Document YBMkK54R8wm3eEk778EVQbeV

P-1 A R a .a .6 - 56Z Z INTERIM REPORT #23 A ia W i of Sediment Samples STUDY TTTIF. Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for die 3M Decatur Monitoring Program DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 JaiSsTimUhDaYKeDsIaRriEPC.ET.,ODREE W1es4t0o0nWSoelsutotinonWs,aIync. West Chester, PA 19380 Phone:610-701-3761 INTERIM REPORT COMPLETION DATE May 2,2006 PERFOREMxyIgNeGn RLeAseBaOrcRhATORY St3a0te58CoRlelesgeea,rcPhAD1r6iv8e01 Phone: 814-272-1039 STUDY SPONSOR 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 Phone:651-733-6374 PROJECT ExyPgroentoScotuldNyuNmubmerb: ePr00P000070600760 Total Pages: 110 P-2 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT EinxyWgeanterS,tuSdoyilN, uSmedbiemrePn0t,00F0is7h6,0,Celanmtitsl,edV"eAgnetaaltyiosins,oSfmPaelrlfluMoaromomctaalnoLiicveArciadnd(PSFmOAal)l Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laboratory PcsporainkctirtnoicglepaSrnotdacnecddoaunrrdterssol4fo0srpCtihkFeeRssu7fr9or2rogtbhayteeEdwxiyerergecetnnioRntjeersecectaioorrcndhe,adnwpdirtohamlotepnrtenlyaetxaecteSthpPetiEotinmm. eeTtohhfoeedlxsatbraaoncrdtaitootnhr.ye John Flaherty * Princrinpal Iinvee-stigator Exygen Research JSatuisdimy DhairKecetsoarri P.E., DEE Weston Solutions, Inc. Date Exygen Research Page 2 o il 10 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 QUALITY ASSURANCE STATEMENT Exygen Research's Quality Assurance Unit reviewed Exygen Study Number P0000760, cfeCoonlrntaimdttlhuesecd,t,V3"aMecAgcenoDtaraldetyiciosnaingstu, roStofmMPaEolexlnryfiMtlgouearonimrnogmRocaePtlsareonLagoirvricacehmr'Asa"cn.SiddtaASn(lmPdlFaarrOledlvAMiOe)awpimneedmraWatpilanhtgSaesere,PrusrS1moocwieUld,esruSierneegdisn,iLmsptCehe/necMtt,eSSdFt/uMisfdohSy!r Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported to the Exygen Principal Investigator and Management and to the Study Director. Phase .RRAFeenvivaniileaeywlwtiRcaaanlwdRDIenpatotearrtim InsDDaetceted 5/2/06 DaItnePvrReinsetcpiiaoparattelodr to DaMteaEnRxaeygpgeoemrnteendtto DSattuedRveDpiorretcetdorto 5/2/06 5/2/06 5/2/06 Lydia^fhaffer Teclmical Lead, Quality Assfance Unit S/< R M Date `Note: All in-lab inspections will be documented in the QA statement for the final raenvaileywticoafl trheepionrtteraitmthreepcoortncalnudsiaosnsoocifatthede rsatwudy. This QA statement involves only the Exygen Research PageSofllO Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 CERTIFICATION OF AHTHFNTirrrv Trehpirsesienntteartiimon roefptohret,rafwordaEtax.ygen Study Number P0000760, is a true and complete Submitted by: Exygen Research 3058 Research Drive (S8t1at4e)2C7o2ll-e1g0e3,9PA 16801 Principal Investigator, Exygen: /IQ JP . /*Exygen ResearchFacility Management: RPErxiecyshgiaderendnR^t eseraerzczhini Study Director, Weston Solutions, Inc. JWaiessimtohnaTSColeustaiorinPs,.EIn.,cD. EE Sponsor Representative, 3M Company: Michael N. Santoro Director of Regulatory Affairs Date Date iw Date %2k Date Exygen Research Page 4 of 110 P-5 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 STUDY IDENTIFICATION 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: P0000760 EXYGEN STUDY NUMBER: P0000760 TYPE OF STUDY: Residue SAMPLE MATRDC: Sediment TEST SUBSTANCE: Perfluorooctanoic acid (PFOA) SPONSOR: 3M Company 3M Building 0236-01 -B-10 St Paul, MN 55144 STUDY DIRECTOR: Jaisimha Kesari P.E., DEE Weston Solutions, Inc. W14e0s0t WCheesstotenr,WPAay19380 STUDY MONITOR: Michael A. Santoro 3M Company S3tM. PBauuill,dMinNg 05253164-401-B-10 PERFORMING LABORATORY: Exygen Research 3058 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: 11/05/04 Interim Analytical Start Date: 04/27/06 Interim Analytical Termination Date: 04/30/06 Interim Report Completion Date: 05/02/06 Exygen Research Page 5 of 110 P-6 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 PROJECT PERSONNEL The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc. The ifnotleloriwminpgorpteiorsnoonfntehlefrsotumdyE: xygen Research were associated with various phases of this Name John Flaherty Karen Risha Paul Connolly Christine Edwards Mark Ammerman Amy Sheehan Brittany Kravets Scott Crain Frances Crespi Devon Ingram Christa Gallant Title Vice President Scientist Technical Lead-LC/MS Technician Sample Custodian Associate Scientist Technician Technician Technician Technician Technician Exygen Research Page 6 of 110 P-7 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 TABLE OF CONTENTS TITLE PAGE...........................................................................................................................P..a..g..e PTLLLQCSG1.RTIIAIEU0OSSSUORBATTOTSDJTLDLUOOEOIEYIFCFMFFTLIOITYCAFATDMFIAAPBPEAGACEPTOBNSUROREIRLSTORYNSNUIAENEFO.DTS.RTIS.N.OEC.IOA...C...NN.A..F.RN..E....ETT..AY.C..S...LS.I..U..E..O.P............T....RN.S............H..A...T.................EA....C...............N...TT...................IT.E........C...........IM.........C.E..................E..I......C.....T.......N........O..Y............T........M..................................P....................L.........................I...........A...........................N............................C..........................E..................................S....................T.........................A............................T..........................E.....................M....................................E...................N....................T.................................................'.'................................'.......\..""1.."i`0g9467532 23..00 IONBTJREOCDTUIVCET..I.O...N........................................................................................................................................................................' Z Z "" " n12 456...0006666....1324ADREPDAENEexFidSArrtdECcerLiaecRRtcYntioEtItIiTPnnNoSTIajnoeCClIclPOASEitdrPNELosMExcPTOeAtrErEdoFaTxuScctAEretTreiadRNocFSunIAtroAAieoPrLMLnrFYSo.oPPe.cT.rd.rLe.Io.idSCE.mc.ue.SAe.red.d.e.nL.i.u..mt.F.r...M...eoe......rn...EF.....St.oT........er....H...d....S.....iO....em........d..D....e..i.....mn............t.......e..........n...............t................................................................................................................................................................Z..........Z.......Z......"......Z..".......Z...Z......Z........Z.Z...........".Z.....Z.......Z......."...]11l1l\4443322 66..56 CPrherpoamraattioognroafphSyta..n..d..a..r.d..s...a..n..d...F...o..r.t.i..f.i.c..a..t.i.o...n...S..o...l.u..t.i.o...n..s......................................................................................11g4 7891...0000666.0...987ERRQXIDCEnEuPOSesTsatEUNrcnEuRrLtCmiNiIpTtLMaTetSitUnoIiE.oOt.nSN.n.SNI.o.TOea.f.nnAO.N.Lsd.LF.iSC.t.Ei..DD/..vxM....iAEa..t..Sym..ST.../....I.MpA...G...l...e.S..A.N.....C...NI.....n...a....D...s.l....ct....r....uS....u....l...A.ma........t....Me.i......o.n........nPt.........L.a.........n.....E......d........S.........O...................p............e..........r....a........t...i....n.......g..........C.........o......n.......d.......iZ..t..i..o.ZZ..n..Zs.Z......Z..Z......Z......................Z...................Z............Z..............22.1111007996 Exygen Research Page 7 of 110 p.8 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 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 III. Summary of PFOA in SPE Extracted Sediment Samples.................................24 Table IV. Matrix Spike Recovery of PFOA 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 ,3C PFOA m Sediment Samples......................28 Table VIH SSaumrrpolgeast..e...S..p..i.k...e..R...e..c..o..v..e..r..y...o..f...,.3.C....P...F..O...A....i.n.....D..i.r..e..c.t...I.n..j..e.c..t..i.o..n...S...e..d..i.m...e..n..t......... 29 Table IX. SSuamrropgleaste...S...p..i.k..e...R...e..c..o..v..e..r.y....o..f..,.3..C....P..F...O...A....i.n...S...P..E....E...x..t.r.a..c..t.e..d...S..e..d..i.m....e..n..t............. 30 Table X. Total Percent Solids in Sediment Samples.........................................................31 Exygen Research Page 8 of 110 P-9 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 LIST OF FIGURES Page Figure 1. 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. PanFdO4A.0inngR/meaLgeFnotrBtilfaiendk,R0e.a4gnegn/tmSLpkFBor,tRifieesdpeRcetaivgeelnyt..S...p..k...A...,........................ 35 Figure 4. Chromatogram Representing a Sediment Sample Analyzed for PFOA (Exygen ID: C0172892, Data Set: 042806D).................................................... 36 Figure 5. Typical Calibration Curve for 13C PFOA in Methanol.....................................37 Figure 6. RExestrpaecctetidveSltya.n..d..a..r..d..s...o..f..1..3.C....P..F...O...A....m....M....e..t.h..a..n..o...l.,..2..5...n...g../.L....a..n..d...5..0...n..g../..L..,............38 Figure 7. ,3C 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 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 LIST OF APPENDICES Appendix A Study Protocol P0000760 (Exygen Study No. P0000760) with Analytical Method V0001782: "Method ofAnalysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by LC/MS/MS", and Protocol Amendments............................................... 