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p. 1 ~-~,ata6~ ~687 INTERIM REPORT #23 Analysis of Sediment Sample s STUDY TITLE Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Progra m 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: 610-701-376 1 MERIjVI REPORT COMPLETION DATE May 2, 2006 PERFORMING LABORATOR Y Exygen Research 3058 Research Drive State College, PA 1680 1 Phone : 814-272-1039 STUDY SPONSOR 3M Company 3M Building 0236-01-B-10 St. Paul, Mli 55144 Phone : 651-733-6374 PROJECT Protocol Number: P0000760 Exygen Study Number: P0000760 Total Pages : 110 p. 2 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : POO007 60 GOOD LAJBdRATURY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0000760, entitled "Analysis of Per fluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using i,C.MS/MS for the 3M Decatur Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laborato ry Practice Standards 40 CPR 792 by Exygen Research, with one exception . The laboratory control and control spikes for the direct injection and alternate SPE methods and the spiking procedures for the sur rogate were not recorded promptly at the time of extraction . .,~~ ohn Flaherty Principal Investigator Exygen Research Date Jaisimha Kesari P.E., Study Director Weston Solutions, Inc. DEE Date ~L{ Mic ae1 . Santoro Sponso Representative 3M Co pany Date Exygen Research Page 2 of 110 p. 3 Interim Report #23 - Analysis of Sediment Samples Exygen Study No .: P000 0760 QUALITY ASSURANCE STATEMEN T Exygen Research's Quality Assurance Unit reviewed Exygen Study Number P0000760, entitled, "Analysis of Perfluorooctanoic Acid (PFdA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Moriitoting 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 . Date Reported to Date Reported to Date Principal Exygen Date Reported to Phase Insp~ Investig~tor Management Study Director 3I . Final Raw Data 5/2/06 512/06 512106 5/2/06 Review and Interim Analytical Report Review Lydi offer Date Tec ical I.,ead, Quality Ass anae Unit '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 110 p. 4 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : PW076 0 CERTIFICATION OF AUTHENTICITY This interim report, for Exygen Study Number P0000760, is a true and complete representation of the raw data . Submitted by: Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-103 4 Principal Investigator, Exygen : / '()~ Z~~d Flaherty Vice Pre siden t Exygen Researc h - s~pG Date Exygen Research Facility Management : 1 AR gwb"f Richard zini Presiden t Exygen R earc h Date Study Direc r, Weston Solutions, Inc . QmhA l Jaisirnha esari P.E_, DEE Dat Weston Solutions, Inc . Sponsor Representative, 3M Company: 441~ &It~- Michael . Santoro Director f Regulato ry Affairs Ub Date Exygen Research Page 4 of 110 .r p. 5 Interim Report #23 - Analysis of Sediment Samples Exygen Study No .: P0000760 STUDY IDENTIFICATI ON Analysis of Perfluorooctanoic Acid (PFOA) 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: P0(}00760 EXYGEN STUDY NUMBER : P00007 64 TYPE OF STUDY: Residue SAMPLE MATRIX: Sediment TEST SUBSTANCE : Perfluorooctanoic acid (PFOA) SPONSOR: 3M Company 3M Building 0236-0i-B-10 St. Paul, MN 55144 STUDY DIRECTOR : Jaisimha Kesari P .E., DE E Weston Solutions, Inc . 1400 Weston Way West Chester, PA 19380 STUDY MONITOR : Michael A . Santoro 3M Company 3M Building 0236-0 1 -B-14 St . Paul, MN 55144 PERFORMING LABORATORY : Exygen Research 3058 Research Drive State College, PA 168 01 ANALYTICAL PHASE Study Initiation Date: 11/05/04 TIMETABLE : Interim Analytical Start Date: 04/27/06 Interim An alytical Termination Date: 04/30/06 Interi m Report Completion Date : 05/02/06 Exygen Research Page 5 of Ito p. 6 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 . PROTECT 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 Title John Flaherty Vice President Karen Risha Scientist Paul Connolly Technical Lead-I,CJMS Christine Edwards Technician Mark Ammerman Sample Custodia n Amy Sheehan Associate Scientist Brittany Kravets Technician Scott Crain Technicia n Frances Crespi Technician Devon Ingrain Technician Christa Gallant Technician Exygen Research Page 6 of 110 p. 7 Interim Repo rt #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 TABLE OF CONTENTS Page TITLE PAGE .. . . . . .. . . . . . . . . . . . .. . . .. .. . ... . . . . . . . .. . . . . .. . . .. . . . . . . . . .. .. . . . . . . . .. . . . . . . .. . . . . . .. . . ... . . . . . . . . . . . . .. . . . . .. . . . . . . .I GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .2 QUALITY ASSURANCE STATEMENT . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..3 CERTIFICATION OF AUTHENTICITY . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..4 STUDY IDENTIFICATION . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . .5 PROJECT PERSONNEL. . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . . . . . . . .. . . . . . . . . . .. . . .. . .. . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 6 TABLE OF CONTENTS . . . . . . .. . .. . . . . . .. . . . . . . . . . . . . .. . .. . . . . . . . . . . . .. . . . . . . .. . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..7 LIST OF TABLES . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..8 LIST OF FIGURES . . . . . . . . .. . .. . .. . . . . . . . . . . . . . . . . . . . . . .. .. . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . .. . . . . . . .9 LIST OF APPENDICES . . . .. . . . . . . . . . . . . . . . .. . . . . . .. . . . . . .. . . .. . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . . . . .10 1 .0 SUMMARY . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . .11 2 .0 OBJECTIVE . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . .. . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . .11 3 .0 INTRODUCTION . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . .. . . . . . . . . . .. . .. . .12 4 .0 ANALYTICAL TEST SAMPLES . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .12 5 .0 REFERENCE MATERIAL . . . . . . .. . . . . .. . . . . . . . . . . .. . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . . . .12 6 .0 DESCRIPTION OF ANALYTICAL METHOD . . . . . . . . . . .. . . . . . .. . . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . ., .1 3 6 .1 Extraction Procedure For Sediment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . .. . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .13 6 .2 Direct Inject Extraction Procedure For Sediment . . . . . . . . . . .. . . .. . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . .14 6 .3 Additional SPE Extraction Procedure For Sediment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .14 6 .4 Percent Solids Procedure For Sediment . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . .. . .14 6 .5 Preparation of Standards and Fo rtification Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .14 6 .6 Chromatography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .16 6 .7 Instrument Sensitivi ty . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . .16 6 .8 Description of LC/MS/MS Instrument and Operating Conditions . .. . . . . . . . . . . . . . . . . . . . .. . .16 6 .9 Quantitation and Example Calculation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . . . . . . . .1 7 7 .0 EXPERIMENTAL DESIGN . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . .. . . . . .. . . . . . . .. . . . . . . . . . . . . . . .. . . . . . . . . . . . . .19 8 .0 RESULTS . . . . . . . . . . .. . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . .19 9 .0 CONCLUSIONS . .. . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . .20 10 .0 RETENTION OF DATA AND SAMPLES . . . . . . . . . . . . . . . .. . . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . .20 Exygen Re search Page 7 of 110 p. 8 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P 0000 760 LIST OF TABLES Page Table I. Summary of PFOA in Sediment Samples ;. . . . . . . . . . . .. . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . .22 Table II. Summary of PFOA in Direct Injection Sediment Samples . . . . . . . . . . . . . . . . . . . . . .. . . . . .23 Table liT. Summary of PFOA in SPE Extracted Sediment Samples . . . .. . . . . . . . . . . . . . . . . . . . . . . . . .24 Table IV . Matrix Spike Recovery of PFCA in Sediment Samples . . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . .25 Table V . Matrix Spike Recovery of PFOA in Direct Injection Sediment Samples . . . .. . . 26 _ _ ~. . Table VI. Matrix Spike Recovery of PFOA in SPE Extracted Sediment Samples . . . . . . . . .27 Table VII. Surrogate Spike Recovery of 13C PFOA in Sediment Samples . . . . . . . . . . . . . . . . . . . . . .28 Table VIII ., Surrogate Spike Recovery of 13C PFOA in Direct Injection Sediment Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . . . . . . . . . . . .. . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 Table IX . Surrogate Spike Recovery of 13C PFOA in SPE Extracted Sediment Samples . . . . . . . . . . . . . . . . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .30 Table X . Total Percent Solids in Sediment Samples . . . . .. . . . . . . . . .. . . . . . . . . . . . . . . . . : . . . . . . . . . .. . . . . . . . . .32 Exygen Rescamh Page 8 of 110 p. 9 Interim Report #23 -- Analysis of Sediment Samples Exygen Study No. : P0000760 LIST OF FIGURES Figure 1 . Pawe Typical Calibration Curve for PFOA in Methanol . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . . .33 Figure 2 . Extracted Standards of PFOA in Methanol, 25 ng/L and 50 ng(L , Respectively... . . ............. ....... ..... . ........ ........... .......... . ... . .. ........... ... ......34 Figure 3. PFOA in Reagent Blank, 0.4 nglmL Fortified Reagent Spk A , and 4.0 ng1mL Fortified Reagent Spk B, Respectively ... .... ..... .......... . ... ...... ...35 Figure 4 . Chromatogram Representing a Sediment Sample Analyzed for PFOA (Exygen ID: CO t 72892, Data Set : 042806D) .. . ...... . .. . . ... ... ... . . .. . .... .. ........ . .. ... .36 Figure 5 . Typical Calibration Curve for t3C PFOA in Methanol . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . .37 Figure 6 . Extracted Standards of 13C PFOA in Methanol, 25 ngJL and 50 ng1L, Respectively. . . . . . . . .. . . . . . . . .. . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3 8 Figure 7. 13C PFOA in Reagent Blank, 0.4 ng/mL Fortified Reagent Spk A, and 4.0 ng/mL Fortified Reagent Spk B, Respectively ......... .................. ... .....39 Figure 8 . Chromatogram Representing a Sediment Sample Analyzed for 13C PFOA (Exygen ID- C0172892, Data Set: 042806D) .. ... . ... .. . . .. .... .... ... ... ..40 Exygen Research Page 9 of 110 P . 10 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : PQ00076 0 LIST OF APPENDICES Page Appendix A Study Protocol P0000760 (Exygen Study No . P0000760) with Analytical Method V0001782 : "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by 1,ClMSlMS", and Protocol Amendments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . .41 Exygen Research Page 10 of 110 P. 11 Interim Report #23 - Analysis of Sediment Samples Exygen Study No .: P0000760 1 .0 SUMMARY Exygen Research extracted and analyzed sediment samples for the determination of perfluorooctanoic acid (PFOA) according to Exygen Method' 0001782 (Appendix A) . The limit of quantitation for PFOA in sediment was 2 .0 ng/g. The standard sediment method (V00017$2) was originally used to extract all of the samples . Use of this method yielded poor spiking recoveries for PFOA . Because of this, a direct injection method (Section 6.2) was used, which also yielded poor recoveries . Finally, an alternative SPE column extraction ( Section 6 .3) was used to analyze for PFOA and 13C PFOA. Analytical results for the analysis of PFOA in sediment samples extracted according to the method based on dry weight are summarized in Table I . Analytical results for the analysis of PFOA in sediment samples by direct injection, based on dry weight, are summarized in Table II. Analytical results for the analysis of PFOA in sediment samples by alternative SPE extraction, based on dry weight, are summarized in Table III . The overall average percent recovery standard deviation for PFOA in sediment samples based on wet weight was 73 16% . Fortification recoveries for the analysis of PFOA in sediment samples are summarized in Table IV . Fortification recoveries for the analysis of PFOA in direct injection sediment samples are summarized in Table V . Fortification recoveries for the analysis of PFOA in SPE extracted sediment samples are summarized in Table VI. The average percent recovery standard deviation for t'C PFOA in sediment samples based on wet weight was 97 27% . Fortification recoveries for 13C PFOA in sediment samples based on wet weight are summarized in Table VII . Fortification recoveries for 13C PFOA in direct injection sediment sam~les based on wet weight are summarized in Table VIII. Fortification recoveries for 1 C PFOA in SpE extracted sediment samples based on wet weight are summarized in Table IX . The total percent solids for sediment samples are detailed in Table X. 2.0 OBJECTIVE The objective of the analytical part of this study was to determine levels of perfluorooctanoic acid (PFOA) in sediment according to Protocol P0000760 ( Appendix A) . Exygen Research Page 11 of 110 p . 12 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : POppp760 3.0 INTRODUCTIO N This report details the results of the analysis for the determination of PFOA in sediment using the analytical methods entitled, "V0001782 : Metbod of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by LCl11+CS/MS . " The study was initiated on November 05, 2004, when the study director signed protocol number PW?0760. The analytical start date for this interim report was April 27, 2006 and the analytical termination date for this interim report was April 30, 2006. 4.0 ANALYTICAL TEST SAMPLES Three sediment samples (Exygen ID : C0172892--C0172894) were received on wet ice on April 22, 2006 from Tim Frinak at Weston Solutions, Inc . The samples were logged in by Exygen personnel and placed in re frigerated 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 MATERIA L The analytical standard, PFOA, was purc hased from Oakwood Products, Inc . and was received at Exygen on March 17, 2005 . The surrogate spiking standard, 13C labeled per#luorooctanoic acid (13C PFOA SP0004184), was received at Exygen on April 15, 2004 from the 3M Company. The available information for the reference materials is listed below. PFOA was stored arnbient and "C PFOA was stored frozen . Compound Exy en ventrY No . Lot # Purity f%) Expiration Date PFOA SP0005444 203 99 03/31/07 13C PFOA SP0004184 3507-195 97 03/29/0 9 The molecular structure of PFOA is given below- PFOA Chemical Name : Per fluorooctanoic acid Molecular Weight: 41 4 Transitions Monitored: 413 -a 369 (for quantification) and 413 -~ 219 (for confirmation) Structure : Exygen Research Page 12 of 110 z p . 13 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 F F F F F F0 OH FF F F F F F 13C PFO A Chemical Name: l,2-13C perfluorooctanoic acid Molecular Weight: 416 Transition Monitored: 415 -> 370 Structure : 44II3 F F F +FkOF F C +--13 11 C ~OH FFFF F 6.0 DESCRIPTION OF ANALYTICAL METHOD The analytical method "V00017$2 : Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by LC/N4S/MS" was used for the sediment samples in this study. 6.1 Extraction Procedure For Sediment Before the samples were weighed for the extraction, they were mixed thoroughly by vigorously sbaking the container . A 5 gram portion of sediment was weighed into a fifty milliliter centrifuge tube for the extraction . After fortification of appropriate samples, 35 mL of 1% acetic acid in water was added to the samples . The samples were vortexed and allowed to shake on a wrist action shaker for --60 minutes . The samples were centrifuged for -20 minutes at -3000 rpm. The supernatant was then loaded onto a C13 SPE cartridge conditioned with 10 mL of methanol and 20 mL of water. The eluate was discarded . Twenty milliliters of methanol was added 'to the sediment samples left in the centrifuge tube . The samples were vortexed and allowed to shake on a wrist action shaker for another 30 minutes . The samples were centrifuged again for -20 minutes at -3000 rpm . The supernatant was then loaded onto the same C18 SPE cartridge . The eluate was collected into a 500 mL Nalgene Bottle . The column was washed with 4 tnL of methanol . The wash was collected in the same bottle as the cluate . Approximately two Exygen Research Page 13 of 110 p . 14 Interim Report #23 -- Analysis of Sediment Samples Exygen Study No . : P 00 00760 hundred milliliters of water was added to the bo ttles. The samples were mixed by shaking and loaded onto another Ctg SPE cart ri dge conditioned with 10 mL of methanol and 20 mL of water. The eluate was discarded. Approximately five milliliters of methanol was added to the cartridge . Five milliliters of etuate was collected into a graduated 15 mL polypropylene centrifuge tube. Each sample was analyzed by LCfMSfMS electrospray. 6.2 Direct Inject Extraction Procedure For Sedimen t Before the samples were weighed for the extraction, they were mixed thoroughly by vigorously shaking the container. A one-grain portion of sediment was weighed into a 15-milliliter centrifuge tube for the extraction. Ten milliliters of 1% acetic acid in methanol was added to each sample . The samples were then shaken by h and, vort exed, and sonicated for thirty minutes . The samples were then centri fuged for - 10 minutes at -3000 rpm . Each sample was analyzed by LCIMS/IviS electrospray. 6.3 Additional SPE Extr action Procedure For Sedimen t The samples that were prepared in 1% acetic acid for the direct injection method were used for this extracti on . Five milliliters of each sample was aliquoted into a 50-mL polypropylene centri fuge tube and the volume was taken to 40 mL with water . The samples were then centrifuged for - 10 minutes at -3000 rpm. The supernatant was then loaded onto a C , s SPE cartridge conditioned with 10 mL of methanol and 5 mL of water . The eluate was discarded . Approximately five milliliters of methanol was added to the cartridge . Five milliliters of eluate was collected into a graduated 15 mL polypropylene centrifuge tube. Each sample was analyzed by LClMSIMS electrospray. 6.4 Percent Solids Procedure For Sedimen t Percent solids were determined using the procedure indicated in Exygen method V0000427 . Approximately 20 grams of sample was weighed into a pan . The weight of the sample plus the pan was recorded . The samples were then dried in an oven ove rnight at 104 t 2C. Then the samples were transferred to a dessicator and allowed to cool for -15 minutes . Each sample was then weighed again, including the weight of the pan . The percent solid for each sample was then calculated. See Table X for percent solids results . 6.5 Preparation of Standards and Fortification Solution s A mixed stock standard solution of PFOA and 13C PFOA was prepared at a concentration of 1000 g/naL by dissolving 100 mg of each of the standards (corrected for purity and Exygen Research Page 14 of 110 p . 15 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000 760 salt content) in 100 mL of methanol . From this solution, the following fortification standards were prepared : Cone . of Fort Final Final Conc . of Stock or Fort. Volume Volume Fortification Std . Solution (mL) (ML) (g/ML) 1000 10 100 100 100 10 100 10 10 10 100 1.0 10 100 0.1 10 100 ` of PFOA and 13C PFOA 1 .0 0 .1 0.01 A stock solution of only "C PFOA was also prepared at a concentration of 100 g/rnL by dissolving 10 mg the standard (corrected for purity and salt content) in 100 mL of methanol . From this solution, the following fortification standards were prepared : Conc. of . Fort Final Final Cone. of Stock or Fort . Volume Volume Fortification Std. Solution (ML) (ML) (g,(m,L) (~~) 1 100 10 100 10 10 10 100 1 .0 10 100 ` of "C PFO A 1 .0 0.1 A set of non-extracted calibration standards containing PFOA and 13C PFOA was prepared in methanol, as specified in Exygen method V0001782 . The following concentrations were prepared Cone . of Fort Fort Final Final Conc . of or Calibration Volume Volume Calibration Std . Solution (ML) (ML) (ng/mL) 100 1 .0 10 100 0.5 10 100 0.2 10 10 1 .0 10 5 .0 1 .0 10 2 .0 1 .0 10 of PFOA and 13C PFOA 10 5 .0 2.0 1 .0 0 .5 0 .2 Exygen Research Page 15 of 110 p . 