (ML) 100 100 . 100 _ l00 ` 100 100 100 , Final Cone. of ., Calibration Std. (pwM-) 0.05 0.025 0.01 0.005 0.0025 0.001 0.0005 The stock standard solution and all fortification anacalibration standard solutions were stored in a refrigerator (4 t 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 ofPFBS, 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 pglmL ofPFBS, PFHS and PFOS : , 6.5 Description of LCIMSIMS Instrument and Operating Conditions Instrument: AFT 4000 Biomolecular Mass Analyzer Interface: Turbo Ion,Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 Software: 1 Windows NT, Analyst 1 .4.1 HPLC : Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosarnpler Exygen Research Page 17 of 132 000260 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : PQ041131 HP Column Oven HPLC Column: Thermo Flucphase RP, 50 mm x 2.1 mm Column Temp. : -30 C Iqjection Vol.: 15 gL Mobile Phase (A): 2 mM Ammonium Acetate in water Mobile Phase (B): Methanol i mi YEA % B 0.0 65 35 1.0 65 35 8.0 25 75 10.0 25 75 11 .0 65 35 18 .0 65 35 Total run time: -18 min Flow Rate: 0.3 mUmin Ions monitored: Aulhde PFHS PFHS PFOS ~,Ntode negative negative negative T ii Monitored 299 -> 99 399-+80 499 -~ 80 Approximate Re tion Tiglc min --4 .7 min . -10 .8 min. N12 .9 min. 6.6 Quantitation and Example Calculation Fifteen microlite.rs of sample or calibration standard were injected into the LC/MS/MS. The peak area was measured and the standard curve was generated (using 1/x fit weighted linear regression) by Analyst software using six concentrations of standards. The concentration was determined from the following equations . Equation 1 calculated the amount of analyte found (in nghnL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software pro8ram- Eouation 1 : Analyte found (ng/mL, wet weight) - (Peak area - in erc t x DF slope Where: DF = Dilution Factor, factor by which the final volusne was diluted, ifnecessary. Exygen Research Page 18 of 132 000261 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study Nor.: P0001131 Equation 2 was used to convert the amount of PFBS, PFHS and PFOS found in nglmL to nglg (ppb). Equation 2: Analyte found (ppb, wet weight) _ 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 (%) -janalvte found (ny,LmL) - anaiyte in control (n&n?.)) x100% amount added (nglmL) 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 1D: C0049478 Spk E (Set: 061605E), fortified at 10 nglg with where: peak area 280750 intercept 3070 slope 13100 dilution factor 1 ng/g PFBS added (fort level) 10 amt in corresponding sample final volume (mL) NQ (not quantifiable) 2 sample weight (g) 5 From equation 1 : Analyte found (ng/mL, wet weight) . - j280750 - 30701 x 1 13100 = 21 .2 nglmL From equation 2: Analyte found nglg (ppb) = (21.2 ng,L,mL x 2 rnL) 5g = 8.48 nglg (ppb) Exygen Research i Page 19 of 132 000262 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P0001131 From equation 3: a/o Recovery a (af48 n8~g ~~QXZ~gj x 100a/o 10 nglg = 85% 7.0 EXPERIMENTAL DESIGN For fish and clam samples designated as laboratory matrix spikes, PFBS, PFHS, and PFOS were added at a known concentration to the samples in the laboratory after the samples were weighed for extraction. The fish samples were extracted in thirty sets, five that were re-extraction sets. The clam samples were extracted in one set. Each fish or clam set included one control fish matrix blank and two control fish matrix blanks fortified at known concentrations . Two sets of fish contained three samples, one set of 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. Accvracies 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 I. Please note that the chromatography for Ph'BS was poor for this matrix . Exygen recognizes this and great care has been taken to integrate each data set consistently. Analytical results and assessed accuracies for the analysis of PFOS found in the re-extracted fish samples are summarized in Table 11. Analytical results and assessed accuracies for the analysis of PFBS, PFHS and PFOS found in clam samples are summarized in Table III. The average peroent recoveries t standard deviations for PFBS, PFHS, PFOS in fish satnples were 79% t 13a/a, 94a/o t 12a/a, and 85a/o f 20a/o, respectively . Fortification recoveries for PFBS, PFHS, and PFOS in fish samples are summarized in Table IV. The average percent recovery f standard deviation for PFOS in the re-extrwtod fish samples, was 1090/6 t 20a/o. Fortification recoveries for PFOS in the re-extracted fish samples are summarized in Table Y. The average percent recoveries f standard deviations for PFBS, PFHS, PFOS in clam samples were 84a/o t 10/a, 93a/o t 13a/o, and 73a/o t lb%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI. Exygen Research Page 20 of 132 000263 Interim Report #10-Analysis of Fish and Clam Samples Eycygen Study No .: P0001131 9.0 CONCLUSIONS The fish and clam samples were successfully extracted and analyzed for PFBS, PFHS and PF4S according to analytical method V0001783 . 10.0 RETENTION OF DATAAND SAMPLES All original paper data generated by Exygen Research that pertains to this interim report will be shipped to the study director . This does not include facility-specific raw data such as instrument or temperature logs . Exact copies of all raw data, as well as a signed copy of the final analytical report and all original facility-specific raw data, will be retained in the Exygen Research archives for the period of time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792. Exygen Research Page 21 of 132 00o264 Interim Report #E10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 TABLES Exygen Research Page 22 of 132 000265 Interim Report #11)-Analysis of Fish and Clam Samples Exygen Study Na.: P0001131 Table 1. Summary of PFBS, PFHS and PFOS in Fish Samples (continued) an ID C0048144 C0046144 Rep C0048145 C0040145 Rep C0048148 C0048146 Rap COD48147 C0048147 Rep C0048148 C0048148 Rep 00048149 C0048144 Rap C0048160 C0048150 Rap COO"8151 C0048151 Rep C0048152 C0048152 Rep C0018153 C0048153 Rap C0048164 C0048154 Rep C0048155 C0048155 Rep C0048158 C0048166 Rep C0048157 C0048157 Rep C0048158 C0048158 Rep C0048159 C0048159 Rep C0048180 C0046160 Rap C0048 f 61 C0048161 Rap C0048182 C0048182 Rep Client Sam 'e ID DL1-F01-IPF001-0-041021 OLi-F01-IPF001-0-041021` 01.3-FOi-IPF003-0-0411021 DL3-FOt-LPF003-0-041021 " DL3-F01-IPF004-0-041021 DL3-F01-IPF004-0-0410210 DL3-F01-IPF005-0-041021 OL3-F01-IPF005-0~0410210 DBC-F0I-IPF001 "o-041021 DBC-F01-PF001 .4-OA1021 " DBC-F014PF002-0-041021 DBC-F01-PF002-0-041021 " DBC-F01-IPF003-0-041021 OBC-FOi-IPFOOS-0-04102io pBG-F0I-IPW001-0 .041021 DBC-F0I-IPW001-0-041021' DBC-F0I-IPW002-0-041021 DBCrF01-IPW002-0-041021' OBC-F0I-IPWOD3-0-041021 OBC-F0I-IPW003-0-041021 " DOU" 1=01-IPF001-0A41021 DOU-t:01-IPF001-0-041021 " OOU-F014PF002-0-041021 DOU-F0I-IPF002-0-041021' DOU-F0I-IPF003-0-041021 DOU-F0I-IPF003-04l41021- DOU-F01-113F004-0-041021 DOU-F0I-IPF004-0-041021" DOLL-F0I-IPF006-0-041021 D0U-F01-IPF005-0-041021 " DOU-F0I-IPW001-0~041021 DOU-F0I-IPW001-0-041021' DOU-FOt-IPW002-0-041021 DOU-F01 " IPW002-0-041021' DL2-F01-MSW001-0-041021 Ot2-F01 .iMSW001-0-041021' OL2-F01-MSW002-0-041021 DL2-F01-MSW002-0-041021' C4 Sulfoqa0s PFB3 PvlluoroEnuswWbnma Analyte Assessed Found Accuracy wst wi. +t- 76 0.432 0.428 0.448 0.440 0.784 0.900 1 .63 COT 1 .34 1 .38 1 .43 0.756 0 .998 0 .952 0.864 0 .508 0 .700 0.738 0 .736 0.780 4.38 4.24 8 .78 8 .28 5 .88 5 .96 8 .12 0 .28 4 :58 4 .36 2 .89 2 .81 18 .4 19 .3 0.203 ND ND ND 30 30 30 30 40 40 80 60 50 , 50 50 50 60 50 40 40 40 40 30 30 40 40 40 40 40 40 30 30 30 30 30 ]0 50 50 30 30 30 30 C6 Sulfanab PFNB PWlooroluoueaallaul~ Analyts Assessed FaunQ Accuracy ww r+~. ",I- 96 0.261 30 0 .252 30 ND 30 0.220 30 NO 30 NO 30 ND 30 NO 30 0 .892 30 0 .880 30 NO 30 ND 30 0 .844 30 0 .024 30 2 .21 30 2 .20 30 9.12 30 8 .96 30 6.76 30 7.44 30 1 .02 30 0.972 30 0.792 30 0.720 30 1 .02 30 1 .02 30 2.30 30 2.38 30 0.958 30 0.892 30 0.948 30 0.984 30 3.$9 30 3 .70 30 NO 30 ND 30 ND 30 ND 30 Ca 8uBonata PF09 t~~lh~aoodan4sulfanab Anmyte Astesaed Found Aacunaoy ww vu. 41.% 33 .4 40 326 40 3 .55 30 3 .36 30 0.382 90 0.230 30 5 .48 40 6.64 40 NR NR NR NR 110 30 109 30 NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR 14R NR NR NR NR NR NR NR NR NR NR NR NR NR NR 120 50 120 50 102 30 100 80 -Lam" Dupkais ND = Not detected at or above Lirrwt of QuanSltation which is 0.2 nplq (wet weight) . NR - Not reported due to qually oontrol result fallunw. Exygen Research ! k. " Page 24 of 132 000266 Interim Report #l0-Anglysis of Fish and Clam Samples Exygen Study No. : P0001131 Table I. Summary of PFBS, PFHS and PFQS in Fish Samples Ex !D C0048128 C0046128 Rep 00048127 C0048127 Rap C0048128 C0048128 Rep C0048129 C0048128 Rep C0048130 C0048130 Rep C0048131 C0048131 Rep C0048132 C0048132 Rep C0048133" C0048133 Rep- C0048134 C0048134 Rep C0048135 C00481 35 Rep C0048138 C004i130 Rep C0048137 C0048137 Rep C0018138 C0048138 Rep C0048130 C0049139 Rep C0048140 C0048140 Rep C004B141 C0048141 Rep C0048142 CD048142 Rep C0048143 C0048143 Rep Client Sample ID Dl3-F01-IPF001 -0-041021 DL34<01-IPF001-0-041021' DL3f01-IPF002-0-041021 D0-F01-11PF002-0-041021' DMC-F0I-IPF001-0-041021 DMC-F0I-IPF001-0-041021' DMC-F0I-IPF002-0-041021 OW-F01dPf002-0-041021" DMC-F01-IPW001-0-041021 GMC-F01-PW001-0-041021` DN4C-F01-WV002-0~041021 DMCrF014PW002-0-041021' DhIC-FOt-111SW001-0-041021 DOAC-F0I-M8W001-0~041021' DMC-F01 "M3W002-0-041021 DbtC-F01-IIISW002-0-041021' DL.2"f014PF001-0-041021 Dl2-F01-iPF001-0-041021' DL2-F014PF002-0~041021 Dl2-F01-IPF002-0~041021' DL2-P074PFOD3-0-041021 D1 .2-FOt-IPF003-0-041021 " DL2-F014PF004-0-041021 DL2-FOt-IPF004-0-041021' DL2-F014PF005-0-041021 DL2-F01-PF00"-041021' DL2-F01-8'W001-0-041021 DL2-F0I-1PW001-0-041021 " Dt2.FO1-MSF0o1-0-041021 DL2-F01d118F001-0-041021' DLZ-F01dF115F002-0-0410Q1 DL2-F01-hISF002-0-041021` OL2-F01-A1BF003-0-041021 DL2P01-MSF003-0-041021' DL24014ASF004-0-041021 Dt.Z-F01-1SF004-0-041021' C4 sunon.r. rFes nnalyce Found wetwt . Assessed Accuracy N- % 0 .3m 40 0.318 40 0.296 40 0.382 40 0.33D SO 0.38B 60 0.712 30 0.782 30 1 .08 40 1 .08 40 O.t)88 50 1 .34 50 0.218 30 0.202 30, AD" . . 30 ND" 30 0.980 50 1 .00 60 0.816 '30 0.962 50 0.247 30 0.218 30 0.348 40 0.330 40 0 .338 40 0.318 40 0 .328 30 0 .400 30 0.333 30 0.348 30 0 .408 40 0.398 40 0.418 40 0.378 40 0.343 30 0.349 30 Cssulfoa,.w PFKs nrwlyne Found net wt. Assessed Accuracy +I- ND 30 ND 30 ND 30 ND 30 ND 50 ND 80 ND 30 ND 30 ND 30 0.297 30 ND 30 ND 30 0.624 30 0.484 30 ND" 30 ND^ 30 ND 40 ND 40 ND 40 ND 40 ND 30 ND 30 ND 30 ND 30 ND 30 ND 30 ND 30 ND 30 ND 30 NO 30 ND 30 ND 30 ND 40 No 40 NO 30 F6) 30 Cl sWonne PFas luti.fyte Found , ..r w. XZ==r Accuracy +J-% 6.18 30 5.64 30 4.16 40 4.38 40 7.40 50 8.36 80 14.1 50 17.0 50 70.0 40 88.4 40 34 .4 30 34 .2 30 Z70 30 280 30 S30 30 846 30 3.45 50 2.86 60 4.72 +50 6.04 50 2.01 30 2.08 30 4.52 40 4.12 40 2.48 30 2,60 30 6.88 30 8.12 30 77.2 30 47.8 30 94 .8 40 98 .4 40 41 .8 40 40.0 40 83.8 30 83.2 30 "l .mboreloay Dupti0040 " 1 .0 q o( sswnplk undforeochsctlao tr~sraddb.0 q. ND o NOtdetected at or above Unit of Quantitatlon which la 0.2 nptp (wet welpht)_ ND" - Not delecxed et a*bows L.intR of Quentilatlon which Is 1.0 nWq (wet welpht~ NR sNot rnpoAMd due 10 qualitycontrol result ftrkm. Exygen Research Page 23 of 132 000 ;~'7 Interim Report #10-Analysis of Fish and 'Clam Samples Exygen Study No.: P0401131 Table I, Summary ofPFBS; PFHS and PFOS In Fish Samples (continued) . en ID C0048163 C"0048163 Rep C0048184 C0048184 Rep C0048165 C004$165 Rep C0049450 C0049450 Rep C0049451 C0049451 Rep C0049452 00049452 Rep COO49453 C00494b3 Rep 00046454 C0049454 Rap C0049455 C0049455 Rep C0049456 C0049456 Rep C0044457 C0049457 Rep C0049455 C0049458 Rep C0049459 C0049459 Rep C0049460 C0049460 Rep C004D$61 ; C004901 Rep C0049482 C0040482 Rep C0049463 C0048463 Rep 00049464 C0049484 Rep C0049465 C0049465 Rep Client Sample ID DL2-F014ASW008-0-041021 DL2-F01au18W003-0-041021' DL2-F01-M5W004-0-041021 DL2-F01-MSY11004~0-0410219 DL2-F01-MSW005-0-041021 01-2-F0144SW005-0-041021 " DBC-F01-MSW0R1-0-041104 DBC-F01-MSW001-0-041104' DeC-F01-fU3W002-0-041104 DBC-F01-1101SW002-0-041104' DBC-F01-M5W003-0-041104 DBC-F01-101SWO05-0-041104' DBC-F01-MSW004-0-041l104 DBC-F01-MSW004-0-041104` DBCrF01a11SW005-0~441104 DBC"F01-MSW005-D4)41 101" DBC-F01-MSF001-0-041104 DeC-F01-MSF001-0-041104" ]BC-FO I-KA8F002-0-041104 Dl3Cf01-MSF002-0-041104' DBC-FOt-IPF004-0-041104 DBC-F01-PF004-0-041104' DBC-F01-112F006-0-041104 DBC-F01-IPF00'dr0-041104 " DBC-FOI-IPW004-0-041104 DBC-F014PYI1004-0-041104' DBC-F01-1F'W005-0-041104 D9C-F01-IPW006-0-041104 " DOU-F0I-IPYV003-0-041104 D0U-F01-IPW003-0-041104" DOU-F01-iPW004-0,041104 D04J-F01 "I11W004-0-041104' DOU-F0t-rW005-0-041104 DOU-F01-PW006-0-041104' 01.2-F014W002-0-041104 DL2-F014PW002-0-041104" DL1-F01-MSW0014041104 D1 .1-F01-MSW001-0-041104' c4:unonst.t'FFSS hAluanoruUnwNanOs Anal7ts ^ Aaaesfad Found Accuracy , ~wt w. +1- 7L ce aullon.e.I+FHS hrsuorolwrrnesuftratn An" Assessed . Found wntwt . Accuracy N- 9G ND ' 30 . . ND. 30 ND ' 90 ND, 30 ND 30 ND 30 ND 30. ND 30 ND 30 ND 30 ND 30 , ND 30 0.868 30 8.32 SO 0,832 , ' 30 , 8.32 90 0 .868 30 3 .43 30 ,O .e84 30, 3.35 , 30 . 0 .880 30 . .3 .62 30 0.784 30 3 .64 30 0.884 30 9 .72 30 0.880 30,, 9.80 . 30 0 .832 0 .83E 0 .820 0 .788 0.788 0 .780 0.504 , 0.620 . 1,80 ~1 .64 0.484 ,,0.444 . 10.572 0.532 &12 ~3 .05 3 .49 3,11 2.87 2 .90 1 .04 0.980 1,20 1,24 3Q 30 30 30 30 30 30 30 90 30 30 , 30 , 80 . ; 30, 30 30 30 30 30 30 30 , 30 30 30 Z77 . 2.88 , 3,58 3.46 1 .04 .-1 .90 0.584 , 0.540 2.18 . 2.18 , 3.28 3.28 . 2.10 2.10 6,00 5.92 7.12 8.84 . 5 .12 5,32 NO, ND 0.895 0.932 30 30 30 30 30 30 90 30 . 30 30 30 30 ; 90 .. 30 30 3D 30 30 30 30 30 30 30 3D c: suuon.a PFos hrRuarooatrwu Analyte Aaseaed Found wr %c Accuracy 92.4 30 91 .6 30 88.0 30 94.8 30 188 30 174 30 NR NR NR NR NR MR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR MR NR NR NR 142 30 152 10 NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR 8 .20 40 6 .80 40 NR NR NR NR aLabOra1Dry DUpAm1R NO = Natdetaclod at or abova Limitof QuarAltaffOn which is 0.2 nall; (wet weight). NR a No* npoftd due to qusNy oonrd nwdc hiWna. Exygen Research Page 25 of 132 p. 26 Interim Report #10-Analysis of Fish and Clam Sarnplt:s Exygen Study No.; P400 (i31 Table 1 . Summary of PFBS, PFHS and PFUS in Fish Samples (continued) EXYM ID C00494D8 C004948e Rep C0049487 C0049487 Rep C0049488 C0049468 Rap C0049499 C0049489 Rep C0049470 C0049470 Rep C00+9471 C0049V 1 Rep 1:0049472 CU0494T2 Rep C0049473 C0049473 Rep C0049E74 C0049474 Rap C0041470 C0049478 Rep C0049478 C0049470 Rep C0049477 C0049477 Rep C0049478 C0049478 Rep C0046479 C0049479 Rep C0049480 C0049480 Rep C0049481 C0049481 Rep C0049482 C0049482 Rap C0049483 C0049483 Rep C0049484 00049484 Rep . Caent 891n ' ID DL1-F01-M8W002-0~0411D4 DL7-F01QsW002-0-041104- DL1-F01-M8W003-0-041104 DL1-F01-148W003~0a41104` DL7-F01-AA$W004-0-041104 DLi-F01-MSW004-0~041104- DL1-F0141$W006~0-041104 DL1-F01-MSW009-0-041104" oL1-F01-MSF001-0-041104 DL1-MI-MSF001-0-041104' OL1-F01-MSF002-0-041104 DL1-F01-bISF002-0-041104" DL1-F01-p1SF00304041104 OLI-FO144WOMI-0-041104- DLt-FOt-M5F004-0-041104 DLt-F81-Iti1SF004-0-041104- DL1-F01-M9F005-0-041104 nL1-F014ISF005-D-041104` DLt-F01-IPW001-0-041104 DL1-F014PW001-0-041104" DL1-F01-1PSN002-0-041104 OL1-F014PW002-0-041104" DL1-F01-IPW003~0-041104 DL14r01-1PW003d>041104" DL1-FOt-IPW0D"441104 DL1-F01-P1N0040-041104' OL1-F01-1PF002-0-041104 DL1-F01-IPF002-0-041104" DL-1f014PF0034)-441104 DL-1-F01-IfF0030-041104 " DL-1f01-IPF004-0-041104 DL-1-F01-1PF0A-0-041104- DL-1-F014PF006-0M441104 DL-1-F01-IPF005~0-041104 " DL3-F01-MSW001-0-041103 DL3-F01-M6W001-0-041106' DL3-F01448W002-0~041105 DL3-F014MW002-0-041108- C4 3ulTOnatb PFn hAluorohro~~wAlenam Arm" Found netwA Assaaed Aearaey +1-% 1 .30 30 1.15 30 0.800 30 O.SEB 30 1 .22 30 1,12 30 1 .22 30 1 .20 30 ND 30 NO 30 ND 30 ND 30 0.203 30 NO 30 NO 30 NO 30 NO 80 NO 30 0.772 30 0.870 30 0.468 30 0.472 30 NO 30 NO 30 NO 30 NO 30 NO 30 ND 30 NO 30 NO 30 NO 30 ND 30 NO 30 NO 30 ND 30 NO 30 NO 30 No 30 Ca 8dfonal4 PFH8 puAuaroh~qa+ro Ana- ely" Found awrL Aesemd Accwracy +1-% 1 .72 30 1.54 so 1 .13 30 1 .14 30 0 .908 30 0 .880 30 1 .18 30 1 .18 30 0,315 30 0 .299 30 0.824 3D 0.004 30 0.862 30 0.676 30 0.332 30 0.838 30 0.84 30 0.644 30 0.850 30 0.744 30 0.'.i38 30 0.516 30 0.209 30 0.247 30 0.238 30 0.240 30 0.222 30 0247 30 0.285 30 0282 30 NO 30 NO 30 0.373 30 0.388 30 ND 30 NO 30 10 30 NO 30 Cp SulfvnaSb PFOS PrlYwpomerulldrar Malyts Fand Aoouracy MtW. d-% NR NR MR Na NR NR MR NR 181 30 188 30 NR NR NR NR 293 30 307 30 NR NR NR NR NR NR MR NR NR NR NR NR NR NR NR NR 17.4 30 18.8 30 13.7 90 15.6 30 9.36 30 9.32 30 36.8 30 57.2 30 11 .1 30 11 .2 30 20.9 30 21 .4 30 7.00 30 7.38 30 8.72 30 B.58 30 139 w 137 90 180 30 1t12 30 -Labaaooq DupOpI NO o Not dstectdd at aobm Limit of t]KwritaGon vAich ia 0.2 nplp (wet weipht). NR =Notmported dueto qudlty carArd =a fiiluras. Exygea Rescarch Page 26 of 132 0002(;9 Interim Report #10-Analysis of Fish and Clam Samples Exygeai Study No.: POO01131 Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued) ID C0049485 C0049485 Rep C0049486 C0049485 Rep C0049487 00049487 Rep C0049488 C0049488 Rep C0049489 00049489 Rep C0049490 C0049490 Rep C0049491 C0049491 Rep C4049492 G0049492 Rep Ctp49498 C0049493 Rep C0049494 00049494 Rep C0049495 MOW Rep C0049496 C0049498 Rep C0049497 C0049497 Rep, C0049498 C0049498 Rep C0049499 C004949g Rep 00049500 C0049500 Rep C0048501 C0049501 Rep C0049502 C0049502 Rap C0049503 C0049603 Rep Client S ie ID 00-F01-MSW003-0-041105 D1.3-F01 "MSW003-0-041105' QL3-FOt-M8W004~0-041105 DL3-F01-M3W004-0-041105' DL3-FOt-M81N005-0-041105 D .3-1 F01 " M6W005-0-041105' DL3-F014ISF001-0-041105 OL3-FOt-MSF001-0-041105" DL3-F01-8tSF00245-941105 DL3-F01-MSF002-"1105' DLS-F01dASF003-0-041105 01.3F01-MSF003-0-041105" DL3-F01-1a1SF004-0-041106 DL3F01-MSF004-0"04f 105" D1.3-F01418F005-0-041105 OL3-F01-MSF006-00.041105" 0MC"FOi"IPW003-0-041105 DMCrF014PW003-0,041105' DMC-F014PW004-0-041106 DMC-F014PW0040 "041105` DMC-F0i-1PW00841-041105 DMC-F01 "IPW005-0-04118b' OMCrF01-MSW003-0-041105 DMC-F01 " MSW003-0-041105' DMC"F01-M8W004-0-041105 DMC-F014+IBW004-0~041105" DMC-F0I-MSW005-0-041105 DMC-F0I-MSW0054-041105' DMC-FOt-MSF002"4I 106 DMC-F01 "MSF002-0-041105' DMC-F01446F003-0~041l05 DMC-F014ASF003~0-a11105' o1+iC"FO1418f004"0~041105 DMC-F01 .WfSF0044).041105" DMC-F014ASF005-4041105 DMC+014ASF005o0-D41105' DMCf01-IPF004004110ti LH4lC-FOt-IPFQ03-0-04f101i " C4 Sultonste "ES PY/UDfebUb11YY1101Yft Analyls Found iPSsed Accuracy rwt wL +~.16 NO 30 NO 30 NO 30 ND 30 ND 30 ND 30 NO 30 ND 30 ND 30 ND 30 ND 30 ND 30 ND 30 NO 30 NO 30 NO 30 NQ 30 NO 30 0.300 30 0.345 30 ND 30 NO 30 ND 30 NO 30 0.318 30 0.233 30 NO 30 ND 30 NO 30 ND 30 NO 30 NO 30 NO 30 ND 30 ND 30 NO 30 NO 30 ND 30 CO SulFonste PFHS P-- ~WOHAK/AvsuronYb lyln , Found at VA . AOcurecy +l-9G ND 30 NO 30 0.285 30 0.282 30 0.368 30 0 .341 30 ND 30 NO 30 NO 30 NO 30 NO 30 ND 30 ND 30 NO 30 ND 30 ND 30 0.388 30 0.334 30 0.398 30 0.464 30 0.270 30 Q.258 30 0.592 30 0.560 30 1 .90 30 1 .88 30 O.BBO 30 0.938 30 NO 30 0.367 30 NO 30 NO 30 0.254 30 0.228 30 0.420 30 0.448 30 NO 30 NO 30 CS SuNonatb PF06 PWnWOfOOC1M6&AM011@1f An8lyts Found AsieNed Accuracy wt *I- % 148 30 144 30 198 30 199 30 173 30 I se 30 118 30 115 30 11n 30 111 30 73 .8 30 72 .0 30 130 30 134 30 81 .6 30 83,6 30 81 .2 30 83.8 30 88.8 90 89 .8 30 84 .4 30 82.8 30 364 30 330 30 259 30 289 30 NR NR NR NR NR NR NR NR 58 .8 40 68 .0 40 116 30 199 30 146 30 147 30 7.92 30 7.92 30 'LSborstwy DupBCafe NO = Not detected st or above Um f! of Quantkafon which is 0.2 nplq (wet weight) . NR a Notmyor4d due bquWnyoonwlnunfalkiros. Exygen Research Page 27 of 132 0002'70 Interim Report #10-Analysis of Fish and Clam Samples ~ Exygen Study No. : P0041131 Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued) C4 Bulfonate PFq Cd Suronats PFHt3 POllraohwwwwlk~~ Cf Sultonab PFOf RwAuaooc4ewrlfaret C0049604 DliAC-W1-1PF004-0-041105 ND 30 ND 30 44.0 30 C0049504 Rep DMC-F014PF004-0~041106' ND 30 ND 30 46.6 30 C0040505 DMC-FOIJPF0064-041105 NO 30 ND 30 48.4 30 C0049506 Rep OINC-F01-IPF005-0-041105- NO 30 ND 30 46.0 30 G005635< DL2-F01-M8F005-0-041218 NO 30 ND 30 49.2 30 C0055354 Rep DU-F01-MSFOOCrO-041218' ND 30 ND 30 51 .8 30 C0058466 DIL2-F01-PW006-0-91215 ND 30 C0056455 Rep DL2-FM4PW00"-0412i5* NO 30 C0088456 DOU-F01-MSW002-0-041216 0.208 40 C0088466 Rap DQU-F01-M8W002-0-041216- 0.227 40 ND 30 ND 30 1.72 30 1 .70 30 13,2 30 13.3 30 MR MR MR NR C0038457 DL2-F01-IPW004-0-041215 ND 30 ND 30 8.80 30 000b6457 Rep DL2-FO1"IPW00440-041215' ND 30 ND 30 6.80 30 00068458 D04J-F01-MSW003-0-041216 ND 30 10.4 30 MR NR 00058458 Rep DOU-IM01-WWO03-0-0412164 ND 30 10 .8 30 MR NR C0056459 OL3-F014PW004-0-041130 ND 30 ND 30 7.92 9o C0058459 Rep DL3-F01-1PW004-0-041130" ND 30 ND 30 7.52 30 C006e460 D0U-F01-MeW001-0-041216 Us So 15.4 30 MR MR COOa8460 Rep DOU-F01-M3W001-Ob041216' 7.12 30 14 .2 30 NR MR C0056461 DOIJ-f01-M3W004-0-041216 4.72 40 21 .7 30 C0056461 Rep D0U-F0i-MSWOOA-0-041216' 4.58 40 22 .5 30 NR MR MR NR C0058482 O0LI-F01-M8W006-0041216 0.384 30 00058482 Rep D0U-F01-MSW005-M41218' 0.36 30 1 .34 30 1 .41 30 NR NR MR NR C0068483 DOU-F0I-MSF005-0-041218 1 .41 30 8.40 30 00058483 Rep t]OU-F01-MSF005-0-041216' 1,43 30 8.44 80 MR MR MR MR C0085464 OL .3-F014PW002-0-041130 ND 30 ND 30 12 .0 50 C0055464 Rep OL3-F01-lPW002-0,041130' ND 30 ND 30 11 .5 80 C0056485 DL3-F01-lPW003-0-041130 ND 30 ND 30 5.44 40 C0066485 Rep DLS-F0I-IPW003-0~041130" ND 30 ND 30 5.28 40 C0056486 DOU-FOi-sISF003-0-041218 1 .72 80 8 .56 30 MR MR C0056488 Rep DOU-F01-M8F003-0-041218" 1 .73 30 6 .88 30 MR MR C0056407 DBC-F01-M3F006-1-041216 0.220 30 1 .79 30 MR MR C0055487 Rep DBC-F01-MSF006-1-041218' ND 30 1 .76 30 MR MR C0055488 OBC-F01-1VI8F006~0-041218 NO 3D 1 .68 30 MR NR COOaNAB Rep OBC-FOI-MSF0050041218" ND 30 1 .59 30 MR MR C005e489 O0U-F0I4A8F0(k2-0-041218 O ."8 30 4 .58 30 C0068489 Rep DOU-F01-M8F002-0-041216" 0.872 30 4 .58 30 C0055470 DL3-F014PW001-0-041130 ND C0056470 Rep DL3F01-IPW0014b041 S30' ND 30 0.246 30 30 0.219 30 MR NR MR NR 9.04 30 6.80 30 'Leboooay Dupllcals NO " Not detected at or ebove Lknff of QuanMtuRon which Is 0.2 nglp (wet weipht). NR = Nolreported du*to qusRy o0n4o1 moult fiiAoev. Exygen Research Page 2$ of 132 00f)271 Intcrim Report #10-Analysis of Fish and Clam Samples , Exygan .Study No.: P0001 131 Table I. Summary ofPFBS, PFHS and PFOS in Fish Samples (continued) la C0066471 C0056471 Rep C0056472 C0058472 Rep C0056473 C0056473 Rep C0066474 00058+474 Rep C0058476 C0056476 Rep C0066476 C0066478 Rep C0056477 COO58477 Rep C0066478 C0056478 Rep C0056479 C0036478 Rap Client Sa 1e ID D0U-FO1-118F002-1-041216 DOU-FO1418F002-1-049216' DOU-F0I-IIBF004-0-041216 DOU-F01-M5F004-0-04121d' DOtJ-FOt-MSF001-0-04l216 DOU-F01-M3F001-0-041216" DBC-F014AF003-0-041216 DBC-F01-MSF003-0-041218' DBC-F0I-MSF004-0-041216 DBC-F01-M8F0040-041216" DMC-FO7-MSF001-04041218 DMC-F01-MSF001-0-041216' DL1-F01-IPW00&0-041216 DL1-F01 "IPW005~0-045216' D1.2-F01-IPVN003-0-041201 DL2-F01-IPW003~0-041201- DL3F01-IPW005-0-041201 D1.3-F01-IPW006-0-041201' 04 suironau vFSS Pefterebutwift.ran.i. Ana* Asaewd Found Accuracy wt +I- 0.840 30 0.860 30 0.792 30 0.818 30 2 .18 30 2 .28 30 ND 30 NO 30 ND 30 ND 30 ND 30 ND 30 0.253 30 0.249 30 ND 30 NO 30 ND 30 ND 30 CS suuonaa PFrs .Wa*0fQk.Kh..