41 Exygen Research Page 10 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: 1*0000760 1.0 SUMMARY Exygen Research extracted and analyzed sediment samples for the determination of pcrfluorooctanoic acid (PFOA) according to Exygen Method V0001782 (Appendix A). The limit of quantitation for PFOA in sediment was 2.0 ng/g. The standard sediment method (V00017S2) 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. FPiFnOalAlya, nadn,3aCltePrFnOatAiv.e SPE column extraction (Section 6.3) was used to analyze for Analytical results for the analysis of PFOA in sediment samples extracted according to the method based on dry weight arc summarized in Table I. Analytical results for the asunmalymsaisrizoefdPinFOTAablien IsIe. dAimneanlyttiscaaml rpelseusltbsyfodritrheectaninaljyecsitsioonf, PbFaOseAd ionnseddriymewnetisgahmt,paleres 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 o f 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 n C PFOA in sediment samples based on wet weight was 97 27%. Fortification recoveries for l3C PFForOtiAficaitnionserdeicmoevnetriessamfoprle13sCbPaFseOdAoinn dwireetctwinejiegchttionarseedsiummemntasraizmedpleisn baTsaebdleonVwIeI.t wexetirgahctteadresesduimmemnatrsiazmedpliens Tbaasbelde oVnIwIIe.t wFeoirgthifticaarteiosnumremcoarviezreidesinfoTrab13lCe IPXF.OA in SPE The total percent solids for sediment samples are detailed in Table X. 2. OBJECTIVE The objective of the analytical part of this study was to determine levels of pAc)r.fluorooctanoic acid (PFOA) in sediment according to Protocol P0000760 (Appendix Exygen Research Page 11 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 3.0 INTRODUCTION This report details the results of the analysis for the determination of PFOA in sediment uDseintegrmtihneatioannaolyftPicearlflumoreotohcotdasnoiecnAtitcleidd,(P"FVO0A0)0i1n7S82ed: imMeentthboydLCof/MASn/MalySs."is for the The study was initiated on November 05, 2004, when the study director signed protocol nanudmtbheeraPn0a0ly0t0ic7a6l0t.ermThineatainoanlydtaitcealfosrtatrhtisdianteterfiomr trheipsoirnttweraismArperpiol r3t0w,2a0s0A6.pril 27, 2006 4.0 ANALYTICAL TEST SAMPLES bTAyhprrEeilxey2sg2ee,dni2mp0e0ern6stofsnraonmmelpTlaenismd(pEFlxaryicngeadekninaIDtreW:fCreig0ste1or7na2teS8d9ol2sut-otCiroa0ng1se7,.2I8n9c.4)Twheeresaremcpelievsedwoenrewloegt giceedoinn 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 standard, PFOA, was purchased from Oakwood Products, Inc. and was received at Exygen on March 17, 2005. The surrogate spiking standard, 13C labeled p2e0r0f4luforroomoctthaeno3iMc aCcoidmp(a13nCy.PFOA SP0004184), was received at Exygen on April 15, Tamhebiaevnatialanbdle13iCnfPoFrmOaAtiwonasfosrtotrheedrferfoezreenn.ce materials is listed below. PFOA was stored CoPmFpOoAund ExygSePn0I0n0v5e4n4to4ry No. L2o0t3# Puri9ty9 f%) Ex0p3ir/a3t1io/0n7Date ,3CPFOA SP0004I84 3507-195 97 03/29/09 The molecular structure of PFOA is given below PCFheOmAical Name: Perfluorooctanoic acid Molecular Weight: 414 Transitions Monitored: 413 - 369 (for quantification) and 413 -> 219 (for confirmation) Structure: Exygen Research Page 12 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 ,C3ChePmPicOalAName: 1,2-13C perfluorooctanoic acid Molecular Weight: 416 Transition Monitored: 415->370 Structure: 6.0 DESCRIPTION OF ANALYTICAL METHOD The analytical method "V0001782: Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by LC/MS/MS" was used for the sediment samples in this study. 6.1 Extraction Procedure For Sediment Before die samples were weighed for the extraction, they were mixed thoroughly by vmmigiLloliorloiftue1sr%lyceasnchteartikifciungagceittdhueibnecowfnoatrtaeitrnhewerea. xsAtarad5cdtegiodrnat.mo tAphofetrestriaomfnoprolteiffsis.ceadTtiihmoenesnoatfmwappalpserswowperiegiraheteevdosarinmtetoxpleaedsf,aif3nt5dy 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 Cig SPE cartridge cTownednittiyonmeidlliwlitiethrs1o0f mmLethoafnmolewthaasnoalddaendd t2o0thmeLseodfimweantet rs.amTphleeselleufatteinwtahse dciesnctarrifduegde. 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 Cig SPE cartridge. The eluate was mcoeltlhecatneodl. inTtoheawa5s0h0 wmaLs cNolalelgcetende inBothtteles.amTehbeotctloeluams nthewealsuawtea.shAepdpwroixthim4atemlyLtwoof Exygen Research Page 13 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study Ko.: P0000760 hundred milliliters of water was added to the bottles. The samples were mixed by shaking and loaded onto another Cu SPE cartridge 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 eluate was collected into a graduated 15 mL polypropylene centrifuge tube. Each sample was analyzed by LC/MS/MS electrospray. 6.2 Direct Inject Extraction Procedure For Sediment Before the samples were weighed for the extraction, they were mixed thoroughly by v1i5g-omroilulislliytershcaeknitnrgifuthgee ctounbteainfoerr. thAe oexnter-agcrtaiomn.porTtieonn mofillsielidtiemrsenotfw1a%s waeciegthicedacinidtoina methanol was added to each sample. The samples were then shaken by hand, vortexed, -a3n0d0s0onrpicmat.edEafcohr tshaimrtpylme winausteasn.alTyzheedsbaymLpCle/sMwSe/rMe Stheelnecctetonstprirfauyg.ed for -10 minutes at 63 Additional SPE Extraction Procedure For Sediment The samples that were prepared in 1% acetic acid for the direct injection method were used for this extraction. Five milliliters of each sample was aliquoted into a 50-mL polypropylene centrifuge 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 The eluate was idrisScPaErdceadr.triAdgpeprcooxnidmitaitoenlyedfiwveithmi1l0lilmitLerso f methanol and 5 of methanol was mL of added water. to the cartridge. Five milliliters of eluate was collected into a graduated 15 mL polypropylene centrifuge tube. Each sample was analyzed by LC/MS/MS electrospray. 6.4 Percent Solids Procedure For Sediment PVe0r0c0e0n4t 2so7l.idAspwperroexdimetaetremlyin2e0dgursaimngs tohfesparmopcleedwuraesiwndeiicgahteedd iinntEoxaypgaenn. mTehtheowdeight of the sample plus die pan was recorded. The samples were then dried in an oven overnight at 104 2 C. 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 Solations oAfm10ix0e0dpsgto/mckLstbaynddaisrdsoslovliuntgio1n0o0fmPFgOoAf eaancdh noCf tPhFeOstAanwdaarsdpsre(cpoarrreedctaetda fcoornpcuernittryataionnd Exygen Research Page 14 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 ssataltndcaorndtsenwte)reinpr1e0p0aremdL: o f methanol. From this solution, the following fortification Cone, of 1Soto(fSpcPogk1F1l01/01uoOm0..0010t0riA0LoF)noa1rntd. VoFlourmt e (mL) 1100 111000 13C PFOA Final Volume (mL) 111110000000000 Final Cone, of Fortification Std. (pgAnL) 01011.00..01010 Amdiessstthooalcvnkionlsg.olFu1rt0ioommn otghfitsohnseolylsut1ta3iCnodnPa,rFtdhOeA(fcoowlrlraoeswcatielnsdgo ffpoorrretpipfaiucreraidttiyoantaanstdcaonsndacalertdncstrowanteitoerenntp)orfeinp10ar01e0dp0:g/mmLL boyf Cone, of Stock or Fort. (Spog1l1/1um0.00t0iLo)n1 1o f n C PFOA Fort Volume (mL) 111000 VF(omilnuLaml) e 111000000 Final Cone, of Fortification Std. (pg/mL) 011..100 pAcorenpsceaetrnetdoraftiinnoonnsm-weextehtrraeancpotrcle,dpaacrseadlsibpreactiifoiend stianndEaxrdysgecnonmtaeitnhiondg VPF0O00A17a8n2d. I3TChePFfOolAlowwinags oCroCnea,liobrfaFtioornt VoFlourmt e 1o (Snog111l/1u0m000t000iLo)n1 25..00 fPFOA and 13C (mL) 1.0 0011....2500 PF1O.0A Final Volume (mL) 111111000000 CFailniablraCtoionne,Sotdf. (ng/mL) 10 251...000 00..52 Exygen Research Page 15 of 110 Interim Repeal #23 - Analysis of Sediment Samples Exygen Study No.: P000760 The standards 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 fortification and calibration standard solutions were pstroerpeadraitinonaisrelofcriagteerdaitnorth(e4raw d2ataC)pawckhaegne ansostociinateudsew. ithDthoicsuimnteenrtiamtiorenpoortf. standard 6.6 Chromatography Quantification 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 Instrumeat Sensitivity cTohnecensmtraatliloenstofs0ta.2ndnagr/dmLamofoPuFnOt Ain. jected during the chromatographic run had a 6.8 Description of LC/MS/MS Instrument and Operating Conditions Instrument: API 4000 Biomolecular Mass Analyzer Interface: Turbo Ion Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 Software: Windows NT, Analyst 1.4.1 HPLC: HewlettHPPacQkuaardt P(HumP)pSeries 1100 HHPP AVuactousuammpDleegr asser HP Column Oven HPLC Column: Thermo Fluophase RP, 50 mm x 2.1mm ICnojeluctmionnTVemoi.p:.:15-3p0L C Mobile Phase (A): 2 mM Ammonium Acetate in water Mobile Phase (3): Methanol Exygen Research Tim11108e1180...f00..0.000minl 66A55A 2255 65 65 %35B 3755 75 3355 Page 16 of 10 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Total runtime: ~ l8 mm Flow Rate: 0.3 mL/min Ions monitored: Analvte PFOA PFOA Confirm Ion 13C PFOA Mode negative negative negative Transition Monitored 413 -+ 369 413 ->219 415 - 370 RAetpepnrtoioxnimTaitmee ~ 1(1m.1inm)in. ~ - 1111..11 min. min. 6.9 Quantitation and Example Calculation PthFeOnAcocnovnecretendtrattoionnasnaorgeraqmuanpteirtagterdamin. nTanhoegPraFmOAofcPoFnOceAntpraetriomnsillwilietreer oqufaenxttirtaactetdanidn nanogram of PFOA per liter for Set #3 (Set 042806D). Fifteen microliters of sample or cthaelibsrtaatnidoanrdstacnudravredwwaesregiennjeercatteeddin(utositnhge 1L/Cx/MfitSw/MeiSg.htTedhelipneeaakr areregarewssaisonm)ebaysuArendaalynsdt sfroofmtwtahree euqsuinatgiosnesvbeenlocwo.ncentrations of standards. The concentration was detenmined 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 1 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 (ng/L) = (Peak areSal-oipnetercept! x DF Where: DF = Dilution Factor, factor by which the final volume was diluted, if necessary. FEoqruasatimonpl2eswfaosrtuifsieedd twoicthonkvneorwt tnheamamouonutnstooffPPFFOOAAafnodun1d3CinPnFgO/LAtporinogr/gto(pexpbtr)a.ction, EquaUoa.& PFOA found (ppb) *= [sample aliquoftPvFoOluAmfeouxnd(sfaamgp/Lle) wx eSiPghBt v/ odliuremcet ienxjtercatctseadm!ple volume)] Exygen Research Page 17 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Equation 3 was used to calculate the percent recovery. ERqeucoatvieorny3(:%) = (analvte found (ng/g. wet weight-) - analvte in control (ng/g. wet weightY) x l00% amount added (ng/g, wet weight) 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. Equation 4: PFOA found (ppb) dry weight = PFOA found (ppb) x [100% / total solids(%)J An example of a calculation using an actual sample follows: wSeitdhimPFenOtAsawmhpelree:Exygen ID CO172892 Spk pinetaekrcaerpeta slope dilution factor ng/g PFOA added (fort level) amt in corresponding sample (ng/g) SsaPmEpvleolaulmiqeuoetxvtroalcutmede((Lm)L) dstoairtmaelcptsleoinlwijdeescitg(%shat)m(gp)le volume (mL) D (Set: -- = == = =-- = =-= 042806D), 42441632006300050088 586 06511.600.454 fortified at 4 ng/mL From equation 1: Analyte found (ng/L) From equatiPonFO3:A found (ppb) = 1236588 - 46301 x 100 420 - 55200 ng/L ^ (55200 ne/Lx 0.04 L) = [454m20Lpxp(b1 g /10 mL)] From equation 3: % Recovery = (4420 ng/g - 586 ne/g) x 100% 4000 ng/g = 96% Exygen Research Page 18 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 FromPeFqOuAatifoonun4d: (ppb) dry weight =4416 ppb x (100% / 66.54%) = 6640 ppb NOTE: This value may be slightly different than that of the taw data due to rounding. 