16 Interim Report #23 - Analysis of Sedimer., Samples Exygen Study No . : P000076 0 The stan dards at final concentrations of 10, 5 .0, 2 .0, 1 .0, 0 .5 and 0 .2 ng/mL were used for calibration . Extracted calibration standards were prepared following method V0001780 . The stock standard solution and all fort ifi cation and calibration standard solutions were stored in a re frigerator (4 2C) when not in use . Documentation of standard preparation is located in the raw data package associated with this interim report. 6.6 Chromatography Quanti fication of PFOA was accomplished by LC/MS/MS electrospray. The retention time of PFOA was - 11 .1 min . Peaks above the LOD were not detected in any of the reagent blank samples corresponding to the analyte retention time . 6.7 Instrument Sensitivity The smallest standard amount injected during the chromatographic run had a concentra tion of 0 .2 ng/mL of PFOA. 6.8 Description of LCIMS/A1S Instrument and Operating Conditions Instrument: API 4000 Biomolecular Mass Analyzer Interface : Turbo Ion Spray Liquid Introduc ti on Interface Computer: DELL OptiPiex GX400 Software : Windows NT, Analyst 1 .4 . 1 HPLC : Hewlett Packard (HP) Series 1 ; 00 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Them Fluophase RP, 50 mm x 2 .1 mm Column Temp . : - ,30 C Injection Vol. : 15 } L Mobile Phase (A) : 2 mM Ammonium Acetate in water Mobile Phase (B): Methano l Time min %A l B 0 .0 65 35 1 .0 65 35 8 .0 25 75 10.0 25 75 11 .0 65 35 18 .0 65 3 5 Exygen Researcb Page 16 of 110 p . 17 Interim Report #23 -- Analysis of Sediment Samples Exygen Study No . : P0000760 Total run time : - 18 min Flow Rate: 0 .3 mlJmin Ions monitored : Approximate Anal yte Mode Transition Retention Tim Monitore d (Mipl PFOA negative 413-+369 - 11 .1 min. PFOA Confirm Ion negative 413 a 219 -11 . 1 min. 13C PFOA negative 415-+370 -11. 1 min. 6.9 Quantitation and Example Calc ulation PFOA concentrations are quantitated in nanogram of PFOA per milliliter of extract and then converted to nanogram per gram . The PFOA concentrations were quantitated in nanogram of PFOA per liter for Set #3 (Set 042806D) . Fifteen microliters of sample or calibration standard were injected into the LC/MS/MS. The peak area was measured and the standard curve was generated (using llx fit weighted linear regression) by Analyst software using seven concentrations of standards . The concentration was determined from the equations below . Please note that the equations in this section are presented in a different order than the equations in the method (V0001782), but this has no effect on the final calculations . Equation I calculated the amount of analyte found (in ng/L, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program . Equation 1- Analyte found (ng1L) - (Peak area - intereepD x DF Slope Where : DF = Dilution Factor, factor by which the final volume was diluted, if necessary . For samples fortified with known amounts of PFOA and 13C PFOA prior to extraction, Equation 2 was used to convert the amount of PFOA found in ng/L to ng/g (ppb) . Equation 2: PFOA found (ppb) jPFOA found (nSU x SPE volume extracted ] [sample aliquot volume x (sample weight ! direct inject sample volume)] Exygen Research Page 17 of 110 p . 18 Interim Report #23 -- Analysis of Sediment Samples Exygen Study No . : P0000760 Equation 3 was used to calculate the percent recovery . Equation 3 : Recovery (%) = {anal.yte found (nalg, wet weight) - analyte in control jng[g_wet weiht}) amount added (ng/g, wet weight ) x 100/4 Note: For the PFOA recovery calculation, the "control" is the unspiked aliquot of the primary field sample . Equation 4 was then used to calculate the amount of PFOA found in ppb based on dry weight. JEQuatign 4 : PFOA found (ppb) dry weight = PFOA found (ppb) x[ 100% / total solids(%)] An example of a calculation using an actual sample follows : Sediment sample Exygen ID C0172892 Spk D (Set : 042806D), fortified at 4 ng/mL with PFOA where : peak area = 236588 intercept = 4630 slope 420 dilution factor = 100 ng/g PFOA added (fort level) = 4000 amt in corresponding sample (ng/g) - 586 SPE volume extracted (L) = 0 .04 sample aliquot volume (mL) = 5 sample weight (g) - 1 direct inject sample volume (mL) = 10 total solids (%) = 66 .54 From equation 1 : Analyte found (ng/L) = j236588 - 46301 x 100 420 = 55200 ng/L From equation 3 : PFOA found (ppb) = (55200 ng/L x 0.04 L) [SrtiLx(lg/lOmL)] = 4420 ppb From equation 3 : % Recovery = L4420 n9/g,_ 586 ng/g) x 100% 4000 ng/g = 96% Exygen Research Page 18 of 110 P . 19 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 From equation 4 : PFOA found (ppb) dry weight = 4416 ppb x(I 00% / 66 .54%) = 6640 ppb NOTE: This value may be slightly different than that of the raw data due to rounding . 7.0 EXPERIMENTAL DESIGN 13C PFOA was used as a surrogate for all the samples . 13C PFOA was added to the sediment samples in the laboratory after the samples were weighed for extraction . For sediment samples designated as laboratory matrix spikes, PFOA was also added at a known concentration to the samples in the laboratory after the samples were weighed for extraction. The sediment samples were extracted in one set . The set included one reagent blank and two reagent blanks fortified at known concentrations . The set contained three sediment samples . For each sample, two laboratory matrix spikes and a duplicate were extracted. 8.0 RESULTS Analytical results for the analysis of PFOA in sediment samples based on dry weight are summarized in Table I . . Analytical results for the analysis of PFOA. in sediment samples by direct injection, based on dry weight, are summarized in Table H . Analytical results for the analysis of PFOA in sediment samples by alternative SPE extraction, based on d ry weight, are summarized in Table M . The overall average percent recovery standard deviation for PFOA in sediment samples based on wet weight was 73 16% . Fortification recoveries for the analysis of PFOA in sediment samples are summarized in Table IV . Fortification recoveries for the analysis of PFOA in direct injection sediment samples are summarized in Table V . Fortification recoveries for the analysis of PFOA in SPE extracted sediment samples are summarized in Table VI . The average percent recovery standard deviation for 13C PFOA in sediment samples based on wet weight was 97 27% . Fortification recoveries for13C PFOA in sediment samples based on wet weight are summarized in Table VII. . Fortification recoveries for 13C PFOA in direct injection sediment samples based 'on wet 'weight are summarized in Table VIII . Fortification recoveries for 13C PFOA in SPE extracted sediment samples based on wet weight are summarized in Table IX . The total percent solids for sediment sample's are detailed in Table X. Exygen Research Page 19 of 110 p . 20 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 9.0 CONCLUSIONS The sediment samples were successfully ex tr acted and analyzed for PFOA using an alternative SPE method, which yielded acceptable QC data. 10.0 RETENTION OF DATA AND 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 interim 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 4() CFR 792 . Exygen Research Page 20 of 11 0 p . 21 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P004076 0 TABLE S Exygen Research Page 21 of 110 p . 22 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table 1. Summary of PFOA In Sediment Sample s FacY9en ID C6ent Ansiyls Found (ppb, np/4) Dty Weight Assoaxed C8 Acid PFOA Accuracy g~nA~ 1p Psri7uorooctanoic Acid (~y. %) C0172892 DALSO-9PP41-040000 NR NR C0172892 Rep DALSD-BPPOt-0-0000' NR N R C0172893 DAL-SD-BPP02-0-0000 NR NR C0172893 Rep DAL-SD-BPP02-0-0000` NR NR C017289d DALSO-BPP03-0-0000 NR N R C0172894 Rep DAL-SD-8PP03-0-0000' NR NR 'Laboratory Duplicate NR = Not reported (kie to qualify control result failures . See Table 11 for m-anslysis results. Exygen Research Page 22 of 110 p . 23 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table 11. Summary of PFOA in Direct Injection Sediment Samples Exygen ID Analyie Found (ppb , ny9) Dry Weight Client CS Acid PFpA sample tD Petfluorvoctonoic Acid Assessed Accuracy (+1. V COMM DAF.-SD-6PP01-0-0000 NR C0172892 Rep DAL-SD-BPP01-0-O000` NR NR NR C0172843 DAL-SD-BPP02-0-O 000 NR NR C0172893 Rep DnL .-SD-BPP02- 0-p000' NR NR C0172894 DAL-SD-BPP03-0-000a NR CO172894 Rep DAL-Sp-6PPp8- 0.0qpp' NR NR NR 'Laboratory Duplicate NR t Not reported due to quality control result failures. See Table III for n" natyeis results . Exygtn Research Page 23 of 110 p . 24 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P00076() Table III . Summary of PFOA in SPE Extracted Sediment Samples ~Y9~n ID - An: " Found Imp. nft) Dry wetqM assas w CNart CO Acid PFOA q=x*cy $amp L* ID YM1luorooetanoit Acid t+ f- %) C0172882 DAL-SD-BPPU1-0-0000 E81 30 C0172592 Rep DALSD-BPP01-0-0000 g4g 3 0 C0,72893 DALsD.BPP02-0-0000 927 30 C0172893 Rep DAL-SD-BPP02-0-0000* an 30 C0172694 DALSO-8PP03-0-0000 2390 3 0 C0172894 Rep DAL-SDBPP03-0-0000 2380 30 M.abWabry C1upYCel e Exygen Research Page 24 of 110 p . 25 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : POOOO760 Table IV . Matrix Spike Recovery of PFOA in Sediment Samples Sample QMglon CO Aad PFOA Amount Arnt Found Amoun t Spiked in Sample Racovsrsd Reoovery (21& (Vtj wet tK wet ' t 9L p/U.SD-0PP0140-00D0 pcw 72wQ 81 k 0. 