*H...r MolyW Aeaesaod Found Accuracy wet wt. W- %I 4.68 30 4.72 30 2.35 40 2.22 40 10 .9 30 10.7 30 209 30 2 .09 30 3 .87 30 3 .77 30 OA20 s0 0.458 30 . O .e44 30 0 .644 s0 ND 30 ND 30 ND 30 ND 30 c$ swtonate PF0a .wIw.Pqd.%..Wk+.#A Anolyie Asasased Found Accuracy (noff) WRIVA . (-/- N. NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR 88.8 30 67.6 30 7.48 40 7.44 40 4.88 30 4.72 30 "Labanloy Dupiaab ND - Not detedad at or above Limit of Quantitatlon wNch is 0.2 nplg (wet welaM~ NR a Notaporrad due to qwilty conlrai re" faihiros. Exygern Research Page 29 of 132 0002'72 Weriun Repoit #10-Analysis of Fish and Clam Samples Exygen Study No. : P4001131 Table II. Summary of PFOS in Re-extracted Fish Samples ExygenID COOy8t51 C0048152 C0048153 C0048154 C0048155 C0048156 C0048160 C0049450 C0049451 C0048452 C0049453 C0049454 C0048455 C0048456 C0049458 C0049459 C0049460 C0049461 00049462 C0049463 C0049405 C0049466 C0049467 C0049489 C0049471 C0049472 CYent Sampls10 OBGF014FrW001-0-041021 DBC-F0I-IPW002-0-041021 DBC-F0I-IF'W003-0-041021 DOU-FO1-IPF001-0-041021 DOU-F0I-IPF002-0-041021 DOU-F014PF005-0-041021 DOU-F014F'W002-0-041021 DBC-F01-MSW001-"41104 OBC-F0I-M8W002-0-041104 080-F01-1N3W003-0-041104 OBC-F01-M5Wfl04-0-041104 OBC-F0I-MSW005-0-041104 DBC-F0I-MSF001-0-041104 DBC-F0I-MSF002-0-041104 O13C-F014PF005-0-041104 DBC-F01-11?tN004-0-041104 DBC-F01-IPW005-0-041104 DOU-FOI-IPWO034%1104 DQU-F0I-IPW001-0-041104 DOU-F01-If'W003-0-041104 DL1-F01-M5W001-0-041104 DL1-F01-MSW002-0-041144 DL7-F014d9W003-0-OA1104 DL1-F01-MSW005-0-041104 DLi-F01-MSF002-0-041104 DL1-F01-MSF003-0-04i104 NR - P40 reported due 10 quQlj4(CwWd result failures. Exygen Research Cd Sulfonate PFQ$ Pernuor0octqnsssMoosts Analyts Foand (nn) wet wvinc Aasessed Aacurac.yl 2060 30 3330 30 1680 30 596 30 836 30 644 30 1210 40 9480 40 7520 30 12400 30 3440 30 5240 30 5240 30 4760 30 608 30 1230 40 2620 30 MR MR 1740 30 2130 30 968 30 708 30 696 30 604 30 668 30 432 30 Pagp 30 of 132 OO02'73 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 Table 11. Summary of PFOS in Re-extracted Fish Samples (continued) Exypen ID C0049474 C0049498 C0049499 C0056456 C0056458 C0056460 C0056461 C0056482 C0056463 C0056486 CO056467 C0056468 00056469 00058471 C0056472 COO;f6473 C0056474 C0051%75 C0036476 C0048148 C0048150 C0048156 C0048157 C0048139 00049473 COent _ Sample ID DL1-F01-MSFOOS-0-041104 DMC-F01-M8W006-0-041105 DMC-FO1-MSF002-0-041105 DOU-FDI-MSW002-0-041216 DOU-F0I-MSW003-0-041216 DOU-F01-M8W009-0-041216 DOU-F0I-MSW004-0-041216 DOIJ-F0I-MSW005" 0-041216 DOU-F0I-MSFOOS-0-041216 DOU-F01-11ASF003-0-041216 DBC-F01-MSF005-1-041216 DBC-F0I-MSF005-0-041216 DOU-F0I-MSF002-0-041216 DOU-F0I-MSF002-1-041218 DOU-FOi-MSF004-0-041218 DOU-F01-MSfO01-0-041216 : DBC-FOI-MSF003-0-041216 DeaFO1-MSF004-a-a1216 DMC-F0I-MSF001-0-041216 DBC-F01-IPF001-0-041021 DBC-F01-IPF003-0-041021, DOU-F0I-IPF003-0-041021 DOU-F01-IPF004-0-041021 DOU-F01-If'W001-0-041021 PL1-F01-MSF004-0-041104 NR = Notropaqd due bquality oorArol raauH faAures . Ce sultonaba PFOS Poflua+ooebn~swlbn~b Analyle Found M)w8twelot Assessed Accuracy (4j- %) 740 30 580 30 620 30 28200 60 4040 30 NR NR 5120 30 496 30 720 30 848 30 NR NR 8980 50 640 30 892 30 1820 30 2070 30 4640 30 92eo 50 &10 30 384 30 293 30 359 30 424 30 387 30 348 30 Exygen Research Page 31 of 132 000274 Interim Report #10-Analysis of Fish and Gam Samples - Exygen Study No. : P0001131 Table 111. Summary of PFBS, PF'HS and PF4S in Clam Samples Ex ib Clsnt Sa mple ID C0056480 OL3101-CPW001-0-041216 C0056480 Rep DL3101 "CFW001-0-041216" C0058481 DMCG101-CFW001-0-041216 00066481 Rep OhAC-101-CFW001-0~041218" C006B482 D1.2-101-CFW001-0-041218 C0058462 Rep D12-101-CFW001-0-041216' C0066483 OBC-101-CFW001-0~041215 C0056483 Rep D8C-101-CFW001-0-041215" C0068484 DL1-101-CFW001-0~041215 C006E484 Rep D11-101-CFW001-0~041216" C0056485 DOU-101-CFW001-0-041216 00056485 Rep DOWO1-CM001-0-041216" C4 SuNonale PFSa Fwlworohu AnaW Aftassad Found Accuracy w1 . +l- % ND 40 NO 40 ND 30 ND 30 ND 30 ND 30 ND 30 NO 30 NO 30 NO 30 ND 30 ND 30 Cb sulionab PF11S hAiqrohmnaulfonab Ana" llnssnd Found Accuracy rwt aR. +1-16 ND 40 ND 40 NO 30 NO 30 NO 30 NO 30 NO 30 ND 30 NO 30 ND 30 0 .202 30 0.205 30 CI sullanaee PFGS rwfY~a~ood~nwrlbnrb Analyte Assanad Found Accuracy w.t wt. +1" 16 1 .82 50 1 .82 SO 6 .18 50 6 .12 50 1 .81 50 1 .77 50 4.48 30 4.44 30 8.80 40 8-84 40 11 .4 50 10.9 50 'ia6cxatory MOW* ND = Not dslrc6ed at or above Unit of QuaeiifafiCn which is 0.2 ngy {wst weight). Exygen Research Page 32 of 132 0 f10s;73 p. 33 Interim Report #10-Analysis of Fish and Clam Samples , Fxygen Study No . : P0041131 Table IV. Matrix Spike Recovery PFBS, PFHS and PFQS in Fish Samples $vnp10 DLSSF014pF0014-00021 ;000arr4 so 0,1e rpe) ot3.FD1 .IpFDD1-0oa1oml ;cWO2SSPF,111Oppe) DL3-F01-IpF012-0-041021 ICOOxtm781tD.1101001 DL3-F014PF002-0-041021 4CO848tttept 0,100 PP4 DOdC-F111-IPF001-0-0410Y1 ;a0wstw$pe e. w pr} DIAC"FD1dPFOD1-0~041021 IOON17rEytN.1rOp11) DpG" F01dPF00Q-40410Q1 fOmlnlOiWcGN10l1 DIAGF01-IPFOU2-0~041021 lOcDwf70 Wk H, 100 001 DMGF01-IPW001-Od141021 (caoa+w pu 0, wM) 171rIC-f01-IPyV001 4NW 102 t IOOw+1a04114100yoei DYIGF01 "IPW002-0441021 Ia00171ftkR101oh1 DMC-F01 "IAW002-0A41021 ;a00Mo191"larpq DMC.F01-IdSVY00i-0-041021 ;OOOIM7t a~ E,14 0~ ~1 DAAGPOf-h1SVY001-0-011021 ;COW8i76ptF.100pwlpY) DpACGF01 .lASYY004041021" tcoae+~7eol~c,s0~~wl DMC"F01 "IdSYV00Y-0~0410Y1" ;o00yto3 30 N. r00 fpb spa) DtLc9.n4l1.0+13-+IlF,Fk0.0.1+.4v-0o4b1a0wZ.1! 012-F01"1pF001-0-0 "1t121 ;a00lsrr 1R K 1m pa tpllel DL2-F01-IPF00-0-041021 ;CaoNiK ~e 0. ve0earol D1 .2401-PF002-0-041021 (ooowls4qcL +0oPot0 ") 6pDnd c4 sWtvrle rF o Amount !n 3npAr ROOmWod RKo+wy 1~.Iw. r1~W4 ound In 9wmpN wlrt PFNo Nn01nt Weol+urd NAooNy ~wt~i CS OWWW" aF0 Ant Found AMnOue! in BDnqle R-awr~d fiOeOlwy +11M wNNt 10 0.30p 6.56 67 100 0.309 62 .4 62 ND e.26 63 5.16 ND 73 .2 73 5.10 12 .6 74 T8A 73 10 02E6 100 0205 6.52 53 60.6 . B9 ND 7 .4E 75 4,16 No 79 .6 60 4.19 10.3 61 50.6 77 10 0 .830 4 .46 42 ND 5 .94, 52 7.40 9.90 26 100 0 .370 55.4 86 ND 74 .6 75 7 .40 81 .8 74 10 0.712 T .E6 7D ND ta .(i0 Y6 14,1 100 0.712 78 .0 77 ND 96.0 06 14.1 29 .6 156 104 90 10 1,08 7 .60 85 ND - 7 .64 78 70a 11 .8 " 100 1,00 61 .6 64 ND 80A 90 7011 131 p1 10 0.968 6 .76 88 NO 7.05 80 34.4 44.8 " 100 0.990 6Da 00 ND 74 .6 76 34 .4 101 67 10 0.216 9.76 96 0 .624 taA4 as 270 100 0.216 812 61 0 .524 83 .2 93 Z70 Z10 ` 375 106 60 ND" 462 90 50D ND" 432 86 ND- 52A 104 530 NO" 462 06 530 4T0 " 924 79 10 0.ew 6.60 61 ND 6.56 66 3.4s 6.35 49 180 O.A60 46.4 46 ND 611.9 go 3.45 56.4 53 10 0.616 5.84 46 ND 6.40 64 4.72 6.56 38 100 0.816 64 s 54 ND 782 79 4.72 72.4 66 18.np, ruld .. .ac..d.M.lpldnp Lrei 096111o"n~f"ri,*Om +n ucwab swine valuealr,abe wwl.rd " 1 .0yaf nnyftto" torooine8on InNraof 6.0 0. ND " N01 doliedOd St or above Ume d GuOnpIWOn wh1ch he 0.2 npq OW welyd), ND" " Not detected st or ohm Lknlt of QwMRalbn which 101.0 n0)0 Not "9hq. NR " Natrpa1W dW qaw"y oaNal rw1! bluns. llrwullwk wWt~ On thownIn TaW 1. New Since 11110 auwnmwy Y610 dim" round09 nWIM, rr00wy wIVM nyy wry OIIpIMytfAmn Ur hpan In so gow date, Exygen Research Page 33 of 132 0002'76 p. 34 Interim Report #10 -Analysis of Fish and Clam Samples Exygen Study No . : POd01131 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) 1Dmpi0 on M2-FO7-IPF0001-00~so0bts1p0e2w1) Drs.fm .IPF60ao4e1021 t~4~ iYt H, too ppe Op1ul DL2F01-117F0044+041021 ICa0101JiipIcD.tODpitpnr) OL2-F01-IPF004A-04f021 rm"127sqc 4 troo vv104r1W DL2-F01-1PF008-0-0N021 looalrsu 1111k a, 40 006 sPftl DI.Z-FOt-IPF006-0-041021 (Ceoula! 3ok J, taD Wr 1Oy DL2-F01-IP1N001-0~041021 ICO9ae1b Npr, topp sprel bt?.F01aPY1I001-0-041021 4COW4139 f0 14100ppolyh) 0.2~F01-MSF001A-041021 t0004e148 eok4,10 oar000f DL2-F01-M9FO01-0-041021 (0004114011pt I, IN ph epY) 131.2"F01 " M9FO02.0-041021 (C0001epkC,I0pp>k+W) DL2401-MeFaa2 .0c41ot1 ICO01141, e0 It, tW P16 3a11111 DL2"F01-AABFOObO-0410R7 (OOOtns9 qk D. 10 oPf e11"1 DL2-F01-M9F00340490e1 ;COON1,12 6p11,140 pr slub" DL2F01" M9F004-0-041021 QC"OriS49110 11,10 qh .4011p4 DL2-f01-M'F0044-041021 Ioo0w14a #J, loo Ae S.p)a DLSF01-IPfOD1-0811021 (Ca001a 10 F,10 PprlOrl OL1-P01dPF0D1.)-W f 027 (aanu50 IL tm pPr splrl DL3-F01-IPF003U-04f021 (rae611411 "It 0,10 PA 111011r) DL3-F014PF003-0-041021 lCOOt6t4S sy L, t00 por ~1 mOwR BPksd su0altift PFW Oun! Am." In SrmPle RbDDwred RDOowly W .e. r .eax. C6 Aging w 9w11p1f va,w NS WmwrDd RoDDwy +rl .a. C6 SKande PFOS Minet Fpmd Amount BDmpN RaODVrad WoDnry wKwt *we 10 0.247 7.00 as 100 0247 62_! 63 110 7.0e eD 2.01 ND 73.2 73 2.01 9s0 72 74.0 72 10 0.346 6.84 06 100 0.946 67.6 67 10 0.338 6 .88 66 100 0.336 68A 6s ND 7 .60 76 4.02 ND 76.11 77 4.82 ND 7.0 77 2.48 NO ' lO.b 81 2.46 11 .3 as 60.4 76 9_15t 72 II2.0 EO 10 3326 7 .04 67 ND 7 .60 76 S.Itl1 13.9 !0 100 0.8Z8 0d0 06 ND 77.2 71' S.90 06.2 79 10 OS3s 7.X 70 100 03'13 64.5 64 WD 6.20 02 77,2 I!D 77 .6 78 77.2 76.0 ' 156 111 10 0.406 a.SR as 100 CAN 61 .6 61 NO 7A8 75 94.8 !AD 60 .0 66 94.D 101 " 15D 61 10 QA16 6.62 111 ND 6 .76 66 41 .6 41 .2 " 100 OA16 Q4.t 64 ND 70.9 71 41 .6 104 62 10 0345 7,08 67 'ND 7.0e 7D 83.0 91 .2 ' 100 0,348 71 .6 71 ND 61 .2 a1 E3.4 167 63 10 0.432 7.44 70 0.2111 8.16 79 33A 40.0 ' 100 0A32 e72 67 0.261 76 .4 70 33.4 106.0 73 10 OA4E 720 O6 ND D.OD 61 3 .66 - 10 .5 70 f00 OA40 E21 69 ND D1 B E2 8.66 90 .0 78 -9nnVw rrWw aomrbft p1Arp W& sIpiYler+Yto, Ihwvbryan aoardY rwoltfry Mlue o404 be Ca4+albd ND - Nd dsbe4d bt or Own LYnR dGuin41YD0ertMd1 Is 0s nyp (we! walOht). NR +Nat ntPAW duPto OuatYaonYOl wwll hIN1n* llsarlyda w1ullY IA ~In TWOII.. Nab: llnep1hbwxnnly bD4shows mweded MwkD-jso1wrYv~Wn ul"Y~11~O~Y hM11MvllWS MMr raw WY. Exygen Research Page 34 of 132 00027'7 p. 35 Interim Report #10-Analysis ofFish apid Chip Samples , Exy0en Study No,: P0fl01131 Table IV. Matrix Spike Recovery PFBS, PFHS and FFQS in Fish Samples -(continued) 9~mplk OL8-F014PF004A4041021 10oo1i1u " pk 0. to 10Yirrr) DL3-F01-IPF00"-0-0i1021 ;G001tu0 91t h. t00 p116 solo) Ol3-F01-IPF006-0041021 0o =4611 478010 ). pliY841w) DL9-F01-IPF006-0-041021 4Wai147 qr 6 tae Per, SPIN) DBG1`01 " IYF001~0~041021 (owl" t".tOpp "pR.) DOC..F01 .IpF001-0~041021 iC4wuua spn .i . mOppo sFlb) pBPiF01-IPF0(k2-0-041021 ICOaNa W 11, 10 rob DOW) D8GF01-PFV02-0~011021 iCOOH14o eptK 1p "pp tprY 00GF01.1PF0034~04f021 Kooalsoipk 0,lopwaoa? OOC-F014pF003-0-041021 (ooONti" spl~ L. to ppo "pwl 09C-F01-IPW001-0O11021 . 10701N61t7pkC.tOpObslta) OBC-F01-IPYY001-0-M7021 (0oow+stspak .ipopr "plla) DISC-Fawwuo2-ao4102i tCawwa)yKO,wppb8pls~ OBGF01-IPW0020~11I1021 ICOOwiG7Aptr .lmprdeplh.) DECrF01-PW0034041021 %aaits3lfta,10ppbqls) pOCGF01 "PW0004041021 tceu"laa"oJ. to ppe syls> v0u-F01-tvF0o1-0-asoal 1010141411'pkp.110 ppYBpbY DOU"FO14iF001-0,041021 Iooow"161 60 R. 1110 NO t001 ooU-F01-iFF00241441021 (C-00t6d Mr a to rob 600) D0U-F01-IPF002-0-041021 K:oa "16ispkL. 100pYipls) O0U-F01-IPF003-0-041021 Iopowsla"1NaC, tp 1 "r tp9mY OOU-FOI-IPF003-0-041021 630,18156110K loom 01wq ASm0OuWn1 C4 &A'WW@PFBS ArMBM.. W* Amount . In Recoo"~d. .fhca~wry Rlrrnt FwM', ;. 1Sn'iottpt' ~n 9mpp " RaoWhd wt . ww~t. Woawy " An* faa~d hSamp* rtt wt Amaulst R" oowrd wt wL Weowry f0 0.764 6 ."4 81 " . NO i 1016 ~ . , 10q . , , D=_ , E.96 88 ' 100 0.704 69.6 00 NQ B.84 ,. , 68 , ., 0.88Y., . 612 81 10 1 .53 5A4 38 . ND : 0 .10 , . 92- . 5 .48 . , , 11 .7 62 . 100 1 .53 00.4 60 NQ . 01.2 93 6 .46 65.0 61 10 1 .34 0.24 49 0.802 102 101. ,,NR . MR MR 100 1 .34 6&4 66 0.092 96A , ,. 88 NR, . MR MR 10 1 .41 100 1 .43 10 0101110 100 0.906 10 0.684 5.84 44 601 66 6.72 57 60.6 60 7.06 ~_ $2 , NO No 0.944 ` 9:614 ' 2:21 835 . 94, : , 110 , E6.0 66 , 110 ' 90 10 .4 , . . NR 06A 66 . MR 0.66 73, . MR 113 ' 180 79 NR MR MR !*t MR MR 100 0.084 70.0 80 2.21 Will 96 NR MR MR ' 10 0.700 , 7 .50 00 ,432 162 , .D1 , MR NR MR 11 ~100 0.700 6a8 OB 9.12 86.0 . 87, ' MR , MR NR "10 0.736 ` 8 .32 76 8 .76 16.5 " Yl ~ " MR i 100 0730 , 70s 70 6 .70 0o.e 64 MR ,.. 10 4.36 10.9 '85 1 .02 8.48 - a6 MR. MR NR NR MR NR MR -~ 100 4a6 76A n 1 .02 66.0 85 1 MR + MR NR " 10 6.76 . 13.1 63 0.792 9.72 8D MR . NR MR ' 100 6.76 764 08 0.742 ~80.0 79 ~ MR MR MR 10 6.66 12.6 . 88 1.02, . ^ .10.6 96 NR, ' ' NR MR 100 6.60 814 , ' 75 ." 1 .02 08.4 97 " -'HR NR NR "lomplu wddr ".oaw&ft spllln0bvW*IprWk7npy;lnr+torn. an rour0s 1wowyr~Yw caardbw cdkJated ND " Nat OeLc1ad it or ow"Llmt of Qutnu)a0on wWclt It 0.2 rya(MIW"Iplhq . NR "NatAporeW dMnb quuRy - YOIrrult hi~ne. RrweivMi mvoe uu dmWin InTabMS N. Mob: 'Ina We sunAAle1y tattle oh.'1Yi rounded 111wd01.ti00YwyValYNwAyvrY dlpMyfnm1M valwas In** rawdoes. Exygen Research Page 35 of 132 000278 p. 36. Interim Report #10-Anatysis of Fish andCtsm Senples Exygen Study No . : P0001131 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) sotqb Dou-F014PF004-o-041027 IcoaWssaye 0,10 sob SOW OOU-F0I-IPF001" 0-041021 (Cmaetailoti,tmp" ape" DOU-F01-Irt0080-041021 ICOOwteNpi ~. toyw sr11~1 DOU-F014PF005~0-041021 (Main Spe J . log wY eprY) DOU-F01-0P41r001-0-041021 (coos+w 10 r.10 sob 111pl+! DOU-FD14PW001-0-041021 (cb101511 Ut It. t00 WIN Spin) 00U-POt-1PW0024?-041021 ICOW61001pu0 .1000 51Yq DOU-FOS4pWf002-0-041021 (caanalpr c,1w we ipr) Dl2-F01-6161N001-0-041021 (C0014101 so 61t so l00) 012fo1-MSw901a~041021 tcoae,asp~~.la~,esrr~ 01.2-F01-Ir19W002-0-04f021 (qooutriti0 rc,wPpp~spri 01.2-P01 "M5yV00Z4H041021 (Dpewtailpt L. +OO wrb Sqwy D1.2-F01448y1f000-0-011021 IposutaOpk C,10 spp811,061 DL2-F01-IAB1M004~011021 (caastappt 0.10010 6plh) DL2f01 448W00441-011021 (COOU1e4 ykB,lo11710 low DL2-1`01418W0040411021 10ean66 0O1. F, tw pp sph.l 012-F01 -NIt1N0011"0-041021 (OpJltpayk0.to00ipey 01.2-1`01 " WVY006-0441021 ICOOis,e6 apk N,10A ipe s~l DeaF014,usiwo01a40104 (COx4aa ask C,1o wr srw) Dec~Fol-Msw001-04411104 1r,ao4000 00 p.106 MelpAu) spked sar ' PM In 8rmpl" RoeDwW Re00rerY wl~t. .rlrl. asuxona.v~ Its aurW -=;r in SOmple RooOVwOd RAoowY wt YIwL Cal su0arru PF AM FouW --A= In Sontplo Rsoovi1r40 wlrR . rntwt. ReCAWY 10 6 .12 13.2 11 2 .a0 12 .0 97 NR 100 3 .12 7E.4 70 2 .30 EE.0 64 NR NR MR MR NR 10 4.56 121 76 0.966 112 102 NR 100 4.56 7e.0 71 0.145 85.6 aE NR 10 2.lp 10s 73 0.41s 10.7 se NR 100 2J19 72.4 70 0.948 ' E3.6 83 NR 19 1E.4 34.4 1E0 3 .40 132 95 MR 100 1 &* 41 ." 7111 3A 80.2 Se MR NR NR NR MR NR NR NR NR NR NR MR MR 10 0.303 0.32 91 ND 6.69 07 120 1ao 0.205 70A 77 NO fla.2 as 120 ' 10 NO 9.06 QI ND 9.12 91 102 100 ND E0 .4 as ND 43.8 04 102 10 NO , 9 .24 02 ND GA! 11 02A 100 ND 61 .2 e1 ND 952 96 92A 128 " 177 ST 110 " 105 03 103 " 182 90 10 ND 7 .56 76 ND 7.2e 73 06 .0 100 NO 42 .0 02 NO 93b 94 04~0 10 ND 7 .96 SO ND LOS A1 1(A 1130 ND 00 .e 91 11D 100 1.01 705 10 O .ss6 10 .3 pl 8.32 I?A 93 NR 100 0 .!!S 90 .4 90 19.32 110 105 NR 75 .6 ' 10e 7E 125 " 234 a0 NR NR NR NR "8rnpsrwiaiw saopaa lhr sPlMrq WetrpN~wnar: rr~aa. en ~oa++w noiwrvslue ND " Notasioeiea ucrab" umll of nii0numion .N,ICn Is 0.2 &A (wot WOW) . 'he d1a~IN NR " NetnparyA Aos to ErUsrCOb1Yd iwi11faIAIxN. RNoI"i nlrAs an Wool MUMU. No1LS lIOOqthis swtrn(tldb shows rounded r0Wlb, weaul~fYvdWr Mryiqh' "i1~MYfiea~ No nhri In 1N raw d1U. Exygen Research Page 36 of 132 0002'79 p. 37 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No. : P0001131 Table IV. Matrix Spike Recovery PFBS, PFHS and PFUS in Fish Samples (continued) 8rlph Dec.FC1-MSWO02-0-o411D4 IoalpqfapwE,+0pppOprl DBG"F014ASW0024-041104 ICap001501,F.100 pO eprl DBC "F0140W003-0-041104 1COGp16t! E0 0,10ppb Soft) 09C"F014I3W0030041104 moon=GO H.1po mb low C6C.F01-AIS5M004-0-041104 ICaplEle3 80 t. 1000 110r) OQCF01-EIBW004-0.041104 IcooN10p EpkJ, in PO Epllrl Dar..FO1 .EnW0oe.o~o41104 Pwpw ep>LloppsEpwl OpPFO1-MSW005"0"041104 Icowwksyt4troai+epw OBC.FOt-MSF001-0-041104 POW" EpkA6 q PO qlhq DaC-FD7-MSFOOI-ao4ltoa FmINie >kr<+t, wopp pw> DBC4014ABF002-0-04104 ICo04"" Epw O, t0 ppe E1010 bEGF0141.7F0024-041104 tooptwep "k P. wp we Itpw1 OrBoGaFoD"7n"IsPoFc0.0+4o0p0pe4$11w0"11 DeC-Fo1-IPF904a.o41104 ICOU9~67ap~.0tpoppESyul DBCrFO'1-IPF005-0-041104 (aWW!lpYE,l9ppb NOW OEGF014PF0084041104 IGOww4ltqF.1oDpp" ipr) 0eo.FO1-IPWO04~041ao4 (Cea~ai Opu 0,1p ppr ") DBC-FOt-IPW004-0-041104 0E040490 SptH100ppYEpliN OBC-F01"FW0060-041104 Owetwp0 1111Y L 10 PO Ow D9C"F01-IFW00M0M4110" (s4miap 9O J,10 PO tpoq Mlaml a7ik4d Gt 9dfv1E F in BEptpb Rpapwnd R4oowry wt .~. rrtwt 8 Amt FOUM In gam* wr .~t ~ FFiS Owd ApcovEnd Rttoorry .ww. Amt FO" In 8Emplp Wwrc tO PF Aaqunf RsoovEr40 rwrt S Reoov~y % 10 OA06 9 .w 91 3A3 12d 94 NR 100 0,86! 94 .E 94 3.43 113 110 NR NR NR NR NR 10 O.EEO 9.92 91 100 O.s00 E5 .0 a6 10 0 .084 9.08 91 100 0 .904 97,2 96 10 0 .032 d20 74 100 0 .052 91 .e 91 312 13 .6 100 NR 3.82 104 100 NR 0.72 19.5 99 , NR 9.72 124 114 NR 2.77 1D2 74 NR 2.77 !00 106 NR NR NR NR NR NR MR NR NR NR NR NR NR 10 O .B20 9.80 59 3.60 13 .7 101 NR 100 0.920 89.4 6E 3.85 406 102 NR 10 0.786 6.02 92 1 .54 42 .5 106 N R 100 VU 90 .0 9D 1 .94 1oR 100 NR 10 0.eo4 sos 100 D.ao4 I IA 110 142 100 O.SW 94 .6 94 0 .564 108 105 U2 10 1E0 10A 9f 2 .15 122 101 NR 100 1-00 90A 06 2 .15 105 100 NR 10 0 .484 9.72 12 3.0 13~D 97 NR 100 0 .404 us 87 3.20 104 10f MR NR NR NR NR MR NR NR NR ~s2 " 254 112 NR NR NR NR NR NR NR NR 10 0.672 10A 9E 2.10 132 111 NR 100 C .672 92A 92 2.10 102 100 NR NR NR NR NR '8nep1v iw10w rs:wdb EnapikiV IMI sID*Acw . p~~. an ooprtM~nopwY ~cwialY~ akulWd , WD = Noldebecled al or obow UM of qwOON1tlen wNds to 0.2 rot(w41 rnlpd?, NR-Net npplp0 duwb qrWly00npOt rplklt ftpaa IINnYyd~ w~WOpEP1EhWpM7phlp 0. NCq: OInp,lhf&su,lwwry WNSahMwp wandpd NiYHs, haaNwy Wlwp erlrvwry rM9hllYNO 00 vwlw i0110MW dft. F.xygen Research Page 37 of 132 0002S0 p. 38 Interim Report #14-Analysis of Fish and Clam Samples Exygen Study No .: POOa 1131 Table IV. Matrix Spike Recovery PFBS, PFHS and PFQS in Fish Samples (continued) BY1v10 Ammst Spiked C4 Uftnefil, Not Amouft ift 8rro-014 RsO0vp40 R4oprwy CB rFHS Ainft F*i"d_1X= 80rtipN RlOOwwd Recovery 0 6u PF Arms Ax" l4ffwuwt in80npIF RlCalrld ReeWety D0U~Fp1" IW40030~041104 I~0040,01 4w K 10 GO 5p40 10 3 .12 13 .1 100 e.00 10 .3 103 MR D0tJ6F01" IPYV003P411104 looawal so L, lao Ar 31001.1 100 3.12 e8O B5 0 .00 107 101 MR DDV-F0I-IPYV001-0041104 fc400011 8,kc.1000am) 1o 3.a9 12 .8 93 7.12 17.4 103 MR DOlLF01-IPW0044"1104 ICaonsma $04 gas pb spin) 100 3A9 ISA 86 7.12 109 101 MR DOV-FOS" Ii+W000-0-041104 IOooww 0!k R to Fp5 fplry 10 247 10.5 75 5.12 13.5 e4 MR pOli-F01.IP1N006.0-OS1104 tamnM fppc r. $oo GOD ~pw) 100 2.97 03.e a I 5.12 109 104 MR a2*01.Pw002-0-041104 I17004S4G4tipk4 tOppb :pllU 10 1 .04 9.48 84 ND 10A 104 l.20 VU-FO1-Irwao2-0-0411a1 (A041681 Ask H. 10a Mb epy I 100 1 .04 e0.0 79 ND 07.6 9e 9,20 DLW1.Ii1e1M001 "0-041104 (qoaaMsoti fo pbapwt 10 120 10.0 04 0 .0" 11 .3 104 NR DL1 F01-Id3VA1001-0-041104 IoOWwqSptJ.100poOtprr) 100 120 98.0 00 0 .811111 112 111 NR DLI F01-M6VY002-0-041104 KOWNUti1kK10ppbtiOYr1 10 1 .30 0.76 d'S 1 .72 124 107 MR DLIfO14ASW00Q4-04110M Ioo041H1 api L. 70o pqY aolat 100 1 _V e0.4 79 1 .7'2 100 9B MR DI .Lw1.usIwOO&oU11a taoaweis,wc,10pob open) 10 o,sso 6.22 sr 1.13 102 111 MR D1J *01-IdeW0019-04110" 0.0,00a410 D.