7.0 EXPERIMENTAL DESIGN 13C PFOA was used as a surrogate for all the samples. l3C PFOA was added to the sediment samples in the laboratory after the samples were weighed for extraction. For skeexndtoriwamcnetinoctno.nsacmenptrleastiodnestoignthaetesdamasplelasbionrathtoerylabmoartartioxryspaifkteers,thPeFsOamApwleasswaelrseowaedidgehdedaftoar The sediment samples were extracted in one set. The set included one reagent blank and tswamoprleeasg.eFntorbleaanckhssafomrtpilfeie,dtwaot klanboowrantocroynmceantrtrixatisopniks.esTahned asedtucpolnictaaitneewdetrhereexetrsaecdtiemd.ent 8.0 RESULTS Analytical results for the analysis of PFOA in sediment samples based on dry weight are bfsouyrmdtmhireeacraitnzaienldyjesicinstiToonaf,bPblFeaOsIeA. dAionnnsaedlydrtyiimcwaelenritgesshautm,ltasprlefeossrubtmyhemalatanerarinzlyeasdtiivsienoSfTPPaEFbOleeAxItrIia.nctsAieondnai,mlybetainscetadlsaromenspudllertyss Fwdeoevritgiiahftitic,oanatiroefnosruremcPomFvOaerrAiizeesdinfoinrsteThdeaimbalneeanlItyIsIsi.samoTpfhlPeeFsoOvbAearasielnldsaevodenirmagweenettpseawrmceepingltehsrteacwroeavsseurmy73m asrtiazne1dd6a%rind. TsaambpleleIsVa.reFsourmtimficaartiizoend riencTovaebrlieesVf.orFtohretifaincaaltyiosnisreocfoPvFeOrieAs mfordtihreecatnianljyescitsioonf PseFdOimAenint SPE extracted sediment samples are summarized in Table VI. The average percent recovery standard deviation for ,3C 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 l3C PFOA in direct injection sediment samples based on wet weight are summarized in Table VIII. FwoeritgifhitcaarteiosnumremcoavreizrieedsifnoTr a,3bClePIFXO. A in SPE extracted sediment samples based on wet The total percent solids for sediment samples are detailed in Table X. Exygen Research Page 19 of 110 Interim Report #23 --Analysis of Sediment Samples Exygen Study No.: P0000760 9.0 CONCLUSIONS Talhteernsaetdivime eSnPtEsmametphloeds, wwehriechsyuicecledsesdfualclycepextatbralectQedC aHnadt analyzed for PFOA using an 10.0 RETENTION OF DATA AND SAMPLES All original paper data generated by Exygen Research that pertains to this interim report wasililnbsetrushmipenptedortotetmhepesrtuadtuyredilroegcst.or.ExTahcitscdoopeisesnootfianlcllruadwe dfaactail,itays-swpeecllifaisc araswigdnaetda csoupchy of the interim analytical report and all original facility-specific raw data, will be retained LinabthoeratEoxryygPernacRtiecseeSartachndaarrcdhsiv4e0sCfFoRr t7h9e2p. eriod of time specified in EPA TSCA Good Exygen Research Page 20 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 TABLES Exygen Research Page 21 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table I. Summary of PFOA in Sediment Samples Exvoen10 C0172892 C0172892Rap C0172893 C0172893Rep C0172894 C0172894Rep CNent Samole ID QAL-SD-BPP01-0-0000 DAL-SD-BPP01-0-0000* DA1-SD-BPPQ2-0-0000 DAL-SD-BPP02-0-0000* DAL-SD-SPP03-0-0000 DAL-SD-BPP03-0-0000* AnalyteFound(ppb, ng/g) DryWeight C8Add PFOA PerfluorooctanoicAdd NR NR NR NR NR NR Assessed Accuracy (/-%> NR NR NR NR NR NR Laboratory D upicate NR = Not reported due to quality control result failures. See Table II for re-analysis results. Exygen Research Page 22 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table 11. Summary of PFOA in Direct Injection Sediment Samples ExygenID C0172892 C0172802Rep C0172893 C0172893Rep C0172894 C0172894 Rep Client Sample ID DAL-SD-8PP01-0-0000 DAL-SD-BPP01-0-0000' DAL-SD-BPP02-0-0000 DAL-SD-BPP02-0-0000' OAL-SD-BPP03-0-000Q DAL-SD-BPP03-0-0000* AnalyteFound(ppb, ng/g)DryWeight C<Add PFOA PerfluorooctanolcAcid NR NR NR NR NR NR 'Laboratory Duplicate NR * Not reported due to quality control result failures. See Table III tor (-analysis results Assessed Accuracy NR NR NR NR NR NR Exygen Research Page 23 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table III. Summary of PFOA in SPE Extracted Sediment Samples Exygan ID C0172882 C0172892 Rep C01728S3 C0172893 Rep C0172894 C0172894 Rap "LaboratoryDupMcnto Client SamolalD Analyta Found (ppb. ng/g) Dry Weight CB Add PFOA Pariluorooctanoic Add DAI-SD-BPP01 -0-0000 DAL-SD-8PP01-0-0000* DAL-SD-BRP02-0-0000 DAL-SD-BPPC2-0-0000" 881 945 927 823 DAL-SO-BPP03-0-000C OAL-SD-BPP03-0-0000' 2390 2380 A tu iu d Accuracy 30 30 30 30 30 30 Exygen Research Page 24 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.r P0000760 Table IV. Matrix Spike Recovery of PFOA in Sediment Samples Sample (C0O17A2LM-S8DS-fB*PDP, 4010-0p p-0b0S0p0lit) DAL-SO-BPP01-0-0000 tcaiTsaed 8pk E. aoooppe Spare) DAL-SO-8PP02-0-0000 (C0172SMSpk G,400ppt Sp*) DAL-SD-8PP02-0-0000 {C0172M3 Spk H,4000ppb SpHtt) DAL-SD-BPP03-0-0000 <C0172Mspk J. 4M ppb Spltaj DAL-SD-BPP03-0-0000 (Coi7jaas spk k, asm ppbSpik*) Amount Spiked ------- l_nofc) 400 4000 400 4000 400 4000 Amt Found in Sample (rtg/p) wet m ig ht C8 Add PFOA Amount Recovered ing/g) wet weight NR NR NR NR NR NR NR NR NR NR NR NR Recovery t% ) NR NR NR NR NR NR Standard DAavvMaraIoe*n:: NNRR Sample residue exceed the apUdng level significantly (3 spiking level); therefore, an accurate recovery value cannot be calculated. NNRoiea:NSoint rceeptohrtiesdaduumemtoaqiyutaaibtylacoshnotrwolsrersouultnfdaeiludrerse.suSltese, rTeacdovseVryfovrarleu-easnamlyasyisvraersyusltlsig. htly from the vatu** In the raw data. Exygen Research Page 25 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table V. Matrix Spike Recovery of PFOA in Direct Injection Sediment Samples Sample Description DAL-SD-8PP01-0-0000 (Cetrosz Spk O,40tppb Spike) DAL-SO-BPP01-Q-00Q0 (C0172082 SpkE,40000 ppb Spike) CIAL-SD-BPP02-0-0000 (00171009 Spk G, 4000 pptoSp<*) DAL-SD-SPP02-0-0000 (C017280Sspk H.40000 ppb Spike) DAL-SD-BPPO3-0-0000 icai7na4spk j, 4000ppbSpure) DAL-SD-BPP03-0-0000 (C01720B4Spk K,40000 ppk Spllre) Amount Spiked --W . 4000 40000 4000 40000 4000 40000 Amt Found in Sample (rto/o) we*. weight C8 A dd PFQA Amount Recovered (ng/g) wet weight NR NR NR NR NR NR NR NR NR NR NR NR Reoovery <%> NR NR NR NR NR NR Average. Standard Deviation: NR NR "Sample residue exceeds the piking level significant^ (3x spiking level); therefore, an accurate recovery value cannot be calculated. NNRotea:NSoint creeptohrtiesdsudmuemtoarqyutaalbitylecsohnotrwolsrersouultnfdaUedurreees.uSltese, rTeacbolveeVryI fvoarlrue-easnmalyasyisvarreysuslltisg.htly from the values in the raw data. Exygen Research Page 26 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table VI. Matrix Spike Recovery of PFOA in SPE Extracted Sediment Samples Sampw Description (C#1D7A2LM-6sOp-aBBP.P400(10-0n-&0g00S0pike) (CotrjtntpkDAL-SD-0PPO1-O-OOOO e, 400M d m tp iia ) DAL-SD-BPP02-0-0000 (C0172HS Spfc 0 ,4M0 1* 4 Spik} DAL-SD-BPP02-0-0000 <001? 2 m Spk N.40000 PpiM 4009DAL-SD-BPP03-0-0000 4C0173004Spfe J, ng/g SpUwJ DAL-SD-BPP03-0-0000 4C0172094Spk K.40000 nglg Sptka Amount Spiked (nflig) 4000 40000 4000 40000 4000 40000 Amt Found inSeinple tnotal wet weight ca Acid PFQA Amount Recovered (ngfg) w ri weight 586 4420 586 25600 504 3860 504 25100 1080 1060 4140 23200 Average: Standard Deviation: Reoovery 96 83 84 61 77 55 73 16 Not*:sine tManummarytable how* rounded rooultt. recovery valuta mayvarylightly from Uw vatuaa ln the raw data Exygen Research Page 27 of HO Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table VII. Surrogate SpikeSRamecpolveesry of ,3C PFOA in Sediment Exygen ID Sample Description C0172892 C0172882 Rep C 0 !72 892 S p k C C0172892 Spk D C0172892 Spk E C0172893 C0172893 Rep C0172893 Spk F C0172893 Spk 6 C0172893 Spk H C0172894 CO172894 Rep C0172894 Spk I C0172894 Spk J C0172894 Spk K DAL-SD-BPP01 -OOOOO DAL-SD-BPPO1-0-0000 DAL-SD-BPP01-0-0000 DAL-SD-BPP01-0-0000 DAL-SD-BPP01-0-0000 DAL-SD-BPP02-0-0000 DAL-SD-BPP02-0-0000 PAL-SD-8PP02-0-0000 DAL-SD-BPP02-0-0000 DAL-SD-BPP02-0-0000 DAL-SD-BPP03-0-0000 DAL-SD-BPP03-0-0000 DAL-SD-QPP03-0-0000 DAL-SD-BPP03-0-0000 DAL-SD-BPP03-0-0000 Amount Spiked (ng/fl) 4 4 4 400 4000 4 4 4 40p 4000 4 4 4 400 4000 ,3c-pfoa Amount Recovered Wet Weight (nfl/fl) NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR Average Standard Owiatton: NR = Not repotted due to quality control result failures. See Table VIII for re-analysis results. Note: Since this summary table shows rounded results, recovery values may vary slightly from the values in *te raw data. Recovery (%) NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR Exygen Research Page 28 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table VIII. Surrogate SpikSeedRiemcoenvterSyaomfp1l3eCs PFOA in Direct Injection Exygen ID Sample Description C0172892 CO172892 Rep COf72892 Spk C C0172892 Spk D C0172892 Spk E C0172893 C0172893 Rep C0172893 Spk F C0172893 Spk G C0172893 Spk H C0172894 C0172894 Rep CD172894 Spk I C0172894 Spk J C0172894 Spk K DAL-SD-BPP01 -0-0000 DAL-SD-BPP01-0-0000 DAL-SD-BPP01-0-0000 DAL-SD-BPP01-0-0000 DAL-SD-BPP01-0-0000 DAL-SD-BPP02-0-0000 DAL-SD-BPP02-0-0000 DAL-SD-BPP02-0-0000 DAL-SD-BPP02-0-0000 DAL-SD-BPP02-0-0000 DAL-SD-BPP03-0-0000 DAL-SO-BPP03-0-0000 DAL-SD-BPP03-0-0000 DAL-SD-BPP03-0-0000 DAL-SD-BPP03-0-0000 Amount Spiked ("O') 40 40 40 4000 40000 40 40 40 4000 40000 40 40 40 4000 40000 n C -P FO A Amount Recovered Wet Weight (nq/g) NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR Recovery (%) NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR Average: Standard Deviation: NR = Not reported due to qu ality control result failure's. See Table IX tor re-analysis results. Note: Since Ills sum mary table shows rounded results, recovery values may vary slightly from the values In toe raw data. NR NR Exygen Research Page 29 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table IX. Surrogate SpiSkeedRimeceonvteSraymopf l1e3Cs PFOA in SPE Extracted CE x n Sample Deechphon Amouni S(npOikead) " C-PFOA Amount Recovered Wat Weight C0172882 00172892 Rap C0172802 Spk D C0172802 Spk E C0172893 C0172883 Rap C0172893 Spk 0 C0172893 Spk H CO172894 C0172884 Rap C0172894 Spk J C0172894 Spk K DAL-SD-BPP01-0-0000 OAL-SD-BPP01-00000 OAL-SO-BPP01-0-0000 DAL-SO-BPP01 -OOOOO DAL-SD-BPP02-MOOO QAL-SD-8PP02-CHX)00 DAL-SD-BPP02-0-0000 DAL-SD-BPP02-0-0000 DAL-SO-BPPO3-0-0000 DAL-SO-BPP03-0-0000 DAL-SD-BPP03-0-0000 DAL-SD-BPP03-00000 40 40 4000 40000 40 40 4000 40000 40 40 4000 40000 kNortnathSeinvealuHeasIsnutmhmeraarwytdaabtale. ihowroundedresult.recoveryvekea mayvaiy nightly 52.0 51.0 3750 26800 47.8 51 a 3500 25200 45.2 40.3 3060 22100 8tendert DAevviaantipoan:: Recovery (%) 130 128 94 65 120 129 86 63 113 101 77 55 9277 Exygen Research Page 30 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Table X. Total Percent Solids in Sediment Samples ExyIDgan C0172892 COt72893 C0172894 DeSsacmripptlieon DAL-SD-BPP01-0-0000 DAL-SD-BPP02-C-0000 DAL-SD-BPP03-0-0000 Total Solids (%) 66.54 5437 44.48 Exygen Research Page 31 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 FIGURES Exygen Research Page 32 of 110 Interini Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Figure 1. Typical Calibration Curve for PFOA in Methanol I 0420000 Sd. Si*E.Nh(PFOA> A9Msnon f i Vs 420 * + 4 0 3 r H 3 0 '" Area, counts Exygen Research Page 33 of 110 Interini Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Figure 2. Engx/tLra, cRteedspSectatinvdealyrds of PFOA in Methanol, 25 ng/L and 50 I X/KOMNH.' M-n>ZfM-AfMRMtt*(StttmHgdtt*:r4f).f **!