4 ooppee0 w) DAL-SO-BPpot-00000 (C0/72!!T 8pk B, 4ooG ppti "s) 400 NR NR NR 4000 NR NR NR DALSD-BPP024000 0 {COt 7240 epk G. 40 ppr, Spiky DAL-SD-6PP02-0-000 0 " '+2nsspk K uooppnspiky 400 NR NR MR 4000 NR NR NR DAL-SD-BPP03-0-0000 tcw?zew aok J. 4oo ppu aa k.) DALSD-sPPos.o-aooo (Ca172H14 at* K. 40G0 PDti 400 NR NR NR Spike) 4000 NR NR NR AwrW : NR Standard Owl"am MR 'Sample residue emee t8: the spiking Iwel sipnoieA ntly (3x spiking bval}; Uraroloro, an aeetrats recovery vsk* cannot be calculated. NR = Akri reported doe, to quality conkipl result aikxes. See Table V for no-anoJysis htsulti. Note- Since this starrqlly table, shows rounded rosWts, recovery values may very sUghtly from t he vawas in the raw data. Exygen Research Page 25 of 110 p . 26 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000 7 60 Table V. Matrix Spike Recovery of PFOA in Direct Injection Sediment Samples C8 Acid PF4R Amount Arnt Found Amount 5empb Spiked In Sample Recovered ROOOVWY Descxi iton we' wai t inwo) wet we 96 flAL-SD48PP01-0-000 0 {CO 177002 spR P. roou oPb sWke) DAL-Stl-BPP01-0-000() (cotraoz Sqc E, 40ow ppb tN++ka) 4000 NR NR 40000 NR NR NR NR DALSD-sPP02-"W D tpa+nws epk ti, 4M rwb sprrsl DAL-8D-8PP02-4-0000 (COtt2at1 SO H. 408ob ppb 4000 NR 3pdkN 40000 NR NR NR NR NR DAL-SDBPP03-0 0000 lcwnssa Salt J, 40oo ppb sWNr.! 4000 NR IyR NR DAL-SD-BPP03-0-000 0 (C0172804 8pAK,40oooppf.813k0) 40000 NR NR NR Average : NR SYandaed Dav4aUon : NR 'Sample resfdue swcoeeds the spOCinq level signifs;anUy (3x ePkirp bvel):lherelore, an aocurate recovery value cannot be caWals(i NR a Not reported due to quality oantoi result failures. See TOW YI for re-anslysis rosWta . Note: Since this summery table shows rounded results, recovery values may very slightly *wn the values in the raw data. Exygen Research Page 26 of 110 p . 27 Interim Report #23 - Analysis of Sediment Samples Exygesz Study No . : P0000760 Table VI. Matrix Spike Recovery of PFOA in SPE Extracted Sediment Samples C8 Acid PFOA Amount Amt Fourd Amount Sample Spiked in Sample Recovered Recovery Des ' tion R ~ ~ VOW91A ~ DAL-8D-BPP01-0-000 0 tco17211102 spk q. Iow nplp Z;plky 4000 589 4420 DAt.-S0-BPP41 -0-0000 (C01T2!lZ .tlpk E. 40CM nft *Pik*) 40000 586 25800 96 83 DAL-SD-$M2-0-0000 tcarn+a spk 3.4oeo n 9 y apuoa 4000 504 388p 84 DAL-SD-BpP02-0-0000 iCOt tttu spk N. aoroo nrq spuui 40000 504 25100 61 DAL-SD-BPP03-0-000 0 J , 7204 so 1 DAL-SD-3PP030-000 0 tCOt72394 so x, 4 0 M WO 3pucq 4000 1080 4140 77 40000 1080 23200 55 Average : 73 Standard D rvlaNon : 1 6 NOW Since this summary tapls shows rounded results . ncovwry values may vary slightly frora ths VOhM In the raw date. 'Exygen Research Page 27 of 110 p . 28 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table VII. Surrogate Spike Recovery of'3C PFOA in Sediment Samples "C-PFOA Amount Amoun t Exygenn Sample Spiked Recove red Recovery ID Description 09/9) wet weigrx N (ngt~ 3 C0172892 DAL-SD-BPP01-4-0000 4 NR NR C0172892 Rep DALSD-8PPpt-0-0000 4 NR NR C0172892 Spk C DAL-SDBPP01-0-0000 4 NR NR C0172892 Spk 0 DAL-SD-BPP01-0-Q000 400 NR NR C0172892 Spk E DAL-SD-BPP01-0-0000 4000 NR N R C0172893 DAL-SD-BPP02-0-0000 4 NR NR C0172893 Rep DAL-SD-BPP02-0-0000 4 "NR NR C0172893 Spk F DAL-SD-BPP02-0-0000 4 NR NR C0172893 Spit G DAL-SD-BPP02-0-0000 400` NR NR C0172893 Spk H DAL-SD-3PP02-0-0000 4000 NR N R C8172894 DAL-SD-BPP03-0-0000 4 NR NR C0172894 Rep DAL-SD-BPP03-0-0000 4 NR NR C0172894 Spk I DAL-SD-BPP03-0-0000 4 NR NR C0172894 Spk J DAL-SD-BPP03-0-0000 400 NR NR C0172894 Spk K DAL-SD-BPP03-0-0000 4000 NR N R Ave" : NR Standard Deviation: NR NR 5 Not reported due to quality control result faElures . See Table VIII for ne-analysis recuNs , Nota : Sums this summary table shows rounded results, recovery valuer. may vary sN9hNy from the values in the raw data . Exygen Research Page 28 Of 110 p . 29 Interim Report #23 - Analysis of Sediment Samples Fxygen Study No. : P0000760 Table VIII . Surrogate Spike Recovery of "C PFOA in Direct Injectio n Sediment Samples Exygen ID Sample Description . "C-PFOA Amount Amount Spiked Recovered Recovery (nW9) Wet welprx t~) {~A ) C0172892 DAL-SD-BPP01-0-0000 40 NR NR C0172892 Rep DAL-SD-BPP01-0-0000 40 NR NR C0t72892 Spk C DAL-SD-BPP010-0000 40 NR NR C0172892 Spk D DAL-SD-BPP01-0-OW 4000 NR NR C0172892 Spk E DAL-SD-BPP01-0-0000 40000 NR NR C0172893 DAL-SD-BPP02-0OM 40 NR NR C0172893 Rep DAL-SD-BPPD2-0-0000 40 NR NR C0172893 Spk F DAL-SD-BPP02-00000 40 NR NR C0172893 Spk G DALSD-BPP02-0-0000 4000 NR NR C0172893 Spk H DAL-SD-BPP02-0-0000 40000 NR N R C0172894 DAL-SD-t3PP03-0-0000 40 NR NR C0172894 Rep DAL-SD-BPP03-00000 40 NR NR C0172894 Spk I DAL-SD-BPP03-0-0000 40 NR NR C0172894 Spk J DAL-SD-BPP03-0-0000 4000 NR NR C0172894 Spk K DAL-SD-BPP03-0-0000 40000 NR N R Average : NR Standard Deviation ; N R MR = Not reported due to quality control result failures . See Table IX tor re-analysis results . No4e: Since this summary table shows rounded results. recovery valuer may vary slightly from the values In the raw data , Ezygen Research Page 29 of 110 p . 30 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table IX. Surrogate Spike Recovery of 13C PFOA in SPE Extracted Sediment Samples Exyqen ID .~~~. uGPFO A omoum Amax9 Sample Spic*d Rseove trd Ro pprery 04>tcriplion inp+9) Wet We iqht !'~) (aC+9) 001 72892 0AL-SD-BPP01-0-0000 40 52.0 C0172892 Rep DAt.-8 a9PP0140D00 40 51 0 Col 72862 Spk D DAL-S D-BPPIYI -0-0000 4000 3750 C0172892 Spk 6 DAL-S0-8PP01 4-0000 40000 25800 130 128 94 as C0172893 DA4.-SD-6PP02-0-00D0 40 47 .8 120 C017289 3 Rep DAt 4D8PP020-0000 40 51 .8 129 CO 172893 Spk 0 PAL-SD-BPP02-0--0OD0 4000 33D0 88 C0172893 Spk H DAL-S 0-BPP62-0-0000 40000 25200 63 C0172894 DAL.50BPP03-0-0000 40 45.2 113 C 0172894 Rep DALS0-9PP03-0-0000 40 40.3 101 C 0172894 Spk J 0ALSD-8PP03 00000 4000 3060 77 C0172894 Spk K 0ALSD-8PP03 -0-O00p 40000 22100 55 Avenge: 97 Slsndar40eWatlen: 27 Noia. Sincs>Ais summaryr table Wawa munded sewlle, reaorery vatuea may vary slightly burn ft values In me raw cla m Exygen Research Page 30 of 110 p . 31 ink-rim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table Y. Total Percent Solids in Sediment Samples Bxypan Sample ID Descrlptbn Total Solids ('~G} C0172892 DAL-SD-BPP01-0-0000 66 .54 CD172893 DAL-SD-BPP02-0-0000 54 .37 COMM DAI-SD-BPP03-0-0000 44 .46 Exygen Research Page 31 of 110 Interim Report #23 - Analysis of Sediment Samples p . 32 Exygen Study No . : P000076 0 FIGURE S Exygen Research Page 32 of 110 p . 33 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0004760 Figure 1 . Typical Calibration Curve for PFOA in Methano l ~ oA?e06D'Sed .SP~ .rdO(IFOI~'Unesl'Represian('7JXvwl~hMnFkY~420r4469e~003Qe0 .04p3) 42lt 4.0a0 3.046 . 3AsNS 3 .4463 .20 3De5 ZBb 2Ae6 n 2.4M6 c 0 2.2e6 o ~.0s6 18e6 1 .6tl 1 .4e6 1 .2e6 t .0e6 aAe4 6.0N 4.0s4 2.0e4 OA 100 200 900 4 00 660 a00 Cenaenb ation . npyL 760 800 900 600 Facygan Research Page 33 of 110 p . 34 interim Report #23 - Analysis of Sediment Samples Exygen Study No. : I'0000760 Figure 2. Extracted Standards of PFOA in Methanol, 25 ngjL and 50 nglL, Respectively , xILYI3$N-f-f+i 10+l t5W s.rd) 4U AOil S AMR ,.+pr.2ofIiasre etlMiawm Anc 1T7:Muratr l~Y1~D~: f.1rOLiep R?: Jllafrhr 11 .01 t2nD u t0o0 SOO sOO 4DO 200 4.62,/ .70 9 .80 A.Y3 TAG` 0'43 t0 ~' ~t16s 1 2 3 4 6 E 7 8 D 1b 11 Ti.,.. , XCA428082 PFQfi (Standard) 4t3A13EDD am u Lnpl 3 of 40 hom 04Z 2808D.wiff Ana: 2G199 counts Noiyht2 .146,4003 eN RT: 11 .1 nin 12 13 14 16 ...-~...-...._J 16 17 11 XY1 2000 I5U 1000 600 DA1 . . O,pp 4A1 ..4.63 e.848 .07 e .34 1 2 3 4 a a 7 8 0 iD Tim*, inin 41 12 13 14 16 16 17 Exygen Research Page 34 of 110 p . 35 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Figure 3 . PFOA In Reagent Blank, 0 .4 ng/mL Fortified Reagent Spk A, and 4.0 nglmL Fortified Reagent Spk B, Respectively , RSryS+t ComAvl PfOA (fAntwrrr) 4ls6+J ft S - - awpN ! Nlillar M2iKQwfd +~~t M+t~baw~aU A00 0'~ 10.6T ~11 .06 0 .~ ,,1 f AS 2o0 .4fl 0 1 .027 3A .00 Jim1G S'R ~ IM .13'11 14 ~a .17 .no 1 0 It 2 3 4 6 0 7 9 fl 10 11 Ti .. ,e mis , R4 aSant Sp4 A PFOA(4C) 413A1300.0 arnu simple 10 of 40 trem 04260DDwdM Area: 302P6 etuak NOpht2 .37oOQ3 aqs AT : 11 .0 min 12 13 14 16 10 17 11.00 200 D low 2 .00 t0A0. TAB 5 .00 1 330 2 3 4 6 0 7 S O ~ Time, ww n ~ Reagent 8pk Y - PFOA ('CC) 413AflOSA amti umpln 11 st q0 Beru 0q280w .wMf kw : 2130300 "uric NtiSht :2.Ode &004aps AT: 11 .1 min 11 12 13 14 13 16 17 2.Dw4 CL 1 .oW 11 .00 00 2 3 4 0 6 7 B G 10 11 t2 13 14 1'S i~ i'7 rim. . min Exygen Research Page 35 of I 10 p . 36 Interim Report #23 -Analysis of Sediment Samples Exygen Study No. : PQ000760 Figure 4. Chromatogram Representing a Sediment Sample Analyzed for PFOA (Exygen ID : C0172892, Data Set : 042806D ) , C#lT2!!2 Pf O i ttMtxowa) 4AL 0.0t9Uaew -rNrpM 1f ~I~f Aow N~NiGt wP? /Iro :: 3dd2tee+wtr iAJpi~ 27i~+0i0Dcps RT tL1o1a 11D6 a0on 2e0o 2000 2400 2200 2000 1800 1600 1400 1200 1000 B00 000 10A1~ 400 0.06 20 0. 0 9 27 .9 69 .82 73 0 3 733.0 1 2 9 4 6 E 7 a 13.00 Q 10 41 92 13 14 10 1D 17 Tkn~, m! n Exygen Research Page 36 of 110 p . 37 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Figure 5, Typical Calibration Curve for "C PFOA in Methano l ~ 042AOdDSed.CPE.~il~13CPFCq):'Ueen'Reyaslen~'1/aPwwlpldinOZr s 40ox+0 .0010(rO .p000~ 4.D~6 4 .4664206 . +AOed ~.s .e +l.eM3 1406320 3 0 s6 Y .YeQ 2.0e6 2 .M6 zzea 'K 2Dd 16r3 , 1 .0s6 1.4e6 9 .0 .6 9a w 0.n.4 4.0a4 2.0a4 0 .0 0 100 200 300 400 600 900 700 900 000 1006 Cseeoptrrisn. a~ A Exygen Research Page 37 of 110 p . 38 _ .~ .. Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : POOU0760 Figure 6. Extracted Standards of 13C PFOA in Methanol, 25 ng/L and 50 ng/L, Respectively , .YCN21N-1- 0GPfM ~faadaMlf3 W7R~anra -*saw** 2 0 416hM PfxlY60twfl>r Anrr; JIM N+ra& NO!Yh i tarNdD eAr RT: 11.I sJu tto2 l000 eoD Ow . 7cJi 400, w o- 0 1 2 3 4 0 E 7 0 10 1 1 Tlmr<, mist ~ XC04200A2 13C tFOA (SVn4arq 41 0A1 i7AA ama sampl t 3 P143 uom 042 0 0E0_+wM Mcr. 26ED9 asuMs H~ipht2lCo~003 op R7 : 11 .1 min 12 13 M4 16 1S 17 11,00 2000 1s00 1000 E 500- 0 7R@ .40.8A5 2' 3 4 6 8 7 0 10 11 12 13 14 16 10 1T T irn~, wdn Exygen Research Page 38 of 110 p . 39 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Figure 7 . 