+ao 00 50 ".) 100 CAW e52 es 1.13 9ee se MR DLlIa-0P0041w-a6eA0BW10.0144"p0p-h0w41r1y04 10 o.9oe 8.52 76 0.9m 9.78 0 lot Dt.1.F014ABMl004-04" 1104 ro100.6eee0R,loo,vbeorl 100 0.90e 84A 84 0.9w 99A go lot DL1-F01-wewo0a-o-"110a loooOowis,ee.10,oea," 10 1 .1e !.!0 78 1 .18 10A 92 MR DL1 f01 .MSwooe-.wl1a IGOOiwm tnut+,t00vo low 100 1 .1e e2.4 B1 1 .1B 95.8 9e NR D1.1401-M8F0014441104 1000Wt70 "pRt .10pb804l 10 ND l.la ?8 0 .316 9.52 92 293 pL1JT-014018F001-0-041104 (coosii7olpkJ.ao06 10") 100 ND 75A 74 0 .315 90a s0 290 MR MR MR MR MR MR MR MR MR MR MR MR 14.3 01 124 lie MR MR NR MR MR MR MR MR MR NR HR MR 201 260 ice MR MR MR MR 303 ' 394 101 'iKiplu ~Iduiixowd M+qMbD Iwal ~IpMIpnh~ Ih~Ara ~n rwab nmwr~wlwpnnaAswkuW~d ND a Na! dmbded dor ebow lind101 Qu4nfas0oe whlefl k 0.2 aOtY Wuvwt?" MR-WOW dualoquIlleMs Nwtr Illna mltr taumerry rhh 6119005 ro1111ueA werrNa, tioowrtlr alum fry lney no 0) *am 11w w41ws in On row d ..% Exygen Rescaneh Pap 38 of 132 000281. p. 39 Interim Report #10-Analysis of Fish andClam-Samples Exygen Study No.: P0001131 Table IV. Matrix Spike Recovery FFBS, PFHS and PFOS in Fish Samples (continued) Srripl8 GL1+01-MSF0O2-0-0d1104 ICAMk71OptK .10Poll Swi DL1 " F01-bISF002-0ON 104 (COOawTtqaLloDP96 spool DL7-F01-UBF003-0-041101 (Clowq : 40 0." pp apft) DL1 ;01 "MSF009-0-041104 (eaoiu72Eo 0,i0oppblpb) DL1-FOti18F004-0"W t104 (COIK"spcf.10prtplr) DL1401 " MSF004-0-041104 Iocw"MsphP. focAr30q Du-FOt-Mst-aosa~041104 (Cam" %k 0. w PO low) L1.1401 " MBF005-04411D4 (ooUfuiJ Ilpi,H, too pe f'Iky DL7 " FO1dPYd0014N041104 87oo1K75 4pk1.101187ipw) DL1401-IPVY001-0~00104 (000awts Ilr a. roo ar aqw.l DL1~F91-IPwo0z-0.a1104 tcW970 i0 w10 vN SOW DL1-F01-PW002-0~W1104 (ODOTw7 0pki, Ioop9 plsl Du4014awa93.0-041104 (CmauW" so C,tOVAlPftJ a1-F01-IPY4003-0~04110" (COIKan %k o, nopoo srrp DL7-FOe-IPw004-0-041104 (0roiars frk 1, 1o ar yeu) DL1-F014PW004-0-041104 (p04947440F,tppqprfoar) Du-FU1 .r"FOV~~-o-a11a (010,"7.>t,a9.1010 $02) DL1-F01 "IPF0020"0"1104 (Cao01"tv qk H. ta PO ipr) DL-1-FO7-IPF0030~041104 femeao4O l,fu,prtlwq DL-1-F01-1PPD00-0041104 (CaOd"m wok J .tODS11YSIw) Spkrd C4 ulfanatr PFBS ou Amount b1 Swnde RBOOveretf Rw.vwry .rw nM .t % S PFHS Cund in 8mOe R1cOw "d Reo04wr7 w*wt .K.6 % CS Sullaamils 04 And Faurd in 3wFp19 wlr. lunmall ROpo,r4rod , . . m 4 RBCOWr7 90 ND 0 .60 55 0.024 10.8 99 NR NR NR 100 ND 0"a 05 OA24 98.4 OB NR NR NR . 10 0203 8.78 BB 01652 102 95 NR NR NR 100 0 .70'b 84.4 84 0.8b2 952 BS NR NR NR 10 ND 5.00 86 0 .532 10 .4 ii NR 100 ND E0.0 87 O.SdZ 101 100 NR NR NR NR NR 10 NO 8.01 58 0.6S4 10 .1 91 1$i 100 ND 82 .4 82 0 .884 94 .0 93 NR NR NR NR NR 10 0.772 0.84 79 0 .650 8 .72 s 17A 26 .4 90 100 0.772 51 .0 03 0 .558 97 .e 97 17A 113 OS 10 0.460 9.0111 82 0.536 9.96 94 15 .7 27A 117 100 0.468 76.4 76 0.988 88.0 67 15.7 100 99 10 NO 100 ND YOB 91 0.209 9.44 92 . 9.30 90 ." YO 020i1 105 108 9.38 t8.7 73 109 100 10 ND 8AB BB 0.234 o.80 98 89.6 100 ND 71 .8 72 0.236 84.0 05 WA 10 ND a.0o Bo o.m 0.2e 9t 11 .1 100 RD 85.4 SS 0.2Z4 9SA go 11 .1 72A " 140 80 18.9 70 108 97 10 ND 100 ND B.SO BB 0.285 10.8 100 202 78 .8 79 0.205 90A 90 20.9 30.5 9B 109 8d 'Bamolu fY1au& myew 1ND plkrwhid61on11Wlly; QrMaO, an aowrne0 FWrupvwlnw anna be caluYOi,d ND - NotBBIBcUdat Of aDaM LInR dOYAIUBao Which Is 021p'p (watrwqlt). IA-NarPI1WA" bVurBr camd rruR 41ba Ia~n47W nw6sn rfo~n1a TIUbAA . NUN;*IPA*Ldi"WIrYIy 7"bY f110wt fOllnnd results, nMCWW7 VOW" Ay MY mBddly hall Of WitosIf to 94Wdeft. Exygen Research Page 39 of 132 0002N2 p. 40 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 Table IV. Matrix Spike Recovery PF$S, PFHS and PFOS In Fish Samples (continued) $pitpl0 OL-1-F01-IPF004-0-041104 (COt9101 tOk K,10 pt.Owf DL-1 ~FO1-IpF00t-0-041104 Icoa0ss+ spkL10ovrs,rH DL-1 4F014pF0064441104 IC0040n to C,10 we 41004 DL-1 .FO1-PF0060-041104 (OOOW07s000.1000008onq 00F01"618W001A-041106 fcaaa07 sptLts po s0ft) DLSF01 "MSYhf001~0-041106 (GOGl10! Opt< 0.1r0 Opb ew) D13f01-MSVUOOQ-0-041106 1om406"i0t 4, >30 PO $001 OLSf01"MBWOOQ-0-041108 1COON0018ph H,100 Ow O0r1 bL34101-h181M0064-041105 t<700Nt008oL6t00obtiawl 01.3*01aA$VY003"1104 tOOOtOt85 40 r.t00pp00y1ri oa .3+01-aeV4004,0-041105 {acouw00 to a.wMr spiel 01 .3-F0144swoos .o~041105 (00040100spkL.f00ppbsOS01 UL3-F01 "MBY4008-0-041106 WntwetprG.10ppYS00a} OLSF01-MBW0p6$041108 ecOwOpf 8o 0, t00 pb left) OLbF01a19F0014W0411oS 1000Wa0110e.fo000900y DL3F01-M8FOOtd4Wi106 Omwsts so 0. IN w0 some) OLSf01-Mty'O"2-6,041106 ~wap~ ",wpn "wi DL3-F01-I,~F002-0-041106 (=4- ii* f6t0000rs00m) 00-F01-A16F00540A1105 (cm10t00lt*AtOpOt+sWs) OL3+01-hIBF003-0941106 (ra0<su0 soy J. >g0 000 so") 8plkrd c4 Amt iN ONO* Jarwt . PFee RsoOWrod ROOOv" y w1wL CS &dkff*S PFNS AmtFound AffsoM bl8unp10 Raoowtad Rieoovry wt~r, w~tw4 /MM Found W BtniFls wlwt o s AM" RraaOVw"d Fy0"y "Mrt 10 ND 100 ND 8.00 80 84 .0 !5 NO 9 .48 25 7.80 13.6 62 RD 9.B$ so 7.00 102 94 10 NO 7.44 74 0 .375 9 .00 86 0.72 15.9 72 100 ND 84.6 86 0 .373 96A 98 8.7$ 102 93 10 NO 100 ND 6.30 84 66.6 86 NO 9 .20 92 139 ND 11u 100 139 1"6 " 258 114 10 NO 100 ND 8.44 84 BOA 90 N1} 9.92 98 180 ND 106 106 100 150 " 283 100 10 ND 1400 N,'3 0.00 06 88A 8S NO 9.68 98 148 ND 102 102 146 134 " 204 108 10 NO 8.40 86 0.?S6 9.66 04 19! 225 ' - 100 ND 88A 86 0206 102 102 log 301 100 10 140 9.08 s8 0.368 11.1 107 173 100 NO 100 100 0.368 106 106 173 1"0 ' 706 73 10 1o 9.18 86 NO 100 ND s4.8 116 ND 10 ND 9.e6 9o ND f00 No taD.B 00 RD 11 .4 114 118 109 109 118 10A 104 118 103 f03 11t1 130 zs< 118 os.9 " 216 100 10 ND 9.32 90 ND 11 .0 110 7b.8 92 .0 " 100 ND f0A 91 ND 107 107 76 ." 190 114 "80ie010 ia0i0us Otto0000ft .v0a09 lwM "WWW0r. rwObrs, m rowa0 iao0.vywku0 mod 0. caMObe ND - Nut debclsd s1 or Woo LunO of OsiOwlos whld~ is 02 aft (n? w0iyd} . NR " Nal ras 01~sd duelo qII0I1qN caM01 m1thduraa. ROwv01Ah eWim mtrMhuqo Ir1 T144 N. No1r.8Biaw 8d0 wmmmy Wk OhawO roaMOa we01p. rrpor0y vOkrs wpywOCymlly,hsy %w s rNnr 1n 1M low Am Exygcn Research Page 40 of 132 0002g3 p. 41 Interim Report #l0-Analysis offish and.Elam Samples . ~ .~ . Exygen Study No .: P0001131 Table IV. Matrix Spike Recovery PFBS, PFHS and PFQS in Fish Samples. (continued) Sample DL3fO1-lASF004W1105 (t00wM 119k K. 10 00 Soft) DO-FOi-M8F0044041105 IC00+wst ft*L. 100pb ~1 DL5f01-M3F006-0-0i1105 IOcw9a srk 0. w ws lepl+} DL7-FO1-IASF006-0041106 !Cw<KUspca,lwpprlymel OhIC-F0I-IPW006-0-041106 IOWa1w ark R . In PR 6o+1 ORIC " F01-IPVII00'y0-041106 {OO0wa3fpkr.1a0RPb") DIdC-F01-P1MDOiAA41105 Icoor,Yw4 qK 0.10 yib siwl DUC-1`01"IPW001-0-041106 IM9p1 "pk Fb t00rpb 6'ae1 DMci01-PW006-0~041106 (c00w1w9pkAtopeioko DMCrFO-OS4N006-0441906 ,oooasw so J, tao o,6 s,..) D61CF014A31V0030441106 ICwr14w " rR K. 10 N 11111081 D41C-F01"MSYYD0.'1.0Q41106 1Comww Sec I . +w pp Sp&y OMGF01A9YYOO40N0 "1106 (CCwaw720 C .10 M spin) D1AC+01-IASW006-0,041106 ICOB.Wq6006 tOCr1bbY6 OWf01-INISIN0060a41 !06 pm~ww ys 6, to pe splal DMCF01-N3YY006-0-041106 IWMiHIfOKF.1WWPNIOW OMCFO7-M3FW2-0"W t 106 IOapw~w ~ 0,10 M sPOel OIAC-F01-MBF00Q4)-041106 1016194" kk rt, +eoROso1+F Dt1o4mGF.0w1w"M.B,Fa0,01300P-O04so1"1)06 OW-FO1-IABF000-0-041105 (CONwswipkJ.100RA11009) ipYced aSufforWO pF pKK/ In Srrlpis . Rsoowad Rs aalwy vrr wtw. . oYnd In Sample ,wtvit. PF Rsoovsnd +whrL Rroowy % e WON" W03 ARK Farfd AmGiX1l In Sample Rsomwsd Rscovwy M1wt rwrA . % 10 N0 100 ND 0.40 26 90A 90 ND " 114 110 13D `144 -1 1 ND 104 101 ` ,130 . 296 106 10 ND 9.112 6o N D 10.3 . 103 . 81 .6 97.2 - . 100 ND 06.6 66 ND 6A ` . 96 61 .6 161 06 10 ND 6.96 63 0.366 ; 9.52 91 . , 612 7WD " 100 ND 84A 64 0.398 ' 10S Y9 612 . 10 0.300 0.04 77 0 .396 ' . q_-8 Is . , eel 156 96 107 " 100 O.aDO 90A YO 0 .796 104 104 . 66.6 166 9B 10 ND 100 ND 10 WD 100 ND 6.96 90 0 .270 , 10.1 96; . ~64A WA so 0.270 us 64A a64 Y6 0.672 11 .0 .104 . . :W YZ.s 42 0.502 106 106 364 75 .0 ' 153 so 389 " 464 110 10 0.316 9A2 92 1 .9D 12.1 ., 102 , 239 250 " , 100 0.310 E2A 62 1 .9D 101 . so .I 256 913 64 10 ND 9.16 92 0 .900 11 .43 100 MR 100 ND Y0.0 94 0 .00 116 117 MR MR MR NR MR 10 ND 6.36 04 ND 10A .104 NR NR MR " . 100 ND a7.a 96 ND 10s , 104 INR, . MR NR 10 MD ax az ND 10A 104 60.8 100 - " 100 ND ; 672 67 ND 110 . 110,,~ 66J, 104 137 'SwW~~.Idw iMCS~d.tlt"yiMnphwl .~n~~rirvfn~. an aoblnw nwosverY nlweorrrol heda+YYO ND -Not 06Uotad at Q Owe LiiNtdCluwn6hllan whfthb 0.2 npq {wet wedOhy. . . , MR "NO mpmUd Ow lu quality oaYkol nrYR lpnnti . RiwIVYW Iwd14an shoomIn TOWN . Nob:9inoIMS erwasry bbh~lo'a aue/N IwwAN. wOSr .ry.tmluw euywry dVqlylfsel Wvpws In 1hM rawOoY. Exygen Research Page 41 of 132 0002N4 p. 42 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 Table IV., Matrix Spike Recovery PFHS, PFHS and PFOS in Fish Samples (continued) !" npl9 DYIC-FO14.9F004-0-041105 (CloNsa9ptK.100o66pRU DMC-F01-1d8F004C-041106 0e0411101 tOt. to X6 to") DUC4014lGf0064-041105 t0o0Mie0e so 0. t0 1*6 so") 0AIGF01-6A9F0054~041106 IGoowsm SIk0,1 W rolt soul I7WCf01-IPF003-04041106 ICa0we0'i 9pk f, t0 hb eplw) 1)wIC-FO 14PF000-"41 f06 (Cm&eoOiPtr,lOCqAeo") aMC.Fa14PF004-0-041106 (C4011E01 30 C. t0 pPb Splw) OMC" F01-IPF004-0~041106 fomtaeul to It too 111A 11101101 OYC-F01.IpF0G5-04041 105 (OOOr010b apt 1, 00 PPb Opus) CAAC-FOi-IPF0054441105 rADIIlem 110,. taow eowl D12401-16lefoob441210l (0000400 40 Rto PO 00") 01.2-F01-IhYY006-a041216 IOmw11a to f. to ,p too) OL2.F01-IPMtOG6~QC41215 SCaE61a7e whG town6rOr) 0L2-P014fMN0050-041215 ta0oswu40 0,IGappC110114) DOU-POI4ISNf002~0-041216 40008"" So l . loop 9'w) DOU-poi-ii1Sw00-0-041216 leo6w"aK,l, leo pp6pw.l oca.Foi .lPwors4.aoa2la ,owe"? 8,en.10 P,.tpl.l OL2" FO14pW004-O041216 (00067301% 1001mrapls) DoU-F014Swo03.0-041216 SOOanaiw9rkK,t.r0 IPA DOU"F014A$WO03-0-041216 SOame~10 :1pk L, to wlb SODS) Amount e9ft0 C4 SUVOMW "M And Faamd Amount In 8001pe RIOOWfr0 ROCOWrp O4 e And Pand 10 81MplSa Remwred rKWe . Recawry Amt Found in 3Wtlple wt WON AMOU01 RecovarOd iw[rR. RlcVI&y 10 ND d76 e6 0 .254 11 .1 10e 11" 100 NO ee .0 e6 0254 107 107 116 10 ND e.52 55 0.420 12 .2 116 146 '100 ND 93 .6 e4 0 .420 110 110 146 10 ND 7.92 79 ND f 0ll 106 7.22 ' 100 No 52 .0 e2 NO 10e 106 7.12 10 NO 7.92 79 ND 10 .7 107 44.0 100 ND e32 93 ND 107 107 4440 10 ND 7.69 79 91D 10.3 103 "9.4 100 ND 75.6 76 ND 95A 9e 4eA 10 ND 100 ND 6,44 84 $32 83 ND 10 .0 100 492 ND 102 102 492 10 ND 5.00 e0 100 ND 644 e8 ND 11 .5 lie t3:. NO 107 107 132 10 0.206 6.92 67 1 .72 10 .6 92 MR 100 0.206 672 67 1 .72 929 91 NR 10 N0 e.0e ai ND 10.4 104 GAD 100 ND 76A 77 ND 95.2 95 6 .60 10 ND 6.12 e1 10.4 19A 90 Nft 100 ND 6eA ei 10 .4 105 95 MR 123 ' 22e 110 193 ' 2E0 114 16 .0 61 701 93 55.2 ' 134 90 54.4 " 121 75 $9,2 100 142 93 22 .7 95 121 106 MR NM NR NR 14 .5 e0 97 .2 90 NR NR NR NR "S"^FyMEMOS Fy,wds Ip*,tplWn01we1 SIlnifCOdly; 10301110~, an a0die0Y IWmrWy hYre vn1o160dIa111110 ND " fbt dOhCrA 6t Or rfEOw LJIM!d Qu~tlta9mWYdt Is 0.4 Opq(we4 wWpklNR " NGtf-paReE OuW tOGU111Cf 001ROI IhUllYAllw . Rtamyd0 nIWIIY "f! ~In TAW 1. Nolr: ehe" 9NS1 wmmuY 1W ONaw rowwyet nnulr, vlmrraV raim0 mr,l wr,t Nphqli~am dasvH~s In 1M wr dr~ Exygen Research Page 42 of 132 OOQ2SS p. 43 Interim Rcpoirt #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) So"" OL3-FOt-IPW004-0-0411J0 Iaooewa Go s, +s P0 Sow OL7-F01-tPW004-0 "0411W (COO00t00 Opk s, w0 pa spr) oou-F61-MW001.0 .341215 9=06+611 lOtO." PPt,204 OOlF4014IBW001-0*41218 (GOOmw OOw " . 1w 0 " so") OpV~M,IHSW004"0"047218 ICOO0u0~ e0k O .+s p~ Opa) OOU-F01-Llt}ilV004-0441214 to00ssr Ow r.+00 pr sqa) DOIWb1-M6WO05-04t1216 Io0oe0m 0ot0,10ip "pYSI DO11-1'01-AOBW00644t1210 (o00aw so M 100 PO Opr) OOWF01418F006~b041210 l0OOO6143LVLC110100OVw) OOU-F01 4A8F006-0~041216 (Ca06Np so 0, "0 PO NOW OL3-F01-IPW002<F041190 1Ca0mu0w0.wOrYfeOn) OL3F01 "IPW002-0~041130 1wOSie+ OM F . log Poe so") OL3-F014PW0030 041130 (a0000w00oa s, 16 hr OpOr0 O13F01-IPW003~0-041130 /COoOwK 80 N,100 Ope to" DOU"F014AGF000-0~041216 4000pp000pt K . 10 p0 qOS) OOU"F014ISF000~0-011216 (CumueOi0L .1e0 e06SPIN oon-Fol-Maroos-1-04+21a ICOIp1010pt 4. 10 711 ") OBCf01-MSFOq0-1-041216 (C00w019p 0~ IN ppb 40y OBCGF01a.qF0064441218 ICOOOOOe07otK1npob OW+) 09CW-WISF0064-041216 (C00001w80 L.10000070b) Amount SOW C4 Arm round tn 80mp10 w a F*88 MnOUnt ROOOwrOd ROoway * .c C6 AMA Found in Sample Iwt~ .t. PF Amount ROCOnrOd went ReOovvy BulfOnau FOS Arnt Maw in 80m0 -wt Recovered ROoOywy ,vw+e . % 10 ND 1 .62 75 NO 11 .0 110 T.9 17.3 94 100 NO 66A 66 NO 118 116 7.92 114 106 10 7 .08 14.8 75 1b.4 Z7.6 121 MR 100 7.06 832 76 ',8.4 122 .0 107 - MR MR MR MR MR 10 4.72 10A 61 21 .7 20.3 76 MR 100 4.72 72A 89 21 .7 104 62 MR 10 0 .304 7.08 61 1 .34 E.32 72 MR 100 0.364 72.0 72 1 .34 67 .6 86 MR MR MR NR MR NR MR NR MR 10 1.41 100 1,41 10 167 100 NO 0.00 72 0.40 1TA 92 MR 72.0 71 t7.40 94A 66 NR 7.92 79 NO 9.04 90 12 .0 61.2 61 NO 110 , 110 12.0 MR MR NR MR 16.6 48 106 93 10 NO 100 No 7.90 60 64A 84 NO 6.66 . 69 5 .44 12,3 69 NO 102 .102 6.44 92,0 67 10 1 .12 9 .00 73 6.60 14 .3 77 MR 100 1 .72 69.6 66 6.66 107 100 NR 10 0220 6 .30 81 1 .79 11 .5 . 97 MR 100 0.220 63.6 63 1' .70 98.6 95 MR MR MR MR MR NR MR MR MR 10 ND 836 64 1 .66 11I 97 HR . 100 NP 00.6 " 01 1.66 99.6 9B NR MR MR MR MR "s,"y4Maws O,r,10d0 o0 Opfdnp l*Vw NWAcvW,OMnfns. anm+aarw ne+owyv" w'na be eskaAt~d , No a Not ditucad at or ebor. umu of awniauon w+lrh Ys 0.2 eyy Ow waget~ , .. MR " Not nyard dw+o auft oonta ~111ourw. nr .n.bds wwft No shoom in Tom* H . Na.:81e00 9.w auirre.q ra0 Ohoa.O n0e+.d n.r1~0. Navvyvo.lr .. .,q,wyw01w), .6.e,9n .d0001e Iw ~d.d . Exygen Research Page 43 of 132 0002S6 p. 44 Ittteriih Report #10-Analysis of Fish and Clam Samples Exygen Study Na. : P0401131 Table IV: Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued) a6mp1~ DOU-FO1-M8F002-0-041218 (CaesNealpt0 .+oq~tyn,} Dou-F01JrsF00a-aat216 (aaos6ao eM N. tmaa ao") CU~F01-IPVYODi-0-041130 (ONWr706041611e6041rl D1.9~F01-IPYIIOD74.0041130 (0001041060 0.10?00 apw) DOU"F01 "h19F004-1 ~041218 Icaoirtt9Pk 1(0prilrrl DOG-F01 .rosFOOa-1a1216 (CmeU71 so J. IOU "IN sow DOlYF01a0FOD4.0~041215 000072 20 K, +0 ppb 61W oou-101-WIsF004a441216 IC00114R so L.100 Slob low) DOU-F01USF001-0-041216 100aW774tL+0 rp6 iy60l Dou-F01 4sF001-0.a1214 (ooaNail0 e. we pa 4pr} Det<FD14AF003-0-041219 (0n0a4746M4taopiPWA) DBGF01-MV003-0041218 ICawe4r4 SO H . (04 Polls 4w+1 DBCGF0144F004~0441216 l0ooee"rJayR1.10rA9oet DSC4014ASF004-0~041216 IOUwIJ7s srt J. +a Ms~r1 DAiC401-NBF001-0-041216 Icaoek7r so 0, " yPel111rq OWFD7-M8F001-0y041215 (Caaw4t66pieu .+wMltpy) D(aC.1M41001M-+eopikN1O, 0to6aO-0t4p12k.1)0 DLt-FOI.IPYJQ050d41216 (01066477 Spk J,100 pph Soft) Dt.2-F01dPM1003G-01120t lDaoOwr 7IAK t0 mb11rr1 C1.2*014PYY003-0-041201 Itmekt" ftAL,too6pe%py Meant 3IAked FOUfW In la9mqe w. onm1.PFBe AfnaRR Rscorrnd R4qovay Of &Mbraft PFN8 aurO wscf Reowwy x CB SWIgraW P Amt FOWW in 86iinp6 rr. MaurR ftwm R---Y 10 O.BBB 9 .24 !4 7 4.66 14A 98 MR 100 O,11B9 US.6 93 4.56 104 99 MR MR MR MR NR 10 ND 7 .80 76 0246 0.00 98 9.04 100 ND a2A EI2 0.716 101 101 9.04 17 .4 62 102 93 10 0.640 910 84 4M 14.5 96 MR 100 0.840 E2.0 81 4b8 103 98 MR 10 0 .742 7.75 70 2,3s L90 of NR 100 0.792 811 80 7 .35 55.6 83 NR NR MR MR MR MR MR NR MR 10 2.16 t1 .1 e9 10.9 20A 99 MR 100 2.19 62.8 at 10.9 104 93 MR NR MR MR MR 10 ND A,46 65 2A9 11A 96 MR 10D ND 84.0 94 2A9 188 104 MR NR MR MR MR 10 NO 7.72 77 3 .67 12.9 00 MR 10D ND 75.6 78 3m a8.6 96 MR MR NR NR MR 10 ND 9.08 91 0 .420 9.08 67 MR NR MR too ND 88.0 58 0 .420 10] 102 1"t NR MR 10 0.253 7.40 71 0.644 9.95 9, 66s 83.2 " 100 0253 72A 72 0.844 66.8 56 68.8 145 75 10 ND 7 .04 70 ND 0.04 90 7.48 13.7 62 100 ND 71 .8 7'2 Nb 92.0 92 7.48 64.0 71 'S~r~pl~ rriA~la~w~d~ ri~1pYiH0 lwel ~CY: - A M.~n aacwW ~oow~y WlwowielMakUYYd ND = Not dwf.iid rl orabOw LhMI d Qunwlullon vrMch b 0.2 fplp (w4l rWpUq. NR . Not spolYld due 10 awlRy camW (WA fi11iw0. IIFwiiynN oni w ~AOrs le TAM N . Maim SIhft6w wiremyLblb fhaW IOwe61d raft". AownfvvkwnuyvnY tll/i9yleelM 614YON" In IM MW dqY. Fal;ygen Research Page 44 of 132 p. 45 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No .: P0001131 Table IV. Matrix Spike Recovery PFBS, PFHS and PFUS in Fish Samples (continued) gpnpl0 D13-F01"IPMY005-0-041201 ItA0f0479 qt o OPps OORS) Ol1F114PW0064-041701 ICaoeuniirf .llot+ppbaptil Mqunt wed C4 Amt In SOrepb wl t~l. PFBS ou114 it0oovrod FLecwHy CS SAID i PFNS Ant Found Mount 3n 8Ynp10 WcovOrod RaoqiOry +q1 s1. sst+d, c8 Sal PF0B Fou nd In Sunpli m0" Iboomod Rocowry wd 10 No 8.18 02 NO 0 .08 90 4 .69 14.0 01 100 NO 84A 86 NO 872 97 4 .88 94,4 9D AsmOs: 70 slrndsrd OrArYon: 1 S ArwnY": 01 atNndnd OMSllon: 12 "9rrw"nYdw uwsds MspWnO ~+IOnMer~IMt O~w~aR sn aeawk 1~y wlw 1'amdbo olWslW ND " Not 04K-NO Si or ObtrwLkrMdQuawdIlOn MNr11 ii 0.2 Oy0(WOt W. OW) NR - NotrspnASd duWID qu "Iry COMM nlnAt 1sISnls . RFSnslyals rrulb an diuwoIn Tom11 . Nw; Blow 1hb wnrqWe doom reneged wwR., toew.y ..rw. nqrv.ry sO,nIlyUa .,n. values In lao erwdeft. Avenge; 00 Otsndw/ OwInYon: !0 Exygen Research d'Y'~, v' \ ~. . Page 45 of 132 Interim Report #l4-Analysis of Fish and Clam Samples Exygen Study No. : Pd441131 Table V. Matrix Spike Recovery of PFOS in Re-extracted Fish Samples c6 sugorm" PFOs DBC-F014PW001-0-041921 (q00rst61 SpcQ 1000 Mb) 09CrF01-II'W002-0-04102f (OOO4at62 Spk D, 6000 PPb) DBC-F014PYV003-04041021 (C000163 80 E,1000 DIM DOU-FOi-IPF001-0-041021 1COOre1 e4 apc R, toao PPb) DOU-F91" IPF0D2-0y041021 (COMI9S so (L 1000 PPb) DOU-1=01-IPF006-0.041021 (c90Wetsa DO K toooPW+) Dpla.F01-IPWOD2-0-041021 (caaet00 81* 1 . t000 nab) Dsc-FO1-MSW0o1-0-041104 p0ooro4ea sp,1uAOO paol DBC:FOt-MSW002-0-OA1104 (C00"1 Spk It, 10,000 PPb) DBGWi-M5V1+003-0-041104 IOOOrcas2 MkC L, 1G,ooo PPb) DBC-F0I-MSW004-0-041104 (C00*0r68 apk Lt S000 PPb) DBGFOS"MSW006" )d111Q4 (o004ws4 apK N . 10 .000 Po) D80-F01-MSF001-0-041104 (f'A04W66 aplc G 10.000 PPb) oer.Fo1-MSF002-0-0411a (C00404le Spk Q 1.0000DPb) DBC-FDi"iPF005-0~041104 (C004948 aPk E.1000 PO) 06GF014PW004-0-041104 ( " 0C 40 50 Bpk F, 1000 PPb) DBCGF01-IPW005~0-0411 D4 (COMM 31* C% MW PPIP) I DOU"F014FWU03-0~041104 (0004WE7 Spk M 1000 PPb) DOU-P014PW004-0-041104 400O102 8pk 1, 1Q00 DPb) DpU-F014P4V006-0-041104 (000"9103 aplc J. 5000 pph) I DLI " F01-MSW001-G-0411D4 1~M:~ K looo PPb) I d-1-F01.MSW002-0-0411 04 (coo~wea aqc C. 1000 PPb) i DL1-F01 "M3W00.~"OA41104 00049W 80k D, 1900 WE) I DL1-F01-MSW006-0-049'104 (coa4aM3pk g, IoWPPb) 2090 1660 896 686 644 1210 7520 12600 5240 47E0 606 t330 2W0 I 2270 1740 2130 I 968 I 706 I 898 804 2860 86E0 3180 1760 1740 1650 2610 23200 low 23200 8520 16200 14400 15200 1600 1590 6520 2640 2740 7E00 1880 1780 1830 1880 'Not lapated due to qudity ow" result hYaroa. Values are notlnclude4 In the waernwyalatwfica Exygen Research 76 107 150 11a 110 111 140 137 81 106 102 100 92 104 86 136 ta 37100 108 88 107 123 106 Page 46 of 132 000289 Intcrim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 Table V. Matrix Spike Recovery of PFOS In Re-extracted Fish Samples (continued) go" D!eacrlatiwi oau-FOl-iaf00a-0-041021 (C0016167 Bpk J, 1000 00) DOU-FO1-ItrW001-0-041021 (GUO4169 30 K 1000 ppb) 1711-P01-1018F004-0-041104 (COD4st73 Spk I., f00U ppb) Amount Spiked I Mda) 1000 1000 1000 ca soitonaa PFOS Amt Found Amount In Sample W4) wet wt Recovered (nofo) wet wt . Recovery t%) 424 1620 110 387 1480 t09 348 1400 105 AYwayn lot sfandarg Dawason: 30 Exygen Research . Page 48 of 132 0002-90 Interim Report # 10-Analysis of Fish and Clam S,ample Exygen Study No.: P0001131 Table V. Matrix Spike RecovM of PFUS .in Re-extracted Fish Samples (continued) Ca suron+e PFOS Du-F014ASF002-04411104 (00"911131k F,1090 pDb) DLt-F014u1SF003-0-041104 (Q00" o472 80 G, I= ppD) O1.1-FOi-MSFOOf}00.041104 (COD4047a Spk Fi, lOOO .ppb) 740' . 1670 ' 1830 1780 DOU-F01 "MSYV002-W1210 100060100 Spk K, 10,000 pp0) OW-Fa1-MSW003-0-04121E (COMME! Spk L, 6000 ppb) DOU-F0I-MSW001-0-041218 (COOBEI00 Spk C,10000 Pet) DOU-FO1-MSW004-a041218 (CoaeMI Spk D, WOO ipb) DOU-Fn1-MSW005-0~041210 (COObOM $pk E . 