<>rmAT*:-Tlfi.mtmpH*t 7 o14ttrom MNNOMT 11.01 Exygen. Research Page 34 of 110 Intensity, cpc Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Figure 3. PAF, aOnAd i4n.0Rnega/gmenLtFBolartnikfi,e0d.4Rneagg/menLt FSporktiBfi,eRdeRspeeacgteinvetlSypk CMfroi . PfO A -m m pt* $ from M Utfawflf Arta:302M eunfc Haight 2.37rG03 op# T: 11.(1 min 11.00 Area: 290300 M unk Height 2J*004 eps HT: 11.1 min Intensity, cps Intsnstly. cp s Exygen Research Page 35 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Figure 4. fCohrrPoFmOaAtog(EraxmygRenepIDre:seCn0t1in7g28a9S2e, dDiamtaenSteSt:am04p2l8e0A6Dna)lyzed C tm m -P F O A t ampU n tfM tn m MlMCO-wOT A n a : 3M 2*eoiw H U gM : Z T U ^tO c p * KJ> T L tm fii 1105 Intensity, cps Exygen Research Page 36 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Figure 5. Typical Calibration Curve for l3C PFOA in Methanol 0420060 S*4. SPE.Wk 03C PFGAfc / * MtlghUnp); y 490 x 0-0010 0 - 0.0000) Arca, counts Exygen Research Page 37 of 110 Interim Report #23 - Analysis of Sediment Samples Exygcn Study No.: P0000760 Figure 6. E50xtnrga/cLte, dRSestpanecdtaivredlsyof 13C PFOA in Methanol, 25 ng/L and t3C PFOA J kn 1 1 W c#artt 1 .t* + H 3 cp $ 7: . j wmpi* Z o f4*tm m W W ftwCT 11.03 11.00 Exygcn Research Page 38 of 110 interim Report #23 - Analysis of Sediment Samples Exygcn 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, Respectively p+m*C0ot*Utrae*t4-)3CPFOA (Uumewm) IflA O T M iiH i 1.01 Pf fr NZIOCOm V 1 2 3 4 7 0 Q 10 11 12 13 W t t 1G 17 Tima, min I RA'iigma:n2t7S2p0k0Ao*ou1n3tCe PKF*OloAh(fQc2C.)e421S*.0O0/337o0p.Qs RarTr.o11s0ammpl*lt 10 at 46 from 42&OOOmM 1101 1107 Exygen Research Page 39 of llO p. 40 Interim Report #23 - Analysis of Sediment Samples Exygen Study No,: P0000760 Figure 8. Chromatogram Representing a Sediment Sample Analyzed for 13C PFOA (Exygen ID: C0172892, Data Set: 042806D) Intensity, cps I C tiT & to 73C PFQ* (HUHk&tfkt:wZm)947USJRb3TTM: *Hwm. 1tammp h 27 * 4 1 ft M 2 f# fa w /r 2fl4 11A7 2.0*4- 2.4*42 2 *4 - 2 0 *4 - 1.8*410*4 1.4*4- 1.2*4- 1.0*48000.0 00004 40000 2000.0 0.0 J--------I r t ----- r . ....................................................., ^ , , , , , . 1 2 3 4 6 0 7 6 9 10 11 12 13 14 15 10 17 T il**, ml Exygen Research Page 40 of 110 p. 41 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 APPENDIX A (ExygenASnStuatudlPydy0tyi0Nca0Pano0lrd.7oMP6t0o0e0ctho0lo0d760) with Protocol Amendments Exygen Research Page 41 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygn ProtocolNumber P0000?i0 STUDYPROTOCOL Study Title: SSeAmdnaimallleyMnsitas,mFomfisPhae,lrCSfleluaroumMrmoso,oVUnctisetaigonnergoitnaiLcgtCiAoP/ncMri,odSSgm(r/PMaaFmSlOl MfAora)mtinhmeW3aMlaLteDirv,eeScroaaitlnu,dr Exygen Protocol Number: P0000760 PE3S0etxa5rylf8egoerRCmneoRislnleeegasgreLeca,harPbcDoAhrraiv1to6er8y0:1 Phone: (814)272-1039 SMpiocnhsaoerl ARe.pSraensteonrtoative: D3SPMthi.roPeBncaetnuo:]i(r,l6doM5ifa1NgR)7e053g25u331l-46a64t-3o07r1y4-BA-f1f0airs Ass*lofis Exygen Research Page 42 of 110 p. 43 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 xyge Protocol Number P000076C DISTRIBUTION: 1) Jaiumhi Kasan, Study Director, Weitem Solution* 2) John M. Flaherty, Principal Investigaior, Exygen Research 3) Michael A. Santoro, Sponsor Representative, 3M Company 4) Exygen Research Quality Assurance Unit Exygen Research P ttria jU Page 43 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exypa FiotocoJ Number: P00007W PROTOCOL APPROVAL Study Title: ACnlaalnyus,isVoefgPeetraftliuoonr,ooScmtsanlol icMAancixdna(Pl FLOivAe)rsinaWndateSrm. Saollil,MSaemdimmaelntS, eFriusmh. Using LC/MS/MS for the 3M Decatur Monitoring Program Exygen Protocol Number: P0000760 approvals JWaiessrtaoMXnSKolcustaiorin,tsSntudLy Director Michael A. Santfro, Sponsor Representative 3M Company ' i Mm. Fla.herty, Principal Investigator "Exygen Research Lydvi{S.hcaftfuer, T\$echnija/ / u LQuality Assurance Unit l Research Date 2 F\ - O X -2 0 c V Dato Pat*i Exygen Research Page 44 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exypn Protocol Number P0000700 TABLE OFCONTENTS TITLE PAGE---------------------------- ---- ----------------------------------.______ _________ _____ I DISTRIBUTION___________________________________________ PROTOCOL APPROVAL____________________________________________ .3 TABLE OPCONTENTS ________________________________________ _________ ...4 B m o o u c n o N -------------------------------------------------------------------------------- TEST MATERIAL______________________________________ ___ _____ __________ __J SURROGATE FIELD SPIKE COMPOUND...................... .................. ......... .................... ........... 5 OBJECTIVE___________________________________________ TESTING FACILITY_______________________________ _____ ___________________.. 6 STUDY DIRECTOR._______________________- __ ___ ______ __ ____ __ _________ 6 SPONSOR REPRESENTATIVE..................... ........ ......... .............. ...................... ....................... 7 PRINCIPAL INVESTWATOR................................................................... PROPOSBDEXPERIMENTAL STARTAND TERMINATION DATES........................ ..................... 7 IDENTIFICATION AND JUSTIFICATION OFTHE TEST SYSTEM ............................._.......7 SAMPLE PROCUREMENT. RECEIPT AND RETENTION.... .......................................................... SAMPLE IDENTIFICATION______________ __ ___ _______ ___________ __ _________S ANALYTICAL PROCEDURE SUMMARY__________ ______ ___ _______ ___ ._ _____ ___ VERIFICATION OPANALYTICAL PROCEDURE....................... .......................... ....................... 9 METHOD FOR CONTROLOF BIAS _ ........... ............. ..... .......... ............... _...............................11 STATISTICAL METHODS........ ............................ .............................. ......... ............. ...............11 CLP STATEMENT............... ................................. ............................................................ ..II REPORT....................... ............. .............................................. ...................... ........................ || SAFETY AND HEALTH____________________ __ ______________ _______ ___ ______ 12 AMENDMENTS TO PROTOOOL______________________________ __________ _______|3 DATA RECORD KEEPING................. ...................... ..................... ................................... . 13 QUALITY ASSURANCE____________ __ __________________ _____ ____ ______ ____ 14 RETENTION OFDATA AND ARCHIVING______________ ___ _______ ________ _____ _ 14 APPENDIX I, ANALYTICAL METHODS___________________ ____ __________ __ __ _ )S 2 s 6 ? Pa* 4 o/dJ Exygen Research Page 45 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exyftn Francai Number: P00007W in t r o d u c t io n T(aPnhFdeOspAmw)apliolnemweaaomtefmrt,hasilosislse,trusuedmdyimuisteinntotg, pfLiesCrhf/.MocrmSla/mMasnS,avlfyeogsriestthafetoior3nMp,esrDmflueaclolaromtuoarcmtMamnooanilictloiavricenirdgs Program. TPrhaectsitcuedyStwanildlabrdesau4d0itCedFRfor7c9o2mbpyliathneceQwuiathlityEPAAssTuSraCnAceGUonoidt LoafbEoxraytgoerny Research. TEST MATERIAL The test material ia perfluorooctanoic acid (PFOA) and was purchased from Sigma-Aldrich. PFOCAhemical Name: Perfluorooctanoic acid MLootlNecuumlabr eWr e2ig3h1t1:64H1B4 hTaraintysi:tio9n7.6M4%onitored: 413 -> 369 (for quantification) and 413 - * 219 (for confirmation) Structure: SURROGATE FIELD SPIKE COMPOUND T(S`ch>ieCenPscuFerOsr.oAga) taendfiewldassppuikrcinhgasceodmbpyo3uMndfrios m CPerlaidbne-lEedImpeerrfLluifoeroaoncdtaAnnoaiclytaicciadl " C CPhFeOmAical Name: 1.2-13C perfluorooctanoic acid MLPTuoroartlinNetsyciu:utimlo9an7br%eWMreo3ing5iht0ot7:re-14d91:56415 -- 370 Pag* i o f63 Exygen Research Page 46 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: PCD00760 OBJECTIVE Exypn Protocol Number: P0000760 T(acPnuhFdrerOepnAmut)rvpiilenonmsweioaamooteffmrot,hafsliotshsilees,trfusuoedmldyliofmwioterinnttothg,eEpfi3exsrMhyfg,ocerDlnmaemacnaasnat,ualvylryetiMgscieasotlanmftioitoeortnrhpi,noesgdrmtslP:uarloolrgmoroaacmmtamnuoasiilnclgiavtcehinde V0001780: V0001781: V0001782: V0001783: V0001784. V000178S: V0001786 """AA""AA"A"AAMMMMMMMccccccciiiiiiieeeeeeedddddddttttttthhhhhhh(((((((PPPPPPPoooooooPFdFPPdddddPPdOOOOOOOoooooooAAAAAAAfffffff AAAAAAA)))))))iiiiiiinannnnnnnnnnnnaaaaaaadFlllllSSSSVWlyyyyyyyioemmessssssisadiitiiigihil*stttssssiieellmballffftrffffyanooooooMoMebtdrrrrrrrnLiyaoaftfttfffCCmmohnLoooiobel/eeeeeeCyabmMmmDDDyDDDD/LaaMSseeeeeellCeL/tttttttSMbLSC/eeeeeeeM/yenrrrrrri/MSvmmmmmmrMnLSue"iiiiSiiim/nSrCnnnnnnM"a/baaaaaa/MtMbtttytttSiiiiiiicyoooooo"SLSmnnnnnnL"/CMCooooooo/Mffff/fffSMPPPPPPP"SeeeeeeeS/rrrrrriM/fffflffMlhhlllluuSuwuiiSooooo"orr"rrrrrooooooooooooooccccecctttttltaaaaxaannnnnnnoooooooiiiiiikcccccc TESTING FACILITY PE3S0htxao5ytn8egeeRC:neo(Rs8lle1eeas4gree)ca2,hr7PcD2Ah-r1iv106e38901 STUDY DIRECTOR JWW1a4see0sssi0tmtoWChnhaeSesKosttoleeunsrta,iWorPinAaPsy,.E1la9.,c3D.80EE jPF.khaexos:na(er6:i(@)601w)07a)0t7o10i-1u7o-430lM716i1oiis.eoin P ap 6 of65 Exygen Research Page 47 o f 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 BxygBaProtocol Nwnber P0000760 SPONSOR REPRESENTATIVE M33DSPMMthi.ircoPeChBncaamteuuoeilnlr(l,6dpAoM5iafn.1nNRSg)yae057ng253tu3o13l6-r4a6o-4t03o17ty-4BA-1tt0ain PRINCIPAL INVESTIGATOR JEoxhyngMen RFelasheaerrctyh j3PSo0huh5oni8en.feCRl:aoe(hs8lele1erat4gyre)c@.h2P7eDA2xr-yi1g1v06ce38n90.c1om DPRAOTPEOSSED EXPERIMENTAL START ANDTERMINATION tIOet rcmitsoibnpearrotip0oo1ns,de2da0te0tsh4awttoiltlhDbeeecaiennmcallbuyedtirecd3al1i,np2oth0ret0i5of.innaTol