13C PFOA in Reagent Blank, 0.4 ng/mL Fortified Reagent Spk A, and 4.0 ng/mL Fortified Reagent Spk B, Respectivel y ~ Rts puFt Castro1- f3C PibA ~tAut~e+wir) NS9+sTL0 awy wwA I e! If t4rw 4Q90i0.wi/l #raa +eot lar0d) 10 .0 Q 7]7 10A1~t0 .0i~2.0.013.37 W.06 e.e3 .0 .06 a W . 4 0 .47 2'04 288 .82. 0.4e /6 ~ 0.0 2 4 0 0 7 6 a 10 11 12 13 14 10 Tim* . mi n ~ Reipenf S* A- 13C PFDr (OC)415.0!l70.0 xnu ramFle 10 046 tram 0420000-waY Area: 27200 oou etr Neia+t2.02e+0O3 ops RT: 1111 mla .11 17e0 to 17 11A1 2>xib 1000- Time . mix ~ Reap~t Cpk B- 13C PFDA (OC) 419.DJ37o.O smu sample 1 4 of 46 fion 0a260e 6i+iff Anr 270G01 eouek Height 24 2r6 004 cps RT:11 .1 We tl Q. =A14 11D7 1 .or{ 0.0 2 3 a a e 7 9 C 1o it 1Z 13 14 /d /a 17 rkr.., air, Exygen Research Page 39 of 110 p . 40 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : PU000760 Figure 8 . Chromatogram Representing a Sediment Sample Analyzed for 13C PFOA (Exygen ID : C0172892, Data Set : 042806D) ~ CtlTM2 fi1CrfGV1(IArrMOMr)1l3ASlf'R6 "w qxrpa 21e~46~Iw~ 6f2NW.MtII rirwe : 3HlfSlcowNer hWgut 29U .000epe RT., l!! Aria 2A*4 11A7 2 .0#4 2.4t4 2.244 2,094- 1004- 1 .404- 1 .2e4 1 .O W 8000 .0 1000A 2000.0 0.0 1 2 3 9 6 0 7 B 9 10 it 12 13 Timc cn1 e 14 14 10 17 Exygen Research Page 40 of 110 p . 41 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 APPENDIX A Study Protocol P0000760 (Exygen Study No. P0000760) wit h Analytical Method and Protocol Amendments Exygen Research Page 41 of 110 p . 42 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Pxyan Pmbont M mber. pooOpTw STUDY PROTOCOL Study Title: Analysis of Periluorooctunoic Acid (PFOA) in W ater, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Progra m Exygen Protocol Number; P0000 76 0 g f~,otm~c Labosatorv Syatsor ~jmesentative Exygen Fu search Michael A. Santoro 3058 Research Drive Director of Rcgulatory Affairs State College, PA 16801 3M Building 0236-01-B-10 Phone : (814) 272-1039 St. Paul, MN 55144 Phone: (631) 733-6374 ..~ fte ! ofd5 Exygen Rescarch Page 42 of 110 p . 43 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Ex~en Pmtocd Number : D00007E U MSTRISUTIQN ; tj lafsimha Keasi, Study Direcior, Weston Solutions 2) John M . Pta}mtty. PAincipa) lnvaatigator. Exygen Reeatccki 3) Michael A . Santaro, Sponsor Raprnrantaove, 3M Comguiy 4) Eacy8 p Rase =h QuWity Assutnooe Unit PayelnJb3 Exygen Research Page 43 of 110 p . 44 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 tixyt o Pmtocut Nmnber : PtWO076p PROTOCOL APPROVAL Study Tide : Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sedimcnt, Fish . Clams, Vegetuion, Small Mammal Livers and Smatl Mammal Serum Using LGMSIMS for the 3M Decamr'.titonitaring Program Exygen Protocol Nwnber: P0000760 APPROVALS if) KAL li Jaiai ', SWdy I}irecto r Weston Solution s r- ~~~Q1 ~ ~ !I l/ b Michael A. S to, Sponsor Representative - Data 3'rf Company M . Flaherty, Principal Livastigator Dat h eExygiRsarc ~ ~~ ut -~a- ,z~, ~ ,,--*~chani A C#izzini.)WsideAt . Facility Man8 a anr.rtt Patygen Res _at n .) L Shaffer, Toetuii gsn Ruearch Qutlity A:rurance Unit Due _ . Pa~t i of6 3 Exygen Research Page 44 of 110 p . 45 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : PUOUo760 BxyREn Pr+ibtot Nurnber : P000U70o OP.. TABLE OF COMM Tt1Z8PAG8 ._. ..__-_.- ------ . ._., -. ...... . _ ..._.. .. . ~ . .... . .. . _ _. .,. ._ .__1 DL4TRIB17YION. . _ ... ..._ . ___, . . .. .. ... _ . . . ., .__ .. . ._._, ._ .. ._... .__. ...-.-. ..__2 PRO'fOCOL APPROVAL. ., ._ . .. .. .. . ._.. .. .._ .__ .._ .. ..____ .. ..__. .___ ._ .___.. ._ .-__ .. .. .___ ... . .. .._ 3 TABLE OF WW7PNIS. .. . ._ . .._ _. _ ~ . .._ .____ ___ .. . . . .. _ . .. .__. ...._ .,_ .. . .. ..__ ._, ... ._ ..4 TEST FtATSRUL. .... .. ..._. . .. .. . ... .. . . _ .. . . _ ._ _, . . . __ .._ ... . . .. .. . .. . .. ._.. . . .__3 SURROGATE FffiLD 9PIICE CWAPOUNII ____._ _ . .._ . .__ ._ ~, ..___. .. . ._. .. . .. ... ...5 OBJECTIVE _. .__. ..____. .__ ... ._. .. ..._. . ..._ _ .. . .._ .. .___ .. ._. ._ ._.__ . ._-.._.. . .._ . . .. . ..._. .. . .. . .. .. -6 TESTWGPJCiLFfY . .. ._ . _ .__ .- . _. .. . .. ... . . .. ... . . _. . .. .. .. ._. .- .. . . _ ._. _ . .. . . .. . .. .. .. .. . .. . .. . .. ..,. . .._- .d STLJDYDIRHC.RL)R.._ . ..... ... ... .. .. . _.___-___ . ... .. --. 6 3PON5OR . .. .. . ..... . .... .. . .. . .7 PRINCIPAL It1YE3TiflATOR. . .. .._ .. . .._ . __ _ ._ . ... .......,... . .. .. .. ... . . .. ..... .. . .,.... . . ., . . .... . .. .. . .. . .7 PROPOSED EXPERIMENTAL START AND TlRMINATION DATES . ... _ . .. .... . . .. ... .. .. . . ... . .. .. . .. . .. .... .. . .. . .7 fD814T7FICATIONAND7VSTIPICAt7OW OF THE TEST SYSTEM . ._ ... ._ . .__. . .. . ... .. .. ._ .. . ... .... .. . ._ ..-. . .. . 7 SAMPLE PROCI7R8MSNt. RECEIPT AND REl~Nt10N ._._. ..,. ._ .. .._..... .. .. . .. . .. . .. . .. .. . _ . .. .. .. . ._. . ..-. . .. .-8 SAMPI.6II)SNTIFICA1]ON ._ .____.._ . .. ._. .. ..... .. ... .. .._ ... .. . _._ ., . ... .. . ._ .. . .. ._,._-._ . .._ . .. . , ._ .. .. ._ .. . .. . .- .. . .. ... 8 ANALY77C',,ALPROC3=.DUREBUMMARY ._..--.,. . ..-. . .,. . . .. .. .. . .. ... . .. . .. . .. , .. .-. . .. .._ .._ .. .,, .. ..._ .,.,4 V6RIFICATION OF ANALYr7CAL PROCBDURE .. . .. .,, . .. . . ..,.. ._ . ... . . .. . .. . . ,. .. .. . ._. .._. . .. . .. .. .. . .. .. . .. 9 TvtBYHOD FOR CONTROL OF BIAS . .. . ._ .. .. .__ .. . ... . .. . __ . ..__ . .. .. .. ___ .. . .. . .--- .. J 1 STAT1iT1CAL1+f6PHODS .__... . ......._. ..-- .__ __.. .__. .. . .. ..-_ .. .. .. .. ._.. .. .. . . ._ .._ . . .------ .. .. . .- .----. .. .__ .. .{i GLP STA'fEM&NT ..- .-..... . .. .. .. . . .. .. .. .. .__ . . .. .-- .-.-_.. .-_ . .. .. ._._ .._. .. . .. .. . ... .. . .. ....- ... .. . .. .._.. . ._. ...__.. . ..._ . ..Il R .EPORT .-. ..._. .. . . _ ..- .-._... _ ... ...__ .. ._ ._ ____________ ._ . . .. .__ ..___..,. ..__ ._ .. . .._. . .. . .. .. . .. .. . .. . t i SAFETY AND HEALTx_ ...__ .._ .. _ . . .. _ . .., .. ._. ..,... .. ... .. . .. .__ . .. .. . ... .. ...... . .. .. . .. .. .. . .. 12 AMEHI}MBNTSTOPROTOOPL . .__. _ ... . .. ... . .. . . ..~_... .. .... . .. . ._ . .. ._13 DATA RECORD KEEPthKi _ . .. _ .... . ... . _ ._._ . .. . ._ . .., ,. .. . ._._ ... .__ . 13 OllALSTY ASSURANCE .. . .. . _ ,, _, .. . .. .. ....__ .___- . . ..__ ._ . ._ ..____ . .__.__. .,._.. .. . .. ... __ . .. .. . 1 4 RbTBNnOT1OPDATAATIDARCHNII4G . . ..._. ._ . ._.- .._ .. . .14 ,r Pao f of 65 Exygen-Research Page 45 of 110 p . 46 Interim Report #23 - Analysis of Sediment Samples Exygen Study No ., P0000760 E.xylva PcaWCOt NumMt: P0000760 '` IPTI'RODUCTIUN The putpoie of thi s study is to pettotm analysts fix pertluorooctanoic acid (PPOA) in water, so il , sediment, tieb. clatns, vegetation. small mammal livers and small mammal reran using LCIMSlMS for the 3M Decatur Monitoring Pmgnnn. The study will be sudited for compliance with EPA TSCA Good Laboratory Practice Standnrda 40 CFR. 792 by the Quality Awurance Unit of Exygen Research. TEST MATERLAI . The test material is pertluorooctamic a ..-id (PFOA) and was purchased from Sigma-Aldtich. PFOA Chemical Nnme: Pesffuorooctsnoi:o acid Moloculac W r* t: 41 4 Lot Number 23116HB Purity 97 .64'/. Transitions Monitored : 413 --o- 369 (for quantification) and 413 - 219 (for oonfitmation) Structure : F OH FF F F SURROGATE FIELD SPM COMPOUND The weogate tiald epildng compouod is uC labeled pcrtluornoetmwic acid (tiC PFOA) and was purchased by 3M from Perltia-Ehner Life and Analytical $CIt~01i. 'tC PFOA Chemical Nana: 1,2-13C petfluorooctam ic acid Molecular Weight: 41 6 Lot Number: 3307-195 ~,. Purity: 97% Transition Monitored : 415 -+ 370 Pegg 3 of 61 Exygrn Research Page 46 of I 10 p . 47 Interim Report #23 - Analysis of Sediment Samples Exygen Study Na .: PM764 Exy}en Prowwt Nwnbtr. tOD0076 0 OBJECTIVE The putpae of this stndy is to perform analysis for pertlaorooctmoic acid (PFFJA) in water, wil, sediWAM , fieh, cMim ver tftion, small mammal livers and small mammal mw for the 3M Dacattw Moaitoring PTov= using the curnat vasiow of the following Fxygon analytical metbodr VOW] 780. "Method Of Analysis for the Determination of Puftorooctswic Acid (PPOA) in Water by LGhdSllrlS" V000178t : "Method of Analysis *at be Ddermimtioo of Perfluomoatatwic Acid (PPOA) in Soil by LG1NS/M9" V0061982 : "Method of Analysis for the DapmfiinMiom of Petfluorooctuioic Acid (PPOA) in Sodiment by I.CiM9lMS" V0001783 : "Method of Analysis for the Detami[ntion of Pecfluoroocianoic Acid (PPOA) in Fish and Clam by I .CIM9/M S" V0001784 : "Mat6od of Analysis for the I3etetminrtioa of Perfluorooctanoic Acid (PFOA) in Vegetation by LGMSIMS " V0001785 : -Method of Analysis for the Detwnieutioa of PcrtluoroQccanou Acid (PPOA) in Small Mammal Uver by LC/MS/MS" V0001786c "Method of Analysis for the Determination of Pcrauaroortwi c Acid (PPOA) in Smell Mammal Serum by LC./MS/MS" TESFfNG FACILITY' Bacygrn Research 345E Rmamb Nye State C.ollege, PA 16g01 Phont. (814)272-103 9 STUDY DIRECTOR lasimha ICaui P.E., DEE Wttton 5oh>tion:, lec . 1400 Weston Way Weot Chester, PA 19330 Plasa : (610) 7'01-3761 Fax . (610j 701-740 1 j kesar(~weatonwlwions .c~m Pcv 6 of aS .Patygcn; Research Page 47 of 110 p . 48 Interim Report #23 -Analysis of Sediment Samples Exygen Study No . P000076 0 aYyyen Protoca xwa,bar Po00A'f6D spoNSOR REPRESENTATIVE Michael A. Santoro 3M Company Director of Replalory Affairs 3M Building 0236 -01-11 -10 St . Paul, MN $5 144 Pitone: (651) 733-6374 PRINCIPAL INVESTIGATOR John M. Flaherty Exygen Research 3058 Research hive State College, PA 16801 Phone : (814) 272-1039 john .lir}wrtyQacygcn.c+sm PR&DPOSW EXPEB3lKENTAL START AND TERMNATION DATES It is proposed that the eKtytical portion of this study be conducted from October 01, 2004 to December 31, 2005 . The actual experimental start and termination dates will be included in the final report . IDENTIFICATION AND JUSTIFICATION OF THE TEST SYSTEM The following are the test system for this study : Water (groundwater and surface wMer) Soil Sediment Fish . Clams Vegtxtion Small Mammal Liver Small Mammal Senun Tho samplw will be collated by Weston Solutions. The control samples will be purchased and prepared by the testing facility. Purehssa and processing Poyr 7 vf dS Exygen Research Page 48 of 110 p . 