100b ppb) DOU-F014ASF006-0-041210 (CaoseN aok 11 . IM ppb) OW-F01-MSF003-0-041218 (000eUee 60 0, 100 ppb) osC-Fat-MSFOOS-1-041216 lCnbO .r epcK 19abopnb) DBC-F014+13F005-0-041218 (CaOee" Spk 1, I= vvn) DOU-F0I-MSF002,0-0i121E (C006eM Spc J,1000 ppb) DOU-F0I-NISF002-1-041218 (CU05W1 Spk K,1000 ppb) DOU-F01-MSF004-0-041218 MooseM spk L, IOWppbl DOU-F0I-AASF001-0-041216 (COD'J6477 Bpk C, 5000 pp*) oeC-FO 1-MsFDO3-o-o4121e lcaoae474 Spk a, uabb ppb) OW-F01 -M5F004-"1216 Ioooeb+7e 80 C, M" upb) OBC-F01-IPF001-0-041021 (CO0rs14e Wk 3,10001pb) DBC-F0I-IPF003-0-041021 (CW0160 SO M,1000 ppb) DOU-f01-IPF003-0~041021 1 (CommSpk1,1000 ppel 620 28200 4040 ` 7A00 5120 486 720 $46 8950 E40 892 1820 2070 4640 840 3e4 293 359 ' 150b s27ioa 10200 25000 aeeo 1780 1820 1720 32400 24100 1720 1950 27dJ 15500 24500 , zaao 1380 1340 1400 Not tapoiied dueb Quwliry contbl resuklaiwes.llaNras an notindudad Ni thesummerydmftk& 124 1o9 122 08 4s 123 174 " 9s 128 110 By 230' 151 108 128 BB 118 109 152 120 97 105 104 Exygen Research Page 47 of 132 OOU29~, Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 FIGURES Exygen Research Page 50 of 132 0002`32 Interim Report #10-Analysis of Fish Eq .d C1am Samples Exygen Study No.: P0001131 Table V1. Matrix Spike Recovery PFBS, PFHS, and PFQS in Clam Samples sample 109OiN03pk C, m pr! O13101-CfYV001-0-041210 100"4100,,000e, DW-014OFVY001-0-011216 (ooowa+ do e, ,. PP" onr,~muola-nG,Fra4s0f0.1e4d0o,44,.2) 15 DL2401r.M001"1215 (ooW&W 004 4,0 ppy DL24014Fwoo1414341215 KvawWeaw K lmWs) DHCG101i'JW001-0441Y10 (000me moktO tpn) DBG101~CFW001-0641215 (0~spkj,woppp) OL7401111'W0014041215 (COOOW W K .10yrld DLI 4p1-CFVYODI4-04121b 00a101Sptl,t00peY) 00U-q14FNf001-0-011215 Mwawri Spk 1t,10 FA DOU.q1 .CFW001A-041218 KDOEMlpRb,Imppe} Amaxd 30ee C4 &Mbrdft PM Quid in s.mpe wa~. Rdew,na w. adoowry +twa AWT n swnpw .0r. He N+iaua a.oowwd wewVy Ce And rwnd r, 8 ,~p, wwwA. as MAaot wow,no n.ov,oy -. mw 10 ND 6.90 00 ND Q15 42 1 .82 0.92 45 100 ND 82.4 52 ND 25.0 a5 1.42 ao.a 83 10 No 100 No a04 go ND aze Ss ND 044 04 e .15 60.0 US 5.15 11.3 61 oze e7 10 ND 100 ND 720 13 N0 W.8 84 ND ?.64 7n 1.51 101 101 1 .51 7.52 57 a9.4 9T 10 NO 100 NO 10.3 103 ND 01.4 6" NO 10d 105 4.48 W.Z OT 4.45 13.0 86 88.4 a2 10 ND 190 ND a.05 00 ND 862 86 ND 9.32 93 0 .10 103 103 8 .00 15.0 32 95.8 00 10 ND 0.40 06 0.202 8.92 at 11 .4 17.2 a f00 ND 61.4 84 0.202 98.0 ab 11 .4 90.0 a7 Aw .rnp: 14 iwwdwdDrWdwe 10 Avweyr. 93 OYWw dOwYYam ti ND - Hot a .h.w .a a o . .ww . Law of ordeftn 0M r os nft " w.o~ Now fbrod " N+nhwl lrb4 00M mund.d walls. naorwy v*w MI MY Wq* Uom I0 vrlws In "raw dft 1W"Or. Ti am*" 0W+A0wn ti Exygen Researoh Page 49 of 132 _` Intcrim Raport #10-Analysis of Fish and Clam 5amplcs Exygen Study No.: P0001 131 Figure 2. Non-Extracted Standards of PFBS in Methanol, 0.0005 jig1mL and 0.001 jtglmL, Respectively r sroo- Praa titr~v) t~~e ~r .a~wAk s er m>Ii~ nrcoaE+Y+yr Am : IM eo.ft Misft Or %512 w/o a a u Y o 10 14 Tim~, mln , @8777B " PFB! (31mdaM 2OOAiW A mw " wmyl*2 of 3! 1rom 061000BA%i4 AhY 1l967 deenb lLIQAt FBI, aPs RT:0.316 mm 0 42 M n u Exygen Rcsearch Page 52 of 132 000294 p. 52 Interim Report #14-Analysis of Fish and Clam Samples Exygen Study No.: Po001131 Figure l. Typical Calibration Curve for PFBS In Methanol 001l06~ FYh.Aw(PFiS~C'Lin.al' Ry~l.n ~4 f ~f'wni~Ynpk y- 7~1i+004x+ ~D7n+0pC1(r- O.iOfip) e.~ .e s.e.e O.Od 0.000 6.040 9.0 .6 4iDd $ ~,Od 0 3-0d 2JW 2.065 7D .0 1 .046 OJOrY Bxygen Research Page 51 of 132 p. 53 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 Figure 3. PFBS in Control Fish Blank, 0.00625 gg/mL Fortified Control Fish Spk.A, and 0.025 gglmL Fortified Control Fish Spk B, Respectively ' AwO~ItCollkrrl "PtBS< l~+IwIr121RM1~ "~rr "s~qPN "N90~ewr HIi15E+nM wrt wot Prr~Q S m. 4 e 9 10 ,2 13 14 ,0 Tim., min RsY~nl f1k A" Pp"f(OC1200"OAOAamu" armph 10 al J! tt .m 001000 E.~ilf , Iu.a :7Y174 909016 iielpUt 1100 . ps RI ; 4A2min Gn.. 8 0 10 iS TIM : min , Ruflnl "Ok I" PFYi(OC)20Y.O=rO "mu . simple 11 OM fm007000EwXf AfN: 33WZO oW1Nt R*4pt'. 700D0. Opi RT :Oa27 nln 7 .6~4 4 1.0.4 4000.0 049 0.0 14 is 70 17 Exygen Research , .,9 . Page 53 of 132 000296 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 Figure 4. Chromatogram Representing a Fish Sample Analyzed for PFBS (Exygen ID: C0049478, Data Set:061605E) , COMM -MM ~t~rR+rerr) ~~M~~ira -++M+! 70wnRew NfiRiEww An- A3fwmb IA$0 893cm RP a4ltiula g Time, milk Exygen Research Page 54 of 132 00029'7 p. 55 Interim Report #10-Analysis of Fish and Clam Samples Fxygen Study No.: P0001131 Figure 5. Typical Calibration Curve for PFHS fit Methanol o" 9e0diFirh .rlWFNS) "Un4aPAaFwqeeelllkrwiFAYn0Y-2.p94004xf? .P1*+008(r .oA7G7) u d < Exygen Research ' Page 55 of 132 000298 .p. 56 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No.: P0001131 Figure b. Hon-Extracted Standards of PFHS in Methanol, 0.0005 pg1mL and 0.001 jiglmL, Respectively , smts .MM Vr..luap be.*%#@rw - ...rft r w3$n.W Maee,ww Ar~w !iAlee~wAr Ml#ft 7A d" Mr M w!I 700 " IO.i2 Ow . aao~ "ioo', c 300- 200~ 1w , o~ 4 6 0 7 6 0 10 71 12 19 'N 16 Tha, min " p27! " PFH9(tlsniarQ700~0A010sinu-tump1.2o19 " from 0E9006EsrifF Awu 331T" eamts MII{Ilk 7300 . oCgRT- 10 .7 dn lam m a 4 Exygen Research . ~ Page 56 of 132 Qooz99 p. 57 Interim Report #10-Analysis of Fish and Clam Samples ~ Exygen Study No.: P0001 131 Figure 7. PFHS in Control Fish ,Blank, 0.00625 gglmI; Fortified Control.Fish Spk A, and 0.025 gglmL Fortified Control Fish Spk B, Respectively , AEywtce~aN "W7lsItY~~rewr)7l~lMaOra . ",ywlaleslroarErERSE,wZr Mrs wet ~rawip 1IsI 0 13 .00 u D 0 10 Tkne . mih Rep.ul *p6A . piNS (OC)3Y .Oi60D rmu .farnph 10 of= Aum001006E .wH1 , A: na 180711 406ek HE12at' 12000. eps PIT! 110 .3 win w ~, 1.OOeA lam ~OOOD~Ob 087 E O.OD 4 7 8 p 10 11 12 13 7" TUOf, RopoN "w 0 " RfHE j0QBYO.OI~OD MW . s+m/h 71 N31 *Ww001006E.wi11 , At=721071 oeunk Nfyht 30100. cps NT: 10 .1 min H U Exygen Research Page 57 of 232 000300 Interim Report #10-Analysis of Fish and Clan Samples Exygen Study No. : P0001131 Figure 8. Chromatogram Representing a Fish Sample Analyzed for PFHS (Exygen ID: C0049478, Data Set: 061605E) , c~rllai" Pl~1e~tAelr.eR)3M~u~a~~..-pwp2oorsprorMraSEMrr AMI: 2l~ri ilwrb IAI~AC ~T.'!~ q~ RT= ZU I~U Y Exygen Research Page 58 of 132 000wE11 p. 59 Interim Report #10-Analysis of Fish and "Clam S$1pples . Exygea Study No POOU1131 Figure 9. Typical Calibration Curve for PFOS in Methanol oeIaoaevun.wr(nosk*ur,..rn.or.ron ell hrwaaAffixro y-1.16e+004x.3.90ei003(r- OL003) 6" d GAGS a.0s M@6 4444 3.a5 ., sars w t S.6~S 2A*6 1 .966 1405 6A94 Exygern Research F t ~ . f d "F 1 Page 59 of 132 aoo30z p. 60 Interiiii Report #10-Analysis of Fish and Clam Samples ' Exygen Study No: : PQQ01131 Figure 10 . Non-Extracted Standards of PFOS In Methanol, 0.0005 pglmL and 0.001 p.gi'mL, Respectively , ssrm-vPoS ~.Wj .MMO am ....Ms iows&.. .awasw+. Arm: ""doom !MD0A, *# A.T Maid tz .b sao- u 70C~ 1w . 0 e e ~ e 0 10 17 7Y 19 14 16 iinH, win ' $l7270 " Fi0l (3faodarf)qpp .0A0.0 amru-swryls 2 0l30 horn OE1EOOEAiM A..: 1b04 NYMt NNOA1:p00. Vs Rr: 14e m1p 7oa aoo nr..s 000 3D0 200 100 0 Exygen Research Page 60 of 132 000303 p. 61 Intcrim Report #10-Analysis of Fish and Clam Samples Exygen, Study No.: P0001131 Figure 11. PFOS In Control Fish Blank,,0.00625 gglmL Fortified Control Fish Spk A, and 0.025 gglmL Fortified Control Fish Spk B, Respectively , Rrv#rt Co~ -MM P"s"wr)IIA6"AO man -aewyA Pol9i Aehr "07pSFrqW Ara: t7Aewab lAtgC lLlcpr Mr !bsiiNlr n u 40- ~zao 234 .4111 0'~ 1.21 1~ 7.41 S.aa A."3 7.?A 0.1 " 0~ O.~J 0 1 2 3 4 a e 7 0 0 10 Time . min RaaO .nt OpkA " riDf (DC)4D0.Q= .0 amu -fnnP1 .10 el3" hem0o10066wNf , Ana: 7100Q oovnMt Height a040. Opst MT! 12 .4 min 12 .10, J 13 .10 1tA2 11 12 17 14 , aa qoOD u Z000 12,49 t2 .D4~ 0 1 2 9 4 0 0 0 SO Tlml, min R.aOsnt So Y- PFO " (OC)iDOLA0J0 rmd - swnyiN 11 of 30 hem OEIEDOE .wM , Area : 2" 7141 oosnll MlIpAk 10000. on NT ; 12.6 min ws 1.6.4 u s tA*4 t~A a000.0 0.0 1 -_ . . x, _. . s a o 0 .,--__,_._-"T., " 0 10 TpnM, min 11 12 79 t2 .40 17 12 13 10 .00 17A11, 17A1 10 10 17 47 Exygen Research Page 61 of 132 000304 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : PQ001131 Figure 12. Chromatogram Representing a Fish Sample Analyzed for PFQS (Exygen ID: C0049478, Data Set:0616tJ5E) , OY"ARO -MM Wiww)4IL6K66m "*awph 2MotR+Rem 61i16MrW11 Awl: !lbl66eeeiIEr lb141tr t161dLqpr Rtt !2! win 1.316 12 .41 1216 1.198 1.0 .6 0.0.4 fOr" r.o.o OArF 5.1344 4064 3.044 2.004 7Aeill 0.0 12 1 2 7 4 d d 7 f 0 -to i i 12 IS tO 16 10 Tithe, mln Exygen Research . Page 62 of 132 000305 Interim Report #10-Analysis of Fish and Clam Samples Fxygen Study No.: P0001131 APPENDIX A Study Protocol POOQ1131 (Exygen Study No. P0001131) with Analytical Method, Protocol Amendments 1 and 2 and Deviations 2 and 3 Exygen Research Page 63 of 132 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 BxypnPiomeolNamba: P0001131 0111 STUDY PROTOCOL Study Title: Analysitl of Perfluorobutanellulfouate (PFBS), PertluoroLexaneaulfonate (PFEIS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LCIMSlMS for the 3M Decatur Monitoring Program 0-1 Exygen Protocol Number: P0001131 gxyrsn Research 3058 Research Drive State College, PA 16801 Phone: (814) 2T2-1039 Spasm Reglmetative; Michrel A. Santoao Director of Rmgnlatory Affairs 3M ]Building 0236-O1-B-1a SL Paul, MN 55144 Phone :(651)733-6374 ruxe 1,# 6s Exygen Researoh Page 64 of 132 Interim Report #10-Analysis of Fish and Claxn Samples Exygen Study No .: P0001131 Bxygw Probool NWeAer. P000 1 1 31 DISTRIDU170N : i) kinimba icc..d, Sway Dhvctor, wton S. olution 2) John M. Flaindy, Prineipat Invertiptor, Exygan Itmearch 3) Michaal A . Santoro, Sponsor RepnevenUrdve, 3M Company a) Facygee Reseanwh Quelity Assurance Unit Exygen Research Page 2 of6f Page 65 of 132 000308 Interim Report #10-Analysis of Fish dnd Clam Samples Exygen Study No.: P0001131 sxygeo PmtocW Number. POW1131 PROTOCOL APPROVAL Study Titk: Analysis of Parfluotvbutmeaultonne (PFBS), PectYuorohextmesulfonste (PFH3) . ud Parflmomocqnesulfonate (PFO6) in Watar, Soil, Sediment, Fish. Claim Vetetstion, Sntali Memroal Liven and Small Monmal Serum Using LCUSIMS tor the 3M Decatur Monkming Progmm Exygere Pnotoool Number P0001 131 .. ir~c4.~,~ MiehCaae]mA. ioz+o, Sponsor Rapmeentative 3M r~ ~ v d-41 /'n Date 1 DA 01* - Page )ofas Exygen Research Page 66 of 132 000309 p. 67 Interim Report #10-Analysis ofFish and Clam Samples ~ . Exygen Study No.: P0001131 Oxygen Protocol Nuabes :P0001131 TABLE OF CONUNTS TITLEPAGE . . .. ... . .....:._.. . ..,. . .. ...... ... .. . ... .... .. . ..... . ...... .. ... ., . .. . .. . ..... ._ ..-_--... ... . ... . . . . .. ... ...t D151'R~UIION.. . .. ...._.. . .. .._ .. ...... ... .._....... . ........ . .. .., . .. . ., ..... ....... . . ... ... .......... ... ._ . .. ... . .. ... . ...... ... . .2 PROTOCOL APPROVAL .. ... . .. ...... . .. ... ... . ..... .. . ..... . .. .._.. . .. . .. . . . . .. ... ... ._ ..__. ... ... . .. . ... .. ., .. ..., .. . . ... .. . ... . .. ... . . . ... . .. _.3 TABLE OF C01V1'EN!'5. . .. ..... . .._.. . .. ... ...... .. . ._.. . .. ..... . .. ... ... ... ... .._ .. . ._ .. . ...... ... ..... ... .... .. . ... . ... .. . . . ._. . . . . . . . ... ..4 INrRODUCrrorl . .. . .. ...... ..__. ...._ .. . ._..... ... . ..~ ._.... . ., . .. ... ... .. .. . ... .. . ....... . ..~..... ._ . . ... . ... .. . . . . . .. ., . . ., . ... ..5 TPSrMATSaiALS.. ..... ._ . .. .....,., .. . ....... ..._.. .., ..... . ._ .. . .._.., . . .....- . ..... . .. ... . . ., . . . .... ..__. ._ .. . ...~._ .. .... ... .. . ... .. .s OSJHCIiVE. . . . ...- .. . .. . .-. ..- . .. . .._. . .. ... ... ...... .. ...... . .. . .. ... . .. ... .. . . ..... . . . ._. .. . .. . . .. ... . . ., .. . .. . . . . .... .. . ... . . . . . .. .6 TESTING FACxL<TY ... .._. .. ... . ..,.. .. . .. .. . ..~. .., .. ... ..__.. . .. .... .._. . .._. . . .. ... . ._ .. .... . . ._.. .. . . .. . .. . .. . .. . ... ... . ._... .. . ._ .. .b STUDY DIRECTOR .__.. .. . .. .., . . . ..._ .. ..__.. . ..... . ..._.. . ... .. . .. .... .._.. ..... . . ..... .. .. .. .... .. . ...... . . .. .. . .. . ...... . . . .... .. . ... .. .7 SPON5OR REPRESBNCATIVE. ... .. . .. .... . ..._ ... ........ . ..... . .. .... . ._.. . .. . . . .... .... .. .... .. . ... ... . . .. . ...- .-- .--. ... . ..---- .. . . .. .. .7 PRAWWAL(NVBSTICiATOR .. . ..... ._ ....._ . .. .._. ........ . ..... . .._,.____. . . ._.. .._ .. ...... . ... ..._.. . ... ..m . . ._. . .. .... ..__.. .7 PROPOSED EXPEkUdBNTAL START ANDTptMP1ATION DATBS_.. ... ... .:_ ... . _. .. . .. ... . . ..... . .. .... .. .. .. .7 IDENTIFICATION ANDlUST1PICA'I!'IDN OF THE 'tBSTSYSTEM . .... .. . ... .. . . .. . . .. ..., ., . ~., . .. . .. . ... . .. ... . .. . .. . .. .8 SAMPLE PROCUREMENT, RHCF>PT AND RETENTION_.. . ...._ .._ . . ... . .. . ...__.._ ..... . .. . ..._ . . . . .... ... ... ... .. . . .. .8 SAMPLE IDElT1TFfCATION . .. . . .. .... .. . ..... . ...... .. ..... . . .. ...... .. . ... .. . .... .. . ., .,., . .. . ..._ . ... . . ..... . .... .. ... . .. .... .., ...,.. .. . . ., .9 ANALY77CALPROfEDUkESUIrMA1tY. ...... . ....... .. ... .. .. ... .. .., .,.. ... . ..... ... . ...... .......... ... ..... .. . ... .. . . .. .9 VERIFICA770N OPANALYTECAL PROCEDi7RE_ ._.:... . ..... . ._.. :... . . ... ..._.__. . . .__._ . ...... ... . ...._ .. . ... .. . . .. .9 MBTf1oD FORCONTROL OP 1RAS __...__...... ... .., .,. ...... . ... ._ .._.. ...., . ... . ... ...... . ...... ... . ... ... . .. . ... ._ .. . ... .. . . .. . i i 8TA778TIC,AL METHODS . ._. ... . .. ...... . ..... ..._. ... .. . .. .... .. ...... ....., . ..,.. ...... . ..... .... .... ., . ... . .., . . . ... . .. . ... .. .. .. . .. . .. ., . . . I 1 OLP SiATEM81iT .. . ......, . .__........ . .. ... .. .... . .. . .. .... .. ...... .....,. . .. ... ... . ..... . ... . .. .... . . . .., . .. . . . . .., . .. ._ .. .... .. . .. . .. . .. . .11 REPORT ... .. . .... . _.._.. .. . ......, ., . _._. ._. .... . .. .., .. ._. .w .. . . . . ... ........ ... ... ., . . .. ... ._. . .. . .. .... . . . ,.. ., ., . . . ... . .. . . .. .. .. .. . ..... . .. . . I1 SAFETY AND H&AL1H_, .,. ..... ....... ._ ... . ._._ .. . ._ .. .. ......_.... . . . .__.... . :.... .. . .. ..., ., .,...,., ., . ... . .._ .. .... .. . .. . .. . . . . . 17 AMENDMENTS TO PROTOOOL ....._ .. .., . . .. ... .. . . .. ... ........_.... . . .. .. ...... . .._ . . ... . .. ..., ., . .., . .. . . . . .., . .. ., .. .. . . .. . ... .. . . .. . 13 DATA RECORD 1CE8P4r0 .. . ....._....... ._. .. . . ... ., .. ... ........__.. . .., .. ...... . ..... . . .. . ....., . ..... . ... . .. .,. . .. .. .. .... .. . ... .. . . .. . 13 QUALITY ASSIIRANCH . .. . . ... .. .....__.. .. . .. . . .._... . .. ... ...... ... .. ., .. ... .. . .., .. . ... . .. ..__.... . ..._. ... . ... . .. ...- "--"-" -" .--- . . . . . . . 14 RI'Tb7vi7ON OF DATA AND ARCRIV1N0. . ... .. . .. ...., . ... ... ... .... ... .. ... . ... ._. . .. ... . .. .... ., . . . . . ... ., . ... ._.. .. .... .. . ... .. . .. . . 14 APr6NDIX L ANALYTICAL ME'CfIODS... .. . ... .. . ......, .,.... ..... ., .... .. .. .... . ....., . .. . . . . .. .. . . 15 101. Posc I of 63 Exygen Research Page 67 of 132 000310 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 8xner proqcot Nuelber: P00a1131 ^ INTRUDUCTMN The purpose of this study is to pat fun. analysis for perfluorobutiumulionate (PPBS), pewfluorobexaneeultonate (PFHS) and. perfluot+ooctancsulfonate (PF4S) in water, soil, :ediment. fish, clones, vegetation, small mnnmal livers and small mammal aanurn using LCJMSIMS for the 3M DeoatKr Monitoring Prograsn. Tha study will be aadited for +eoenpliance with EPA TSCA Good Laboratory Praetice Standards 40 CPR 792 by tk Quality Aasuranoe Uoit of Exygen Reem-ch. TFST MATERIALS The teat materials are perQuorobularlen11t6nate (PFBS), perAuorohexavesulftate (PFHS) and perAuorooclaneaulfnnate (PFOwS) and am all supplied by 3M. , PFBS Cheanlcai Nalae: Pafluorob>aranewlfanate ^ Molecular Weigbt : 338 supplied u the potanilm salt (C,FaS01'K) 1A Number. 101 Purity : 96 .7% Txauuitiona Monitored: 299 -->" 99 Structure: PItiiS Cheamlod Name: Per#luotoboxanerulfooaxe Molecular Woiglrt: 438 supplied as. die potassium salt (C6Fj3SO3-K) LotNumber: SE036 Padty: 98.6% Tnneitlotla Monitated: 399-+80 structure: F Page i qjr63 Exygen Research Page 68 of 132 000311 Interim Report #10-Analysis of Fish and Clam Samples Exygcn ~Study No.: P0001131 Exygen Piooocol Number POOO 1131 PFQB Chcanical Name : Perfluarooctanewulfonate Moleodlar Weighr: 538 supplied as tha potassiiun aalt (CsFi7803-R') Lot Number 237 Purity: 86.9% '1'raaaitions Monitored: 499 -~ 99 Sauctura: , F F F F F F F ~;'SD?' F FF F OBJECIM The purpose of this study is to perform analysis for perfluorobutancsulfonate ('FN), porfluootibuaeawltonate (PFF1S) and perfluorooctanasulfonate (pr-OS) in wow, soft, redbsont, fish, claua, ve8ststiou, small manmmal livors and oosall mammal fduoq for the 3M PeCatuL 1Naitoairg Progr+m using the r%k currant versions of the following Exyg+n walj+tical methods: V0001780: V0001781 : V0001782: V0001783 : V0001784: V0001785: V0001786: "Metluod of Analysis *'Uw Dstsamwsation of Porfluorooctanoic Acid (PFOA) in Water by LGM$1MS" "Mefhod of Analysir fa the Determination of Peztluorooctanoic Acid ("OA) In Soil by LC/MS/MS" "Method of Analysis for do Determination of Perfluotooclanoic Acid (PFOA) in Sedtumt by LGMSIMS" "Method of Analyaia 61rr the Ddenninacion of Perlluorooctanoic Acid (PFOA) in Irish and Clams by LCIMSIMS" "Method of Analysis for the Dekcmkation of Porfluaooctanoic Acid (PFpA) in Vnetation by LGMSIMS" "Me" of Aeulysia for the Determination of Perfluomotanoic Acid (PFQA) in Small Mammal Livor by LCIMSIMS" `24lqthod of AiWyk6for th Delehnination of Perfluorooctpnoic Acid (PFOA) in Sumall Mammal Sam by LCMSJMS" TESTING FAC1lLITY Exygess Rwinoh ` 3058 ResenrchDrive ' lomk State College, PA 16801 Phone:(814)272-1039 - Pw 6of6S Exygen Research Page 69 of 132 000312 Interim Rcport #10-Analysis of Fish and Clam Samples ' Exygen Study No.: P0001131 sKrpa Pwol mM6*r po0oi 131 STYJDY DIRECt'OR Jsioimha Rend P.B ., DEB Wetted solutions, Inc. 1400 Weston Way West Clhcgtar, PA 19380 Phone: (610) 701-3761 Fax: (610) 701-7401 j .kestxiQvatozaolutioni.com SPONSOR REPRESENTA'TIR'E M;Aael A. Santoro 3M Company Director of Regulatory Affairs 3M Building 0236-01-g-10 St. Paul, MN 33144 Phone. (631) 733-6374 PRINL7PAL IIWRSMATOR John M. FZaietty ExyW Research 3058 Raaeecty Drive Statoe ColleBa, PA 16801 Phone (814) 272-10339 jolm.tlaherty(a]weyaen-vom PRQPOSRD Il:XPERllIhIENTAI. START AND TZRiWIINATION DATES It is propoaed that the wlytical portion of this audy be candmed from Oetobar Ol, 2004 to Dacsraher 31, 200S . 1'he actual experimental stars and anvainadon date, will be included in the snet r"oa. pa&v 7qI6s Exygen Research , . Page 70 of 132 000313 Interim Report #l0-Analysis of Fish and Clan Samples, ., Exygen Study.No. : P0001131 Exypro Frotxol Nuuber: P0001131 IDEN'i'IFICATION AND JUSTIFICA'11ON OF THE TEST SYSTEM The following are the test systems for this slady : o Water (groundwater and surfto waW) Soil Sediment Fish Clams e Vegetation Small Mammal Liver e Small Mammal Seruln The samples will be collected by Westoti S. olutions The control maples will be purchused and prepared by the besting fsafiity. Purchase and processing details for the control samples will be included in the final report associated with this study. The test systems were chosen to access do onviroaraental impact of Pros, PFHS and FFOS in the Decatur, Alabama am. SAMPLE PROCU!