fhreetphaoicsrtt.ustaul deyxpbeerimcoenndtaulctseldu tfraonmd IDENTIFICATION ANDJUSTIFICATION OF THE TEST SYSTEM ThefollSWoowailitnerg(agrreouthnedwteaattesryasntedmssurffoarctehiwsastteurd)y: e Sediment ea FCSSVimmlesaghamaelllltsaMMtimaammi mmaall LSeivruemr TbehapsuarmchpalseesdwainlldbperceoplalreecdtebdybythWe teessttoinngSofaluctiiloitnys.. PTuhrechcaosnetroanl dcapmropcleessswinilgl Papi 7t>f65 Exygen Research Page 48 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygen Protocol Number P0000760 wdeittahiltsbiftosrtuthdey.control samples win be included in the final report associated TthheeDteesctastuyrs,teAmla*bwamerseacrheoas.en to access the environmental impact o f PFOA in SAMPLE PROCUREMENT, RECEIPTAND RETENTION mMWSas3ftbvoMuaeraaldmdutieeylitwaamiar.o.b,co'an*ihtrll*okit.miayTlepT,ahinltnhsaerremientxdnhdhueeewsnnmatafiqtmliibilietltplosl.ebdl'odee.fasifsndTTshwdoab,hmci*edtniy*pratpaol*bmeecte*anp,2ltrrovconeWedcfcuguemsoieiranvrtebmakemeftdiiprPleoleonnelaast,tffnifssnEcomaaofrxmlolatylhrlpregleiclesSepmtnseasoadtmrrudmtedpiwcramyleesiiinlcasavltoglrleecyvdliEiaoavrfaunteyrentvordldimidrnaoewnaepnnWddiemtahnilseneydmsntztithaotnheailngdesll WpFacrisocahocte,errdsd,siniifnmoggil,t,aotvaeEntghdxeeytsgaeatedpinopi.mnroeTannmhtdeisstaesemmsaapanmllleapslmylewta*icmilawlmliblamlelbeuletishvesoetddor rise(sasdemrreeepcfleAreiisvpgpeewdreaniltwdleidixbtheaoIt)up2.rtoCfcTue-r8hstse`h>eCseder. ssfraaammctppiolleenss wwwiililllllbbbeeeceusnstetordriefudfgoerfrdtohizneetnshteuadtfiye.ld-SaUtmPthaCle.ltmimSaemmoamfllaclomlslaeemrcutmimoanlwawnildlhotbhleee ssbetlorouroemdd frozen at S-10*C. rTehpeorrteacnediprtaawnddaptaroacsessoaciinagtedofwtihthe tshaemsptuldesy.will be documented in the final SAMPLE IDENTIFICATION PnCnlauurhbimmrooorbrbmaeettorrao..traoyngTarslahaypemshisiprc,elefe(eatractehthntacstweaimilsnlpuhplmeteobwoiedeirleelnrwbetiiedflilaetsdbhseribogyuunngetihdhqoeuaueltlaababthnoodreraattwaoonrirylayllyssdataiimmsctapiplnllogepurrrioeesffcheeerrdeeeunnarcccehee. sStaumdyp.le Storage conditions and locations will be documented throughout the FegeSo/fij Exygen Research Page 49 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.; P0000760 B tytt Fratoeol Number F00007M ANALYTICAL PROCEDURE SUMMARY Reference!: V0O0I780: V000178!: V0001782; V0001783: V0001784: V0001785: V0001786: A""AAAA"""""AAMMMMMMMccdddddiieeeedeeddeddddttttttthhhhhhh(((((((PoPPPoooPPPooodddFdFPPddPFFdOOOOOOOoooooooAAAAAfAffAffffAAAA))A))AA)))iiiiinnnnminnnnnnnnnaaaaaaaSVlSllPSllSllWyyyyyyymimeoesss*iissdaiiigiiihiiaa*sl*sssstiellemballtfffffrffanoyoooMMoooebtdrrrrrnirrLyoaatttttCddthmmChnhhhLb>ileeeee/eyembmaCMDmDDyDDDDL/aaMSelleseLeCeee/ttttttStLbSCMeee/eeeeMerymr/irrrr/mMvrmSmmmMmuLSie"iiiiSmiiirS/nCnnnnnnMb"aa/aaaaa/MbytMttttttSiiiiiiyioooooooS"LSnnnnLnnn"C/MCooooooo/Mff/fffffSMPPPPPPP"SeeSeeeee/rrMrrrrr/ffffMfffllllllluSuuuuuuSoo"ooooo"rrrrrrrooooooooooooooccccccctttUiiUaaaaannnnnnnoooooooiiiiiiiccccccc PTnFohOmt AeanbfooovufnePdF.mOeAfo.odTsheufsienaal nreaplyotritcawlillcoinncdliutidoentshecaispoambleersosufmsmepeadraitnintogtotthael VERIFICATION OF ANALYTICAL PROCEDURE mAcoentltharbooodir,saaatnomdrypaledcsdo.endtTrtoohlethstaeemsmtpaslteurbicwsetisalnlvcibeaeawuminsiecbdroepfmoipracdtthteee.inptroepsaorlauttiioonnsoafsfopretrifitehde wwppsucfcSbfFbioooeeosoaoeaioleerrlnlntlttullfrfddtetteghtltllanwrieuecerrdo)iosisotsofnaunaet.aotrritispdononnerwbTl.wdborggeiuiwchucslsirtalfeItanUweeaTCaatmsdptebnncOboheeo,iepeeeertblrafnaoslitioaituusge5elnyldtsaolldol0tgfpfidmaolwwfo0o,eiinefkbnnnpEsddefmls"aslhxtaietttnhCehcyaonefLdliovagkcdseevPe(eopa(hssPSenFlsPbctprilFpaaOegheFebiwiOdmkcchekeBAcyiletneSepleeiS.slnof)al(arai).e(esnonnEet,scsuqaueldhxodpuiwdtopnynTiapinTweivgwtslhlSrherpyaehlenoflcilitnelsygloekoiubet/hnwnwerouSoesetsesrpaEicmboeltvsoctbloewedehhoeimolstreidli5ffstupulxprftPa0lppmlseoaofrer0ppeeornceuePtidlporemninkotyFfrensgedPiifiOtourect/seoFaoPlLndsArfiBfafFebniwwfilmSweaoOsnlfea,iiaaePpilteActtmdihPFlhelnhieedsFOnepePasHccblAAmFm(faaeolPliStumOalnlpocPlld2naaAleoupaHee0ckslclntldo0lSehtsade(lewnaXctocmwdtimoHPtceaan.iinLalFiolpDlnllttaTOnolrtienPehoboawhSAr)daeEneslset Page 9 o f<U Exygen Research Page 50 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exypc Protocol Number P0000760 aenacdhhwigahtelervseal)mfpolre e(veexrcylutwdienngtyHsealdmpdluesplcicoallteecsteadn.d Afiteltdhespteiskteins)g wfaiclillitbye, cdeoxetntercaremcnteitnrdaetimionnethwdouidtphlaiccPcaFutOeraAcaynadannddwptirololccheaoslssceokdfobthrerboifuaosgr.htifthieed deastcraibeldowproacneddurheigtho Fpatfwhmsoiarioeziegemltrlicthlhdphplaea-e.olo'slaeldsseieAnlaoiav,aenmtlecbdshltdcpeehSauildeaegefdrinoa.ml/tladcreSotbAeyscipnotfaplaeiitrltner,ncaiodocgdtdPooncaiftrrea.maoteyolcamSacepisilahdnirk,iemiteenoayrcnotpn,rwkh/wldleberoifaosndaovcuegewrcehxgsogbmtihrlusneilaaoatsccabtsumeeh.ttdetniiehpootuaflrnnHeodadC,ardtOewi-EtesosPPiadtcxnlhFEmrylteiOwgobbpbleAeeileoetnedvhatetwecclwxPpelhoitlFirsrlpllcloapOleeaoccecrlsnAtecsteusdtiiodaaofpauiimnpebtrniednlebepwyrolbaditeoltdoeoulhcrlndpbooeeadblwelidelac5les.tgoat0echotwrt0ieiemnpedpaaamtinnchneoLhdddeer Fncfooeoreordterlsiaefmcbhhgaolell(dtauemmbrseap.malneFmdocaarnlesuemlldwivalrelelitrnm,,gtanEmesxeaymrfgueaemrlnspeiswpneenpitlaatler,asEs,taoxaprynpgdtleuypnboewalsyipl5(lrt0oseupdpymplleLolynpea)p,tocuolvbylaelpcesrucottpaiAoymntleetkrnhsieet. twhmseaiisgemDtthihpnsolghledeofivaaaeccblticehluieatfrynoal,adcrebtyiaofpaicrrenahoddtcoEaetrvotsyesapcerhrdkaiennocdotrkhwtsrofeonoreuurcxgmobthrniaasccs(aeh.tmnieotuprnadlCaetei-toswPtcnhFirnieOwbbleAietedvhweePplxilrFstlorpOaacecleAcstdioefuadiherteidebnobadtdteouhldpoeadwldiecl.toateowtremeaaainnnchdde Low andMhaigtrhixspiking SeWdSioamitelernt Fish leveSlsLpfiSook4wOrinneOPgganFc/LgghO/elmAvealtrix l4Oonkg/fkg VeCgleatmatsion llOOnnggffge SSmmaallllMMaammmmaall'SLeinvuenr llOOnngglfge sie defined below: SHd5Oi0gc0Ihm0PnFLgO/eLvAel 4400nn*jt//gx llllOOOOOOOOnnnniggsVf//ggga 100 ng/raL Sp"iSCkOi-nPOgFngOL/LeAvel 4400 n n g g /g /g 1lO00Otnigg''gs llOOOOnfnV^ftt lOOng/mL Rlaaencevcaceuloylrsvas;iecshryioeowwsfielatlvhmbeeer,aqifnauitclaielcluiietdpxyeaadtccooitdnnptfrtrooeocelbifseisinaoambnleprateloepdusomratdc.ecs7uc0rraKibcyeadwndailblo1bv3ee0.)d4etAoerfmsttihaneteedmfobernytitftiheodef PawcraicotuerrratoctoyaomjufpPsltFiefOyaAntahsleaymsuipss,leesso.lafTbohreCatfooPrlylFoOcwoAinntgrroeslasusmpltpiskleetsositrueedsIytnawbblieilslphbreepprcaeorcenidds:iuocntedanidn bog* tO oj 6S Exygen Research Page 51 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygrn Protocol Number POOO076O Two control watar blanks Two control water samples ftxtified si 2JOng/L with ''CPFOA T25w0oncgo/nLtrwoilthwPatFeOr sAa.mples fortified at 250 ng/L with ,JC PFOA and at Tatw5o00c0onntgro/Ll wwaittherPFaOmAp.lei fortified at 5000 ng/L with ,5C PFOA and TVPeh0re0fl0ua1ob7roo8vo0ectaaeannmotitptclteeAaddadr"eM(PteFotOhboAed)eixnotrWfacaAtteendrablayyntdiLcCan/MfaolSyr /zMeddSiea' ccDoerdteinrmg intoatimonethoodf METHOD FOR CONTROL OF BIAS Chanooamnlytorzgoielnnogefoabtuilsaeaamswitxitltwluboreeleosvdfedelmascoshafemfdcarbttiryfi.xctasfktriioonmags.ruenptrreesaetendtactiovnetrjoolb-ssaammppleless, afnrodmbya STATISTICAL METHODS Scatalctiusltaictionwoilfl abveerliamgeiteredctoovethrioesse, asspeacpipfliiecdabinle.the subject methods and to the CLP STATEMENT RrtTsAEhetheaPplelpniAesdrasaeatstTusprsoeddtSenra*ycCttdteaasAawmtntiovadaeGfesnp.wtotahcociiolksdwlnasdoigLltuuuleactdbl(tiybesonuderesaphtpmiaonsllriilygyecbndodPeetmedrovpapiectalhrbtitfiaeyicooneSrncmpestShoetienwdansniaotdtSnhhra)tderuscddrihu!etyaruprl4deol0nyDrcttoeiCfrndraeFotncaimRndtionrct7aahop9omsap2stn.lapeidctleiasTamtbnaShlenceepnedotaGfnwrtisdhLniostaaPhr.lt REPORT AaIot,tfthibneeaclfobrnellcpotowursmtiowgn:ilol fbteheprietpudarye.dTbhyetrbeepporritnwciipllailniealvuedaet,igbauttcwr oilrl tnhoetirbedelaimiginteede Pag* Uof6S Exygen Research Page 52 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exyttn Protocol Number P0000760 . Tofhtebnsatmesetinangdfaacdilditrye.ss of die Study Director, Sponsor Representative, and cAhasitna-toemfoeunsttoodfy rGeLcoPrdcso, mmpulsiat nbceein(athneystruedlayterdecodrodcsu)m. entation. such as _. TAwhseesreurrsaeingpcnoeertdUednatinotdrtheegdaSarttdeuiddnygsDdtaaitrteeemcsteoonrftasnbtduydMytahinenasgpEeemxcyteignoetn.ns aRnedsedaartcehs fQinudainligty! Atcinhnoucepdmoyesrbuspoecborrfjrieatapchnttteiedodmanpeinanotaghtfleoyotntdhtihuecweamelaxrbsmeaepfcreoottmhlraltooun.dwsat.lIeybfdtAetihceinanexylcamclcmuoteldontyehdd,doiiiftdtioicoinaisnstesniopaeenchmchoepnsptlsowaoagyretehyed.idastocimenidnet,chthletuohdsdeteuwpdoriynol.lljyebcIeatf Description ofthe instrumentation used and operating conditions. AildeDveenrlte.ifsiueldtsanfrdomdiealdlasteatstaabnlealwyzileld.incCluodnetrsoalmanpdlefnourmtifbieedr asnadmpfolerstifwicialltiobne aRcidheefrponortrmietfisaifeeitcondagtiatrnitaoimavnlesllcceohhvfrreaoolm.mstaaaTttnoohdggearrraadlmmoacssna.dtfiooarnceootcnfhtrtohalensaaalynmtaeplylietn,eaepnaedcahakmschawrtoriilmtx,abtieongccrlluaemdairnlaygt Adsllucwiriclul mbestdaonccuems ethnatetdminaythhearveepoarftfected the quality or integrity of the Location where raw data and the final report are to be archived iaDaAdlmtiederneedrntaciidtttfiioymoornnteahsnn.aotdtrsptiThcgaeobrntreeSrodpeafcobmttnhyioeseonnfrordseRempteooSeprntrtfuteotdshewyeaniftDlitlniaisatribelbvceeertioe.snprig.gonratTeltdshehreeaadalnlmdabneednddai(tmnheedetnhretbeayssfhootanhrlmsle cfoSloertfautrdhalyyne SAFETY ANDHEALTH Laboratory personnel will practioe good sanitation and health habits. Eesuxvbpetortysaunrcreeefasos)of.npaebrlseonpnreelcaauntidontheshaelnlvibroenmtaeknetntotothperetveestntorinraedfveerertnecnet Paf* W e f t ) Exygen Research Page 53 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: 1*0000760 Exygen Protocol Number PQ0007&0 amendments to protocol