49 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : p{1404760 psnen Protocollii mber. P000p760 ,.~ details for the cantmi sronpks will be included in the final report la3ociated with this stody. The teet systemt wae etto'ca to iccea the environmental impact of PFOA in the Decaau. Alabama ares. SAMPLE PROt'1vaMTlT, RWSIEF''T AND RETENTIO N WateG mi . sedimmk f* ela+m, vetzCtatioa, small mammal liver and small mammal aarom mpla will be received at ExyYen directly from Weston Solutiar. The details of'ssmple peoarmaeot for this study at outlined in the 3M wodt plan entitled "Plwe 2 Wol Plan for Sampling Environmental MeW The numAat and t7pa of samples collected will vary depending availsbiSty in the fiold . The total neither of samples received arid sruslyzed for each matrix will be docuumted in the final report associated with this study. Wator, sell, and sediment samples will be used as recaved without further processing at ExYean. These sampla will be stored rafngsratad at 2C-8'C . Fish, clam, vegetation and small mammal liver samples will be processed according to the appropriate analytical method (see Appendix I) . These samples will be aimed fraaen at 5-10'C. Small mammal whole blood samples will be centrifuged in the field at the time of collection and the scrum fraction will be used for the study . Small mamnul seruu will be stored frozen It !5. -lo'C. The receipt and processing of the samples will be documented in the final report and raw data associated with the stady. SAMPLE IDENTIFICATION Prior to anRlysis, each sample will be assigned a laboratory ample mforcme qumber. The reference number will be uniq u e and will distinguish each laboratory sample that is processed thou~ the snalytiesl procedure . Chromatographic data will be idariified by the laboratory ample roremuct nocnNer. Sparple storage conditions and locations will be documented throughout the amdy. ,. . a.Se a of 6s Exygen Research Page 49 of 110 p . 50 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 Fsnea Trobcol Numher, P Opep760 ANALYTICAL PROCEDURE SUNWARY Refiuatces: V0001760: "Method of Analysis for the Cfelertnination of Porfluorooctanoic Acid (PFOA) in Water by LC/MS/M&' VJ00176 : : "Method of Analysis for the Detett_oination of Periluorooctanoic Acid (PPOA) in Soil by LC/MS/MS" Vt>t'l0t782 : "Method of Analysis for the Ddcrmination of Perfluorooctanoic Acid (PMA) in Sediment by LCIf.fSlMS" V0001783: "Method of Analysis for the Deter_ninadon of Pertluorooenuwie Acid (PPOA) in Fish and C'atna by I.GMS/hfS" VatM1784: "ivtatbod of Analysis for the Detamination of PerOuorooctanoic Acid (PPOA) in Vegetation by I.C/MS(MS" V0001785: "Method of Aralyeis for the Determination of Perfluorooetenoic Acid (PPOA) in Sma11 Mammal Liver by LG1V1StMS^ V0001786: "Method of Analysis for the Determination of Pcrfluorooctanoi c Acid (PFOA) in Small Mammal Sawn by LCJMS/MS" The above methods use analytical conditiotu capable of separating the ~ isomers of PFOA. The final report will include the isomers sumaned into total PFOA found. VERMCATIOiv OF ANALYWAL PROCEDUR E A laboratory control sample will be used for the preparation of fortified control sunploa. The tell substance Will be made into solutions as per the mdhod, and added to the matrices via a mieropipctte. For water sampling, Pxyga will supply one bottle per sample coltected . The bottles will be 500 niL precteaned Sci/Spee Premier wide mouth HDPE bottla . These boides have been routinely used for PFOA sample collection at the testing facility and have been Chown to be free ofPFOA. All containers used for water sample collection will be shipped to the maple location containing 100 ng of 13C PFOA (equivaleat to 50Q 091L in the final sample) . Sampler w'V be added to each oontaina Iu a voler-Otric fill line 01 200 mL . A field duplicate, a low field prike emd a high Eeid epflcc of each semple Will be collected . The low and high field apikea will contain PFOA as well as perfluotobvtRteaulfonate (PFBS) . perfltrav6vtanesulfoaata (PPHS), and perfluotooctstwsulfooste (PF06). These compounds We inctuded in the solutions used to spike the strrmplw. The results tor PFBS, PFHS and PFOS will. not be reported in this etrady. Pacygan Will supply one field blank (control water) and two field blank spika (cootrot water fortified with PFOA at a lo w Page 9 of QJ Exygen Research page 50 of 110 p . 51 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : Pt)O00760 ,, . .. ~ .. Exyj+n Protoeot Nuw+bez: POOOU96p and high lcvcl) for every twnry samples calleetsd. At the testing facility. each water a rApk (oxahiding fleld duplicates and field spilros) will be attracted in duplicate and will, also, be fortified at a low and high cooceattaport with PPOA and prooestod Onv& the described procedure to <btettaittc method u ctuzxy, mand to chock for bias. For soil, eediRwit, clams, and vegetation, Exygeo will supply one 500 mL pteclwmd ScilSpec Pannier rride mouth FIDPE bottle per sample collected or a zip-ad bag. All coNanatlbt gs need for sample collection will be shipped to the sample location. Samples will be added to each container or bag in the field.' At the testing facility, cub sample will be cxtractail in duplicate =4 will also be fortified a1 a knowa concentration with PFOA at both a low and high level and processed tlaro ugh the described procedure to determine method accuracy sod to check for bitr. 13C-PFOA will also be added to each esmple in the laboratory pri or so atcqyction at the level specified below . For small mammal liver, l3xygm will supply a 50 nsi. polypropylene cantriasga tuba Fot annetl mmamst sqvyn, Exygon will supply a collection kit for each sample conlaniug serum separator tubes (red (op), vacutainem noodle holders xid>,eedlet, trader pipmek and polypropylene tubes. At the testing 4cility, each liver and an= sample will be extracted in daphow and will also be fortified at a known concaNritiom with PFOA at both a low and high level and processed though the described procedure to determine method accuracy and to cheek for bias. 13C-PFOA will also be added to each sample in the laboratory pri or to extraction at the level speci fed below . Low and high leveks for each matrix are defined below, MsMx Low PF4A 1tlgb PFOA C-PFOA S 1k4% Level Splidu Level Spiking Level Water WUSIL 5000 ng/L 500 n SOD 4 ujVg 40 4fl n Sediment 4 DI/K 40 ujIg 40 n Fish IOngfS 100 ng/g 100 niVS Gluna lonwx 100 Alva 100 nxht V 10 Owl 1)OOlWZ 100 nIVE Smell Mammal Liver- iongIN Sma11lr1ammal.Scrum 10,Wl ! 00 vIlIC 100 n 100 cal. 100 ni/mL Reoowriw am unticipatsd to -be botwew 70% and 130% of the fortified kvela; however, The exact, pta"on and accuracy will be determined by the anatyds of line quatity cqnt{ol sonples described *bova A statement of accuracy will be included in the Anal repo m Prior to s suplc aalytis, a laboratory control spike mtdy will be conducted in water to )uglify the =e of 13C PPOA results to establish precision and accuracy of PFOA eemples . The fRlloNring samples are to inc prepared : Page to of is Exygen Research Page 51 of 110 p . 52 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0t00760 sxrs.A Po+oaa Number poooa760 ,-. Two convot wow blanks . Two control waha ssrttples MW at 250 ngjL with '}C PFOA Two control wata saatples fiirti&cd at 250 g!L with t ;C PFOA and at 250 aglL with PPOA Two coattol water samples fortified at 5000 nq/1, with 11C PFOA and at 5000 ag/[ . with PFOA. The above wttples are to be tattraeted and analyzed awarding to method V0001780 entitled "Method of Analysis for the Detertnination or Pe[fluorooctaswic Acid (PPOA) in Water by LC.lMS/MS . " METHQI? FOR CON'1"ROL OF BIAS Control of bin will be addressed by taking representative sub-samples from a homogeneous mixture of each ma trix from untreated control sampk:s, and by analyzing at least two levels of fortif cations. S7'AT7STICAL METHODS Statistics will be limited to than specified in the subject methods and to the calculation of average recove ria, as applicable. GLP STATEMENT All sa peds of this study ada11 be pet i.attned and reported in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 . The final report or data package (supplied to the Sponsor) sbaU contain a statement that the "study was conducted in compliance with current and applicable GLP standards and will outlins any deviations in the study from thaw slandards . This statement will be signed by the Study Director and Sponsor tteptwontative. REPORT A&aal report will be ysopued by the principal invastiguor or their designee at the axictution of the study . Th e raport will 'mefltde, but will not be limited to, the following: Paye11of6J Exygen Research Page 52 of 110 p . 53 Interim Report #23 - Analysis of Sedinwnt Samples Exygen Study No . : P0000760 Sxy{eo reotoeot tvua>ber : raoomaw ,.. ., Thc mine and address of the Study Dinxto[, Sponsor itcptescntative, and of the testinj facility. A wtemcnt of G13 compliance (any rcl'ated d=nwnution. such as cha+n-of-cuatody records, must be in the study rwor*}. The signed and dated statemont by the Exygen Research QuWity Assurance Unit tegarding dstes of study inspections and dates findings were reported to the Study Director and Managaraeaft. s A description of Ow exact analytical conditions employed in the study. if the subject method was lbllowsd rxactly. It is necpsary to include only a COPY of the analytical slasmod . Any aaodificatiom to this mAod will be incorporated into the repmt. If the method is photo-redK Ced, the project umber and pa p number must be included on each page , + Description of the iaauomeatation used sod operating conditions. All results from all sets analyzed. Control and fortified samples will be identified and the data table will include sample number and fortification level . ~` R tive Ch tpm raim ona taUgnO aofsotprteeacihntaeliach matrix, including chromxtognrna of a paadad and a control ample, and a chrwostogram at s fortificauioo level . The location of the analyte peaks will be clearly identified in all Chrormosuns, All circuautancea that may have affected the quality or integrity of the data wil l be documented in the report Location when raw data and the final report are to be arohi y od . Additions or cortsctiau to the final repoit shall be in the form of an stxnaximent signed by the Study Director. The amendment shaU clearly identify that part of the report flot is being altered and the reasons for the she Wona . The amatdrnant will be signed and dated by the Study Director and the Sponsor Rept o ntative. SAFM AND HEALTH Laboratory peasoanel will practice good anitstiom and health habits. Every tmonabte precaution shall b e taken to prevent inadvertent exposure of puaaot and the environment to the test or reference suMtance(s). P*e 12 ojdS Exygen Research Page 53 of 110 p . 