(1MMENT, RSCUPT AND RETENTION Water. soil, sediment, fish, clsm,,vagetafion, small mamma! liver KW small mammal am= uimapiw will be received at 8xygen directly from Weston solutions . The details of sample pmwrament for, this study we outlined in the 3M wo& pin entitled "Phase 2 Woek Plan for Sampling Environmental Medis. The number ad types of samples eolleetod will vary depending availability h+ tha field . Tlia total nmnba of maples received aad enelyzed for each matrix will be documented in the find report ssvociated with this study. , Water. soil, and sediment sarnples will be used 1e received without further processing at Exygen . Then samples will be stored refrigraated at 2. C-8C Fish, clam, vegetation and ana11 atunmal liver, maples will be processed acooiding to the aippnapxiate analytical method (see Appeaft I) . These semples will be stared Sm.en at S - 10-C. Small mamma] whole blood maples will be caItritbied in the field at tha lima of collection and the tisotioa will be mad for the study. Small mammal serum will be stored frozan At % -10'C. The roceipt and processing of the samples will be documented in the final . report and rawdata associated with the stady- ArYe 8 of 6S Exygen Research Page 71 of 132 00031-4 Interim Report #1Q-Analysis of Fish and Clam Samples Exygen Study No: : P0001131 Exype Pmooeo! h%n6w Pool 131 WME EnErrTMeA7r0M Prior to analysis, cub smnple wig be earigrod a laboratory setnplc rcference nmnber. The retierewe number will be unique ad vuil] distinguish each laboratory sample that is peooeaed throuotout the analytical procedure. Cttaomatogrtphic data will be identified by the laboratory sample reference number. Sample stomp conditions ad bastions will be documatted thnoughout tkte study. ANALYTICAL PROCRDURE SU1Y144iAYtY ltefetencea: V0001780 ; V0001781 : V0001782-: V11001783 : VI1001784: V00017g9 : V11001786 : "Metliod of Analysis for the Detecenitutioaf of Perfluorooc .rtanoic Aaid (PFOA) ite WOWby LCIMSIMS" "Method of Analysis for the Determination of Pertltorooctanoic Acid (PFOA) in Soil by LGhG4IMS" "Method of Analysis forthe Determination of Pcafluarooctanoic Acid (PFQA) In Sediment by LACAWWS" "Motltod of Analysis for the Determination of Palkwrowtanoic Acid (PPOA) in Fish and G1ams by LClMSIMS" "MetiW of Analysis for the Determination of Perfluorooctanoic Aoid (PFOA) in Veptadon by LCl1v1SIM5" "MdEhod of Analysis far the Detamination of Perfluotooctanoic Acid (PFOA) in Small Mammal Liver by LCIMS/MS!' "Matbod of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Small Mamsnal Serum by LCIMS/MS" 1'lte above methods use analytical conditions capable of separating the isomea of PF'HS, PPHS and PFOS . Tba final report will include the isomers almmed into total PFHS, total PFHS, and totai PFOS fouM . VBRV3CAnN Of ANALYTECAL .PSOCEBUM A labortitory eotarol sample- will be used far the prepantion of forlif5ed control ". lea The test substance wig be made into, solutions as per the method. and added to the Matrices vie a mioropipeste. For water satYpHag, Bxygat will'supply one beftle per sample collected. The bottles will be 500 mL pteclesned Sei/Spec Premier wide mouth KDPS bottles. These bottles have been routinely used for iluorochanicil sample Page 90f6s Exygen Research Page 72 of 132 000315 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P()001131 Exypea Protocol Number; P0001131 r" collection at the testing facility and have bow shown to be free of PFHS, PFHS aad PFOS . Samples will be added to eaoh container to a voleuncaic rill line at 200 mL A iield duplicate, a low field spike aad a high field apikc of each sample will be collected . The low and high field spike bottles will contain PFBS, PFHS and PFOS at well as parfluoiooctanoic acid (PFOA) and , 1 .2-13C parfluoreioctsutoic aeid ,(t3C PFOA). PFOA and "C PFOA are included In the solutions used to spike ,the samples. The results for Pl'OA and ~C PFOA will not be r+eporud in tbit< study, Exygen will supply one field blank (control wroter) and two field him* spikes (control water fortified with PFBS, PFHS and PFOS at a low srsd high kwal) for every twenty samples c. ollected At the testing facility, eocb water sample (excluding field duplicate; and field spikes) will be axtractod in duplicate and will. also be fortified at a low and high concentration with PFBS, PFHS and PFOS aad processed tbmujh~the described, procedure to determine method accuracy and to check for bias. For soil. sediment, ciam:, mid vegetation, PatySen will supply one 500 mL prockaaed 5cil8pec Premiar wide mouth, HDPE bottle per ample collected or a zip-t+etd ba=, All eontainaalbags used for earhpk collection win be chipped to the sample location . Samples will be added to each container or bag in the field. At the testing f>toility, each eanplt will be extracted in duplicate and W3 also be fortified tui a known concentration with PFHS, PFHS and PFOS at both a low and high level and processed through the described procedure to determine method accuracy said lo check for bias. For small rnaatmal Svar, Exylon will supply a 50 mL polypropylene eptstifaSo t:ub,e Forman, tttalnaral scrum, FutySett will attpply a collection kit for aeh ample contairuS sawn separator tubes (red top), vacutainera, needle, holders and txedles, transfer p. ipettes and polypropylcrre tubes. At the testing facility, each liver and swum sarnpta w111 be artracted In duplicate and will slw be fortified at a known concentration with PFBS, PFHS and FFOS at both a low and high level and processed through the described procedure to detarmine mathod anwrrcy and to check for bisw . Low snd hi " levels for each matrix are defined below : Katrin water Low SAM Level 540 H kin Levei 5000 n L ~ Soil Sedicamnt Fish 4 .-- 140Y5" 40 ngla 14o0on-- ---- -- - clan 10 n lo0 n V ou 10 190 nWR Small Mammal Ldver 1o small Msrrmrsl Setuat , _ 10 no/ML ---~ 100 n I QO nghnL--------~ Par 10 oj6T Exygen Research Page 73 of 132 ooo31.s p. 74 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P0001131 8x"ea Pmleool Nwnber: P0001131 Recovarios are anticipated to be betwem 70% and 130% of the fortified levels; howcrvor, the exact precision and aot3aruy will be dete+nmined by the anatyila of ttte quality cotNrol tatttples deecribed above. A statement of aocttracy will be included in the fta1 tqtott METHOD FOR CONTIKIL OF BLAS Control of bias will be addressed by taking representative sub-samples from a hotoogtaeoua tltixtttro of otoh matrix from unttroetcd control sarnples, &W by analyzing it least two levels of fbodficAtions . srAnSnCAL nSTRODs Statistics will be liatited to those apedfied in the sttbjeot oaothods and to the calculation of average recovari#* as applicable. GLP STA'IEMEAI'Y' AU up" of this study thalll be pafiotmod ead reported in empliance with EPA '1'SCA Good LdtoJawy Pttfce Standards 40 CFR 792. 'Phe Gnal report or dadt packaye {atppliad to de Sponsor) sMll contain a stateruent that the study was conducted in oompliattce with currertt and applicable GLP standarrlt and will oudiae any deviations In the study fbom tllose s. tandards This sMttarlertt will be signed by the Study Director and Sponsor kop"antativa REPORT A final tbpott wili be prepared by the prlncipai investigator or their designee at the conclusion of the study. The report will include. but will not be limited to, the tbilowing: a The nune and address of the Stady Dtreotor, sponsor Ralmsentative, and of tha teeting fiicigty. A statement of CiLP compYaooe (any related documentation. such as chain-of-custody records, must be in the study records) . 10-1 Pass! 11 n/a! Exygen Research Page 74 of 132 ooo43s7 Interim Report #10-Analysis of Fish,and C1am,Somples Exygen Study Na. : P0001131 ExyVaProwooi Numcbor: P0001131 r~ e The signed and dated etatattant . .by the . Exygen Research Quality Assurance Unit regarding dun of study inspections and dates fndingb were reported to the Study Director and Management. e A description of the axsct analytical conditions employed in the study. 1! the subject method was followed exaotly, it is necessary to include only a copy of the analytical method. Any modiScstiona to this method will be iaootparatod alto ft report. If ft method is pboto-reduced, the project number and page number mug be included on each page. . 17vacription of tlae instrumentation used and operating conditions . a All results. iibta all seb analyrud Co" and fortified samples will be idcatiSed and the data table will include sample number and fortifwation Lerel. e Repreve<stative chmnaatograms for eech analyte in each matrix, including chrormtogana of a etartdard and a control sample, and a chromatogram at a fartification level The location of the analyto peaks will be clearly identified in all ehromdegrams. e All circumstances that may have atfected the qtyxtity or integrity of the data will be doemnented. in the report. e Locations where raw data and the final report are to be archived. e Additions or cot.~ectiass to the final report shall be in the form of an amendment signed by. tho Study Director. 'Cbe antendment shall clearly idcatify that put of the report dot is being altered and the reasons for the situations . 'Rte amendment will be signed and dated by ft Study Director and the 5poneor Repraseataave. e All applicable requirements for reporting ol'atttdy results as per 40 CFR 792,185. sAnETr Arm xRAI,Taa[ . Laboratory persoauwl will practice good vaaitation MW hoakh h. abits 0 Every reasonable pcaution shall be taken to prevent inadvertent exposure of personnel and the enviranin" to The IM or reference su4stanoe(e). Pap 12 of6s Exygen Research Page 75 of 132 000318 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P(}001131 Pxyrn riotooal Kuiaeer . Pooo1 131 AMERidM1EN1`S TO PROTOCOL All significant chsnlles to the nalytiorl protocol outlined here will be expressed in wddatS, sired end dated by the Study Director and Sponsor Relzrerentative. Amaztdtnetits usually will be issued prior to initiation of study plan ebettSa However, wben a cheose is required without sufficient time for the ieeue of a written aaratdmont, Clad chan,gc may be effected verbally with supporting documentation signed and dated by the Study Director xW followed with s written atltxndmeat ao sooa as poetible. In this cam the etfeotive date of the written amendment will be the dote of the documented c1tRAge. Copies of the siped amendments will be appended to all distributed study plan copies . The original ameeduent will be maintained with the original study plan. Any deviatioas Svm the study plan or from the analytical method see provided will be documeated Imd reported promptly to the Sponsor Representative . DATA RSCORn xEEPMc 001- Records to be maintained include the Poliowing (as e,pptopriate): " Ssenple moms sheal(s) " Sample roeelpt records, statne hietory, and chains of custody . History ad prepreMloa of standards (e4ack . fortification, calibration) " Description of any tnodiEiceatione to the method . 8tatnumont run shee% bomb-:heeb or toga " Analytical data tables " All cbonutographic and instrumental conditions " Sample extraction and anelysis dates e Acomplete listing oftitt:dy personnel. signaturn MW initials " Chronological presentation of ta11 study correspondence e Any other docuenentatkm necessary for the reconstruction of the study ChramYtogrtlmt;- Au alromatogmtu wi]I cootain the following; e Sample Identification, iqiadon datc, arrow or other indication of the area ofiateoest, and ia,feotlon number comspondinS to the run . " Additionally. fortifications will include the Amount of enalytc added aRd the ample number offt sample the was AWfied. " e Analytical ahndard ohrutnatog~ratns wili additionally include the concentration (e.&, ItglmL). Palo 1) of 455 Exygen Research Page 76 of 132 QO('319 interim Report #10-Analysis of Fish and,Clam ;Samples Exygen Study No. : P0001131 PxMrn Protoco1 N: umber ?0001111 10- . As part of the dooumaltalion the following sham will be included in cach analytical set a run sheet Iisting .tHe ssmpla to be run in the set, and an instrument oonditiona sheet de=-Wag the insttutneat type and operating c. onditions 7'ho ;QA Unit of Exygw Research will inspost tba study at intervals adequatc to aswre compliance witb GLP's, ad will :oport the lsndirw of audits to the Study Director. Exygm Manageatee<t, and the Sponeor Representative. RETENTiON OF DATA AND ARCHIVING . All had copy mw data, including, but ncl litnited to, the original dtoatstograaas, rroricaLeers, ooereapondenoq and results shall be included with the data package submitted to WStudy Director. Mew will be archived with die WOW study plan, sltteadmente, MW repatt, and all pertinent infoaastion from the Sponsor. The teating fitdlity,ahall keep all electronic raw data and any imstrument . equipment, snd ato:sge loge ~ for ft period of time specified in 40 CFR 792.195, An exact copy of ft materials eubmktod to the study director will also be kept at Bxygea R. esea- rch , Exygen will obtain penrtiwion froam the study director before discarding or ratwming sanmp}es . ' .r+ Exygen Research ' `'` Pav 14 of es Page 77 of 132 000320 p. 78 Interim Report M-Analysis of Fish and Clam Samples Exygen Study No, : P0001131 Bxyien Pioloool Nmbei-Paooll3l APPENDIX I ANALYTICAL NETHODS V0001780: VOO01781 : V0001782 : VOOO1783 : V000178< : V0001783 : V0001786 : 'Method of Analysis for Me DoAnoinstioa of Peffluorooctanoic Acid (PFOA) in Water by LCIMSAW "Medwd of Arlalyria for the Datamumitioa of Pcrfluorooctarsoic Add (PFOA) in Soil by LCJMSIMS" "Metbod of Analysis for the Determination of PerAuorooctanoic Acid (PFOA) in Sedisneat by LCIMSIMS" "WOW of Aiudysie iPor the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Cllpns by LCIMSIMS," "Medsod of Analysis for the Dotomiattion of PaflaorooctanQic Acid MOA) in Vayetatioa by LCM1S/MS" "Mettiod of Analysis for the Deteaniatioa of Pertluorooctenoic Acid (PFOA) in Small Mwaml Liver by LCJMSlMS" "Method of Anelyde for the DetamiuetiAn of Pertloocooctanoic Acid (PFOA) in Small Meamnal Sam by LGMSIMS" Exygen Research pop 1SaJ'6! . Page 78 of 132 000321 Interim Report #10-Analysis of Fish and Clgm Samples Fxygen Study No.: P0001131 Exygea Prowcol Nwnbar: POW[ 131 001, ANALYTICAL METHOD Kvo"rr.mew vweonio KwAod dAaWpY Ur IYr OrwrdoWu of 1vftOnoesrls AM (PFOA) Ir Wow by rrnuws AMY" Twft FwHipc frrsenAorweA lOOi Ranawh DRivw sats Lbllp, PA 16i01 Appwndft FM] Cemoft Bus Tw4~icd L4dw.IC-M$ 16Mw1wwai Um r+- Exygen Research Tv01 ?law 7 Aov 16 oJ'dS . Page 79 of 132 000322 p. 80, Interim Report #1 U-Analysis of Fish and Clam Samples Exygen StudyNo. : P0001131 sx,vn Pfflmwi WUWAW : rocoi 13 c LA fop . nib 4cd ic m ba wII) i 6r a beYioo u6 qurimim dpwfluaaoauqic add by 100 lUqnld Cbf'aarolieft cwipled to c uedcn Mm ~Camwde DweekrtS~Cf~Ma) ~ wyr. 2.0 Soft 2.1 AuWn4abwn. .drl4h.rawrrpWkwL cm.urI , utoswie~ .>Wruy . .r~~~o~t~ ""f"~Y 3A 3rqtltR"iimawt 3.1 At brclOeLalIwtwrrUforaYnObn. ].2 NO wrpA 9wowiau owed ow tiraoe rpww. 3.3 9mpiw MEW faRipsrd 1im14 6t Wewad eo Sqpllibpte a room 3.4 All wqlKwwl w qrraOb'IYsH)~1hri belei ~Pwd far wunclion 34 ARV r .qtlY.4sirWey PAWN leadt r omnda4pa 81-3= go fbt -S dwoW ad to 4powao1 w4d At The ecvxtioa. 3A 9LWW 0 .0"q "ooe~w wi4 b. R.a6cd in tbe "00614 Pin bf this p*& 4.0 1GYW Mil 9enlOY r~ 44..12 wNrrr.-r-p1Krcsr.c.rr W u ~a~.or~.Ae+~r-Ac.e,aw~anae 4A 'rwlraoetroaAdd-~i~AUrlc3 5 .1) brNent rd 1q*@rR 3.1 A N#, I np liqlW dgreYe/* OW" Of PUDPW U7 IA 2 Hlr"lqn"W ai1A awdrbir vol~oe l~J~ohr CRYd4 of i~jeetip S-I00 pLaowmeYd r eIrdnaYrrlp~aYnnrUr{~ . !.1 A bvlw 1v Orlwl ~w iW fw' /Wc isrt'rfkp ind qrllintbw 3.7 Amlrdwtlwlroia~YU4fwN1yL0A0001 t. 3~4 SOwLlfyehbb~l~w~l~wewl11yilmbbr . !.3 13 sl.AlperY0lW0, lP~Gavilb14 WWL 3.d lltycMAD EIw*bm e0td00da. 17 113mS.IDlB mawsow&beaha i.t 7 wi . ebr Nl"LCvWti. S'.9 OI~~r~iwYa 7.10 Awbirlim" (1MiCOt PL aw 1o-190 OL), wilb 4*owY4 dps. sit Won Rip Pak Vs 6 00 (to) 1Cti W8 araldpa rq. : .r+ rsYt 17 ofbS Exygen Research Page 80 of 132 000323 Interim Report #10-Analysis of Fish and Clam Samples E.xygen.Study No.: P0001131 Ex,gen vr0=01 N=dm: POW 131 wrrNw" _ A LpA6s1145 waw WOWr, vwoino ( IA WnMf ss..iu3 sars.e.a.u~w amp~ais.v~t4pdr.i 50 aa,polyvwrUm "+rwK woir wL 6.0 CWOw11o0npMe tYro 6 .1 Aoar*W CAVA FJiwvhw RT {Rey9bor saisKffaa t.t am it $e rwn . sr (e16t:82366"062t30) 04 6 .3 =rv4w ("A),;C 2 nlI ArmiimAmvbMin Wrwr 6A lIYIOelbnsQl) : Wr1111101 6,3 On"lrayaa: MMUMW NA 0.0 63 ! .0 6s i .0 2010 117 ua 63 now RMO 'JA {dfmd 35 0.3 )f 0.3 . 71 0.] ZS 0.3 73 0.3 6.6 yoedeaYnbeoa ISpL(pa6simnwiba~aiuqiu70pL~ . 4.7 qndYpdm- ?w1cAm-wMmdoWWwd odi6wN-orrvR 4.9 Rr11wK -23aAuW. '~ alOr"OOwi~~YlOiAG"d~d O ~ {Oldfb16 ~YlO dIrI~Id Irt d'd0~ b a0d~fu 4le I~LC s7Kwi. 7.0 MSOAS 9yp1d 7.1 i40ft a76proqSYliVIIdYf IdRA( apda, awjllorlij fID -1769 oNL. 71s OM wrdWaw w lnnedW 0 a piide ad MY be d~n~1 m omn to awlei~ OK 16a6+ySa . so !"OvA4asof8obqoai Ll i6slibliw 1.1 .1 2 mit4 roosium won k wIK is paprd by oddiDS 0, is " *or woolwahm 446" lo 1000 Ml . NWpw. AN-Nr rd- ary 6e pmpuw6. iW7-4A-: On. Pop /a 065 Exygen Research Page 81 of 132 000324 p. 82 Interim Report #1Q-Analysis of Fish and Clam Samples Exygen StudyNo, : P0001131 ExMsa Praoeol Nrallxr : PoDO)131 tay~.rrr rOwd oiF wlaw r~r. wanw AIrA>t .rncu Mxruoo 1 llm irliw~ a~ie Aaid (!'POA) in ' atu by LGlfSfiIS 9.0 ilu0lMenlpnalbu kl SIw1iRi Sa1~RalillalAiw iafitan 4 Ll lwple a Awlc aohrt{on 4l-100 p#omL 4! YPOA Foy walShins SO mg alawlidal fmdrd (wirwfai far rwhyj ani diloM 1o 100 wL wilh Ir111oA 1a a 1iS~mi.IDl!E bal0a, 9.11 A Ff raAsi. Ano4arir wlntea 4!lPOA Y ynvrad 6y hrYWall w rI. e! ila 100 POhnL 10UIUou to i /r0 ws)wna of 100 wifA nrthwi in 0 [is ML U" 1001119, 9.1 .3 A1.0 PMhb 10e96em4a aoilt4n alPPQA ii pnpand by bAn" I n e11.of pr 10 P/IwL"eWdm Yafrlwluseaf l00 wIY~ ~nrnN in a 127 rIL IDl81m1b, 9.6 .4 A O.l ~ll .lbN/atlar adllqaa elPFOA fa pepaad by brfnbin j I U mf.a!lal." 1~LWrierYadedr0llleeolSOOwfO~mwhr" lin a 17i mL LI~!'RlolA~ . 9.1 .5 0.14 A O&I POhaL Ri06wiw wwel4s or PPOA 6r !mqmW by bdsaaY IB 11L o! 1M O .l P0ct. wbsieo so a Retell volonos, of 100 with ssOrr "It3 ni. tDP! FMde, Ybawet wl R~ti>swliw wfWlas alaYMa1a46 la a nMNnar of rpploltlsY~ 4'C ald aea a016U IE[ a ~u+cimlee poid of 6 manlha (Moodosdoa< .. ~WL 4.4 WrdadGliYqllwlolutkw 911 6CAISRwS ollbnaul aa.aouaa we Prw+oN In HrLC w. . .. The wwrrVa ,r,4,& ,w Pwo,w,d *NO an as.ata. a.K.dwe, ier6ed rarpw . 912 7b lbuorGlO r a cypiwl atrPIK addfliara) "w+aaiuWala nxy be ~rrpwr . not Cw,wwaio 1wY11eWw v$kaa4! cwoamwof eewlrme.uw Whom P"1111 Comm alrrlw Cdllrrioe S .eroalD b"a"O 41 la 1a "Oil 46 ft"as "Er A xc. .rM br-1 Im ia eo xc.eayy-i la 4" 410 lao xc..ry)a no me 41 250 xc=do-l w Th, too w 40 4o 4D IN xc...wn" s 1000 XCWAA&74 " aYaond sousiondn alOr aYcalkq aolrlar6 fu 4qw1 Y 6> la inlilal am elrapw, rwY bswwwYrim otllw aewlnM dwSj she extraction (SPE). 7tC " waasriutiwum wrdri. rqe4ar' Pop 19oj6! Exygen ltesemh Page 82 of 132 000325 p. 83 Interim Report #10-Analysis of Fish aiid :Clam Samples Exygen Study No.: P8001131 01*1 /" Fry6Cm Protoo0l Nwaber : PQQ01131 waw x.&wvaoona AxA<rmAl._11i1111=0>, 0 ~o A) in Wclor by : M A.71101fmAld qW6m (Rope 1)101j w8jill,1mamif With mch fk w"1110111" MAUbd Y"ZA tl0wrilw0omlalNc~iwwo=dOdciO{3"m1.PolypuyyYrWba oI rC 10 6"C. c~ a tw wrolsO. !33 ANwawwluowo alloombrllooo of n+adiadr mRy bo I - u aods& 19,0 l11cCOli lic1ily a0.! lbeh b1oh, of orriploC smNC6 (bliodly i9 or lwc) mid iodYdc w Icca wc tul6rrt ooero! (MOW 61dt wise H1LC 'WOW) od iw myem olIOFa amIY1d U ImOn71 amwYstb01 (Id "M01 Wilm to Verily Moadrd rsewcy !pr dr hskA. ~Ibir &M will be sPedboll ir . .p~l..fol r W~ s py ~oj~ ~ ~o 11.9" ftaplollxosdbo fl'.l " 114 , 11.3 11A 1(ooo~e40 e1Lof rnqL sir apwdo0 o(wwpSO diloWw44 MI. +i "wr .r ir. 50 rL pmWapylw aaptilr6e on (IEe61y a ,oceK, chYoc lid ari CpkAlw b Cq PI Onu'isoC (I 1. 6 mL) by pmtm6 10 wL mhhrnel foltorodb3mLoflRtCww(^2d~o~hoc) Doaotlctoohoaurundry Laodiorvioae wrMmwl Ca RPi ow0idw~ Aoord oiwecHhi1c wi6i-d eL 1011 rdyMR COW 3 sL of olwle ink jradvMcd 1! aL 6oVppylr acoCiO0" (6sY valmao -Sm1.} 11 .5 ANrIYasLvilwiair6& - m ) LCM6'MS. ILO ChMrYwoliy 12 .1 bjoet Fo miiiino Nmrl a! sL etrt6" awls ad IOAilioi emeyle imp OK LC+9iMIS c,niou. A ah'hu0m o0adr6 cnuw 6nocds arA follow ski ..abra rrpks. 122 IA"d.drofKNWlmtcop"gibilcotlrMffvoaoMove aenosomwanlbvt1r auOo kWh" Ym mall" In 113 OWN Got of rciwq WilcWoo OWN* mwwl b iaclv6e0 K ibe lcOnie6 owl ct 11w OW of a 4m/Is rl. Fxeroyt WrWwdt mm h. {III~I~IAFI lA1r~Iq ~Y 5" 10 Yql/11~" MUe WrltYVt. ~a wtin a~t ol arole/ oWhcYw ifw6sds mm be 1Nonod et Um beginning Of o ui b6Owd iy o~cY1 odilnda oandri Iwruipcnn! cvvy 3"10 -mplsc (r aae~tforo cwnd aA af wtioolW YoWordc). 10 slNw aao. atkaaINA ewi6wiacqm6do wtietlte ra 11+a titlm 1AiWI" ia r unwled . lls um linrc vrWd au w for quo0u0oa . Llnpr pn6md ew+w ae 60mqlod 6n " o adyis rylimr wipisriaa odnL 1!c wsi66tIN 91P- aea r4pj wr 011, PaYr JO af'6S Exygen Rescarch Page 83 of 132 000326 p. 84 Interim Repart #10-Anslysis of Fish and Clam Samples Exygen Study No.: P(1fl01131 Bxyyan hooocal Hwnber. POOO1131 IlMMwnrMA , wwMer@rvoootno -ki,I1rT A" i DelMERMWOMraaeOeakAdd(PPQui3m Waewby LCMYi4 werr adihraliax "AM ooneewtrisa wYK DIwLM 1 .3 (vr equivalena) wAwesafw"M 12,! Swph wywrw elrwM re weed elrdri rwporeoa. Iiay amlWa gm weeeEwuYed tee~orr AaY W WYeslOdfer and r+nalywt, 13.0 AeeepI...Qawle 13.1 ClnoWpWmaw daV apw1t ata dw*ter iw r 369 emu Qon a prai af 41f aaa 'Or 4ri am perrA oa~aar p "e MA aniom .rhils ak Asylerria (3W rr) nP~ Or Iw afce~boefmri4a 17] liellrd bleie ert asl iewie ~POA x YwL dw~ the I,OQ. If e Wok oe~hfr !'F~DA at br~e ~w~r IA~a SO e e now Wetdc w71e a~W w a11Woe1 ad iir ~dn srans be waurcrd. 