ApRtcsfesOmRhatuhlfpeulreaefelpaliplrepndtgonpiehcrryistgwoecesntoisisegrhssadvuepete.elanideelnnanndsaiCttsStggdonawauiopceattfdniiia.tprdvctv*eyohniooeeweHvwptc.p.osiaruiiodrfiAecnomiwteshwttitfmthd.n.aeeertegnvnhienwAt,gtenweTtaiaerensdlth,mrsnilsyimigeoiwtbepndtanoteenhomeoeetneddtvrddsaenimoiigtanagbaucaemitdnnneusinamocdueeamtehn,ldnaaeneasdlndtsalndhnaamayafmtmgatrlneewyoetaeeddadntmsnciniitlcahdtbtlsdnae(wamorbyhaldnewoieteelgqetrnplniihseuedslrtbtpelioasumreouahtwdebSotoeadyyttpitcdbyeluaoowpldedppbtlslhibarypspetdieinheoeorabDeoonutrolfemSmudetitrflr.etoteioapeufndcsrictifdentuolnItteydynttfomoidahftrtiiieatoachnvDthalhtieeedlienitierodshrronddebenecatiecawsunoStSstlwtimaolrsipmfpytilierobyheols,eltnwtnunuiatsttctsfindehhehoootadhdydeeerlrr DATA RECORD KEEPING Records to be maintained include the following (as appropriate): HSSDaaiesmmstcopprrlliyeepttraireonacndcekopipirfnteagprneascyrhoaemrtedioots(dn,ii)softiofcsraattaigonendh!airtsodtostrh(yse,tomacnekdt,hcfoohdratiinfiscoatfiocun,stcoadliybration) AIACSAnahlnsclmrtaorcolupmhynmlrtoepiolceelomaenxglttateidrnctalaoamictsplattpaiiiotnhpraeneghbseaileocetnnasfdat,sanbtatudienodnainycalyhaopst-eftrs*ruahsmdleolaenostttesniutseaodllr,ycalcooigognnrsdraiettsuioprnoessndaenndcienitiais Any otherdocumentation necessary far the reconstruction o f the study Chromatogram*- All chromatogram will contain the following: a oSfaminptelereisdt,eanntidficinajteiocnti,oinnnjeucmtiobnerdcaoterr,essnpoonwdionrgottohtehreinrudnic.ation of the area Athdedsaitmionpalellnyu, mfobretirfiocfatthioens!awmipllleinthcalutdweatshfeoratmifioeudn. t of analyte added and cAonnacleyntitcraaltionst(aan.dga,r(digtacahLr)o.matogram will additionally include the Pag* U of63 Exygen Research Page 54 of 110 Interim Report #23 - Analysis o f Sediment Samples Exygen Study No.: P0000760 Exygcn Protocol Number: P0000760 * AainnssatprlyuantriMtcaoRlftsAeemto;odadoitctujnonrnastehnsothcaetbeoltinsdtteibnaegerftiobbleilnosgwamtihnpeglesInhssetteortusbmweeninlmlt btymepitenbcaclnusddeeotd.paiennradetaiancnhg conditions. All vplicable requirements for reporting of study m ilts u per 40 CFR 792.185. QUALITY ASSURANCE TtSothuaedaQyauDAreirUceocntmiot rpo.lfiBaBnsxycygegcweaniMthRaGensaLegaPer'cmsh,eannnot,dliawnindilsltphreeecpStotpshotenthssoteurfdRoyledapitrneignssetenortfvataaiulvsdeai.tdsetqoutahtee RETENTION OF DATA ANDARCHIVING Acwwinhliifrtttohhormhtmhtahaetreltdiodogaontcrraaiofgtmppoianym,caklwtrahaosgewtreukSdssphuydoebanemtpsatlosi,a,trnt.ec,idnoacrtmlorueetdshnpinedogmnS,dteuenbndtuycs,teD, finiarnoenatcdltolrrriee.mspuTiotlerhttdse, sseahtnowad,lilllatbhlbleee painoercrcrtihliguniivdeneenaddtl Te7slq9hsu2eoi.1pbt9mee5sekt.inentpAg,tnaafntaedcExixalisycttytgocorsaonhgpRaeylelloeokefgsetrsehepehf.omarlalttheeerleiacpltserrosinuoibdcmoriatftwetdimdtaoetatshpaenescdtiufaidenydydiiinnresct4rt0uomrCweFniRltl, Erextuyrgnsinngwsiallmopbletsa.in permission ftom the study director before discarding or Exygen Research Page 55 ofU O Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygen M unter P00QC76C APPENDIX I ANALYTICAL METHODS V0001780: VOOOl7 8 1: V00017S2: VOOOl781. VOOOl784: V0001785: VOOOl786: """AAA"AAA"'"AMMMMMMMccccccciiieiiiieeeeeedddddddttttttthhhhhhh(((((((PoPPPooPoPPoooddFdddFddPFFFFOOOOOOOoooooOoAAAAAAAfffffffAAAAAAA))))))) iiiiiimnnnnnnnnnnnnnaaaaaaalllWSFSVSilSllyyyyyyyiommeaaeaststsadiiiiiiighleaaccaataaieelmlballtfifffrftyanbooooooMMebtdrrrrrrnriLyoaatttttttCtChhmhhnmhhhLbl/eeeeeeeyCbaMmmDmDDDDyDD/LaaMSeCeeeeeseLll/tttttttSML/bSCeeeeeetMn/nyrrrerri/MSvmmmmmnrMnSLue"mi/iSiiiinMmrSCnnnnn"Maba/aaaa/SMtbMtttytti*iiiiiiyooooooo*SLSinnnnnnL)"C/MCooooooo/M/fffffffSMPPPPPPP"SeeeeeoeS/rrrrrMrr/fffffffMlllllllSuuuuuuuSoooo"ooo"rrrrrrrooooooooooooooccccccctttttttaaaaaaannnnnnnoooooooiiiiiiieceeeee Exygen Research Per*li oja Page 56 ofllO Interim Report #23 - Analysis o f Sediment Samples Exygen Study No.: P0000760 Exygea Profooot Nimber P0000760 ANALYTICAL METHOD MaftHNwfc: VQQOITtO AarijitkalTWtFaiiiOr: IlflCMMI tajfiM w ch MmHRCMWIHwch. PpAriv14101 c-Ak TfM*MiC*MI UirMr, LOW teye* ySv!*/$?Jm T ' Vitfw iiW Op--BWinrt frw--cfc bvM DM -Djud u k. M hp; 7 Exygen Research Page 57 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exyim Protocol Konter. P000076C itliilNwfcar VWClTlC 10) lett LCooffrNCv/Mftw5vooOBMlc ACM(PFOA) imWUarby I*npi*e MMbyIMWi c*0O*fmMbU*km(mLmCALOfiqMearMBft)cPWMnC--rm. igai^Mhjw Mo/pwfhnMCMMie 2. farpopvufcy 3.0 3J..54 3. *SpA1nm1*w<r--j*wba*a.yiaaml*UfdlmaaOccbmn*wakqaptmOttwtaowU|bpmMnMnaaykaadrli1aImimttoa4dgaHk)abbncc-icMtlO-inaioip.bT.k-jar.tlaund^-3tit0a0i0, *,,*. -5 1 far uu *0 I^ M iria a W ) 10 **U33 MNWipraifaaMrrin-Hiwii-PiiawmLATCf*iaCkaaaAdapa-rAid*.-CS.Sly.lMaap<aa*<k<>aada 5.1 112111S51.5.544?3f 2nlIAA5A1ot05mildL*MlMfUJeyLwLj*m|Onh*AMil*KMfbUwPwIiBLidIlfwNCMlbiNpMWppiWMpfMMro*lcf^trl*it*biwnEaCMH{nJ8--mpOirIy-WIyIMhitOmlrowbOwtwpohb<bIUHi^dw-m*ftM'Ma.ioi|*>OMi3NwmOo0gOymn0*OrlN0ie>ktv4mbiUb0u^*1iLijsmmCr*MbqUpS>cMibnohSfa)e.piwfmtncf.ujwkfi* 5-2002 111110 AViwmplfjcepmPa(IkSV04aIeO4O||OL el)iOIMI SPC>1e1mwiCi*pa*eeMbl tea. P*gtJ7ctfM Exygen Research Page 58 of 110 interim Report #23 - Analysis of Sediment Samples Exygcn Study No.: P0000760 Exytea PtokkoI Number P000C760 ! _ AHALYnCALMEIHO LCAd/Mft | 7 J.U SfB to n a i m b IM . S.U Om riftp pr t lia f iy ^ 3 0 l>ofrr a U tebw 3000ty 11 Andytwd O if c i >hn>*m O (lU y M n i Irin id r L 2.1 n <W i:BS J2ljO > 12 TtopoNoac J0*C 15 W k t a W : a M J m tP nsA corn ia W tor 14 y * a T U e ( : W.Dm .1 15 G n tito ta p v Sm AM J 10 U) tA aoo 33$ IL A <5 (5 IS 4$ FU Sata H I tfflL ta fi) 3$ 0.3 33 15 75 1.3 15 13 M 11 U U m ilili v a --: IS v L tu a te iiiS M M d to M iK iH jB id 1.7 U Kb Ud c -V m m t eap*datteoffWMIPinIoCrii)WaniiaI,rn m u pt aodm y W cU ajrt ter MSAtt 7.1 TOfUtMUUMtlMMMSdMUSeiwpnan.* U M s r a d e U M y b * cUp4 to 19 1h1y l iU-Ur fOMvPUi nmin i to1000mL *fwor. fry Dtiiat 0.154 g f Exygcn Research Paz* 19 &C3 Page 59 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Bxypn Protocol Number. P000016Q M .1 AHALYnCAlMfnK LGM&M5 Add (TTOA)in 1oi--U>f --------U-k- -H--J-^--m---L<U(*3mWsk^*jkw. yeily)iidikkto lOOmLwHh .IJ .1.4 iImAAalL0tl2.J1<91r2fi5LIngfeUkMtL1L>I0NPLhMiDtOjbtMMg0htBIebi,MLfioMhttwih*Mi.ktbiwolrbtMutefuWcUmfiOaOdioAAvkoiiritapapwr/oep1ft0Mtb1a0wi0JitybhuWym-rwurm^tlf^O,uonnarmifmiur,in*,I 11.5 AOOl piataLtH titntmmM m fOA li pr*or4 hyMaa 11.4 w10wLiofa*lU *(ULLMD illhi qNfhlUO M fe 4 (h a i n h m o f oo w ** Ag pofOMKll>i WdyM4*CtohdMk idItmMIomh 0o bwbioimmmbpo*rteidoOf oiommoraritot HPLC wutr Th* MJ 1>0fcOeehl ii typkal e v ie OOWwl jmybt ,,xastti-**MIiCM1140O* _--_t4a1MIeCMoOytt_______ 444444a000000_____ m M1M20Id03M350OAiA00ntjana| jfc* m nSrfT XCtwidyy.1 XXXXCCCTiMnamrMhnMiy)Yynj.4f*3i Stn*sttkMio0llPE). Exygen Research Fgt 19o f65 Page 50 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Boten PkUocoI Numkcr PCCC0760 MMbritfAatoufcr) ANALYTICALl*rtH..O..B.. M IUl i u t a iiM jHam l) I MJ mKtmft 94.4 *Mrmc dml 4CKM, aMpdotiwfcw td 94) Ata * MI*.e!* W M I d M M M M M w iWaolCernlwM)iwli ...... pwMelewviiyMihBkeekmmmb M d ai b e n n o M n m (M bw cI pik n * * iiv IW P !* " * ** * * -- >* * f * * will k " ' r i h r * taBX m*L "r tLiy m n tm.***or*w.of.m(*M!H*>hmo4mHMt0.m,*Lw*.lknw.uma .1.1.1 9" *"' **C* * n l>. )**U).W^HxuHfccfo>10mLidIjrm>i-Jl IL j LndM pk c n tfiM n d C *3 ra c a rin d fc . M cactliM t. 11.4 n> kU -a|.lM K M IM . CoOt5LgrdMkUn|hud t u * fr f lu mim lO U tA O . m t fertlM Ulapk i 3 ) *AKMM*mki*Mi*mK<| mlaaadOfMiAfi>sKMstfaMcMpttHdlrHitfifcBtaMVim.pmaittaMnMilLivlabUorti iw i f i m i< M w > fW ty H o jm ^ U b A fM a l W inrimM the **M, di M*taMrr set bocf a4 .<MUW.*.Mh*.*.BO.l.i"iT.Mi.d.B.**.^.My.*...*.MM..W...d.MM...M.M..M.Mr..f.t*f.bcB..l.aJ.b.wi.Mf..ilM.td.*wd.*iMMhwmuMtiimfmrnUtip^anmmimte*BoMimttwM+tryMMca5a.a1mg,x&apa.metitd Pag*20ef6* Exygen Research Page 61 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Bxygcn Protocol Number. P000076C |kkfftieiitwedKtekAtefrteteteDiAwNtAeLMYLrTCiIcCMiASL/MMtSeElTnHMODicteteM^f*fTMO*wb)wiiveWeini7uiety | m m a te m te mmmt tm m a ttim mta$ tm Lym 3 3 <or qwvikni) 113 SiacentwuprUanmimlyntfiewctmewiptenrmi*ciMitermi*mAteMteatret*eiilwte^imki itm. mAaniyymM.inpto dw no AufBiowi 13.1 n r--4 UM L|MItiKe 4te13tet a *opwtroerrri>i*wtepsiitme rt>it ea* p3f4o0atemmteym, wuhttliite 1SJ ItieitUeatkit*liroUltieatTbi PfMPf O!*t*e)iffmeuriiTriiTpmfWlhmOi ATHnmnmiffSe6nraritjirA~p.n1KwtimTr:t*e-eiwitMe LuOkQim. *Jf*i 13.3 fttUeewfmMcutmmeAmltmerKiirnai etmhetpeiivriOlmtfenimkNcmi--i*htWyreitttpeA--gmmafliyfae*lpHurAMo*Kyi mWtmuiwtnmeicr>tm^eiiktMiee7liHmUt3eiiQtotteeHm.o7t0f 13.4 Aay tM rmm m m M femri n te * ite te li rotte by u w | m Mi U J fkItacOetrpemLtiOrrpiitrttmrie<**I*mmAtempNmaeir>omtOeeottrrttoieot2lti00et1Uet4teittene*idiri*aotdmleifttieit]ettMeeetiatmeutvmeeittieteyntpmmeamei itrnrftiii,marinot.eudttaetrhbtici Il* tieMn teifcf otret e MteuOtteentieMoattteenriea teitietemtealptetmraomntiey nd. km drft man thu 14a%rijltieictrei ntee--tesfrttittteena.tIefttee tteeiiMialyUmndi.te i m orii i t i iritt w*tM 14.0 Cinteteli l.t fUt^e--itletteemVtyptifereiMerMa*mwI)tLtm)eHati$KtItuettaietmiml liimyliiiBtcpetrwmi>m: {Uinr*iWnpPMAMfanrop*afn*etnto^nLi. EST (te a r by r te te tete ro tirn r w m dUriod, Ifm cm a ry. Put4ftn Pagi il ofS Exygen Research Page 62 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygm Protocol Nwrfeer POOOQTOO I HMnlafAMfrMfcffc.DAMWMAMLL.vCan.MrcfSPAMwnfSatinmKnMumnliiUypKXMinWlfty | W * f"c"HwM1Mu pMrtnw1ttlritlaumlinlii fMc pMM lmfPwPOA;p.im OMian. nie MlXMdMUifU Exygen Research / fr 22 o f65 Page 63 ofllO interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exyica Protocol Number P0000760 ANALYTICAL MYEMT01H7OI1D AMM4fAotfcnbJtr tOftrwnutarLdMGMrfSfMwffttu w r m ite A*W(FfOfc) laS*Uy Am btaalTaMf fro lty : BWSrtyatitwKo--Cwwaane^r\etfAOcrttMl 9f. T U , C - J i . ____ MTMCcaMl Ul;4ar,IC-M5,Bay*pa ta w tk / Vi?wiMw^ Opaatw---,--8--i-/--y---K--------i-f-t j 4 l Exygen Research Toutpi^ac 7 Pa&Utfto Page64ofll0 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 fixygtt Protocol Nurobor P000076C Multd hrlw AlUUrnCALMCTSOD 10*4SMS e A*id(PPOA) m tot by 1.1 leapt u **? tr<ieO****d"o"rO*C*M* lS*iqMm*Sd)>riMnmil. pqdilijHr t"tmiMs adorroflnaxUMMKui Iut C**1f"-i)*ia|>,l1>Hl,<lmdht>m4tDtr3jl1rrr.fli..a-.l, .yd ..l fa. t, 10 31.J1 H--l`.T|l'|l'ifT'arn'im^.IidIdk f cri.in.lin .tlii U > M p n M M d to a n d D w illM i. room 3. X3 IAdliy toiltaodtto damaMid iM raMd itcoaddittoofda nitno1n ia--n tMliMfe>rUmanftdp.J` AO AtalftMViamrt-KtarMtCivm. *OAj4 uIntniinlii-aiuiamrnnl : i A.lili -f4i|mMi >aaidai n uK m aL L S N um U a10 II 1134 11 1I 7t AAniknilMMmqw*MMi*gltr*|tkmma1A'tlq|fUncoHimiIttinona*ttttlo*domi tpi*1arnoql*yli.M4pl(qn3alnut0>Hlio-dfl*fIiift0l>nimlOipJlLnwHma.iMAn1in0qimIl0lmfm.Ma3y0gin0i.00.tli0HlMm^fi0LM0Iem)aL1.aOp.gHrV.MoI^Stii'MUoaSfImp.oofaivntout fl-to02 lAAdW lCriollal. 