54 Interim Report #23 - Analysis of Sediment Samples Exyger. Study No . : P00007 60 Exyym Ptoloco2Tknnbet : BOOOO750 AMENDMENTS TO PROTOCOL AD aig3tificaM changes to the analytical pnotoool outlined here will be expressed in wtiting, signed and dated by the Study Director and Sponsor Rapte,sonutira. Antendmmh usually will be issued prior to initiation of study plan change. Howmver, who a change is roqwin d without sufficient time for the issue of a written amendaunt, that change may be effected verbally with supporting documentation signed and dated by the Study Director and followed with a written sitfpidtnant as won as possible. in this caso, the effective daft of the written amendment will be the date of the documented change. Copies of the signed aeomdmems will be appended to all distributed study pun copies. The original amendment will be maintained with the original study phas. Any deviations fine the study plan or from the analytical method as provided will be documented and reported promptly to the Sponsor Reptacesaative. DATA RECORD KHEPlLYG Records to be maintained include the following (as approoriatc) : Sample tracking sheet(s) Sample receipt records, storage history, and chains of custod y History and. preQrxtion otstandnds (stock, fortification, calibration) Description of any modifications to the method Instrument run sheets, bench-abeets or logs Analytical data tables Ali ehmmatogt'sphic and instrumental conditions Sample extraction and analysis dates A complete listing ofstudy personnel. signatures and initiata Chronological presentation of all study correspondence Any other documentation necessary for the reconstruction of the study C h roa lI tograme- All chromatogtams will contain the following: Sample identification, 4ection date, ana+v or other indication of the area of iatereat, sad iqiecrian number oormpoadinS to the run. Additionally, foriiScWions will inctudo the amount of analyte added atxf the ample number of the sample that was fortified . Analytical standard ehvmatogratsu will addilionalty include the concentration (e .g. . 14 Yqa1-). Paj t J i Oja Exygen Research Page 54 of 110 p . 55 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Ety;en Tnrotol Numhr. P0000180 r- . As part of the documentation the following iheets will be included in each analytical at a run Sheet listing the samples to be rim in the aei, and an inatrwaent conditions sheet describing the Instrument type and operating conditiont. All applicable requiremeev br reporting of study rawlta aa per 40 CFR 792 .195. QUALITY ASSURANC E The QA Unit of Bxygtn Research w ill i iect the study at Intervals adequate to aaau+e compliance with CU's, aad will report the findin of audits to the Study Dirocoor; fiuYgeu Mw ayemeat, and the Sponsor Repreceatative. RMNTION OF DATA AND ARCHIVING AN hard copy aw data, ineludins, but not limited to, the original cbmwatograms, wor>;sbeete, oocrespondmee, and results shall be included with the data packap submitted to the Study Direclor. Then will be archived with the oriyinal study plaq ametxhttenq, fiaal n..pon, and all pcninertt information from the Sponsor. The testing facility thil keep all okcbonic raw data and any instrurnent, aiuipment, and storage lop for the period of time specified in 40 CFR 792.193. An exact copy of the materials submitted to the otudy director will also be kept at Exygon Resereb, Lxygnn will obtain permission aom the tcudy director before discarding or returning tamplee Pep* 14 Of a,1 Exygen Research Page 55 of 110 p . 56 Interim Report #23 -- Analysis of Sediment Samples Exygen Study No . : Pt?000760 GxY grn Pwowc rrwober : ?ocwa 7s0 APPENDIX I ANALYTICAL METHODS V0001790- "Method of Andysis for the Draraist:iti m of Pbrthwrooetffiwic Acid (PPOA) in Water by LCJMSIMS" V000 1 781 : "Method of Analysis for the Detamination of Perfluomoctacroic Acid (P'FOA) in Soil by LCJMSlMS " Vt)00t782: "Mcthod of Arnlyiie for the Diccanurntion of Perfluorooctmwic Acid (PFOA) in 5edirneat by LClM51MS" V0001783 : "Method of Anatyeis for the Determination of Pcrflurnxwctanoic Acid (PE'OA) in Fish and Clam by LClMS,rMS" V000178A : "Method of Analysis for the Detetrrrinadlon of Perfluorooctenoic Acid (PFOA) in Vegetation by LGMS/MS" V000t785c "Method of Analysis fox the Determination of Perfluoroocumoic Acid (PFOA) in Small Mammal Liver by LC&zms,, V0001786 : "Mdbod of Analysis for the Determination of Perfluorooctsnoi c Acid (PFOA) in Small Maaunel Serum by LC/MS/MS" Pag. t~ of6~ Exygen Research Page 56 of 110 p . 57 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Exyvca ProtOooi Muenba: Y{100076Q ~^- A1'IALY79CAL MHTHOD NwMITwWw VOOOt7lP M+iat t Y * i1 MtM Dtlr4MMa Ithdvw*ochmb Add (MA) Is Nat, by LcqALSE AaaVtieal7rdylaWW. RBAN y nwA 106i IIranb Arivs Ss QILK PA 16M 1 AlP--db!' ' +, c~ ~ w1s~~~r tar Gwi1r DAN tad:wi Gdw. LCiY, mcy9w Rr .rek ~ /j~ OM ViostMw n40pwrimM &~y~alww.c~ Tag Pm.: 7 Paps 146 o/as Exygen Research Page 57 of 110 p . 58 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 ExyEcsi Ptoaed Number. pOpDp760 S''~1 wwl+nrv wMt34o A.YALY[)CA1 MITFIOD wo .w v~ ww7r aSeiiae ~iwe "Wes otinwwoqciric Atl0 (lFpA) M wa . by L0OtiAts 1 .0 tmp TUN resod'w M M atiMMjwr 6 *s bell" rd qwMWAUa ef mjk.,mmmi, !!0 y' Ily~hrbtwuw Uqald O~esraOM1W w Nd e a andwa M. M~- Aru4m WGf~ mnv. se e.ky Lt Atwrabm v~ =61d, wypreon, 22 CWWA d appspt W e NBD7 ba!!M b&WthM My cbm,,,j far gapr ukty 1A fsqrl .qpttit~wt 3. 1 wl W a0 eL dMti wtpM lratistNa 1.7 we aatt pApa osswoM ada0 M w . mylK U itqlw !w " X8+Vwud d-10 be tl4raa o Kuilanle go toom wowKSM& 3 .4 All asfmpIsi wi be iMaw*Yiy Woo f vft. Dwq wyNd for arnnim 3 .5 Any 4rINw asapl ft Nidw em" M aaYdApO r-3000 qim Its, -S mwt. .r on q ..ra.t vow he ON assrs .iiaa 3.6 iaqls aoMo60 P~ wil M psifioA it Or avip4y pt on !er tma Pti a 4.0 1i w4wtY aad S~tiaada 4.1 War -@LClt.r 4.2 NMomnI-t1pRCa++ 4.3 Atzssarirs Ane-A.C$.lyMetCw sda AA rea.swsumi. .lCa - *pWAai4 zo 1eCnWUtrdaqmpmat 53 A 6i*j rY~wm Wpid dtmtqb& pd arable by pwWiag ur m Z wMea pu'vpN iAtlt ~ .rial~ .adtma i~et+ar apttpN of injxan~ 3-700 *Looms" *4 4niwa 14w fp"e4rwu, CUWNlh 3.7 AdtrlfebasWqlprAlYllrpUkialhfaljqtiqqyaltlj~pp~ SJ Aaw7tiw11d m acaW KtMft is O.pqOl 5.4 50 teiL 69swo 4 VNgSOpyIaN ame Gyt NDw. 5.5 1! sL dymolti MbiroNMw Dow &V Obw ss nu w i.ow.o pw .. cealoaa, wasoaa" f7 12$ iLLa?1aozow4h. .sWd m 5 2aaLdw iOlCsldkk. 3.39 DiaiorYppAlai. MO ~A~ rMpeawops. .rlo)oorc>. .t~ai~ ...w ;~~ Sep Pat Van aa t16) ICI fMerui4p . v=a~ PW I J q/'6i Exygen Research Page 58 of 110 p . 59 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 exY2ca Pnotoeol N+mbwc roooo760 ~- ~ L"~" ~rt+~rr . voonra AtMtrMAr. Msruoo ~.a~w~r tr, rm~ ~0 wMAdrRruA) a Wrrly LCAdNI/1 sa2 ara+nws . .~diHa s.u ps~w~w .r*.:osowiitayymyb ..~ .a ..rww,~.. C l AwilialOei:Plrqlre2lpGl+ldt leiwii ft tlos~Al~. 1y Oar:ustfo.as213D c2 T~rwR 3PC 6 3 U" Phw G11 : 2 Nf A=MNism Awar ia WWr 6A ffs" !l,w (s) : U *rri f.S on" lw"W. 75Y!lmlil 0.0 1 .0 I'D i0.o n s FLrRrs % A XY !o>L~1 is 1s a3 u 3s o.3 :f ls 1,3 23 63 u e .3 7s 0. 4.6 k)Oq7os Ve:rt: ISML(rap6~inw~r~/br a~ia~SlppLj, 4.7 QYMihll= PeJc Am - ralnrt O eid n4bw`m avva N Rre7f~ - 23 rrMw. ~^ Yb aMM~IWaY rw amid~d r o pdM ~d mryl~o4mpd i~ a~et b wd.i. Ow MC ryw. ao suna so" 7.1 21ods RNeMray 2i~PO~ MM eodr, wa~ilriy+l3 -+ 36i ndt. ~s Naw -WW- w isrndd ft Wade MA wrr be dapd r adr to /PWAM IM M6W qw~. IA hqnrieetOdwonu 4.1 MoYiblY- A1.1 2 wN ~eYqMi~ ~s a w~1r 'r prpr~d bq.-28i[A 1 $4 K of earw$wl memo to 1000 *L Of.0, exa.ww+rew .w a tw~es h~t 1 w~- Pa~. ia ~as Exygen Research Page 59 of 110 p . 60 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 Hxnb Ptameoi NwrA st : Poooo760 r-~ .o,r www ...wa~rw AN,WYt9CAlldlTNM Micd o[A~ria it'4a DMrwiwkn Ad! ("OA) : wwr 4y MACAO 9.e lr.A.aR.~raq0. 9.1 >It.i~lOrd?Ir1{fl ..tio.loYO .. 9.t .1 It~ra a~Y2rMlql{M-la Py4[.Ort!(1A Yt v~dtf~ kt rwY at ri~d aYOia+~ GOnNhd i1r l~ity) Na dNk le !00 nd . x~lh srOasi rs Uial. tDt1l011M . 9.1.2 AIO~AW.iWtlfadMMWii1~lfArWlirD~ObYOcinpYw d. of tlr t00 ~1 . ~olulkw b a Eaal volaoa ad tdf wi6 mrarw N s W~[ tifi iatM. 1.0 AIA~aLAeiRoliwlrlMiaoo/PtOAitpnpradphrtnCeOr'~ siotOk 101+0uL wri0w a a fiirl vaAer d 100 wia arie..a ~a .lu 1L LOrEloltM. 9,1 .1 A0.1 ya+nLfaYEsOoaao4irwafOAiapnprMDyOnspy in sLdfr 1 A M,OW . rh ooa b alml wlawr Of 100 vdlY waNrael in r11Jl U1.i DHM1 W R1J A .0010t OL 609=6= dWM a[?POA Is pArM y brltAinO l0 soi. of ft 0.1 WwL 10ktios le a tiW wprw of too wa *Arri iaa 12S PL LDM bode 9.1 .0 Tbrrir WA he6sarisu eLier at M bs wass0 in a ra6irtpa a 19pfaR6 W) A"C as Yt rNbN Qw a assi. 9vfv1 .1 6 womhs &aw dr3iD M*q.Yiea. 9.2 s ndrd Catibriw ioWaw t r 9Z1 LO'AI>tlltt! adfAsYam luYtldr rr pnqrM 's HPLC artu TM Mu tatlay MOrlydr we peameQ th CaaO U aitacti" poceN+fr. iYieiad te rOOla 94.1 Tlr Apw41t ir, trOiW aa IPW AdOfdaatl roncmVallms sur be lnOrd r wrVd. ~ Oamwoi M P605.4. Valsd Cwrrnw"d orhdOWka V~ T ,iOYOwM 4iYeWaa div. 3006 riDI i fiat-WU f6 IOi Ad YS xCl.ddyy- l (G tao ao So XfaraN7y3 u soo a uo xOMWems !Op 140 40 170 xRDwqyy ; 00 a .1W z~yy.] I 10Q'M 3Z M WN %wwMrs4 TlA mrrd aorswn tlm efOa salbnaeaWvl is a pul ti i+ + o feilid maaYiaq dr r aw a~starauW W &riy Un satrrctioa ( r fa. XC - aeaed nNb+iw vMira. hM i J. . Poge 19 of 6 1 Exygen Research Page 60 of 110 p . 