1!3 ~W ef ~rd~ie4 r~eId- *ON mi be between 70.170% Of lawbwrR vw4Aw, If aaoaM r" !a cow" do esyhbA laali. IM GUM wt e! wytw daft be nOmen4, ANY =We 101st awelre 70134% dwM 1 enlrtrl by do nab* so de~iOS it re-eunaRon Is wanwrL 13A Aq all1ankn Ipnleii &W 4 k a Mimfoal anther by WIM IM KM* 8noe Iwt, wy fa adrdN taw ft aiwlUdoa of Ys alihralen w. ane ltewwa,'. do 1W frine of+itbyeled eINnlla~ sIrlr& Nrt eald be wlrlW =AIM MweA 30% 4t *l WW ON" et atraopl neetude 009- 11.f '1'Ir awwYrha tow"" (q fk aiiawfw eaww hrxred Ma se a.0!!! ~' a. 0 W U alibntfoo wed1r "A o~Wb ft. ibnin. men ~sOAe~ w~e a~wt wr wiw a .ywc i~a .nr opnwon. ere w rrr6 rtr alwtlw wl ocrww woaa be nwyw4 uA IreLa & . bwwwa 1rbrar ad w~IIu .w1 am drift siws aww i411w'W~~IadJYwI~R uabatialdmr3iRawwdsthilwnll~lihin n wlydoal w dm do sa ~ be wwlru0. 14,0 Cdwletlar 1a1 ur rr LrwerO sinliw r aSwl~ en wawr ot PADA fbrml (OWL, bow "pod asy oft r and" VA" QWw nFania~ a I en) pp~atW 1y do Men LIw aodww vMwr: 11'oAhead C*Vll .1-gBaYusL :LYarslelx DF [F- was Iy*1dA IIW fW vehrae vu dilalel . Ilaurwry. h,eewr Pare 21 vf6J Exygen Research Page $4 of 132 000.'32'7 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No. : P0001131 0011- Exy=w Poomool Numb= P0001131 a~,l.w~w up" U.rovaomro ANAL ir~qdoaiu~sewla~~ aa. n--v~ rw-~-u_l-o-r_w^e_+-l~p~1e--A-CM ,s 1~ +'rv- nn!! wr_, .w.,w--r--s-y 1CAM" 1e3 For irrlplr Isd>wi vifl l-lowu wianlls of"" Pfor lo ex uaolion . -re 111n Ihlpwiu squdim p sYWsr Ib pRa~lls 1wws,. R-F+YM` [rpl .aJeellmdGas " w1ybL~dinoonall(~rIL)~ xt00 w*%WUWdl@Ll /ww Exygen Research tw1Wi Page 22 of65 Page 85 of 132 000328 Interim Report #10-Analysis of Fish and Clam Samples Exygen StudyNo.: Pa001131 8sMen Protocol iVumAeY; F0001131 ANALY'iZCAL 1ffMD IldlodlArbrt VOOpI71t ldrirw dAw+IrzIsUr IM LahrYOn dfhefhwwlrW ANi (lmOA) b $afl pr LCIMSMO ArlHlw rrftFwiYer 131oRO .aw 3es Ku~i,p,cv# saaCapaPA IM APPM.w ar r.A ' 1 ~ TOohda11wr1~~ 1G1ds,la~Rw.r wlula 4 Dow /^"1 oalft Exygcn Research TOW how 1 Pap1l ofb3 Page $6 of 132 000329 p. 87 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 EMM Pol&cWx,raWr powijI iq~u R~ Y17CALA1 e LCJ74:fL11i 1(Ad N~iY01911n Aad(rPOA)i4 i1bY 1 ." Scope 'lfr4 e~elfod i n be qbyW >br 0e feolwlo~ aoi paeitetiao ef~is add by 190 riotea..ee. Llquid t,um.rpuper oampl.e w . wadues Mass aloemaawefe IDnermr (ECMdai6) (n eaq. Lo simy . xl Al.mpobon., all, Lborsoorylnedon. L2 Ceauult b pqAel~ 1RSD0 blbi IIaAlInO rty eLroical foryioper ~ufny Oncriiao. . , 3.0 SeM01e N eI Yme~ 3 .1 Allow 7 .~ No rrpbru~rriu~ i~ ~rdrd br eoil ~r~lr . 7.i 3tWIw OW Yriq1ipiY1i 111" be albwq q s9ui1L'bal1e b mom M AU ruislwurrt W dsnau4liy aiRei Yebw1wr04nny1ed For acru6eu. 1.S /ropfs aollwtim preoN~~ will ht peeilied in IW amplaii pin for this 4h Raven WA Molasses 4.1 Wear-NTiG0a6 42 Mrod-I!lLCYaOe 4J JlMEN&rrleewile-A.Qs.Aey~uttlte0e 4A !tlraenewnoie Acid- OPWAI&kb SA Lanweat r1 dqaiPwi 3.1 A Ai* porbnnuw Opi/ dwafeloi/rpk eWu11t Of rnpio0 u0 a 2 wlvM qldpN Idr " YIA111f oOleer hpeAR 6OPb11 Of 1111%tiAll 5-20 ILL aeuuuerdto e "aim Mass Opeepanws (LfilM7ll4l1. 3.2 A 4evkne eo11ea1 Nor duafer0eefi >tNesaqwr mod qwonNrlau. $a A.,lylie.lw.e.e~+dleerrr.r.~,oo.ooools s.4 !0 sL eiPa"rlyru0>i=wuMlYie abuL i.! Ib ML diqowbie OdyPODln ; mmilsf Nb6L f5..67 D1i2rgr4ob2Ul4.tdwesnwloIwO-Nbe(oSaOn-t1e0e0aW,a.t.00-20ouL). 11.11 UP 7ar.,am."olw..,lla,.uvww. akm. sao 3.11 Awaplrw0ssliNplPwhpkMV1U00i0ft0(LWr41010"9 1sr0l0sp[WdW,w4iltphRdispoaeYl.Upe. f.]1 a.lu Ilfalra.eca.eliarra.Mknlaa. Iwzw? ^ Aass 24 pjdJ Exygen Research Page 87 of 132 000330 p. 88 Interim Repart #10-Analysis of Fish and Clam Samples Exygen Study No .: P0001131 Sxygen Pcotocol Number. P0001131 3 14 wdw.ou.,ammw. U,s cw~e~awav+a.oe~,t~o, se ar.vmyp~ovr~ee.~u woo~u . s.o aa Aw~ial~ma: nuqrw It (t.yreea kimnfia).21 MR =!o men. sp l1AY: n'^~"'~ UO) u Tuwponexce: WC fs UktiUlh4w(A) : i wH AAnodno Aoran Sn wwr aa aw6wpa.w (s) i M*MnW Ss aftdiewirma.. : 111ot.ioAMW u 1: ..0o u a 2n0e.0 2css plow sAk ss as 0o1.)s ~IeS ooas ye o .s ti tqrfie.Ya4nnK 1f rL (or e.i .a.. .a o,. a.fir !0 )Ld.) . i.f Quadrl+e twl .4..-a+~su urard od~e.do. wrv.. 44 1taK Tim -?3 mlawr. '1'fu /lur~ OO~W001 w iYrJ~da~ ~ ~d0~ aedaU'b droj~0 in adveo . .aivin In 1aLC eymm 7A H$Mi lysIIEI 7 .1 Mac llevaqRy lipdYwAptMmode, wMilucia, " 1D -* 'J69 nJi for pEbA. 7b rwseafllllw a~ ir~r4dr ap~4~ rd nry W dun,ue ie omw a o,d3 ..a ama e. we ea 7 .ar~ersoweiew Li Pesos LL I : .w w...wi. ~oK.b ia wss 1~ 1~+vn .e ry saaa o. ~!~ , .r ~wwod~w ~aWr~ ra 1000 mLafw~ea. Alteeb val~rKap'w ~~L ry~3 a+ Page 2sqfa Exygen Research Page 88 of 132 000331 p. 89 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study Na.: P0001131 /'~ Bnygeq plotcsal Nvmber. P0001131 se"ab+..eb =fOJWO " M:aoD - 1.orLenrs MOW' .rrvooolnl ie AM (IPFQA) im Soil by 9A', -IendedlerPrYlor ~-[ swam x"Wrattesda am" ;lWss a aYdl roinlr of-f00 pyaW of tBOA Iy w440iyi 10 oy . , 1KrrhAfta1 W~drd (c~npnd b~l~y) ad d'>e~ u 100 nL wiM arhrol las13fi1 . LDPR bas1R 9,1.1 At0 pomL ft1Rfplba ooluion or IlOA sa Pn"Iwrod by brinony In , a"1. of W300IIiJb6loAtiw to a fiW "humor 190 wiTh mlaeul Ina12SmL LDIA bolqr. l,1 .3 A tA fylaLlwtiSiwlk~ w41iw of rPOA is p~pr~i by bna~i~r 1v . mL d~ 10 ~w1. rolulba to a lbnl vrlaee af l00 -ilk panhnaa is+ l~lA V.,.5 9.1.6 . ., a 123 ML LOPE been, A Q1 qlrfl.lY1ltloatfoo wiuimot!!OA Y yt"ww by btiebbV10 al. rr~ 1.Or~a~ior b ~ firi vNus~ o! i00 wibwwlrd la a 12! >114L11PS b~U. A 0.Q1 Y~L wnfinliu " ~~n rflFGA in O~iA^~ ay ~n4~t 1a wl. din Li MWal. solatfoe so a Oa .l vokvw or 100 with awllweal io o [Zf sL IDl61tau1t The aoat and Wt4a0op aollllior am b be *WW In a Ibl"yRaor r appIOKIpst+ly 4"C add a* *&a fbr a Ipoziur . period ore alonlis t~ItD .rrofpa~rria . !s lroddAUkwkniolrdar 192.1 LGWWaYYIiIIW arldrle an lnOuWil iDLG wner 11u aailledo MM& w poowed dam* Ow abWbll prow0ure. 1/111" p WE11M l.Z.T 71u hbrnir! in s blid,otqdn adioorl wawMl+lkn may be peyrW Y rded PmYCoae=mWka 1r1i11rlla wfllr~~r ("wrMnliaaor dfaAm"w vow= ToffdCwmal Cdd="M C1libamn Undue, ED It 41 ft" uptiftio," IN , to w as xQaapeyy"I 10 ?00 40 f0 Xcw~dlyy-i lll 107 b l00 Xcenmddyy "3 >.b Ire atbobo +a eo asp !oo xxra.ar.WwAyfytas 1a M n rb foba ~r.tianm,,s '1Do moo" oonowoWeo oriviolibrllmrlatod is "peel W, la in Wdid OewWrJal. dais 11o oaoornsWa of OrIWldiel dmwiriw a"wCNoe (BPi). XC + Wrn1 e/fbalka 1lmaud r.ps on Page 26 ofdS Exygen Rescarch Page 89 of 132 000332 p. 90 Interim Report #10-Analysis of Fish end Clam Samples ExygCn Study No . : P0001131 Exymen loocol Naa6ar: P0001 13 1 I" apyr>turrr rw~t~r vmaiwi ANALY!lCAL ~ '"~o A~~D~~ia~~laotaHOZo LCMyI4 ~FOA)la3ollby 911 A WO 211Wdmd Mslmdr (irpm Mask) 1WItLtXWmp viih "Ch !let"riYii rea~1. l~7 ." ~n dl auwM aalihnWn d4odm* is 1$"mt. polyymVybin tubes r 3'C w 6'C, apti Iti. rwaa 9.U Allrrrroqanrrd orefirntar of rIrltr* maybe prepared n no" lee AAdi3t(7p 10.1 Iheh 10011 of weylw apmpW {lypk+ky O6 Or IM) OWN Yrcbd* ai WON am myml ambl (anYo1 tdmic riy S rL d mwUeol) aed m wageii naado pAIIIN u Isew eaerUmlar (lob Crikel spike) to veMy poWirY~mvq -Mrlwel 10,I RRaqir" mr ffr hIA Ml hYwalorY diplianr Od low rlll be swirled L a. ~ m .mrced. r eb p~d. 1110 ewl"nw ..wM r~.rRim fund .h,wn. 11 .1 W ! / of Y-Y !Ne !0 ALL polypaNWead6(Np Met (h~Yfy m III Adds.4ot.mr..d Ma amaC..wfM own",rat -u mla,w. lla TmrA1 b Ma +. aA11..wr. wfi+ ..r ...k.e 1x -le mieun nA YiSK A1 rwUri a.el~rlse. rr It 10 CAL vh0 wamr in the $O mL pollpmPyldu /" 11 .5 OMwftPIr-la MlMwx-)ooo qn . 116 Candid- 11r C 3V6 arlttQM (1 F b ML) by Orr4S 10 ML mrlnaol RQwre1 ry 1 mL ef Ifl'6C ww~r (-I&ppyw). Do am lot aohmn me dry It.? Lar Orrd) do imopli aa tM roomlf{aa0 Cm 8!C wvid~t Discard dam it,t Mob wft s rL 100% meOrrl. Cebct S mL of alum inte aradmaed 1! mLPhllr+oA= *wAA&p sQw (16r1 veDre - s oL) . 119 'Arqpar+0u1 04 dM11m*qV Ili1CVMS. 1u cwqmgsvlviw 12t vj t)rmrNrimmtdrohwdmd, rmpb rd fielilM rm01~MW i!e I,CA~I~(3 M7iM A r1111M110R S " d i/ 11M AiCdr ad klqoW 111 l22 31r1mi0lN0A~mn~WI~L~I lrrl /W Of1Y0n eaoowiYitir Ihrtb art6~L~1rU/ir rarl~irlwt t?"3 As rb rt of n4rlnd 0dlbmim AdW* -wt tie iroludeA Y Yrc pyY~ ad a 4e m0 ef t fr" lmemW rrWwh mum be Iulqaw~blarwRrl~'S" IO~P1w aMmaidlrmltn.oatirsawof ~$461 00- Pagr 17 af65 Exygen Research Page 90 of 132 000333 p. 91 Interim Report #10-Analysis of Fish and Clam Sartrples Exygen Study No .: F0001131 ,0111 H:"m Plafoool Pulnber. P0001131 eq~ ltrwr AlIALYITCAL 1111<7110D LOMM wwrl >w.~wva~wrst ~o Add (PFOA) in Soil by *Mood nftrba atwiwlb MW w Willow o Ow Ysholnj a a wt [o0wwd by =mead aaltitWort t,lnirdn luwnpwni" wsy ! "10 manFlw (In rr fer n MUM wt Of rlraebl wrdsCs) . TX "w aw, ntrWtd alibsdmikatAi rR bY W Ark wd irt iKjrotmr in a uwtatn w. I2J1 Un IYItI[t W&AW mm hr qnWwOn" L1Mat IWoYd OYIm me =brow altilyYtiJ I[wt" 1~1"1011 Y4 IA[ rp~Wl_~ ~pOrl YO ibra11011 ~IwAnd mwrtntios ude~ IIfWLyaa'17 (or aqwvsla~l! sweOIYIiIt t~111ti 113 iNWb Rlpoall Ilww oot mnd rlrdri eqoluu" !1q anylu Owl wwl!WtWd wwFelris7Yww Y frelYr diluted u/ nra,lyW. 17.0 Aa4troaat>tia Ii.l t~nnt~+w wwl allpw~ aP~ al a dnu~Yr ~ Y l6C ~tu Ilan ~ Mwm dli3 rtla The "13 mu MrW aowFd_n lo an_FFOA Wait whik the l11 ~SYlti~awl wl oa~pl~tPOA Yw1s Ibw 11e l .OQ. If s ltlrt ~bWir r10A t+t knlb S7 "wlbrn So := a MW bLnt Unpk sr Y e3taidatr Or aWn wt rtrl Y nmaol~0 . I7i )vooMlw Of 11 rpd4w Ed aMkiY W&M nrlzal be bawm 704M or tldr Iww vdtrr. lf s oo>wra! spun a1H iwnil4 Ills ampiLbla Bmku. ix ~qn 1w .t r .pta Yara b. madgati. Any wWix spilt. wtulds 7o" 130% IYw10 b awlwhl by 0" =gym U dMictili+n if nsatwction Is raa." 17A Aay aUYwdtr swAtaO *Iwd b Y a qBikbd er1Uer by rwi" Ow Huw am 7w4 my yn usludd hmr ft edorlYiaa of ft odtbntion sum. IIO+wM, q+a Powl iwwbR Of UtklpA nIbIrICVt IOdrb dW MA 1118 oak" auk ow a=d 7VA nf tbs OW aotfaba e( nctrrcud r'ardaOl 17.3 It arwhMwt eNAfeiGal Qt) ms anlibcalinn owva ynernsW nwN Iw aQ.9Y7 QI 70.q3} II aYbntion reulY 6ll avhids lblin IWrn14. 1hm 1/, C/d~ll tlllpt< ~be ItIw10 logo" ~k9ti7W pY[tiNan, mid Ihe rrdadYKtbWnInvrrtH AtnaIdbYistWy+ad. U.6 A+wfn limr b0wwtn rYlad ionpla am not iri!! mom tiun ! 4!i rllbq K " , AIInL U1~UIY70lI tile0 am qtandti twl limq altbdn ntanWaS us tYnOn wtlwtI Wwnurbvd Ap t;yf' /"1 Page is 4rd5 Exygen Research Page 91 of 132 000334 p. 92 Interim Report #10-Analysis of Fish and Clam Samples Exygen StudyNo.: P0001131 Rxyri Peotoool Nwmber P0001131 amman .A N."wNwwYavoeonfi 34.0 C+1ndollar 1"i dpri~R~rtiw lo s.kdY~t1a amao~t of PPOA latrd (ix ayL, UYswe6&w pwlc awa) wlf~ be ~i cwvs (NEW wprsim pOrwat I , 'blom-Ly- a r+1mp-: PiqiAlmdpyR.j " Rrlcrra_ :re~n xDR slor OF -woW bywliok "e e..1 ralire,rr &1w1, iiamewial.. 141 lyt SOON hMi wdA I0m Mseurl of PPpA peim e MaetLwi, we do INIOw1Yg "oiiaa b wkHmr b (~Cmt nrovmy . R-004, [IaWrrijwh=diwAFL1 "xrlbl"hsdixoerrel(WM K100 +o7bs"MI"pu 14.3 Um do 60wdW aPrnfam lo airsl do ronoLoR of PBQA fad in n61L No owl, GPrl >'!oAa~tl~Y>~ fC~9A~r~ ~.~.Qe.~..a a.ew ~+~(s d 11A W 11r bOowBq rqwlbx 10 wloWdt +fr rusrt of "GA faund in yph tmdr&7wk ProA hand (Vpb)aoy .dlM -PPoA rwai (pw) r (loon t wm aiiasnc)l r., ., .(7 Pap !4 oj6s Exygen Research Page 92 of 132 000335 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No,: P4441131 TucrlVa ftuwvcl Nombkc rooo1 131 AMYTICAL METHOD u.&W*Jmdw vooonrl mooed d AWyPU 14r&@ Mls~tlw OfFaBOWOWUalk Add (Mot) Is /AWyliail T" Iaoiltty: 0 3r- n Arwroli 3038 Raroah C" SarCeRVklA l6101 tow air `?,....~. (-IL4 rs.Wdxcdtmd nr.rwae.l.a44, s .n.el. .aoti 1 .4W ~ am v~ess~.~oax ap~w~u.~y~r.au..~a 0-1 Exygen Research ZbYI ?am 7 Pan 30 00 5 Page 93 of 132 0oo3,3s Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P0001131 1" T Lxy`aa PLowcoi Number: P0001131 lwwlrww~ "" h of Md 11"r/ Nutbn VOpbl7lt Awr ww lfr , Is Aei4 ("CA) in SWirome by il'JIASILS 1.0 Saw 'lbe erllrl Jr wl+impb)ed irie Yolrdor rd ~rriWion of yw0earvaamwic MW !9 1* P~rhra LiPt1 mavily oaq4i te B Owner Man 6P+ati'metio Drear (LI~IS~L9) is wdm~A. 2G laft 21 Alw" elwveerhli-rwyPendnw. 2.2 Oorrdl IIn aPpepddw 1=1S bebn Yu1111y my e6Menirl5v pipw ufny P--d- 3.0 Simple Ro pinownt 3.1 At bwt30jeflntwmpirkraonadoa :5.2 No rsPq peww" i Mew hr abiroan a. mpler 3.3 Sroir Aon1 altprwad Yauld be 4ldbah0 to wluilibrrlo ro ram ASUMPUSMM 3A mwt irflelal~Jy ofwi 1N~n boily uirPled far exa4edan. 3.4 SrepiY oe0rctloo Ploorrrs will be iPralhd in ON rlooplieS Plea for IIKs e.0 114,pOrlSfrdrb a.i wow-1"t.CypY 43 RLlrd-IlWpb 0 AodkAdd-lteqrtWMe 4." Anneniw Araaa -A.C.l. iwpot (aide 4.i hRboreoelwelrAdi-iOMKOAlol 41A Lu4mwl Ed 3420009 !-1 A NO Peh-uor Brim dewrrlrpO erbie of P-visi al se x ahwllr eAtypd rl" a vrlrLY valrr tyeaberm~rW d Weafot 3~2a0 pi,e.ewnrt a s w~lw Ilw kro6'a~wr QC7~i). 3 .2 A 4nbe a eellwtnw wa tw Pelk Wr~rll~ aV 900dud". ! .3 faalylintirlrrrP~befsrdYltto*Awl S . !A !Y aQ. dlrPowrllr y0i)prr~lreerolrdlnr Wer. S .S :! eaL IIYPewfL polyp --- edeltlyr olbr. S .f plPrn6lemiampimll(la10111f.t9G70011L} ! .7 170" pd, I~!! a~ww.ual~ lealL !.1 2rL elxe I1PirCvlrl Idt. 3.f OkoOIAUlIPIIIr. a .lo s .11 AwrMiPnySrrP~t~{lcova,leao6oaUI>s~.IaClIotaSoFoePe".aaifyt.m.rPaobi. aya 5.11 WE version midM i , .(7 paw )f of 65 Exygen Research Page 94 of 132 00033'7 Interim Report #10-Analysis of fish and Clam Samples p. 95 Exygen Study No .: P0001131 Eayyeo Protocol Number: ?0007 II I Us Yog11m+ SM1 "s RefadeYOadWker. ~c.r~e O~.lre a<~+..:~ so d. ~ty~y>~e ~, r 300o m~ 6.G Clkier00ieid,fe Slvaw+ al ruuyuws.+wr. :rw~ .e.slr [x~erp "e sawwaal . :.1 m~ a so ~ . sw . ..~ aso6.osxual ~ .. (1 sA rjre(a) ; 63 on6WJnow= s sN Asmoslum AcAse in Wow hilorwf ". I zMmW yllA 0.0 6s lA 66 1:! 2s 2" 4S 234 t f Flow RW SS lmLdmiat 37 0.3 9! 0.3 73 0,3 T7 0,3 3! 0.3 4 6.6 'I*uM Volwjg lu yZ .(sa be tm .eeeato me weaee 30164 0.7 Q+riYNea: Yak Mee-wwnl .e-ana odibntioe e .sa llml*mr: -t>>wmw. 0111. 7>te ~ow maEitlaoe w Ioom~do0 ee a P6de e~d ~be aheoled io ader ev or6adw dul4irC9eeftL 7.0 343M3 gym" ' 7.1 1We~ 1We~+~+yNe~lir+ 11k1A aiole. aonieoei~ sl7 -~ 76! ~VS fer )r1b11. ~i elOr! Oe~1l0Y~e ~Ode1wag" ad mlqtte OWIp/ed in elderOp ylwiae On UYlli NeAl11L 8.0 larwao. or:.rri~.e all MUG nr Rt .l 7 mlt elY~alilew eul~ b wW~e 4 R+P~~ ~' eddinlG 0.131 0 of p11pl0oium ao~Y b1000 oL OfwYer. nor) 04, Pass 97 oJ6! Eaygen Research Page 95 of 132 000.338 p. 96 interim Report #I 4-Analysis of Fish and Clam Samples Exygen Study No.: P{1001131 Exyooa Paoload Nutnbor P000113 1 lb1ral~+ it YT~CAL ORfHQD 'o waa rrrr rwo~~o (~fOA) tn 9adlmaa by i.Z eau.aio.lohY~aa 1.21 17i amlia aa4 iw aar b pi ad by aMft10 mL vf aulio aw1 to 1000ULof+valR Alnwnawlwwwq1rpwpKrL 0.9 Ikrla~ llyralla~ !.1 1M00~1 ~A1ir 9.1 .1 Pwlra & auk aolwlww ~t~-100, oCPPqA Iy rvflhia110 mr danbliwl rrlr'1(awwuad Ibrl~,~iiy) aed lltas Ie 106 soL wnh aobod bi " 17_l~rLlD_iE iplb. _ l.1 3 1R si6 0~l~OO IwInL wlrlia~ la ~al ~~bab In a 123 mL UM iwda 9 .1 .7 A l .0 hraL ~ olaial dPPOA ia ra~ul by wiyYK 10 aLaf9a lO IyMI . ~Waa la a IIeY wlumr a1100 wilY waJod ia a l7f ~Lill!!lar4. !.). " AOtIl~A~L.fi0llolWnaelrtOSpfPPQALpItip~e~lbyYm~1Y ~f.of1fl11 .AlOImLPOYUdoq to a !W wpwn o! 100w1tb awwiwl in a 125 mL LpM boltia. l.1 .! A OA1 lral, frYierin iola*na d PPOA ir P+aPrad bY brlalYka 10 rL of 1w 0 .1 h#AWL, alnloa to a Aai rolwm of 100 w1* mAori k a 11s uwL LDR Yaala 9J6 11lOlkil b11FWdOq Wieqoma aa ab~~lenG in a ~rern a~Ot1~11~ t'~C ad m/Yhla IE[a Mitlmlpll /QlOd Ord IIIOalhi >~ ~4 ~ tj !2 fMM1u4CAMalier9aiolaw l.7.1 1+~1d161aalilutf00 A"!/od1 an P~'ad ia alwhrid vla diluiian 6MOLINISLO .8 "boom 922 'fl 1ilb&y ia a allow Waryls: aOdiUoual oaioomeatiena may be C~wr~~Waa,d sar-dl-i-. - - d1arY/rllw YAM Diuda Cewabaea IloNt 1s0 V too 1s0..o0 laa to 2 lo tlaobo t1 o.0 s l0 1a os too Page 33 q(65 Exygen Research Page 96 of 132 000339 p. 97 Interim Report #10-Analysis of Fish Lnd Clam Samples Exygen Study No .: POQO1131 g.xyyes Thomool Number t0001131 r+ bmwxiwr" A1 .iLIOetBOM 60MMor t1i71wn~~ 1141 NawYw V000170 Add A) =DY raa sae. waaekmemmade* ft Ixs,lw.l.ora umvr-m ..w Ielo" at2'C l01'C, R 1v'at51 rlpYa, !3A Abwalt r~tvaor wd w~eanlnW~l "lllaa0aella may !r ~wpaod an aaNld tOb DIM34UO 1a1 er w10 .r+ .1~+" nrull~ (a,~iwur >~ .r Iw1) .wK Le1ws x ww owe a&wlad owed and um anrwlad saotola AeiRd ~t tmv,wi 102 ~"Iwlla~w >0mr6s0aa0a"or~wilaaxo. w ww 14 r~ ~~ a+~~"r"l1adw~+vuaac+;cne..a :Irl pwfy wrrw t1r Ibe Iw po1~t 11.9 s..w1a11~m.~.a 11.1 w.4la 6 11 dam* 11p. 50 .Z rwl"7lw+ e0aoimya aabe, [ronify aa .Le11.lr,laea wmd Io61 .dA. 11.1 Add 37 ml. d1K amti aoie, m0, valta ad IlrM an a vwiss action eater 11 .5 C101ri~aRafBrat-3000~tur-~Omfila0li. I f A Crildm Ir C IR aawldpa (1 & 6 a" 1y Pwi" 10 mL matlwnol iulowatiy3o,.L,nVr .c .wr(" tIbop+we). oo ao11,1 oolumno n,a an 11a Load teaal1+) n. wWlw m +a .mdio.w C,. sra CmasW ollCara 114 Add 90 r1. .r allrmmeal r d . xdfawn 4m in m. bonoas or da w mL nrtilyr MW Cap, vana Sod 11a1W aa a wi1R nation abdw fm -30 I1.1 ~191fW6wi~J010R01~ "70oio~a Il.i Dwa~ IYe atillral awlo la nwaR8 aati0rl. CdI0o1 /r aiwla. 11.9 Walh tb MINIMUM "M 4 q11. at MOM" Cetiaal OM duW d add k r We tlrraerwladls"11J. 11 .10 CmdfliaasraoN Cp 3fE oesrdr p ~.f ML) by WIUci10 mL +nalaaal Wlio~+ld ly 30 alLor1UPLC wOar h2bopllaoy Do ml IN Oak" ruady 11.11 Aal am.011wi la -x00 ml. .r walr +.a bN on B. a.eoaa aoeaiden.a 11.11 sra .aww Alto ,Itm -s aa.1aoK mlmaaA se s.p1movr1aa .a111a,.a11. C(eManrw+sam-w. -ors "is ML) . k+o ,r .au.W u.u Aa.lyaa .a* . .aia0+aea..,rwLCnAwlw . )apf;r, r+ P%r Jt 4jaJ Exygen Research Page 97 of 132 000340 Interim Report #I 0-Analysis of Fish and Clam Samples p. 98 Exygen Study No.: P0001131 r011 Exy2srt Protocol Number: P0001131 Da7M ~~~~ wIwONYF~RV0W17t7 d at LCUM ) in Sedfimnl by I3A tiawalo~a~l 111 i~w1 W~ roraopv of wlkallwiwd, wAAe nd axdllq/ wlqw bqo Ihe LCIY&10 qti1Ya A dYYniu ~dri0 ar plwv0r aod WOW dl 111 9110d"d!.!OA OIII11 arra111~ 111 r11e111! /+tar Illqll COIIOw11Alion lta"St surele YoYidYnwlyYertar. :J3 As w1Yw aR of ~rrwd a~nelas rluiuda ewa be inch" at drc bawvblb av! t "e ad of a Irwb wt ftedrds mm be iwvpaml bwwa WAY 7-IQ woylw. AM ev altowdw. all GWn eR o( orlu7lratwn rhn" nb we 1 llyralr6 at to byirias of a mat Ydeww by - N~alian rlrwlrilr Ylrwalwi nW !-1" wlaOw (w voovrol !br a wooad ul W kvldlid. Y rMt oar, ralYYlra nrlwo wwl be the Grlt and ban hjeotioala a eu~b wl . 1]A UWt Now ahIIWa - arv11 Or 4uesdudaa. Lierr alrdnd aarvw arc ~IrnN1hrb~46yliarw n~anriea Ua waipYK efvwkues vunw vdlaadw il.drd eenaabadon w1a~ b(wLyu 3.3 for aqllivafenll wilboosayww ILS /f1AVb IaolOqre Aw11 ad anewd Mr*A fMyeaNb Any Ynlplp dnl w.erl .mdr~lrwpalwrrlalda e. Warep+11e aid,oe.lyned. U.0 AaaWwew pllula 13.1 avow~Y/ass eaul aIolr b PIYI of adrylwe ion a S!9 amr !av a pWnn 9(411 mm 7161 413 10n111 ana1 a1 a dw lFOA awea,vAWs Ihs 4a1111"eYa (70llnla? 1111 ~ a " Iw ererbo.eloasar. la2 me" e+m ma rot eoiY rrol+ K wwa ve"or OM on iAQ. Era bb* aovdsl !!OA at 11"1M /uhr Oue Oi eNlaL, 1Yv a MW blrak wll~lemr b ela~ad 1Aewlb wl aa~e bew.eilleord . 19.3 llnwwlw4f oo11YO1 who st smaaia Vibaa A" I* I 7Q-130%9( Ihi falor ralrr Us eevbai AU bHoelsbida ile acampt"liniu, w wdln so at eweor doinll be ee~albKlsd . AM eraie spike arjude 70. 170% 14aW1 be awlaabi by Ifle IIUfrR 10 d111tmilu if laafal,iion if I3A AnyaeUYalYae lord faat Y be a 49111" eWia by wia= So NO 3ear'IbaR way be rteladw be baladrdall of IM edibraliun elr.e . 8ow"wR Ihe wall number deleackal allbnelaa aeedwh *wt oowd >w pldom MM a01 *am aft of as 10611 aRAIAf at Otleoqd ftRWw6 19.! '11a wrrhllmi wv1lfeirR Ily Is oalihnlflv bKrw !OMY aww be AN* Qt= i0A,7). it aWEnliea nwdr 611 amldr Ynra limiu. Own Ip/MpGq O"4 Malt 1a ohm Is a*R Sa~Yla1- eyWalivn. GI10 The rlvrdrir areedevaar a"afrolOrYauW be erNysrd. BqP"07 0111- Pare 3! vj63 Exygert Research Page 98 of 132 ao0341 p. 99 Interim Report #10-Analysis of Fish and Clam Samples Exygen StudyNo.: P0001131 Euyy6q NOW*) Nwaber. PODt)1131 /"`. b".arr" ANAL L1'JIOINS w+aiK10" vwonn 0 Mis aaem by 13,6 xntUiar IYttw twtwew w60adb Yd MMlw swrt not Cri6 MW tAMm * 4 K v,tYn r a@OdeN = . i<ulullu lbasddA aaewda We limn within m~wd~ied nwlba IYe wt ruK w ~eaalya,d. 1 "0 [SkWadar 14 .1 Nwlbefdlvda~4paYo~le*abWUeft=opmtofPFOAloued(inqymL. briMPaat woo iiytL aWNY4 onw (Soma niinsion Persimmon) 6emwdby ii birLpmaa!lwar eropow ylQA1OW (rylmlQ- QaLaer .iooaoao0 a DA rbts DF - duory%tM w.1k.t ..bawIlbot, ifnaowory. 143 la wAlw bRIi10 WO laffos amVA4 0l PP" prior 10 WAMboo. moo 11m blo+vs 41r11r (h wlarm fttwowit naorery. " [ kW m~ye~ ~mi G~f~a - rW.1w11o~wdireoaMW (ay~Lll lOG ma~adddhf~) l .3 w. r>,. erwbmo .awlom w o . ..ms aw . .m.ma er rrw (mma !mwmr. b 1105401 TFDAfarO(pb)-=IW(sS) WA w. ir. ~mrLS"w~~ ~t aaw~.r) roae~,~.e. a. .nmme or rvoA Ih~ma r.