111*0 Al l pigt i l (100.1000Lnd 10.100ulltwadapootok to. 111 9 M l V d <*<1g)iC lt S M 1 1 111 M v M d M113 UH t A tioiori Pat* 24 oft l Exygen Research Page 65 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 exygen Protocol Ntxnfcer P0000760 l APULVnCALMireO LOMS/M5 au Acid(PK)A) a S~glb~y ] 14 CtnauiDf^UclyvM)J..(U4 CWwfl*lmicd<toi fb te otyanin| SOtaLpeSyprofrlaantm M5000 cpm. 11 13 ITbW{Qw--hMnlhydbeiifUli--beirWfannCtsP--iaMniwf9-cp4id(x--Amn)r)i::c:ixW) eM2tpeMfMlnAateWml m{TeyMA--eMWfwelWiieaXta2r.1-- 30 16 fc^weinZO1)Zjo0i4VJili--r lJjM%6iO2teSs55AfcetaarMuM33773533354iiKAiahoM61616v.3333J3fw0U)*liL). 17 QunrtMbia feakAm ~tm daaa4B 4*tibM aearTa. I I H H T te t t le in if . VtWtteiinCDKea./ " ** TW above B lfe ilM V e M n M m e p id a n ls a g r to cfeaapd ordert 7.0 M S/M SSytf 7.1 Mel: Bocfcf n y N y iv t bCEMwe4c, loonitom n 413 - 369 toft fot FFOA. 10 fnyrtiefSrhii--iTytot*eb*eevS*rpKeiSrinlfalesyaileaBto.roled u apud* d w*y to cbanfto io order to 1) MttMemea L U 2 BM mummte t water Jr yr^an d by adding 0 15* j c f ace (1MOn L fwater. A ta a tw vHb m i aay be$M penl Pag* 25 of65 Exygen Research Page 66 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Bxygen Protocol Number: P0000760 HauS ttoE ICMSMS eAeM(rfOA)iMlky 1 tmimAaNffialli iMfcJi 9.1.1 ** * fJJ hAA*mfiLWtt*LmfvOt1t*pm2f\aEpt)Mtiiert*nL1.le0LAA0*tUoDmMMlr*AHtMiifemmflbele*aLe*.tt(t-Lffiagl.I0ialrOmtarMitMOaalMoM|it*|f#iaaatTriAfTj.FafPnlPrfOiiOrfv$Aro)AmmQsfdcpdMAptifbWmyp"wLwONiwObyw|f1rihc0Mdmi0eamwJ|fLMi*lOwj wIiiOiohs MA #.U AAlIUil1(2Mi*Lk0iaLa1)aL|OitijilLgiM.|tUtOftiat*DrLtoQat.Art.tBfMrAorfibartLlCfTtilfLlbbMat..f*DslLnMtwmMttaMlkMMm*fIfrMEF>O1AAmii]aifynotl^pMifMMa di*b--bTyyl1^bn0o0-wi-w^yrinlf9ge jFltfcnufrr e m a m i mbk Di Itlimrmy itt ft mfl .2 fallimi nifcrti iltiliim >il IXMSMI m fcntkm mmimit n |npan4 In HPLCaur. Th* **2 TMWmttMWmiitIwoio*atfaaaMlatypamiu)^ M w Md w |ili. tkffM |b * tts te b o a poecdare. i JJirto--I oacaMiou nuy be fimiCimmm+in. fftn ifin bai to i- M UVrt*Mif*im0nm-- 110 Hm*tm i C iw ttl r a m am n CaMrwM f V nM tfni.) . 40 49 i Cbbbrnm & todiD XOiwMyyA XCOHdr>'l IN NO 140 49 4499 INJ# X*4yy-2 XO w ttyyJ * 4 XOwNdyyu HO 4 w ____g L 40 Xi nCn-anaiwl i it,tteoaM--kiuowfllMtoutfttabmcttr.iicHain rtw mntoIrWMt N1Orwt la * XCM NM XCa*AWA mtotiw [SPE). Pag* 76 o fW Exygen Research Page 67 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygrn Proteeo) Niunbar P000Q76Q i Maio>itlW- itefafcOaAa^ihiriLn<CrcffAttttaLMfliSogirniBotaail AaiifrFOAtfSolbT | 12* fc&J AmStAatti2a*aa*nafCaanittfamaatfafmytCdaoin*taa.tta**aaatamitaMoktSwt<ftacocaieoioM(itonakiMtaga.trantdaodMotataitcr/tt)oaBtUt at-mtdJLf tJ W lI t* ach palypppyim* * my bopropini * ta t Ba1tta IBS SjeBiBtaaaeaaimfittnraaModrltMpUaiitnftHiatBlkdafnuoreaitemfatftamactaraiieeonfyltlpamd6fkatittraaaB*artoriatnp*n>bcttMbatadacanraktiaka*t(toealetpayyiwti*mrtb--dato$aytt--am2--L00to*f--MIodcttataam)dhmMpwil)iawmptiiatkibaya)twipedawacv>Uefret*iafm*yi IM MJHUJi lnl.ji tl.J T<--BAVOJBLb--ielM*U--rMMdan*iol*5iia|h*wtf(ilBttd--arympLt--abtp--ee(y--tik--TattJi*aaf-)ameatIiCanmtDuMaLttntenoploaaMSast^lermHaePtlMatIPmtnapdacttlkaabbin4--BttoMm0aladtt'Oaknlmap)iieLtO.nntpa(k*otaooetaiintayaZpatap$atmmar.roiowfiiilpaa^a--ynnaarLaotenedbt}k--)caCobtDyautMMoatpBrSa--atPBa*MhErrtatJfaiotilmanargini-odaofna1ept:biano*aulL.y.at(pcnhtruaotwOdt*pii<*ytsdtaylomeynnoneii 1IJ tt.f BAIJaodnLyvtpatowato<nfir5UoapatLfaada1ai0ic0--%ilttwnibmaih>a--nt.ay1tUa VC{OaUtntStaaAtvaioS5t.oml.-oSf arottUa.* ina paduatoi taMta ttz.1 \U af122 1I--AhtnCoaaataMt--iIyia--Baa---fit/miMatMfairr*cimttilP--okIFitaaQMt#aAtiainctaaaao--nmMrritp/)icod-tflatittiemfaoataplitaea* iva mtiptaocoiltiati aMnadtpbteloImwa thalel orman maaantrtatoal***k ana fe tactadai aa tbatt fepSvO Page 27 of 65 Exygen Research Page 68 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Bxygn Protocol Nxrabar: P0000760 ..........* I StobaOafAaMtototoDali*iMnbui.amaIlciOi*iaMif.PIaaMatfTlttaMaiaPto 7A cid fW O A ) m Sod 114 11] ->aMMbU|MMn-a-MtaM-oambM-iMlMM1cMaa*timtqMob*aMMt"ytM!oMt.'aoMMaaia*la.iMbalI)InMMHmIa|I*bMlaimMytmalmMMMllMimMiiaBatfro*a>*aMMamiyMqMao-raaMal--baaMtCaaioLiH-abmaMbliMaim"UMaM.Mtftwo-MiH*ihUi<i1(mM*laUiaMtawlat]airoiwriiMn--MiaMt1l|aAMXin1l*Mr/M-O(icMaiaS'clai-Mga1<cf,0aapaal0Msaavi1vKcaaavtIivMacaaMaMrkviaiil HI110 A101o.1c1MX--kUbMtaaoaataOMdMoaraKabtavC*Maa4attrooMnn-MaaaaLnata-WMalaof1t(vfM--ot9TMabIB4maWT*amM--aOmat.Uaonfl*aiatlSV-tM)otaaoolnmivaTm*MiomwaanaloTaap*ajalbmMiaaabtafyaaaap-daktamtlaFoamw^ffmtOaiaaotnbaAtaatobolad*y*tiiaaknM3daol0awau.aM.aAam.hiaa.4n.pyM*>t._l.oi.XMtattob.oouWaa*mrilbnxOtuaaoiAnapifpiamtMiwilkotaiaooimaaoJomi1o.Joiw*0-4i|u1nQ3atui0okaa.KipI7taTaokaf. 114 a Madeal awller by ib< to Mu|t ' HauabaMami.ataoaaaBmMil aauaaaabtaDHaxaafataoMamablbmmniobaarMafiaaabractwoal raaanudldanb*a IIS Tbbaa*nnan(aath1lstaonesasaftlciifaMeat<oKaatMo rmaHmbarilaaia 110 M0Illta4oaaaHalatalwMlajlbaiaatatolotMMaoalMMtbbla--aianatMloanaa4MaatolaaKf.aaataIaoafi kn*yaalaainaMaotitoaoaycnatlaaodpObl.aKOlatoaanHaaalyMaaaaObO.aMU ato*a n b a a aato Exygen Research P ap 24 o f65 Page 69 of 110 interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygen Protocol Number: P0000760 IT f t.o..m...t.h.. AKAlVnCAt>liWJ VQH7H Mahodt/A--ly ^ f c r ^ n iif wrLioOwUaS/P/MarSflunmnmaiir A#*(?yOA)i Soil by 146 CH--lari-- ^an--bylkaMawl^Mcaaavuopiop--; npaiiai pa-- n>m i)4 I Uw X fcixw ti -- -- *a cak-- n *c one i ofPfOA fewrf 0* a *fl, fPOAfcwrftwl)-fl itafinlv 1-- y(K)a141 F*orMmma0ama iAn >ntatawtf iwMMiikine--ilaeiaeai--p wtoNof--PToOvaAryp,rior to cxtraeiioa. uk [--1mh*fand(magbl4nr-tmWit(,*iehiia)<noaocroUa^pl* I4J toi*nI<IffapabW>bwiog a--iraa to-- t tba m o a t of PFOA (bund ia ng/Vto p q a o-- a * ***>* ^mnf* *M4f) - 'ib i i B T T rid ffl M i )) 144 hUnmad*oarMbyiMa ihib|Lefudoa teufe* * mmum of PfOA feu* ia nt> P A fa< to t) * r w ith t - 0 A t d (pjik) I [|* 0 * / mi W a ft)) Exygen Research Pag* 2 ? o f 6S Page 70 of 110 Interim Report #23 Analysis of Sediment Samples Exygen Study No.: P0000760 H xyf Protocol Number P0000760 AM lyoeai 1 W > | ANALYTICAL;MvoEoToHmOaD tfbyLCMMO BMSU^SMIgCRoeROewm^eekPtDbMantrot l(PM>A)te AioeUIy. MTmCtmhablcim^fcr.L&CMIJ. 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Exygen Research Tttthvt I P ettV tfiS Page 78 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exyfao Protocol Nuifccr P0000700 i AHOM#xMrbnyolfQ^aMUr^&nnMnpIoinpneirAca(?-fOA>i>ri<biid | \A U b$$ 2.0 m>lalMM--yfcyHMBin#nMiMM^r(wrrrmlirqrMrni Ofawlln--piri^--bycwpta ft tartcm Mw I1X.1 ACnJ--nwylii>M MwWwPfcfrl*ihMw8fDtr8ybfntfcetxmha.adfrnmy rt--icil fcrpwpw wfrty XO l33a.11yliXSMwpfNtM4mIM bfn m tm iMfretrretfwfr-- HnnfetAwoficiak aift Iw jm fe 0mm etan# nwi#rHm4M1ovnfef>l arwtarianartaai--ri0T JJ fB iM w 31 ba y r i N m the m y th ; plan lor this 4.0 ^ 4412 WAmn*tM-HrOtaL-iC?*LC*|dc KS pifOMOO#)-llMfMtpa#43 CeM(12440Ow*l-*e*c 44 4i f5 4471 49 410 PtLP\a-iMnAp--mnomafowMmtlyMaMAMbh-LfaldlcCOUdU-wNM-:%yifhchMa-Ma)t*-ea-Raoftpfap.Mi*aMdnMparwtdpeai*d* 51 444iM111131BPWMnoiBfhpMMliiM-.SAi.CpJM.lAa Mp tckOral* 5.1 3531 AaAtAtadLnhharoariia#tcjaftMataepafqtlMMifbatpanfWtphaanMQtetMMar--M#tfciHHadao^fpiwtmUtMIfiaiMaMrjaiiwK#AfirMfiiftepctttparafMM--tpOi'p---eOlhaejaMiCqocO4Hepol<prha*cgM1a*nfatgt)a.po>w/Mfptj.atfat*P5-3QQ2 Mag* 3 4 o f 63 Exygen Research Page 79 of 110 Interim Report #23 - Analysis o f Sediment Samples Exygen Study No.: P0000760 Exyge Protocol Number. 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SMiMtwf Mta il iI2nSbaiLd piMwMiqMml nflititufanbyrteftafitanukwtiotaabibaecMmS, Exygen Research Pffg* 41 o f 65 Page 82 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Bryjt Protocol Number POOOOTSO JpaiMiii . uwMmvvaoanu -200011.7 M i|>>, r DtuoiOtuamMfcoboyftPCthffOfaMrtDSOManoxAciri(?fvA) ioKili aad 114 DkO-f1mM0<i Wm m C UMCUWt.nOHMS In.Ou ti uUvlatL6nnla.ald*pa. rra.tofruf.po., 1.1.1I.J1.10 y * P t*MW*1--al0.OM a!.Mo0'>flM0if0Mt.--bh-Ml^OMiarat*fofeOlIeli|a*-tflmO-.oli*blw-- niahial.NOm.a.dmtcka.bOSi.O-2m0Lowdif.eM*On<*m. 1111 **' >*I>P,W|1-- " "*-- 1 --pk t -2000 rfa HU JMJ l 7 kWl l MM MBattMad McoakiinMi t Mh . tn.CMAMn 1toOnMtw, mm, 11.1 loiaao H .O w ngrdalreaiiuM adM aO to.ttc.iM a l Llf I,lU`!II AtAMreM?p-aikay8ia1l!r4*1tiM1aMSvapaar--piidafoMacfaimMk1iHoMPo^mmnmaasaidol'%lritiaiUtoola*iayfMtM2LeMwu^a|LrfakWirioyiobpHfvmIofa^*tac.thfwcila*aa>oaniMt(wka.a<wh4r0i^TiMn3Mftlkuu*oim 111 lOMhAMriMMMlma. mmAMomAekm Im U--MP*i*uk pnadi awdpkMmoowall ,i2 12J eiMM^IwaMau#bwo*fl*ea**ca--bM**rpi*^o>n*riita3VwiiuI|M>Iai*MI0auW`Maaa^^*wUl>y|ep--ioalkMoa*Ma^fM<WIM*Lmma*a*oimiucnMpW*aahMafWeaucoIMfeawbtMfvorltouofmauiaafpusatMaitbycwonaidnarrrfeiitbntaMktolaowaupeouwow|wdKroraUaaifMMnf^udcwienoaioMnarirwinylfrati5*^at-Mh1uwa0 12> lfm 1/a *MnaBofpA am M MaaLjau U (r Exygen Research P a g t4 2 o f6 S Page 83 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Bxygn Protocol Number 70000760 fl HifctmMhtvoaim MtodafAMNteta*ePAiiNtOAoLmtoYmtTokICeyLAf7&LtktoaofioIiHBn<MWaMcAcdfffOA)ruito \ l i i SbanmN<etbtqkodm*mtfootmo *malmaaMubtoe toutrotfo4dHmmApnt oemra.anAal*yyudm a n ta t \M A11c1o^tmecOM 1X2 113 Ib--fMb4a1k*3e*H4m>MmMlNtIokf*fieOM44AUa*inmtepoAbrpa*muwip.miPamaPan<0aiitAtrAoXaMmufeM0aufi.aiJiftaaptbtopriofMtiea,outtotiPraFdO*aaa.mnmtwbuMaXaL.dJO*.e1Q*wJ.0hjnHip4foief J>4 4Am toto tonWtoeiaalamatftottatobcyoatltlootobtetoMeH*it>atam*l. UJ aaafbita (ft) to oilAtaiBi curve* w m i l i **l--l*--r%nt--Bbatot*orlttr*ooaiapt ot*mo*iM*BtoUytwotottoatltta*oo#atttIooaTmtia*oit--ro*iioh4M.njMaulmUytrdtnoit*.od>rriwfMt alyuuMtadop.omt fofitmiItm,oiatniwdiitahtioin Ml UMMtot4Mobo<yv*tntoM*to)*tot*oaaiLA|iyCatoLtMa taayiawyi *tff?CA fiud (ia hj/rL, FPQAtoad to ta P ^ n to tf t.o* )U U to ttto a i|to to i0aovaRtoa a*fTFOa fcto la wstL.to PFOA to (rto) * *toftx(D flBUlPfl PP* fitorfcywtohto to) vto* *u tod, ifnatmvy. P at* 43 o f 65 Exygen Research Page 84 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Eiyjcn Pnnocol Number P00009M OmbrlCMUMi c A c M tn O A In ria k m l 14,1 y*. MT f*ew* tagmim MlnhMpvnMrnWtovAwy. w 1* 