61 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 ewo Pmwa r,ombe, roaamM am.,wr+ r.~ .+w.r~.rwou, .rucrncm.ssrrad Mwr .rMr,wawu~~t ..wa .~rr.mtwoea.r~.A~a~ ew~ry aLC~a+~s 1" A an rdrt wb+ix our" Now yrK LaawM etY wue act wrdAWevIa"tewil. 914 IYw A aMMd aiitw" MWrb's 1 S maI. )alyrwPyMn Mla ,~rcrs'C,sra,ww~a. 901 3 Ain.t . .oF.w .~1 owea.nlb.. et .n+~a~ ..y fe pnpr~i u .~.+w. t0A B~taA tl r lal 11w0 MtM d n"tw rsaarl (qlrMq x a I.a) aru mode r hrt so two" aatlb! GM~ 11i Yoi NH .C wow! 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M 87NOD w~o6 MrIMS~ vaoo~ ns MAW dAadb~ b br NrOwraluM dlw0~rnr-wfe Add Mrowt a airn w...isame bur"w AsYydcd rarun~lriitf : ft" snap" 3w no .Re am. 3eie CoUep. iA I6001 Mf~'M BY ~`t^r1 ~---A/~ s~Irs/rnJ Dal 7wYunl Lft*w Ep M Raw* IP`~ Yiw TniMo4 ~. ~'+1yn A~e! 2014, Pf" Ty81yN: 1 P~s ~9of6J Facygea Research Page l 0t7 of 110 p . 101 Interim Report #23 - Analysis of Sediment Samples Fxygen Study No . : P0000760 Bxnea Pioroeo) Numbar P0004160 hM+~rrN NM1otMu~lrt vaofta are, = 12"VICaATL I OHM , ., ~e;e usmai~ asr .trS --n runMvisa i .a sw This anYo/ i s a w .ybri ~. . btr I+.rtiw t.1 ynrriwria sl rrlAaboaxwa +eK Cl f1'~ Adsso~ li~i~ G4ra~roi4~7 owqlM a a arr~aq Msu s~wnwtMit D.Lrar 00WOM : mom tread . w r to stdwl t .1 AM.4s .iwwai>1b r*wrPutior. u cmoN tawawd+~utoaMa.>t .aft +arbwjw arwovwktr 1.1 At bowl aLetwotoomploftr tr.rir MO loiltwdamnplMyyrwa tmm+r.r Mwn isBn tae. 1.1 iqb eo>r-'ti M pwsi m wM be apo:iSeA to dn aotpl~iei pion fm ebw 1.0 1wrY taN SIrWtY Al WaM. 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N iAat comm, aii~ N,4/Yd1 mw la IlM Sql wA Yrl iljtaloa f11 am* wt 12A 'Jr MW MadvO auw Rr o uob4tloa LiNu AaWil cwn in pewd Orla wl,,e p liaaar Mvv aioa wiq IN .cillnlna util ak ua rwaw ca66aCw Maaerd aa.wo,daa uiss Mard.yaa 1 J (w WMn i~w ) 001 01 yala~ n 123 laqla noun "NW no ar,atl aWrd tAaa w Any amps tku ao ad ~acd n~naw lbwid Da fatMrriLitad aN nwJyaad . "pier- 00Page 61 vjd5 Exygen Research Page 104 of 110 p . 105 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 sxysb hwoooi rll,m1k : poW60 . . " wr.a~~ . r~>mewr~ r.o.+wr . wla~. MOM AuY/at wA~ As" O"A) .: . . _ Mt~d fmr by LCl1aSnlS .. . uo ~atrw t~.r ` . .17 .LCia~rur~erMo. .prcora~ .,/14wiYwvw~.w .vreti . . Ufn 4M. The M3 tar l ow be rfOA raaA wAik qs +oMi3 l~ nr..r w. a . .ral t. q.sy. ti] ~1Mdt ~w so w" IGhA t Mnit pow QA* 1M LOQ if . W~Y MMiM /!pA K Iww 1MMM an 10 siML diw t MW Link 00008 WAS bb 661160 Old 2040AMaN WAM 1W 04XMCMC U3 R .itdtMOl Wir M" 4" srsl. 6t1..7a13oxor . Yrt Lta rtLa HK . trwi OU 66 aduiL y aarpvbM tiin, o+e . ,a~iw w rtw~{r iiaY N wirYrM . Nry nrri+c 7iks wddt ao- 0" iwl/ M men" by ON wtyM a dtunilr it .enaion is +rtrrrMi 13 A Aq stWpWw au.id ft" It be rM dW arYr by rrt{ Ib H.ye iaw Took mw be wiMdd 6pe to nisLi : of do nWwrw ewv . 60 ON won" of 40VAt O MrOri4 M maW M euJ4deHow" ""tam wowt2Dfldtb W4 wwYwetmfw6 Y *I, i 133 no wlwitMw twMdW (1q IbF W1wWe arrN l~e~t s~r be i~d9i (AJ i0.lKj, if "Mali= wnb AU .tiWt fMte lime. [kn ~a}IiW M W wtt M Yita IN YjmR MW-OW ap Mlw. rA trc to~de~~r b rrnrt ttl dttt ~Il/ N wwiYsM. 174 twweiw Oaw Ir.wl rrdri W uwpiw rww wl a%A most am, l 4 1/whw* ao w tl)*A na Uat wi ft wacdriA .qoUdl:ou .+Rhin in uw7tild nwtletbnlww bowruiyssd. ' 1~.0 GkNWw l 4.1 t1wtY.filbr* tOtWoatalwWs6w mom tflPOA fwed(iu tinnL rd an P@* r* mug !t ttwdd sum (low npwiw pwwMUS/ pww0by 6t Ww Ly+a atMU+Mfpa: POA bead 4*W4 - aIdLx2L--YOwMI a DPi diquot picqr at" W~' 1Vdof Yy LYf>)11tD td1Y W~IIt MY mIWM , ttOtOtMRRY. . N14YIl1tiCpf ~ ~ . l4] Av tryl L`Iifoi ri161waiw ~oiatt ef 1FOA piw rc fuatcuae. va wLlbww6t~wrtwabaAwutvR~rwuray. Rent-7 (%) (ww .ry~~aSl o+lrauai.w.s.ttw4)I ,,tan wwtern~u ..~. . .. r-~ Pore 61 0165 Exygen Research Page 105 of 110 p . 106 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 &xraea Plorocot Nms6,er : POOOO760 Vi1~~ Yf~Mli~i WbI7M W4W AMAbrnGAL SALTROD /WiMU Dowmem W Grp n alr W s.,.l by LcnAWs ' Aa~d~i~Sn~ll ~~ 11M ~t ~~11b0~1 b otMl IIII rmmt 0FQA ~WOd M ll(/tRL la POL ~ *AM 00) IFFOA - (a (MI Mq PW lidtti ~.~ Page s[S aJ6J Exygcn Research Page 106 of 110 p . 107 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 RESEARCCHH 309 Research Drtr . State Co Isqe, PA 16901 Phone: e14-In1o3o Fax : a142311 580 MQTgMAMENQME Amendment Momber:1_ EifedM Da1s: QVIQO Exyprl3hNly Numbeq.eM= ClMd 8tudy Nmber: None --' pop t of t DESM IPTI~N OF AMENDED 69 10N 1) Anatyiioal Prooadur*9rnrwy V1i001780 9sWat 9.1 2) Var#WstJOn of May" Pioosdure AM~R 1) Add to Section Y.i : Sactlon 9 .1 .5, AMrnWs wafpMs datsndards may be used to PtiPwo aftmaM amasnGratlav of stock solutions as nsosssary. Alternate levels at AortlAcatlon soiutlor may slw be prepared. 2) Low and high apkhp levels of the ans4bs for each m .trtx may be altered depandlnp on sample size awlMbls for e*action andtor to cover wyts oanoenoatlons axpsettid In the samples. 1) H ptNr 0onomlra0ons d standarcie need b be popered In corder to spike the sample, boliie4lK hipher NMr&. 2) The sample size aYarabb for #rtMN R1wwnN Mr and U rlxfl iMYa s1riAldr than eo~ . SpBdnp at the prsde~errninad levels in to protocol " Me spiked Ox nanlraAfon bear than the dotadlon dmlt. Moo, the arrly* levels in to voter samples are aa~eded b Wooly aocosad the An}daNm~Nnad soft levels ~ the proloeol. When the *We In ihs samples yroatky wooed the spidng Iweb, an soma b reaNery value csarwt be cdoulaied for the GC sampie. HVer epiidnp Wools in the bottles wIA cover the anWyta oprxen67tlons a~s~ed in the water ternpias. W,ACt ON STUDY The 0 .0 1 LM is 100 nr. a.rnpe nplp for a ornal e 0.19 sarnpls d a,aernrawu" . sme0 merturwi War and Is 1000 nprhnL for a Higher levels of spiklnp 1br tr wsier samples wiM won that more QC recovery data can be used, 04- ~,~ . r (~ ~ D eY E:xyyan t>w+U Wview 1adau (a' . , irs~YO w+aoola~aa- _ : . . ' ~wNisrwmrErowa Exygen Research Page 107 of 11 0 p . 108 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . ., P0000760 RESt:ARCti 3058 Research Drlvs Phone: 814-272-1039 State Coik~gt, PA 16b01 Faz: 61~-231-15~0 AmerKknant Number Effadw Data Exygen Study Number PROTOCOL AMENDMENT 2 Pape / or 1 0N07l05 PQ001131 qiMt Study Number Norte 1) Report. page 1! of OS 2) Test idate+lals, pop 6 d ft PF08 trarNitiOn matlb W 480 .s 99. AMENDW 1) InsC~d of one iMnt report, krtarkn :apoft wNl be lac ed. 2) PF08 tranaMion moiNta ried may also be 499 -> 8t+. BaQNALE 1) Due to the sXoe "ive 61m of to dn6aEs, kiEe ft reporis wll be issued to aibw the dbnt to receive dsft h a tkmNwwrnws meow,, +4khr ~wn' 2) The AS 4000 ICAU.44 MONta dated 4 49 9 . a 90 PFOS trarultlon w1th greater saarltl~Aly tlan ths 498 -a Q9 aaneilion. IMPACT ON A'jUDY 1) The cient rr41 be nbit 90 too" and nvisw the dais more qui*, 2) The 499 .a 80 trnntRivn an be detected with pi+aaiar, sondtlvMy; tMr+sForr, gNlnp better dracrr4ograpl y. n L& . sk* Mrs N-F~ im, ~ i~ Datf or. Aw ~+t e v.n.+ a.~ . f-MfR-Ox svaror e~Cr h p~s~w~d4 uw ~ Exyqen G)A!J FtwNrw l.x.l U/Adty- ~ ~' . U4RARY 97e V000025 4 _. AD1NNt8?FtAT NE FORM Exygen Rescarcb Page 108 of Ito p . 109 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 e 3058 Research Drive Phone : 814-2721039 ni RESEARC H State College, PA 16801 Fax: 814-231-1580 DEVIATION FOR M ~ tas X Prqea speci8c Deviation, faa'tity Deviation, Date at Occurrence: 04rzt3lOt3 Exypen Project At : P78DIP1131 Deviation 5 Cllent Ptojeat # : NA Rebrenoe M : 06-0Te ReuulatoKypjv_er. ~on Tvoe : (InchxM W for methods and SOPs) CiMP X GLP X Protocol Method SOP other Wl : NA None Notebook Werance : NA Samole t7eeulvtfon Login # : L0008191 - Container NA Lot 0 : NA Summary of DeYletten The three sedirrldnt samples In L8191 (C0172892 -CtI172894) were originally extracted using the sediment method V0001 782. Poor recoveries were obtained for PFOS. PFOA and "C PFOA. 8ecause of this, the study sponsor requested the use of an etternstive extraction for these compounds, as follows : Direct In jection Method ; Before the samples were weighed for the extraction, they were m bced thoroughly by vigorously slwkhp the container. A one-gram portion of sediment was wooed into a 15 - md1ifibr centrifuge tube for the extraction . Ten milliliters of 1% aoetic acid in methanol was added to each sample . The aamples were then shaken by hand . vortexed, and sonicated for thirty minutes . The samples were then centrifuged for -10 minutes at -3000 rpm . Each sample was analyzed by LClMSIMS skcboeprey. Using this method sooepteae data was oblsined .fa PFOS. but th e recoveries for PFOA and uC PFOA were sHt poor . Another attematNe melNod was then used for PFOA and "C PFpA, as Wows : Alternative SPE Method. -The samples that were prepared In 1% acetic acid for the direct injection method were used for I is'extracttan. Fme m ill ifibrs of eeah sample was etiquoted Into a 50KnL polypropylene Cenalfuge tube and the volume was taken b 40 ml wtth water. The samples were then can trifufled for -10 minutes at 300p rpm . The supemstent wes ttten leaded onto a Cie SPE cartidga conditioned with 10 ml of methanol end 5.mL of water. The eluate was r8scardod. Approximately five millers of methanol was added to the cartridge . Five mkNNters of etuete was collected into a graduated 15 ml- polypropylene centrifuge tube. Each sample was analyzed by LCJMSlM S p. ray Cause: ~ Preparation _ Analysis instrument Cttent Request X Imbed: More usable dais was obtained . Other UBRARY 10: VOp01840-8 ADAMSTRATIVE FOR M f i x y g c n Kesearch Page, 11 .190t1 1 0 p . 110 Interim Report #23 - Analysis of Sediment Samples Exygcn Study No . : P0000760 CHEM EHSR 236 1B 651 733 1958 05101 '06 73 :46 NO706 03/03 ~ Qi-It ~tOQi 4t :0pa Frot1a1011 fOUKIdR + 5-411 ~.011IQQ7 f-!1 f ` , . . . . '~ ; . . +: .o: . ~ i ;, . . 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