~>.awenb ~ woA bmr bN1 &rwA&-rPOA Wuwippb> = Itaox r nai .oba .IwH rv, 7.17 Page 36 af6J Exygen Research Page 99 of 132 000342 Interim Report #10-Analysis of Fish and Clam Samples Exygeu Study No.: P0041131 PJySai Proloeol Nafa6m: POOOZ Ill APiALY9XAI. KOtOD 541oaltlnbrr. Yp01FlTp I~IaYw afA~ ~r 4a DwRw4a11ai atiA,rpwr&aeftrale Aald 1!1'OA11a i4Y sad Clar fY LCJkItIM6 na.lrror r01ft}"Mr. a . m x..W" loss e.wah o*4 sew NOW !A 16101 Apprmd n. 1~'r. ,+. C-4 Pod cNew Talriaa! Iaadu. LC-A0.8t11Raucri , . .1l44 DM /- I1 Exygen Research ad P"a : 4 Pase 37 of 6S Page 100 of 132 000343 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: PUOQ1131 ExAea Proloool N%w*cr : POW1131 u~w~hwwr iww~e~ew .vooonu AMLYa~CAi.1~T80n ,aamwa~7~srwa~w~u~nwars~v~aoaaAM fPA m a1 Pd . OWor br LCAmIAt! 1 .0 "6W " This wlLa b ab .np1oy.'for i6. iml.tio . .d quafYd.n .(waworwawrio reid by IlSsb Palbr~ea LWFI Groneoopapy oouplad n a wmdan Mac. 6pd~am~le DwnOOr V/hMQis fii aadrLMa 7.0 Swky 2.1 AWqWOw1Mff*w,M1)F"dM ZZ 01MA OWIPPOXIM KSM boon kod&4 my chabical INV" jarety pwaw- 1.0 310"k RNP6-w I Albow2gSdowasimplebransmOm I3.2 Soon OPW be I - - b9ft# usecdon, Pbm Ow hom as"Is In a bw passowr as hm"w" wa dry WL Plan dw Mw" L% "NOMM bm WM th twon VWW gvmwgu Ig SHOW hr dwxwo &W and Plan do "now In k%mmon , a On* of 0144111h6 33 lompb NOW" yeoaAow wiU w WOUfad !n !r tumplfns plom 16r WS . d.0 RiivY ird 1lrwdrdr : 1.1 We*-TR1.CDMft 13 Aowodtrjw-t4f.C rnda 43 Cobow(170"IOOerw-Arprtyadt 4A M06"-11:i.CVvdW aS MOM Oal 09-70o ON" -REMM 1'++" Lf Mwhil(f"100MiO-1HOmiMO 4.7 42 1 rrl-AMC ~~" 69 alo Ln,lA.rwmriYyiraeildudw--Rurr1-Ox0.'So&d ' .a. +.u "roln,a~-w.,wsw 4.1: ---' A*@W-A.QLRftpWOr8* 4.11 ewOmm.snarols Add- Wfm&AMft xo rrrw"rr Il9qre" 7.1 A MA f~I ro-raa ipdd olronutaQapb capnrtk of juroyind up io ] alvrnb OPWi rAR n vat" VOW* 64"a so" of *Was 5-2QU pi. raweqda atwdm1twlheua~CndWY) . f.! A 1 1, rp0 eollul mr do fOrpnb iirplYe ad qnr~ewim 3.3 Aad3dalMannayrplpolnwdlwiv lOOOUIg. aye3Kt 00,11 Page IS qj 63 Exygen Research " Page 101 of 132 000344 p. 102 Interim Report #10-Analysis of Fish and Clam Samples Bxygen Study No . : P0001131 ^ H:ygeu Protoonl Namber. P0001131 s~ .~ra dq0 . AXALSTICAL r I~ Qoutiy LC*41iAK/ ~s~rv~aim Ifn~ SA Rulr7 ~w~ar. 17~. Si 1lSaL (Wla. S_7 f6 ~[.6~~i7patylr ~rril~ 1~ ~.i I! a[. Url~Y~7P~!'~ S.9 tli~Wl~mim'INY(3PlUAl,1OP700sLj . is .,1u6 :1fs3,a~eLl.m1~tluEKa.wcor~lrr~alawrl. t~ La~tlw. s .tr Aid- 51..3143 AsavIaPPIAPMwt.W(.IOUas(olootprul.or.tr. .laatavoos7NrrW7),. ~~po.~lakr. e. u sas ~omtM.rwpo.w+~k.,rqperrpoML raYSwrbm esu.2000 rpu 110 mwresse+CIO= 6.1 ArdP*l1 CAIMs: DLapew RP dwlwaae 3darllkl, 2.1 mm x 30 mm, k+ (TlN~i~lOS~017130? 61 ~ (A) : 1 MW AWmoir 11aft in WOW i.6 IWWI~Mwpf1 : i1YlYnot f~3 awaiwthr~rs: 3'9Mbdd $A OA R 110 65 zIoL.Ot a u !Zs 6 rAw Ra" !~ ftaLlri~! 0.3 53,3 6.3 7s 6.s Is o.s 35 6.3 de WMk=voh..e u ~1. (~a e lna...r so x ovoh ~ w uc). 6.7 Qm.*Mkm : 14.tAn.- .xwmr $r.era a.libkstioe o^va . 64 br7faK -2Sairwi~ TW dove wdlekos in Ieiodr0 r a "ift wd mq 6e aAmp1 a order w jl Me rw itFt.C ryr~n iWJofI I"'r Pap!Q o161 Exygen Research Page 102 of 132 000345 p. 103 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No. : P4401131 HxypaPmtocol Nnmler : POD01131 - MAWafAm4pin far a. a cl.aatYc.Cn"W1 w.ewraor .vowna Acid (110A) in MO-ii 7.0 MM 11"M 7.) Olod". iYelo~ Nylh'e MR)t wpda, wmltorin14i1 ~s )N rN : lbr PPOA,' 11a ~bowoatWiwl w faludad NIL VA" Ed MY be elmlwl a ouo 10 Updod"ONJOW ~~ L0 F wrimaftaYalan 1.1 A1abk rim i.l .l 1 ~1 aurlaltm reA~Y ia w~ w PnP~nd 6Y adWnf 0.1 fd I af w~awiwa wwtno 1000 mLofw~r. i.1 )<aaaotiaa Solttlkn 111 7% wewYk sidim mv&Moi bpwr-nd OYdiwo1vin17 Iof waaAic aeldl.lrwl.arMrrw. IJ3 11011 'Dwd Adillwoiilste in MOM b YnOKb by bWinIM1 ) Ml a[dlrllpddt wiNet la a lwl vadwr s110 NIL with Wom. AlIlteMwaltwtw My' be pegwed. !.1 llat+ltad 1rywYlar 9.1 i1ladad "teaMaqt6w"aa Ieioeim 9 .1 .1 lc~is a MpA aalWiw d-i001y'aL of YTOA by vaon110 w1 a[amlYlkal tewdrd (oaratud hr yarilA wd dNaoa to !00 mL aith arlhrai in a 13S-mL LC!/ roltlp 9 .1 .4 A 1 .0 Jefwl.lbYpnqall mwll0a of PFOA it ytrprd by Yei" ; wL o!>a IIO I~IhttL wbdir b a 1W ~olawa a(140 wilh menwrml ir a l4! rL tLf60otW . 9.1:3 A al Iy1rL fttiIlwWoa wdtnlaa alyOA Is pappad by Iwinliag la mLdtlta 14 Iy4aLaolatloo to a tad volute of 100 ri6t aiedm ir a 123 wLILA1B Iaqa 9.IA A D.ol Ir11at. arfli~adm aanrtaa ol' "OA 1. pr.rwad >tr erialia, 104 d 60 0.t rymL aaSatiee to a /oal rolwwr of 100 with atrrad 1s a 123 n1. Lurs bama. 9.1 .9 Tim MA r0lnlioaqan rolllwa an p b Mad in a nbilwmrn yprodrlaly 4'C wf aw rai44 hr a arxlwwn pqrd ef 6 awodr bow dr dre et~wwdon. r've4a1 Nor 40 ofd3 Exygen Research Page 103 of 132 000346 p. 104 ~ Interim Report.#1 Q-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 rr01111 6xysoa Ptosoool Numbor. P0001 131 sY"O11.wor MAW Alyui.lfiLAi YR'JMoD by clnr t~reunYn r.ar1u.rYfvoeonu -r- ;. rr.e .r 91 wMimdCdfkwMoslolriuuu 911 LClilll+l~FSadlYfdiwwrltdYwp~lpndieraWYSdriYd%pdvn Ate. is yFrLlY~l6crdw mdrtisn. 931 TM bll0~ ir a ~Ial s~p1Y : rdi~md OeneamruisaY mY1' be Prp"ralWf1. ,~,nl~,~ afFoalfArllYS VWYw Mild 45 r. .l cmuontim f 10 tA 7A UO tA lA 100 Of ~A2f 0.01 r~.Oaa6s lu0 l00 oOA.OmOfs wl l0 111000 OADI mmtt N 100 . OAOOS Ya.7 O~~A~Oa ~sa~d~ uxaaYfiaR-11018h b0ulel prC1s A"1;vprsitmoeft. r,7.i AUlrwvrl~rl"aelOauewenelOttial~frWrd~mYwOnr~ Y Ow~ 1060 irohluf 17i 1a1 Bu! kid) of frP1w wweW (efqefulr 20 cc MIN) MM In*& At 120% Owe 1AvwII 00w01 E/ 11u0 dlrW OO~OY fto/ d aOUiA ooo"atrrlor ObaaMel y"lo "lts weewy sr as 6mxli . loa Imf~f~t,~rf !i.~derr I~r.n~wr~q&.Y .au be dpuola.u ia 4r~0'~ei9beIx ~It/fo)K~ 11A arrbOsdYdaa 11.i IFw'~ $ 5 of Sowi rFk IN* $0 wL PA On -UifilP tub" (~b y 9M"fYFYuu lllasl wWxnnri). aw AN 30 ML efAMONIMbud OWN ee AV" mlioR drvr lor-I S minYow. t13 9YYUi~wl~le~AwaeAr-llCUr. I IA ?sk ad we0iia IM illZ hYw d dlulr tluVdwlnPi Awlff . 13 .5 Pa* fu 10 di. !!1 IdW la wqwor wM 1 i Aofid4 7 i lslics 101. 2 Y ratSuR ad 1 t LCNHI. Aaddao In oolwtrY %f10 20 ML of mMrol. # yp pl, w oO"Mk DYWrd dl aYiYa. De net allou~ M oN.nw m 11b Iilmts to 135 mi. pYwlspW AM* by Audoy wAA *A M% ft"IbY&NOMiu 1o10ew Ads" Rim 11r Adit WA lelusr ow'bum" by mslY" am d.M4 Dry llw am awrlddy eNen we. eilhs y,lwdrylu~ a~ a ~a otoiety~a . f~(Y Page 41 qf6J Exygen Research w ;. Page 104 of 132 UU034'7 p. 105 Interim Report #10-Analysis of Fish and Clam Sampl.es Exygen Study No.: P0001131 1'- ExygnProaeol Numba: P000113) nyrrlrr~a i~bi/ N~a~r YEeena) A1fALYTlOAL Mif'HODI usWaa ofhdiammoodonsio Actd ("OA) n Fi~h Wd Crm. by >ICJaaarMs 1f a oe~ifiqe a w ad. Deq~elrylru ft" ommalaioj wa+pb r -loao rpm : f1r ~lo a~elr. 11 .1 Dow(kmwlleol se 1o aeodiboqaill WE oeluma Rtleiinside Themovehof so PmW4W4qd ra*. coo" ft 415M in " 1-45 ML summum PqWhLPm AWL Add 14 =L of N*WMiw 0 So mqb in 0. * mal. combillap tb. . 1140 Bohm** MlVkAPb Ot-3*VJWAWM a W11*40M dWw. pboolhoubminall hr-lbooramm. "31:1"3 Caa*&p do 50 mmL pdypmqwbm IA= ountolming moWk d -2000 qm PN,,A$PW && ad DoMbin, *J& *0 OUW ftM #A ijjiLWl ItI A 4 IIA' 11 .)? IUS AAM 3.4 dW of 1-90mell W Om M*mq in 6m pvmr4bwW limak wW vool de c"WW romme Wftam" vv - 40 4 401% = *.@W bV@UW$2 .Lf2%&vcwrb* .ldi. .v-mmm1- OW FW4"" MA twirl so WAMINI". Tmdw 69 aftaft to KPLC Visit Ww" dispo" Opm ANgMi I valigaimboVWLCMIMA. 13 .0 CV001"Vviry , m kdm 6W amme mmomma dom* "Wimpil. mww ad h1dow sample bat OW - LCIi4t11a aj*a A a6'Yndea iraedad MW DweeOe +md Dulow al1 ILl , 14aDrd aflPOA ealnVeadlaD to d lert Dee or leaea canoaitraliae k.el1 mwt>ts ia~W ia aa elYl~eat eeR 12 .7 ,-Au afiw ma elsalibnlbr elrdudY run be iuaLdedat the lejenlag sod K dr r oft mew+Y OIL llw4ade Nar be'n+ewa~ei bKw+a ovnry S" Io aul"n .1i 0 a9KeWw. a falb eel of oallblatien aar0ardf coy be iyepd v Me YagiiaD of a ma 11Uoead by ealfAeuien tlraads ialeI wwl wwyl"1DarfOr (b aamlet Or a mud so Maundu*l. In -dim cm aa1'indom dmda* tpeit be Go JIM ad lm iajatiua in e nr. 12A eUam1qwyMae ylaednd ~ hr pfalllMiM LJanr wewdaud owvw am pamad iisdewlyei byDaar wDoMaien ewinD lhc wwDbuq ofpwkerw verua saDYwltn elaal~nl eoupMaNm uY~ MWLra ).3 {a equivalamr) aDAw~" 491Yw NP edt ^ Pap 42 of65 p. 106 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 t ExWaProeocot Nwnbw. P0001131 1kww~wrreA AYL AKn4YTtCAL Mlf110* !f 1 ~s~a K Claf 17LCIi!lIM~ 14"NrmYw Vdp01111 ( ) iR itb Yd l2! l~wpr n~e~r iao11 ae1 Kewd wrdnd r~p~w . My wnplw IAaI rtp~d a~lknd rwplll~w eAauW br IIuYurdIIIned Kid rawalyreA. 11.0 AswpWACdrlir I:.i Ciliprreqmo moor *owayak9( 6Ir6Lrr rw aNi! me Min t Par", 4(413=L 7* 4U -p-1aNI dr 101w plOA Mfa. wAlle Ihe A+/orAa(M!omoY) III (Is IIUIOKCrY1~ OrR30L 171 UAW bl .iiNot ad enllb rpoiA Y luwr YUW 1hm do tqQ. V a 1bek mrdiiPPOiA d Wv&Swlr fim pS ppl, Ma mm, iLet Hepr ~e 6~ eArirl~l Iw rW rt ~rRbwir~d. 133 iooerrllw a! roomel Mltrw mod IMIUlxW1w rrc be lelrewa 764 M% at Y61sw~ alwa Ya ao" M ~lkp iiL wdd~ th Iloo~ir>th 1knAw +Ar ads we dreplw i1wW bw"Klna" . 13A Any eeEiocWw am" hood to Us m oIrriml wAdrr by win= dr Nus ISeor Twl, ow 1~ ark" Am be nil:ulYOe at Mw aliSrWam Now. Hnraw, IM rrt Iwnll'w o! tdi6nda rYadmip Amt aeold be aeh+ded mrtaetwrd 20% atom rrl radrrefrhodonlY iy4at'L 13S Tw aaaWiM oMdors W 16r nlqiwulw alrwm pnwllud mpK be :!.l93 (!l= iQ.IK!). it man" rrWb Y wtrb ".r 11ain. Ih. I eGr rqi am r . Mm w .qj*hree.n "orodOa, re dA. rdr~ rir nlwrt rtKrplr~W W wrWlord . U." Rrwdx rtr blrr~a RmiOooio ad wllpra war am rill aw" don ! 4 %vifMommumbihol Iw . groom" dole dril etowdi IAr fixol wAtlhl = r4 YoN mm Ams Ou frt unrtD" awrl~d. t" Cliodrt{r 14.1 Uru, foNwYtqwMo . ~ ahlrrnu aw~n .rrpoA maea tu~ w^~lwd on 1uk Ow} Mho OR w~d~d Ow" (NOW '01mrlon psMslenl par.rlby Ihs mew y.x wMen papm "OA Fowl laS'aL) - MmIAML:.WQC1o0 4110" 143 Vw rr ldowr~ rq~Wiwto aoerwl ~ a~or! ~t1P0A Aird !u nVw" n M'0A 1b%md (ppb) - +.0rw+1W (d Dr -pclrDy, .WqArLd ..Lrs*wdfAr.d icnwewray. w,. ? eaY 100, pqge 43 q/63 Exygen Research Page 106 of 132 000349 Interim Report #10-Anslysis of Fish and Clam Samples , Rxygen~ StUd.y,No.: P0001131 Rmysaa Pramcol Number. P=1131 14.3 ft iM1iw bBbd WW 1W"0 aomuM of R^oA prior ao exlnctrok a* to ~Ilowfo~~qwlip Is WladWh dw palm mm". FACDVyA%1[Mtr..aWd .a am - s!~INUpriw eeevacwol ,oo a.ryr.mw o" 001, 001. Exygen Research 11p 1 YfI Pap 44 of63 Page 107 of 132 000350 p. 108 interim Report #10-AnsIysis of Fish and Clam Samples Exygcn Study No. : P0401131 sxnw rmumoi Nun*cr: rooot 131 ArrrwAsiwxxrwi,cwAe<r, MvEoot0aloMp M~Y~ ~II~d~1~r"eDIIIflIf~qw d~AYewelr~it Aclt (r1~UA? N YIFIIn byIRAWwti AryOod Twft Pal" AIN 1rr CMI,"!A 1f101 Awcowi Dr. Ofte ~,,, FLS~ny rVbRwra~l. Q~rrr, i~p~r~ trrne~ Exygen Research TOM Aws 7 Pass 45 jr65 Page 108 o 132 .1 C (,~ :.J 51 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : PU001131 Exr,a.< rro1wQl rr,mbw: poooiis t r- 7npip+awwa MIcAi. Mtrsao MtidF4-" voppirw a by LdAtB l1O Sin .rauaro, . 1 .0 7% NOW Is t In qhrAd fwlb. iolrfoq ad WMdtadoa otpelanavalpaqio =0 b IN# Ferf- Ul~ Cl -, ip's awjPkd to a w0uw Mw 'J3oreawleia DOWN (t.CA19fIL91 in vWnMm 1.0 SONY 2. I Alraaa atiasrarA h"nracy Awdaw. 2 .2 Comb ib apptOptisls 161308 ba. had* any d :a" l fa. qcopar aaby. 3.0 OaRlekabuiwrot 7 .1 N 1wt 7D j olutatat0l, "r apaoMao, 3.2 i>uaplaabaiAla roeawd Winawadoa . Pbea On kesaa mnpk in a holl iw~Oilba"ONAW va *Y ift ft"sw moo" In Owain" bm qft is 6am awsp v"040a la GILT" (w , I - doxwol SW and ph" aw .1 in 6050 AMW WH tirm of a] a.qa ooiboYwn paoaadarw will be .p.rJSaa is Ya wmirrq pri ibr this rVOL "A Rq"011rliY!/rda s.1 u wAoo~awom-tijlif.a-c,tranaWaP.a. IJ Calo {t30"" OWN -iatpeevaea 4.4 16aqt,rl-RFLCVaIs as aA seinto"tiaota.oi.o=0onotatnaub))--xR.o.om,oar.a..a. 47 awwaiaOLC4% -1090pa" 4,11 1"ooaara-rPl.cpia to L.AWOMo add- Raaar pae. 4.10 DwWOWNINalnflasa-lu3mtOatb a.ll TOWtbe-llwarpsla 4,32 Aa-aadiwAnaWr-ACSAaqlatOeda s.13 luiuonaaaolo Ibfi-~I~na"J11ddd 5.0 imotamawd8qitipwrt i.l A W* Mebtwwi IIrY nhmavaheraiO aaptilb cf pwopin0 up w 2 altwn~ rltY a w1Ww rahatta WW" oflajada6 l-2a0 1IL00~a0~ala " Y~drt WIaO~aaYaalall~. fZ A OtWa1a alld mr iY brtwlt ialWdioa atid qw6adoa, 53 AulYdn11a1aqosewAkdnaJq ao 0.00001 & ryrlw'7 Page 46 qf61 Exygen Research ,:. Page 109 of 132 000352 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 Itzygen Pewoool Number: P0001131 Impllwwr MALfTICAL Mn UM by LC413q ifA~l hwYe w~0i 7f~ in Ya~ma~ 3.4 OalqG WE - r. _ 3.6 go :L6~-I-l-r-pr-a----Y-t-a--t-a-aaYiweel0ea 3.7 1s 30L s.~ pl.~..+l,r.ylr+~6ou~.lao,~oa13. 3sN.1fo 1z2~7ci1..tNs~xEvtwcw.l..l-km;tle. aaseollbn. e1.n olves.u.,+rwm .12 i1qkagr(Iratooep. ..r1o.lo0hs), .4mMva .w.up. s.17 !!!:wYwpw A+Mww. se.wmT1y. 35..1149 wc.eenlhww..a.@>arllos.tqi.eetso+.r.polyrnp3le.awbW.I2aooqn 6.a cw+o.wanaloarro 6.1 ANSI)" Clelorr. flmpbw RP tR,qmw sciwNNtey. 2.! mm x SO MM, SN ("M~, t37if4f2q0) u r.op.+..: 3rc 6s l4sWg#lhwiAl : 3 mll Aronewlma Aeren. in wMar 1.4 M"Phme(B)i Mowed i.f G4Ai~t1~ SWaradW %e OLD 63 lA 6! LO 2S 20.4 13 224 6S Mew RAW %a MAW 35 0.3 35 0.3 73 0.3 7! 0.3 3f 0.3 ae ly.A .voa.c 6.7 QUMduli= hllt Aw-anrl ~Irdr4 ~Y11n11w ~. 6,6 Ilwi'fltna _23wb.rc '19~ ~m+~dfllrol ln irlsddu 4 ~Ys ~ed ~ lc alw~f~ M aNn ro uNdr O~ eR .C iy~l~~ 7.0 Nf"t+yllr 7.1 6lore Bl~aais!' NOW" WM arok moeYwrlet 413 -+ uA VIA Set !qP7 a1T doffAk Pap 47 oj6s Interim Report #10-Analysis of Fish and,Clam Samples p. 111 Exygen. Study No .: P0001131 $xyB,as PrOloOpt Nluihar: POODl131 Fayp RerU16 L6ib7e~Ar~aii YZICAL. iwarwii~lioa by LOWS" deWel IMWrV00rf17aM Acid A)ecVeruroa TI! aboro3adiliwrarn buwo0edo a OdOG and ary boahaupd In order so 0 .0 tw0ealiro/SoloUor 0 .1 b1aLAalbrc 1.1 .1 9 ~t amwdrta aoeuwG walw 4 qeparal)y eddia8 0.1 f4 j of 1AOadqaaoelelele I000 mL o~wolw. O.t &caoiioaBoluNom i.9.1 2% alool6l0 lioie il wOnlol ib~rqRad Uyauolvine Z sof loooibic rid w l00 rL orrWeeN. t.2.9 70'K Di~Rl~dlowaeorrhO in u111no A1cev~ 1y bew~i 3 ml. of~i~e toa' Malniw~ ot10 ~oL~i+<t plewia. AfwmoeYe+mae eaaybe OrepoaL 9.s Bredri regaratiea 9.1 8aaind JloeId9oRlhatlm Bdotion 9.1 .1 rwpaa a Meek MIl0ea of-100 pOlIhlL or Fi0u1 by wei0pip` 10 my ^ of eswiyeca{ slowest (ealeoled be rurily) Will Qilvb 0o l00 awl witd ayhlW 4 a 123 mar LI11'B lot" 9.1 .3 A lA jqon6 hrMioelkn eakllUr of/MA is poqond by briapnlt i af. o( Ow 100 prwI. solo" lo a Ooal vobooe of 100 wide ewLriel In a qs mL Lo~laeolw. l.1 .3 A0.111g%oL RAiBarYm eeloIIGa of FFGA is ynpored by lria0ina 10 mLdrw 1.0 Ill~al, eoMioa to a Baolrolaeo of I00 widi roalmol In a 135 vL LDM WOOL 4.3A A &01 yrbaL feltiBaNr robaiea ef 1'FOA ie aee~rW Yy bnaWaO 10 laL Of Oa10.1 WisL rlarioa to a Onl Votons of I OD with wwrent W a 12S aL LD~l6loala. 9,14 oil , 41 ~peo<baWb. PC had au eabls he a arxiwun fww of i ipoolle pasirdoofppaftfw. 92 SlrdaeaCabhlwlobudar 9.2.1 1.C4LVIfB pMkadan aYlrhuG w yaqaa0 ia awlboool via dilution af0u 1 .0 Wa6 fetlilkWioa oloqwl. Piy,4 m' 001, Pop 48 of67 Exygen Research I . ; 1~t Page 111 of 132 000.354 p. 112 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001 131 Sxyoen Ttotocol Nuel*oa F0001111 c""".' .,'1 aflAeNiYlfir YOi+ar DYnl4 Qanoe4Kfa L1 .C0 il .so lloat o.us got aaa Io NO am" OZ to 0 .1 lo 1l0a6 Ma O.o4M1 O.M 92J 9W* A 10 096146a arleAdl i~ 0 Ix6d.1.1~'lt a~ewro.+rort benls .e PC of e'aavaa .mo ." !2A Ahlnnnr .aiwavir Bad cwwwara(m of ,msdoa. my h . pro" a 10.4 Ilqk3R BJr 10.1 aarD boa e! wnplr arrrd (qVlnYbr 14 or 1rU mre indaar x lost aw -wakwpd MOW pd No rownd ooauaw MW a twwn loa ,o8Nrrtd . (1+ .wY.1 .vas.) * . .ay pi .. .a~rd sl.,udnnse"aor wa .a mow* aw~new. rd nawpietr.,..yfwtrev..spe.edxre.. c JOW ia tti "ft ~ Fir kr Ns IAJKc 11 .0 3=qna.Oabo 11.1 rrdr, j 5 .t ft- ryw rro JO N. pohlpOprlame emtrirulla laxas t9YAqy ~w~w4 Mv~wrN dx wtq. 11.9 Add Ihd. afawmadvile W idoe aa s wal ad" drka h-1! aaaa. 2 1,3 CSrCIhp Y !C xiL Pa7Pro1ldwl 0" o0nnieFAa Wrpl! ~ -2000 qm exae29rw 11A lae~ml aaait~a~alQ! t"r al dloi~s me Mr`~YyNSata 11 .4 faek do 70 wL iM nir in wqww whY 2 g lloeldl. 2 S Am yl . 4 g aedbrb t01 I LC4ft CoalGfm tly a*Aaea witl 20 =i. of slbwal, On ip w1 . of modldla D6oad aa r~a Do aol Wwr Ow odwan p Ilb ~r iYn 125 rt pwioW &*A y exnfag witb ft 30% dkwaywfieblendYaala Owaawwirlfer MAN er frh wldi 1o6wne Boom, 1 1, nl1 ly xrqiwrl (OM ti .w) . Dry !a Be" wafrluNY before oft aGlat6y lk,ft a w " swwnw afmrarri I LT Damns 6a avow an la aaadItiaaut M anYrn SRni irfa Ilw aoaL of OR~ruiyf~l AML GbLM ft BMW in du l2S ML dlapf1eG paMhW OBIL rya~r7 I--- Pap 49 o/EJ Exygen Research Page 112 of 132 ooo3s5 p. 113 Interim Report #10-Analysis of Fish and Clam Samplcs Exygen Study No .:- P0001131 $x"eaProqool NumbOt: P0001131 I111Ai.1TICAL !WY'[II00 - by mmmm 1 in eyaptloU 11& ll! 11 .10 le :1r . A"90s11.drwodpdlYtrll0 ample is lw so laLeuavUopahe. Yr1a Ou wyla apYbr-10daw a~ ayinwtira11akK. Cwari010a Ow !0 al. ~olyp~l~w Ww eonealMy ar+pie a -2000 y~a ka-Soirra Dow ri. mom am No Wow aPis oetwom. Called On wurs filed die wrs Oapahmlewl Sea ad wa*a rA Ihe skew 1Yoe1 die leithl 11 .13 Itptw)H 11.I IYwOA Il.lt yaYt. MW. ha I " *W of ioaerol w do w.x 4n IM rm-alW.a A.n IMP ' aaso,nlla R1WM 0~ ofta pow7 I (st -c 401% I1 .14 Malls do rl vrlrra,ly aYlYO 2 m.l of 2% mantle aeii in madlwl lo .y_paar"nlad Aand Mule o"roira .._ra lIYRW 11 .7i Auab~~~~i~~YLr: 1].0 CWinaOPOY 12,1 War6s wrwwwo afv-ir+aodrd f-Pb md fheNilrd saaPla iaq rK , . . I.QVISAlli~ A allballall aiv0atd raw PrnwOs and f011ar all . Iil . ~Ilrida afl'fOA ooma~l~i'si lo R Wlt llw waiwa eaaoaaeation lawb a1w~U irl~Iwd f~ aa arlytial ut. .~ (~J. J1~ =Ib apl of wlbsonl talpoilbop aYpdRb must be ieeludrd W the h~1Y10 aa al Ow r at a aaw/Y w1. 6aaaa~d waadrA auk be IAr".rdral.r omy sl0 mIpla Aa .1 auwna0w. an wlnn +a or 'ion md ealinu, . aYrra. my Io Wrolr r go lapilmai112 or a pl foliwnd ly An" cahLaeiw atullula Wr;sw1 svuy 3-lo pmpiw (loaoooa .l !. . w .a .+ at of,.rt~w0 aloe.ia). 1a oi0t. tu.. .anaet.a . aY'rai. .ar8d. aualloUr Am ad bet iq.olim 1% 4, ample wt. 1Z.a Use hear urYrd orti+ !W 4or111a0aa 11rv aYndwA We" we Oralaad tr4tasr11u00' Wla~tywell oahlllh waidWt2 ofywk vr y_ltiro allhodoa almdatd aama0atloa fw1021Lrt.yai 3.2 (or e01iqlBtl 123 2r/b iwPO~ 11wuti aos aoad aYednd +rpanaaa" AnywaNpl"" wawd Rtedritaywr aYwllirlnls ilrrd aud ewealpaL 13A Awptam Q11uis 17.1 QICaw1owon wa " ahorr a penY of a YIIyAar !oa q 769 am Aoat r yaaq of4l) w. 'la 417 aan pomit wnw'al' b do TIS1A union, wbilo Ow daorr iea{If0 aw)n~WS11M lerdrnlaadfsrW . fq.aW, ^ Past 50 oJ6J p. 114 Interim Report # LO-Anslysis of Fish said Clam Samples Exygen Study No.: P0001131 FxWn Proboal Number. FU001131 *oMIwa..ii Tiiaaea~~ AiiALYRGl~ . ~D b1ommR NOW u.rW.vorix4 Add A) a Vyptalim 17.7 1Wol WrtnmpR Irl urin!!OA a11aqH ~aalar da>I11W WQ. If a blank ce"ninnIMli0A Y WO hr11tr Em 04 pp. than a now Nwlc fmpli mo . a aYwr .~ a .lk. r ..aa n~ar,pe,a . 1 >Wn~Iw af owWOl i~ aai ~alAa~c~ mua Ya bawaen TOUQ% of Ilai 1oaw~ ndw, Na aand+lllw MIA oarida do waarible Umin, the a~r .nat.r .rtrrwwaw.aoqnere . 13s Ay adileri~ anslanl two" be a f4eltieq Out'- Dy wl14-0s 1%-I= 71R mg 6a wdadd !ma din wkalMtioo o! CIA eapheulIO ana Hnnwm. din OW nnww of ol6pliu aa+dari *wt vorld be =aladad so nn uowl7dK of1Y 1nW ~eA~tefaer~ win" 17.3 'l1n eanaiaas eaalRoiW (1t) hr aaNl.Uba aisvaa ji w~ew~d r-r W ia1l2 (It~ M . M) I! Wia" Varlr t" Down am Unwa. dim I~loprlnln Op rns be WW 4 NOW 1nM11anMa1 apRadon. 1ol nu ~u.~ra attr wlawnt rt .tuql~r~6ow awrdywa. 1sA a+rdao Bnw boom Mr+trwn And uaylw must am drie am than t4 % a" titlla nnorl*d Ann, llnbatiarthm MA mwaaft riia i{mh whMn ri ra~deal waMr IYa wt nwtw nrnlyud . " GSIwiYYann 14.1 lM tla >lllar~+~ar~a ~wlelnu ~a rronl af ~FOA 6uai Aa uywL, Urwl on pnah ewli rig ua atreri am {ilnw rheeniae hraauiask /"` j raNdAylalilw[WaIllwwnpopm: 1FOA 1bu1(a&0 -QmkIts :kimmila) (1f 11rIr R9nw*~ItbnprOnnIR qWnnroaoR of tPOA bud in eWNal. M doom /!OA &nd(prb)- "wleWd* w nr-fa~ .M~kaa ~nnt wrw+r.a a>,oa. uwar,~. 14a !W u*w 60" rIA IIM nnwWA At MA Prhr lo aceootioe, am tr btloa+.t,il" 4e aalslw Ow Praaa wooMy. b-rcw- [ra+ .ht.annaa+raf - NW*bnadl.a..ralarrlj w131w .aa9a aura ,,ao yIriYC i Pap J/ of as Exygen Research Page 114 of 132 000357 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No.: POOO1131 Sxypa homcol N. umber P0001131 ANALYTiCAL NISlHOD 11N&edN=b~r : W0011i3 1rldr.+drArdrTa W omrrl. Yrwa .uww.r.rtyrw oq .w~ ou+rolo AdlMFOA) h lw.a AWJydal rwNo$ WOW . , amo swus Mt1WwaltDAw ilwC~ PA 16101 A"MVW Dr. ~` w~3r3e~- .- s.Wlo.l l..+a, LoWlll"Mw~s . .~aSzt.ro~ orr Dar hd Tyr : 7 Exygen Research . Page 11 S of 132 00(1358 p. 116 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No . : P0001131 /'' ^ Pacyssa Protoeol Number: P0001131 . itpla"wr" I~w~rNUrrwwirrs Ah =~~~'e 6trmai Lirrh7l.CMMa ) in 1 1~0 lUvOs !00l1h,ttsrirdiaei .tie~le~i hrOuiWaIla~r89~aakP~waaeerrwx s~r~o!y,wnrio. aI~~aeaRrlorrcouirL~lePnd~d G~k.<o~an.l~Y.priothpauswra,qW 4 a widwn Mw zA drAcr 11 A6rqseMl~qaWi1eeWy pwrIton . ]3 ~pIiar Ld 6ahi 1r~lia0 ry shamioal ihr piapw sdny -- 7A ~ lwria .r" 3,) Alluns :O1an.MqbLrrbouao. 3.3 $"Ow iYaY be "rAn rxlrwioq. ltfx 60 iom =M* in a ieep 7taorrur o1 ~fa .ifb &7 iea, aGee ufa mmpla. te eaaninen rd Iww aor k Sawr rrap svwedW p al1Lr for oa6oa diwa4l- lobrradoa tral rd Ih" Iw wApk In ACM aerye msO time d' irdria AuarYly,lf fitw is r Iw"afirrt~a~moru of arqk (-Nw than ~~aaalaasahYad . 7 .7 Slwjtr OWWWO I ow0iwa~VAN lr pa~ oiAd k Of 9ep0og PLM The uh PIOUL 4A R~yaaradSMrladr 4.1 111,rr-F1PLCvvh 4.2 Nalbrol-IDGC pib 43 AealorYdia-HfLC/p/r 4.4 Amraahr ArYn-A .Ca. LyrlOwie <d -hiMawtwdeAdd-sWa.AWA 5.0 kerwrt ad Bqu}aut 5.1 A fa~6 faA- Iqai1 +laarnrpqY rraNa of Mr*ei a0 is t [91Y~Ya Kd/prd w'~ i r~d~le w1Yw fr~ialra~i1e af i~jrelifl~ S-?Ou rLtwr~ ta atrlrr INr i~ara~rr(LCJ~I, 92 A4vv$nf*odWMvswA@ft -- -~-----S.3 . Ai*,lforllrlarrerpahralrde~os0.00001 ay" 7A 7!rl.IfyouNr~ol~rap7lwraanvlAysplba. 7! 1ld.dfVoulA~artdtqratia ! .f Di~rwrk~irpi/Iel(30"100aL.100"30hi.L 17 PaRNP-WALM but" 32 7 ri.rbr Ftl1.C dN1dL i;;7, 7; /^ PaN 53 o/6J Exygen Research Page 116 of 132 000359 Interim Report #10-Analysis of Fish~and Clam Samples p. 117 Exygen,Sdrdy No.: P0001131 Exyrnlhotoco1 Nuomber : POODi131 urs .r w.rr.roawa+ AK"rnCAL MX"M _ .-e(Tdrsndrole Aeid (TPOA) in Sm@H IlsrI llnsby [ .CMWM 5 Dfqo~w~~. l.910 (1Od100D VL ad lp "IO91W). ~i9r dhpoapietip~- s,u "~> sa : 2ftVWWAk==uw. s.ls 7ilY.iiWilr. s.u wrw,.~w.Ow- 6.0 MON-WoOk srft- 6.1 AmWy"CetrsROOM Rr Rq .mrSMWAO.2.100 150MM SP ~ttlos.oatt~o? bs t~npurrc WC 4s N~Yfle /1~ IM : : dMAanodup Aaew in wwa 64 lwldw 11m(W )AgboM L! fltzfwwlwlw; Flow Raft ao tt ~s Wjobs1d u a ss o.s a9 ts 7s o.s 32."Z! s! fS 7s 9s 7s a3 6~ f.7 1Pmiailu~uo~`do:fTrWrItI tA! my!-(nalnrbuelisomaeedwueAteeraLeVrauaeahauaSmo r1 .y. as R,wT+.~: -s .b,rr.. lw~o.w.~"w.dao~IdMrPlLCk4w1r".Mrr .aw r" ~pd~. .rr~owN wr~w meraa a 7.9 bs1rA3 e"uw 7.1 1(dar ilwiwr~syW~dw1OlY mad~. m~tndni f13-r 3Lf Nz for 71r Yew eeedkbru rn babe r a Vfda Lid arW be OwW fri aav to ~W K9Na vjww rq..t .r+ r P. as 34 ofss Exygen Resemh Page 117 of 132 0003F0 p. 118 Interim, Report #10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 ExyPe Protocol Nwlber: POODI 131 ^ aaw " Ow`w w,"ftiL 1'I bIR771Op ~~ef u~~ Atrtwi.rlaa MrIY Llva by LGK8A13 wrwnrir,.vooonts 1 in u oaI roko.a(MmOm u womerim i.l.t 2 .16 ..~~i.. wlr k .rr a pnwnd Iry Wliea o . t s6 a ut AWnpft rs4lew Idy b, p ~w4 9.0 91oYrd taI wlt~ !.1 9~atlri ~IOdrA~w1Ylcdanleladoa O.1.1 1a'/ep0r1i a1g"oI*MOmALUdde(aavol!a-HIaOOOBIlyr1paYLAqo}f P ledMdObOyWwuats1r0i0aMtIL10rAmtah rarlWrlba ,u.a[.t.cl~falOr. 9,1,2 A tA phlL >be~eriaawia4wdlFOJ1 Lprpwdbr b~nyaj I rL ofthe SOD IWmL nobllal to aQonl relwne of 100wGb 4otAerl aa lussL LwsIIa l-U s0.1 r,rm1.aifiation.hrir or rraA hpa~+e.e by bNa,Me III mt.att)w LO roYmiw to a Wt web= of 100 wil6 slhwl in .IUS .r.r.oew~L..w k..L OA A ZW " ad bIIIAoIAlso OohIlOrm w IW r1aa1 ia . w6lpara a oppoadlllldy 1'C u0 a "ida !r a aabma padot of 6 nonth Oval tw61eclpWodm. 2.11 itrlnOt.SllYedalshdar 431 LClMWaalikadon Ma0w*an - rad In maqirol via diluNoa afOa 00.1 pAaL hd/nlioa aallllfr Mr R1bw1Y~ SS a ppwal srpbr atbtbiW aallnnaniaw mny ho I ad r owdaL CANWOWN dFdoa" Vdr 17ird b Find LYaemanlim UI to S1..oo IIL; ';2 7A loo 2.0 lo loo I .o to loo o.s lo ttoo 44 MINNIM& Is 3254RL LZIAlrnaow "woft bonkr ' 4,U lad 2'C la f'C, ap w ~Gt mollIM Alqtelq rolww~ aad cearseemliwe of Aadae& nry he piepwd rc awid . ry,Ar+ Pose 33 of 01 p. 119 Interim Report #10-Analysis of Fish and Clam Samples Exygen Sf.udy No.: POOO1131 SsywPmlocolNlvrber: P0001131 rolwlrwr~f MAW .ICVrreAL fa11nwn 1Ewmel I1rRbyLCAI$IMS wtsl rw.aw w~ouias I (lfoA) in Cata1D 30.11, " aawih "tip 10.1' 1101h Iald of rsylr oatraolel (Q'llWy 30 x Iw$ wus iacWls r Is" am y,ateel~ Wad e1 two awwwd seamoh RRil-O r lm, . eeaoo~oreaepdieooboJepiello .othlosadwal 4MOVOY Of *A blank '10.2 Yepi:onww fr IIaK me Ieu .+Qr earlioro s spItw wu Yo lpooifioa , ,oklYop!libwowNwylonlKlAiolRdeet $1 .0 11.1 Its SfJ ~+'11A = 1 8 alwapb iabtt0mLpolyloaqylw eenpi lob" (~onify+w ~plapo q~ ad ~c 1W11. Nole 00 alnpme +rr'~iu d liver May be s~oie~of d~P~ioo On rqbalr wdle6lo Jhr+w . M4 ralw so to oavVh bra Ilnivoia,o 9(W arL 91=r 1w= do mowf~e~~-dpow~ba1o !4m Into a Is al, ' na bofa~moeulteYe dddb!r-.10 nm[w+eo am +wniaoetion alnlw. 1 i.f ~yeiO~We y-70i0sP ir ~S mi~r. ' n.r Doonl ft owlwawe[ YOO s JO mb fl+uAlo omuiAfe ours oW aid 3! aiL ot.rar. ceawiaa to Co 8tE orrNiwo (t s f d.l by lowiaf to ea. wtAuiul ~llnwl Yf! od.ofWUC ~sar (-3 ir~eeel . l3o aa le~ eelwae nr~ dry ' I1"! Lal tio erpleeaeo~d0leaed CN !TE eralya Dweud eWn. 00-1 11.14 13Y MO +l wl. of r11r+oL (.bpeot 2 wL Of oluslo fnp e pWekd IS sLl~41'l+~T' umN!W Ow(fisal ~aW *21R4 11.11 NrprerylwodaEeloowolooyL+f'JMOIW" 124 13 .1 1. `Ow MOW ofwaY etofu; aa.4b w0 bAiloO saup6e inw the eI IrL A WIielYea r4eArif annl preoe0e a0 follow al 1;.1 llpirdo ol arloiodly lo ot ]wn tw er a~aw eoouna+ltoa It+'ols esat tie IeoloOef Is ftaYlyial r- Iis Aa em, .. eteor'bnriaa r .dw~lo male Iwek~eoe w urc bqiminf nrl r do of 9(a wq* Ls . iwod" am h idaep.aa rehv.ea ..e4' S-lu emtpbl. AM w a11wolivs an wwir0 w! of wlibtiti0a yteofrrd6 may hr Wood n Ow Ovgaio! af a on dlmwee by oelibruiaa wand" L~Irpruf w~0'!-t0 o~1w lto aoaoat 1w a wowd oa oir~Wo~Oq. u+ ei4R emy calibration prdaOL epuwt 6e "e bat YW hot iajwaiaa in e 17 .4 tJr~inr am" ewyw rr SroYmiww 1Jnr oaadarl owr aft yaaalrl bras eob% by liewesolrrdae odaf S& wu#A"eflwk erw ey. se+ 001, Page 56 01-63 Exygtin Research Page 119 of 132 00(1 .3F2 p. 120 Interim Report #I 0-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 r I- ExypnProtxoS Ntanber:pppp1131 LqPDYM" ~Nu Afrr~lLJrtr 1YL~6 1fAN IhA*w VOOM7IS nas allkalba aaa6~d owio~dan rWas btwq,pm 3.3 (or paWahncF abaa qwM iT! fi~pU ~eer alarl4 aK rsowd ae0rd rwyAny n"lea dw wewi wwkrd eayrww Uw~bs Mhardtfiw4 wd ~wniyud. 11 .0 AOeapuw Orilei~ Ii.l t1MoMOOPr MW +m a PO! o[ a da&ar we 81369 amu iee a paem 4( 413 ~ MW 113 rw jalrt aaaapm66 w ft lFOA Won, wMle ihe Iw~Yrles (700 awr) nynMpu IM kw otaAan d"da. 131 lidMed 1Yett >to1 aat aeeYir rAOA r brnk VaYV bwt Yr LOQ. if a "Mk omwor "OA a bwY rear " 10 W& "a a MW bnk ~pk ahwl bot,ldr6 wd M arlsae re be w-awwwL 113 IrewOw otaowd A!o ad am* Win mrt Ib inwaw 70.1 Ift at Ass irw veIw. tf a Pont apb 61h id" do aaalp7aYle qmia . Ib wifw at of Me61r ilwll ba n.Mdd. Any maCiz 1Wite awddr 10176% AYd" b erIbmd %y Ota wlm p wlamiw If rsae4aedqe b WMEr" IsA AV oWkVfU rerdM Iho1 a a a aaWioA awll~ by "Wag e.h lt%V 9aor '[a4 rrlr 1a soYY6 !m as WerYYea at "a aWMtroa am. Hwanr, 6@ ktd rir at eM ala drdrdr Ow aork b aohdsd MW autMowl 30% *(*A "a riwlw4falr6aab ijaolal . 13.! 'lb nlwlaYn nsMeLn (it} hr aYrwofwi arm /rrawd mm b am pt' 40AM it a1lnfle4 mrtr OII euWAi & .w Iiea am AWvjdM ar~nln~~rtaafa~ryiar ~W Cre a~rW Iya~~ ~ Mr 13.6 POW= do= ba~ srMW n6 ww01r ow aal "iR mom ftn 3 4!i wWfr u waqYod nr. uwUruoa isa Ad aaewh tAl~ IinN rGqin .aYrlPlerl m " r Or re arl b rweaiyul. 14.4 O.Iwdri.r 14,11 K 4~ 6olwwlq pa~elo~ Io orad~r lb wow~ of M~D+~ exnd pn qrmL, OrW as pot ra) aly w alr6ad a- (liwV rhrwioa iiaapuwnl !aswWhria Mr 1Wrm w!~ peormw r~DA lb.d f.6rdJ-Q46kao~iaY6oit1 s ~ r all0r.c baier d." i>f~ 6~alarbywYaY IYr IYrI volwr wr Q14rW . ifnaow~ay. AN" &@W- 10 P606 .17 0111. Pap37 ofd] Interim Report # 10-Analysis of Fish and Clam Samples Exygen Study No.: P0001131 EygasDrorooolNumber P0001131 fi 1"1 !k wqlw knttd wU1 ~:~ d!l~OA ~irr a sraodon . wr drl~lorip+~aatwlwsd~~.a~oo.vwy . lKwwY(W " ~toplardn~ri 8~'al"} " awY ,w~Wur~ la omuyi(xyn~L)] , IBD ndlh~/016(4raa.} 11.3 1H~ 1~ lplkwlns ~ aamrws ir rnwu of lFOA !wd in ryyml w i70A Uai0 (pp>r} ~ VsWU+wwIWt(R) Exygen Research s.vv .n Age.i8 of 65 Page 121 of 132 000364 Interim Report #10-Analysis of Fish and Clam Samples Exygcn Study No.: POOUI 131 B"aP~o~xnl Nueiber: PM 1131 ANALY77CAL W1= bf4elltwmlw, Y'OOOI Hf M&" dAzNk*wr &8 INwsYNw dPorpwnwwik Aek (rI0A)1q 6aa NYwwd fw~ ly LpMqM AWyYWTinYKPdpp^. luylwBwr+ob 3Wi Rrrrrb Driw 8u4 {Wkx& PA 16W1 A/pVwasr- POW ^aaoo~ T Tab" IwM* W-M1. )hypo Rwwiah islular DMA Exygen Research Tomft.: 7 Paye 39 0163 Page 122 of 132 000365 p. 123 Intcrim Report . #10-Analysis of Fish and Clam Samples Exygen Study No. : P0001131 I', BxySea Prutaooi Numbat POODI 131 ~.ir~a ~ua.~wr .voaoius 1(awd 11~ tiY Lr1MMrfS )aSm t .0 SO" 11b romi irlo bi uqbrd ArtM IwUliw rd Qu~Nnfw orp~dl~oiwc~uwk si1 by M# 1whm Lihi1 pswrmeby ewW to s sire~m Mom fPOotDmwia Dnuw(LMw9a Mdl mwrW wveL 20 iWw 2.1 AM" sbwirAYYQd~ef'FWdm Li Cowuk Iu ~Piw AISD! bdMs liwdli~ say dWWAW Au vmp,r s.ky pwwqa~, SA iOy1s 1twWdMM" 1.1 A1lwwtmLetIWwoqblxaYrti~n . 7.2 NO sWp41~~wwbV Y seem ms ~ raplw. Howww. 0amri rrom rn~1r ~t u~rd feea~lwrtytl~t Is ioar Iq~u~idas ius. S.S SwW!r eeUrlloa powlww wAI be MP8dad i 69 woD1iK Ow Ior we Iq Rr"rM W 91wdw8 4.1 WNw-IVLCffilh ss y($d=wl-lIpLC VoA 4.!- Awadh3W-ilLCVUW 4.4 1lssedunAMuu-ACASjrrywtOeO 0 hrMrmerricAdi-2*sA10riR SA inuAMr rdl"lpwt 3.! A L40 VuI IirWm AaOaYM4pp oIPOW of pirnpi4 iq w 2 a1wrM ~0 ~ ~ vakfle wl~ Y0wlu arr*w of ifijGow* S-2ol> pl. eoa~~ew! u ~ tnlw 14r ~eawr (LCM~MS) . !J A~wlwtoodYaawaral:P40tiA+pMOanrdqVMduW@& S.7 sw A SO .~t .1a4 W.rurwL~sI~SpPYi.~r~y.fb~. w.doi~saM0.w0u00a0!.s. aa lS .taa4errr- r . .=Mhoubw Ss !.4 Irid.LMwaiu-fwfoiwrnwucawa.tww. aui.niaaaoa.c> e.i 2rl.elnrlli.cvWYie 110 Mr . iaaIM Nr, .d MOO yi,% ,r* e*arrti elp. . s.!! wwnaRratvoioa{1plCUSraaQalepL s.12 6rsnwyi.aiwiwd 5.13 v.+.M ry. :or, Pw 60 0J'61 Interim Report #10-Analysis of Fish and Clam Seumples p. 124 ----- s Exygen Study Na.: P0081131 Exyjer Pra6ocol Number pOppl 131 wapar."Iet AY4Ai .YflC4L INiTHOIa bc Ow 16111111 swm by LC41SAts unlr N,rw Voooi7w llaid 1 in Sre~U 5.14 ~ CoaoiAi'o~04~l-13 oLt .afqlmieii ti mLMyPnlY~uleo Y]000 iprn . 6 .0 t;ltrmropaphis=ywru s.l A..1Y" coiW rleelesw uO .yrM seuMea3, :.1 .. 10 mm . sN (7l:t p70b~10917Q +62 T~~ f0'C G] lh0i1~ l7w(A) : i d:! Amidum Aeo1ime A Wow 8A IyaliOWRr(B)i 11, ml 8 .! dradirot lteIa~ lirUM Ya OA if IA bf LO 25 u00s.0 =ass Flow Rw ~ lmilmw 0.3 35' 0.) 7is7 00.3s 35 oa Y.6 lyulfn voluaa b PL (m be Yasrom+to . . much os s0 pLl 0 .7 G~+~Iw: P .icAw.-a.at~pRdawaYawn. iA Dws7"i~su -riiewr '1L! Am 4o~diMaww IYmahd osu pdll ed pity bo a0rnpl ie ars ee e~inW 0a 1QtC iyrm 7A A(EMt3ymsem 7.1 ~aloeao~aar t~rew lt A.+., .orae~, 4u ~ sav ~ o: IM olow eoMiliarr m IrwdM r o Said aW say be dmpd in order io mpiwau>r m!YS 90a i." lrperhdlelifbs lt .l llalAeVae i.l .l 3 w)l wr0oir roMr (e NOW io rn/oeod by addft0.1l4 0 of ooeiW~ ~ p 1000 mLof w~pr. ANmsAorelueKtnylrpapwv0. hr fuf I rAr. ar yr6s Exygen Research Page 124 of 132 D Interim Report #10-Analysis of Fish and Clam Samples p. 125 Exygen S.tudy;No .:; P0001131 ^ Avft Hzy=eu hoEoool Number: P0001. 131 l4mriWrt GlAullmli" r A .YALY'ItiCAL MICTBQD Ywwl Samtir tc+MSW lw640Wn"w vae01+1 " w in I 9A 9t"o6sd 1"rl~llilll~ !.1 9tndu~'SbddPbosw~ti~alehqiee 9.1.1 ppn" delta "o0lfioi at+100 RfilaL "!9lOA b7+asigldnx 10 iaa . , a! rlyreal rlrl/Id (onwWbr ~lnity) r~d 4ilaw ID 100 nl wit", , 1 wilwlin a123-at LDPL book. 9.i .! A l .0 ILg&nI . Aeifwiw wlWpw afPI<OA Is J "7 , , mal. af t1r l010 pjUL "olrlfo" b s lirl voladw of 190 wish ortlrna . . la " It! aL LDlBlodL 0613 A 0.1 yglaL 9lrdleaiw "oGei "s olI1+OA !" a r'sad tiy bdr4*I O al, "CI6s 1A~L lalaliaq 1" " IWI "elaw d106 wilw aW~noi in a t2f ~Ll~iB bcW". 9.1s Tlr A"dcwd beIRenUr " shrlrw w b i" Amid is a orMprow A do do vipmanklum Its Soo"dc4a"="&" 21 UMAL%S 016MO AMIMM MV"WW in MOmmol. VA dil9figo of IFA " WOL hordsmadmin mowdem. : .12 The hbwhgis t"" examb: addlilwal oooommWoom mey be In"0Mebt -eg6momwotperag- uism, Vow link MAN-L) OW DOW41169 tau Rest COWWWW" jUjgL- W IA 0"0 l00 1.0 .6A . 10 100 O's :'a a loa" 01 0 .1 i" rc,o Pc,ya lo dLm"ae">". 177-wL UWWW MVw-,,*A1Ii bottled '4.Y." AMMAN ralwnw d o "oomoaplr Of Wnloda WAIF be PC" a+ WWWL Iao Mmas"lur 10.1 Z"IY YdeY at avollw "mAo"" (47low 76 or NO am islub au low r" MOWN on" d hw ta11ww1 *010,016 11114,11111140 a know p"aalaRri0lw{In101wY1mom) 10 YOlly p1 ""IelICa) nwvRy fur Ow home, la7 1bQYlplpwq" 91r &W Ml 1 "a0lwty dapliudK and Wim wilt h" Md6ad ial6t Quality on"" pm Or44 rJmaL r4l.o .r Age62 oj63 Exygcn Research Page 125 of 132 000368 p. 126 Interim Report #10-Analysis of Fish and Clam Samples Faxygen Study No.: POOO1131 A--?Aft Exyse.Protocol Nm* .: roao1131 R1pOlO1w1 MEO W AKAL 1!w YWALM IArrreltwrs yUnAwa NrAd N-rYe Vi0ei1lL AM (RF T in 1 1-6 t~le estixioo n . : Ile111es 1 .L .rmple+ro .loataar~+Py~~lw~~eeatrauly ::an" wabee Rd er .Ix *ft MM do ,6eao,e ,rolem,ee of esrn, roe~ u /q .Vi., .n ae no* W. ewtwib fur an. ls W raremealeee+ebawe[7DaiI . Cylfqidr lua vavsbr-1 .t.dr. HA lYrelr t .L of N . momp1e ,ft . fspeeettr pkem Ire e ls euL 21 .5 MA! maL aleeAOnheUe 111111Aeke Ipr " ,4p mlenln ee e vdr .eeelor 8idsr. U-6 dea7Y,e we "Ow el )IOOmm 1<k-3 mlaw111. 11 .7 1Peerll !e er~iwiort bno . M ML aiuyanfik eeimmilige tube aed ed0 7s ML oewYr. In NOW" (116 4 ML Its Ooa~dea ~e C4e mi.1 ti91 pee~R lo meqaeol lbllelnily!l .LefN!l .Cwels("2dWWw} Aoolleteelrnu,~undry 11 .9 }.etQllw~liaeawllfaadCp!>'!er`f~ye, DYadelere. 1 1-M Illele rM -f wi et iebrd. Cow 7 o), of ehWe nAa a yadue,ai 13 ioil.Veb'PbPP~ 'IS amb@(ftel ve" se- 2 a,r.l la.u A.dy-rrp6r .u.lUeeaahr.qt .G1+N4e5. au cwanowsphy 18.1 Ljeoc k e.. ..not .r .rh eY.rA frrpls me biseea .ryk We +,e LCAaIlfO ayenr . A awbtwfiae eqindd iayt pnoede and 1bAaw- eN 1I$ Mod"efldOAMR~/~p awRleiaelwd iuvvv ".& et 11Y13M Ot ~ele 00aCaUtlltlop 1evele 12.) Aa ollie edafadi4ntiea mtrlAltds mwt be fre4del el aw byierieg and r doe erd oft ervle M. sluiievb mum 6e ieeeerw+oi betwea e+rrr S-1 u rrpla As as aYeriw, a *lm we of edIbnRMe e1mArde mey re Wemi s do 1@Om*4 et e r Mowed by odlYe+rion nrqwue f~ilket~a" eN~intire de~aea mad De dm Ow eel be i*"o inIe 19.t !JK Urr d.id auiwe Ar vepduN. Ueeee MesArd eurva ue pmemet At de ww11M by IYer mpwelar r1W4 lAx wraeftorlwk em wnr eitbwft reulaC aaiaweMiw rrir4 1YtmLraw ] .7 (or e*waleeu f 9S 9eMib eeqore eliwM ao1 moved nrrrd ~paww. Aey samples do meeedeordrd uqe~ww AeaW be Oa1ladibrea al,aeeNye-e . ~:ys ;is h Page 63 q/'6! p. 127 Interim Report #1Q-Analysis of Fish and.Clam Semples Exygen Study No,: P0001131 t3cyM Poorocoi Nmiber: P=t 131 ^ 13.0 AGOWAMCI*k 13.1 (7emakwas wql Ari a pak ida au6bw ion at 16i amu ham a parest uf 41 J wu. 1b 41! ar prsal oorwr6widx a IN; tlpA aaYOe, wlwk Uir dw/i1w io (7M was) nprar` lir law ofowhw fosiaa 133 IIwh00.tW0t4 OW no aaYalo PlOA n 14wk /wnr 11ON Ilr LOQ. If a Urot onWu t!'OA xt WON ~vYr don 10 ryhn4 dm a new blank ar~k wula xWiwi ad 6r~lYe wl wus >te~ra~~ad . 133 -IQ~+wir etvatd ~~ rd swti Aih NO be bRww 7F130'M of thie lamm arhrr. II a ow6o1 WON " k ,udaida i, aoeaptdols liwis. do aeis aw d a41ne "w1d rs n-awn+elnd Any xarr6t qtks oiRaidi 70l30% dwAM k Ovals" q 6r arlyw p ixwmiss N K"awaeias u wreobL l!A Amy atiliIlir xlr4rd 6wd 1n 6a o evellotleN ouYkr Iy wi% ON Huro tdnqr 7w4 irr 1,r swladd ion 1tM odoolAmon of do cal>'brxion cum . 11hlwxr. qle Will 1WWblr' 4t alwr60a xlbOrr111Mt Wul4 be aohrle0 not mat Mind ZOfI dAr1oW ME" o(steadtrY iajraYi . l) .S 71b oondqies udMwt (it) hr ealiYelirr errvw poKaerd MW be . ip.9RZ (Rx iGlfi). 1f pBbscim lwrtol "II auhldr on liatiu. Lhen apMoprirY am saw be NEW 16 04rc Yw4aweal orwwtioe, urd thc xanlaA orlL twr'n'on of IwoY fLwW w Iaandyxw0. 13 .6 yNnou{aa *w (a+rnw anido wl rwspln mur wt drift nws u+ri 3 4% whis4 si rrlyiod wo. psawnqqw tlma drift oo" M Iimr wNeia an yrlydod m 11m 1M 0 vow be rearrlyui. 1!A Qdnlxoer 14a tr. d . imwly h.a1a.w ealeYuw d . mom orrroA rama u. p&L eaw a .,[~-~ xaal uW~ IM wwosr snne (u .wr ~loa paNeKStit /IIIMfWd by tw WINEj.ysI ptwwq r10gmA1. t"rOA AMA (+&x6) - (PJIYWL--kaggil x DF x diqda Ilaar stop D!- Laaitywhiab "xlnl wluma was bluw.0lf preewaty. Aliqaoe BOW ' 20 162 pae rmpls EAtOai vOh lmewo rrsas e6 PFOA paor b atnuio~. ow to l4lrr* ow1fMwada" ilrrag" naorwy. RsvYwf (%)~IOOd~iwdGulmW-xWy%foonliaooe_4v)(~ymL)~ a100 r+dtba0l*d{eshri .) PyrA .w POP 64 1y63 p. 128 Interim Report W10-Analysis of Fish and Clam Samples Exygen Study No.: Pt?4U 1131 BxypnProtaol Nrmber: P0001131 R~r+~A l= A~ lw6 fC~ ~a X~09AMNM WON DOw'iWalol ltrrnl 5~ly I,C11dSlMS wwe~ Mrr v~a~~r aAcid -(-P- FUA) in Small 11.] , Um$it AQmftqrllon 10 Cplvrtt IYe roount of PPOA ebmd in nWmL m !!~+ lfOA "w1(~Y) ~ ~~hL) Fxygen Research !q, tot+ pop as olds Page 128 of 132 0003 r 1 Interim Report #10-Anaiysis of Fish and Clam Samples Exygen,Study,No .: P0001131 RESEARCH 3068 imeardh DOw State Collap, PA 16lDi PMaa: E14272-1Q39 Fax: a14-231-f5M M ENQMi Arllendnw9Nxmb*r..L E:f%1RiYe dalat 4111910~ 6cypsn sudY wriae PdOE131 Cpaal ft* Hlumbar Pw1 d 1 BECIM i)An,y" Proa.dur.surrmay VaooIraO:seak)rs 9.1 2) Ve~illoallon dAnaylica! Proadure Nom 1) Add lo Ssc,ifon 9. I: Sacdon 9.1.8 . AIEamaba V104M dsbndatds may be uud 10 pr.par.aD.rn.r ooao .nadlon. ddock sokaior~tas naaary. A~blevels d roA~oala, .owuau m.r .ao ba p.pa.a. z) Law and NO :plkkrp 1r+wis Of tha Ml elpba ior aadi nwtrbc may ba aMsnd dap~dlip on sample, do awYabb for***don andbrto aovK anayla oor>antr'aliaxs aPsckd In 1M samplas. t) MqMr cmneanaiqons of foendard. nasa io be pr.parnd In ordar b spilce ih . :ampl. badla. at nlph .r I.M.Is. 2) lUaufipa shs avalabla for amall aa~_ ir nrnd liwr andsananvraaanalar ltws . .i o_ ~ on iower then On _tn~t. _ llbio Ihaa Ilah_ q~ at rownd walrr vWng listed In Ow p1+01D00l. 1lY~ F 1h! bwaltD~ woo" ready 1baD~Cd ~pRtktQ levels, nw~y valua an~otba cala~irfrd for1lra AC wr~pla. flVphaf apikhp Iww1s in tw bodies tA oaw to analrb oonoarMailona m3pectad In the walar samples. TIM L00 Is 100 nplq for a-0.1 9 safnpla d anal mernal Brar wd Is 1000 npIFN. for a 0.01 MI. sarple dmatl nwmW sarurn. Higher by*d apildrqfor ft mW sampbs will anam that: MrsGC raooywy data can be wed. " r dS Osm OWW QAU tbn+lew1al azlei lt Exygen Research . Page 129 of 132 0003'72 Interim Report #10-Analysis of Fish and Clarn Samples . Fxygen Study No . : P0401131 RESEARC H 3050 as~d~ o~ Pw~: a~~-~t-~o~ State Cottage, PA 76~Q1 Fax. b'14-231 "1Sb Amendment Number. E~hrs D~ ExyQsn Study Nunber I'ftOTOCOL AMENDMENT 031~0 PO009131 Client SWdy Nwnbar Pep~ t of t None OMO OF AMMED SECTION 1) Report ~p~ 11 d68 - . 2) TomLisle -a' pop dd 86 : PFO$ fasnviNonmonl4orad ~9 -~ S0. 1S Irnbod da~rMrl rspaak Inlrlm~l~d. ?) PFOS bansrton monllond MNY 00 be 490-.), 80. m wA! be issued lo, allow tlhe S breosiw~~rl~wqr,lk1~ x) 'itw API 4G00 LCJIYI~IIdS rys~rar dntaot to ~190 a 80 PFE33 ~n!+qlon wlthh prs.isr ~rrIw~ISy fh~n Ow 490 ~ ~ "arrllon. 1) The cwnt vwl~ be aft blrOSR~ and rnA"~ w ~maa qulddy. 2) The 4~4~ -,v 80 k Mg w be daiscwd %M ynaYr ~esldN4r,lhwsfaro, 9" ~r a... o-i.~obra~prre.~al~w . ,~rswf o.~. is , . ~.e. s-.o~.os f~~af Dft 13cy~n Q~W i~wlaw ~~ LrIWtY D,11DGQ12~bb-. : _. . ADWNWMTIYE FORM Exygen Research Page 130 of 132 000,373 ,~..,~ .-..:,~ ..._...,. p. 131 Interim Report #10-Analysis of Fish and Clam Samples Exygen Study No .: P0001131 09-20-Z905 'Ot :3ln Fro~1FSTON iDLUilAIS .+ . , T-314 F,QMb4 F-47t 3St0tStEe.cRowabm*hfDtHi"6601 phrons : a14272-1039 Fax: i1A-Z31-15i0 DEUJATION FORM - X~Proyed Spedfla bsrltGon ,. ,ftClkyiOw4rtloo . 1pale ofoaaurrsm: o6Mb Oman Peolset 0 : MM "I eiprn PralKt o : ~ NA -; , .. ~ lndudb Dayiw" !lsFa.ncr#- : ms~o~ arM8 p67~-,(,M , A-4 aINP --XA~ Pre+ocol MfOoa SOP x Oaw uw NA M" Nawanok mWens: NA LOP* : u12s1J1.4M conhlnsr4O, : ~ CMoo-0s Lot Il : -NA-- Th~ e p~ wwW~ dwM 90 w,kol tnd brtNfedccnirol ssntplMof nchnraUbc wYl be snalys+ed; hows+ror. MW dam wssnot obahed FM wasutpd sOw oontrol for he allsly* of thswasix ctsm " Csusr. T_ PnpsraUon ~ MsWb . ' No nepndm improl on Vft WMy. - htsmso - CUM RseFuest X MW . Dwi~ . ; I tntiestiQaeor Clu"AssYf"nCt , ' v nom sa n 4 v . $1~~ snt ye DSfOt $ponsOl Nlpltl~5fll~NfK v sta Dsls M1fe . Exygen Research *. Page 131 of 132 60 3 7# Interim Report #I Q-Analysis of Fish and Clam Samples Eaygen Study No. : Pfl001131 00-i0-2001 02 :3lpe FrorWF5110lI SOLUTIOqS + T-304 P.014/OD4 h43T , , RESEARCH 985r3 Restwdl Qri+re Phane: 81~1 "27I-1Q39 Sta~e Colkg~l, PA 16M Fax: a14"231-1580 t~IfIATIt~W FORM 1 1 x Pro~t ~pavi4stion ;_._ Fsc~iA+ Devlakfon , Qaee at Ooagmanee: ,,?~7~a11 a"~O+n Prod 0: P7eola1laa Draiation 0 '. CfOent ProJelct * : 14A liwlt~rSnoe it : oS`- aT +.~-.~-. : (11"d1-is l meows w5~~7 OUP X ou+ ot~a Now Pboacat tr~ 202.~o s.~atcn 5" ' War.boo+~ nRr.rw,o.: w4 luWhod X SGF' laq(e+ 0! t .~,.~ cbnbeiner0 : _~ Lot1k : NA 1trxmarr et CJa~ArHans SL Z714 (3D7G _ - ~ ~ - ! (B Toklefrs) v~io1wr1 tha ~Otplla!!Dn dab~ 0fQ~11,31~d. but Rt:544 (folnwn) uud to M" $1.4114rorpkld an 0080604. iLZ114 W= uand to stiaithd~al AO~tware prsp,r~d foeThe 60 s~cfionfrom t?1Z71~F Qa+oitph 01~7A5, C~. ~ prrparstlan ~, qnalysis ~ Insttimaet r, Cllset ~,~, ~ anepatlva KnpiC! orl 1M ~y. Tolu~na wtit usrd only as aaotveat for4heg~'a Pro~r~n~ J. blmev y+l8klfiatnsl~ wrhich is 'the oonEing Sgent was not axpied. DaY4~iC~t 94riied . :! 9ludy " ~~ ~ItYlWursries ~ ,,lt ~ rims f ~~,nn~' t lb.t~"+i t~a0, ,~ -- ...~--.... SponsorRaprsiandflw D Csa SponrornMllgemfnI r!r -.-- Exygen Research Page 132 of 132 U00 :376