1. U* RmwyfH)* *5i555 Exygen Research vi* ^ofw<yj Page 85 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exypm ProtocolNunbor P000076C AMNA*0LwYdTNICA*Lr METHOD vdooitm tabbed TaaiPatyr VWMiHtO'LCWMI MH (TOM) H tBMamStIwCKowBbwekwe>*n*D*artlvitt) A#FvedBy PToo-HckCafove--altLOJMyLr,LCC-MSJ.BlL**\ ]( >* Dt a / M f U / ________ ' Vfegfrwitai, OpiwCBm,ExypaIwfwh Exygen Research Totti Pipe 7 ft*** I S 6J Page 86 of 110 interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exypa Pronoat Number P0000760 afAmtyrnkkeSe erAnfmrAuMHt?nmlC^AfmAWOi.MMm&tmTnBtiOUmDink A (TfQAJ~m Vagi*** f 2.0 MiyTjayn*wi--biitioiiiiDfpftaMlm--r a(pIiCtany/MaQUS0/jMutJSf)eCMfclnUclaaaamofrttyou'uctmimpiM-- i/apM futinfdfwocwMomk X14I AhnnkncaftUm tnutiaiitioti*fcM4wtioirclHHwl*X9nc< ufay 3J fnplatowiaiM 35.41 a$AtmfoMctifphiMflmtalaattaoXitoaoag4.raptiffSaWatdaaimletpmioi6eImfiO*lmapmMAtoimBmtan<rwtttfaroawaia*atnMyopai.alciiaK*g.ttloP.itmttoottiowhAM*ke#trolicainibadaltwtSomawau*mdae*f 3J S--aabjl*a>eeftartojwxtot il ta apanfiadfcaiiplag planftxdu <0 togtowdtoto 4444444444444.1111437341itt1320 W^UAaatMoarriM--HpltfeHfUCL"apC*ti--4frLeMC*)|in*~ i - SUD7tAlaattafaartMcopto*MatonilafMcwi-lat^gtio1UioiifaLiAinM--li&llBwyoCi-wiXaHrKtlfoAKia0l-amibit4Ard-4)1t$i.M-a--<topttUgoiMMp.MeaitpaAfeagt*todaoidaaO**nia 50 h5.w1r--AjpaLMtuoMiO*tipaoi.faiaittiiofhopaaaa--daa*fweittthoS1M4aanMcatltatooa*tntaooapitaaortw(tLecCeatpe0er4MaSap04t<of)p*u*airpyeucjtinfp100> >3 anapiral talMWija lli a fm to n 0.00001 f. Pagt 46qf65 Exygen Research Page 87 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygcc ProtocolNunte: P0000760 UAKtp*fcrmmr wAnJwUnimboyCLACrLtfwrMlfMtywtTttMooOcmPdc ArtdffTOA) mVwaooT1 3}5-.A56 iN iyn^M Bt 30mT Mfrfwpjtoan--jfrf t*U. 3>15MJ3-...J1.1M1u130 WPO2Dt>tEihSiILiMo*fi-Mfswi>lMtMiMULiVm.iW(mpwiWny<M^aNLn*TaCHww).(vi.l(oWwT3oOU--b.tiota0Ic.k0h.MjiU.W1m0H.O7`12OTQ7).U. 3.M C tn ^ a p .M .K l| OOix i (.o ciw orewis>--f.1 u11343 G*WTMaeMaNfqajyUa:Mwl0aia3Pca0tFoR3iriM-Ba0<f3(3ni1BaT1m):CJ:Oa)-n3MMOokMhtimaAaljaafMM(al(iaanaAlaoaUaTtriianmWlttae).ilB 10 1.0 33111.030 (ee22959ss *73317353591 Fkwliti 13 J 001...333 M1U7 lQK^miKiHTOImiwiim:V-e23kHAwaaMkISMABaL.a(ao-baaHratlactnaudoai*eamnmraHOMacairsvoe.: rW a to ft otadUM m ia ic a M aa faida aad may h ahaai|ad A aadar i MSMSsmi M IM > Baa*a<^NataA*MltMiaadacailsna|41]-.Mai':fai Exygen Research P a g i4 7 af ( } Page 88 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exys* Protocol Number P0000760 I . . *AKmmOiLMlTMOD ) M bi .........r..*.w...D..--.....bleyuLiOiwMrSfNMrSflm w ocrwwk A rid flT O A ) V u m "oiftotMto^MmeSWUae^*MWle-rorte* b(to* bdwneedmorierw 10 1h1to 12 a 111U211oio.d211Bqbi^it3o2kf2i0atwbMtHfUi^titUotoiPoNmWbtorKftiilwoiitiO)QotptaUMLrbktotbottfo*wiaw--NdliOmOiirtl*oot.LaiiBlcloirumf^wBltmJikvmropiiknJwpyaryomffplcjOiwwbauytLbw>Myitmo^n|tloo|gftuttfloawMic3.cw*Lk 04 hto n n tfik tm --yb>pnpnO 9.1 gUBttoil 5ol*b-- 0.1.1 0.12 MJ AmaMAM#ltlOLat4loolodo>)wMByffMjtttOoLeooi*t4MLlbaf1w)Orl)04fwtt9Per1MotSpt2ibiMliSijHfMMlctHLofe.Cl(bBmuBwtiona.MoMmfr--e-edmbMwtweoO>tl4koI^i*i*irfmU.nFfopeiPlfaLafrrOftioOtAyvtTaA)iePlemFwpOejsfAvnW1*pb0wy01r0Nwwf0tyi1wb*b|0yhoi0rh*biimnNdwLaw0>g*l*fiO.fejiinni*1*a*0ll 0-1.4 0.U 4H*A1P0e(|UiMkddM*MLBeimia*H*wMtU1n*dfLyitetto4fttI*iwoptCIniLSpmmiwBMDtAiimobW<dLl.tmmitooWMthUotlcotwm,mferw*tbfoifemT*tOoifmeAeaiue)1mNvpodpwiieiuRKpnawe#dilotob*ftyi61pb0nnr0toetnowrcmiht*hit J WfelCbUbwfecIffefeBi 92.1 lfCfkM**1A.0Oufntn.htiotrotWwFBtortOuBluuktotwpwpmd ionh--n)mdilm>on Page49qf`6S Exygen Research Page 89 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygan Protocol Nimbo: P0000760 I ^m_M__t_e_te_o_f_A__ia_f_r_n_a_f_c_r_t_e_r_t_e_m__m_ubiwyUmf/PWwrMnauSwMiDmmiroa ~(ptqa; k VtmiuKm | 92i jaa411Mj44 Voten MJ io 2J li 1 IO w M ote* teL) 10 l0 100 1 110 10 ita PM Cten-- tii foM D IM 0. MMMOOiS M tt Moaa i la lZS-oti LPPE iirrtw mm cfs te te * ay W pnpond m 104 Bote ImUp 11.0 1 50^ S11l11Uaw2J4iplaSA("*B>iBfmtTaaectidia*g*rw'WaJtvabi--aiyl*anHSdantvlLfkeJpwjMyitaoeL#aWftB(ieh*mmKebWBepTM"ialMlpaaM*--atkpimfdaedmtimyeiuF^lrlif0fanaapb**mm>t)mbtid4lem*a*0*(^o0et*ij*ipeupiyyoacBwinjay*heaAmqpewwn*)lytL.irwrii2*pf0oe*acmliyamWnwpitoeadrrpicnbtcyf)ecB*kam*e*afeami*irnfy*w&to<liia*ltd-blch1nbkA-1>htm^*m>cpbifasiactucukifatb*iee,e.*d 1H1.J4 Ui 11.7 *Dt*t*at eereta*a*neatc*mptb*at0*ymeyt*0,*tHan*etkter*irle^fkMat1m*mefl*gs1rgaiit2ekm*Iiae5Cmuofr.aa-?.naBNn.tmtatH(iiteio4etl*nompt meaiCtDmttaoealairtm*ocWnet+tMoaeeta)n>e.tnoOaciultOtK&leetteiBywltpcatettKtcoHttmekakem-af2.tftbaa1payat2Dnte5foewftroniDidurrammainmamklt2an.0iittt2tel*ontt*wt*ati*tetttetealemMmfmetna+ebaraifny-nrirtit.awtteJoeOrac*iatrHl.tl,f. P*&49of6S Exygen Research Page 90 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Bxysct Protocol Number POOOC760 M M (AaaMib*iE ULYTIC4L HCTH WUVM8MS t***(rroA )S VtfManon 111111J.910 ASCMief>Mcrifmf^tLpem^tfpetml9etm0^miBLm*|h*tbm-91A0mWe--m<wlfeikeBwSt*wt5mt$t*Um*+L6%eriK*KBepftlaln*ri.*tW-2.00 1111 D M r| iitifMlMiillatiaDb tiMMl iwV*Kiwg DMh Bi AmCoklKMBtfftbada nttefMe mMm) 111L.1IS1 >1.14 XAMM*tMaMtatMfctaMpMpfcwMlWUMtaiIfKNmnMrbt*BiyilaMMaalt l aa ftA*tmLntLaitoytsfMt2HpamnAiomerft>(a m<m4Am0im*MCp)th.i flaak iMim an* Ho 1I1U-1I5 AItataBtbar*ta1|teMaMmf HdoFclwCarfjawlaLaO*M0S*A0C*4. 1 R*at. 12.1 l imy I MJ fcrtlri Bpli uMathe Ul UJ SMlMe4lWeM4iniaecrm?hfMOmAlmmwrtMmiaimnyafeirekcm4aMtlfme|nlio*lwaialtvdawfia*ekfineew9et aimMMwriiilcvDhw 12.4 0t'UApaaomAmutfmmMnmimMmaMwfbmtmMbamii*btrMANifbtrtbmoaArWaamMM$ttiommoMdmai4mktymtmalmf<anbmvrfjm9btrt--SHottmaA>foIcK0vrotM*aatriayatca^fMbtalao*tMtai.moMI*MBbAamilatAammfaitamtANvimLtfljl^mil.maIlMmnmwAbimdmajwarmtimttM.ftmaiaqOtraMkorBpcaitb5mtMlnm*o1fn.tJ0opatorf*nmrfanalatpaelvltno*etdasiI 125 wSb Mam9acbklaimMAl)nB^MMaiwBminkfcomonoMMkiaaowhtoiaBalnWdWaiiilMfmiintAomtmei*bsJucMlMadmp*wLdajtaw. 14 (oc aquivk*) wAmlyyKmd. p b tto< IY0 A12o1--rmtQmarc^owmMiClBBmrHMmtamta.|(w1H4a9Ha--MU)t1nllyMr--W<iOM^aWtloaltoolta0off*aewibIiNaAtmidliwr3rr4Oi0dAah.mmmmhrmn,wfcriaMre*m8 r*a*r? 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' 14.2 UakaMoaim^udoaBhairaRilaa SiofttO A htad a iWaL a WOAnhllllM -grOA had M(avfallialai|h(nUl ) DP k a a byadl* Ihn fail ataaa nadikud, Hmmmtrj. 141 I*Kfaall^wl aaihbriiaMiiaoadba blaal--n aanpaati nfIfOA poor a a w n i IW ajlSI* [a a la d a a a d ta^u.tyMtoUWad(He^af)a l i.Ma ra|(nKD) Page SJ o f65 Exygen Research Page 92 of 110 Interim Report #23 - Analysis o f Sediment Sampies Exygen Study No.: P0000760 Eiyfeo Protocol Nuiaber: P0000760 AMNAiLMYTIMCArL MVEMT0HI7OI5D riUmt VjLC/MBACt AAtM (fTOA)liSua i8bOMcNraCm0M0f*MtMftcb.t?lkMAvttol A*p**dy TS*lM5Vn5lV5L5m\i*. faij LC-Uy li fc qq yI---w--u--t One /VJoitao*i/FPjlwaltMiLlMri/,0|in/B/n.>_i,_B__yf_I_ww_n_fc Dtc Exygen Research Tctolfepr. 7 Pag* 52q/ Page 93 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 B xyj Protocol Number P0000760 ^9IUnM* 1 ANALYTICAL MEIUOO '1 Um m I tivwbyLC/MC/M9 nAel4(7roA> inSmall to Scapa ml t "i* I f r-- arrtlolifnpA*iuti*CTb*Ooi-ir-o-l-i-P-M----a---f-i.n.. i , riop o*f.p7flro3iopc3lro3oie Uamotauyrtmroal h , pop MpTOMoraakowMOlawMlCyiMriwtiMolaomu15.11 AtiMiSPr|ooMrMUupmoruini>drcWn4KrKaCaT. oau. rM uki Im a 1...1 l'af"oA,r,*.^i1>1"-!nol?l1o-"A?p*.lrloTuJop--aaI^F*l'iaX.nVraoitHaoaMramo*a^arrainaoodbilo<niatavroomualrimlocakrlxMo>iuolatlotcoamri.ortbiooawaMiourfrfoooearedalritonMeetuiparnioHiutioauIlMtrnoocaiiilkkhriun>or l appolaao4Saaotaato 4<444.1411J WMAitmmoawaeMiawmnro-piKo-ManHMxAl-:raWpuaa<:TMLMOpCaatpr-o-iAdt.|.CBJ..li4UttaoiiGtai4o Aulr,"ot*tfor,orotrno*"4"wT1Oia4"valMOIm*mvoiotiuop romrtjUaocOa^aMorUcSaaTpUMoWfp.rfoirnjaaicuo.pj.20u2 11f5.11i1 1D*1Muripatottfaif>rpalaan1au"ulu*iln!i1Hr.Hr)a*rPonnir(orXrfwflit.M|mh0iniioanUut,rolotOifiHMocatfpO.l.0Ol0ato0atrt0to1..a I1.l7 Impa-LuctbuaarWwlCoMatMiolibMi.iuditopitp Exygen Research rat* S3 of6i Page 94 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exypa Frofpool Number: P0000760 t Iafininamllyltiimcaba/lyymwLCfrhAaiwOocfotcCiwicAdd<PP0A)vkoi3eoi7*il5t W5i.n11 Um ww H a^ i | T| i M^ l 4 * (utlsm>cLtiOiOMrUti,dwe*bwf*.posbtetip<. 117 snm m m m m U M . 117 IW h m m . 5.U W mMMteaUaK. 117 C a*rtlO vafctaicvkic l5m Lpoiyp*eyiew lub 3000 fpm i 50m>Sa11 fiM b iiiJ r ii w nnV ! r r f r . j . . . iniw iiiii).! \ m XPC(M tlB O L O K IM ) 12 T m jm m m M M olkP hm O B ): 15 (M M P H fv : tiin tw i) O1.ft 10 200 ZU JLA 5 a 2S 67 Pfev&au & b <mLtak 73 J 77 1 ) 75 0 ) 73 0.3 7$ 9 i 1174 Qhpieb>enehVnerlefmw :k AL3mttL-(MM brtm a\mMaMteddtoiMm&mn&<oo3u0m*1^ 7.0 MM689)tfMi e Bhnexp Nifrtv W.H a attnaf 4(3 -t 369m/z fcr w oa. Ib i Aon N ttiM v i I M t fd and u y b* cbifad i* dar k Exygen Research Page 54 of 65 Page 95 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 BxygeProtocol Mirobor: P0000760 \> ^pIW > Mfpjpf Miljfariba~DMwmc^MnIiUiacamagbtfyNwLrCrfrlMawBSoMwpBwoJg~IA9Mc~*Mi1iK'T*fMPAw)Vi~1aCin01a7H1J to U Iffciitiinfftiimi io NtOtmLmomiwM rp w n d toyMa 0.1)4 t of 9.0 IfIHilt9t9li...PlM11...S2f MiAaAtwtafLOilLf0a1nf&noa.H.l10iZiftnrtMfumpySlcTftialntwUWaioMLrl1lt.i>L0.nifiwd|l9ciiDlimiaa#niyStiiattjef&iHmtointthntaKdiaiiatM*Lt.tLitTiio.(fonLaonialtpoiOat.iorikmTinnfaiaEi-wttrami1etnl0afokiMa9imif%SfpF*Moa*TifmL*lPOv*fi6O/Ao>fAoleWth*piadeOnn>orApAfnoabp1b(ma0>yla0OnvlwOt9aabiutygollyhOibrbibOritmugM*wt>eLtlwaOiwnmiOmpi1t*n*i0l 9 .M fTpWMdomdeMMiMyfACflUakddiana boabiai**A* mraianto# mMeantoy a m o al*n ftife 6 msoopritom I n iltiM o ffa M u p jj 9Mp0m9CbKhnOMlalniaM 13.1 023 TaLVfCffMaaMil anaftmftUwLfatcltOyMpoenodiAmnttwmilri*fliMrmfaOnthiaaMndl im#wo)viaditai oeiilratiM a ty be k99OC.lJ2MfpJ4iciuOMKaMU1.aAS.m9i9l9it/nPufiHAaMtCaaaflKlmPnmlCVbrmne1z1.1II.tOfO*490onomingmaMii-t-mea--drDm-aff*DTmtoim11No*M00Llo#99ta)-m-n-1i-t2-m5-hmaiL.iTiLanfDalMwFrW54wI91mtM.444)o0bIaJaimoaaoybnaoynthgabfaidnlat a*<*n Page 55 of 65 Exygen Research Page 96 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Bigrfeo Protocol Number 000007 UMXwtovWIIU I M ^adefA eafrnalalaP*--ime.lYinnl&-aud.PMiir..i.i.K...woacluAddffPQA)ieSm 10.0 1--MUy i m Umkr n a n a 10.1 I"n k M0 *1f0*oMaMinnI mitaHre)oInMoalirifMr)-3c0aand--mlasiatcaa)amciaMm-irAtiBa*derlaadiutauIkn I0 J ina0-ia--MMyiafacamiWanMI--IfMtilanMpij ipdaafcOicaan n d ap*-- ri ba ----a iri 110 StRfllfalMltV 11.1 I1J /BUiMnd#--arla1ia1frtMaeefil--raK1ndnn--a--rdi*aa>miriiJndOaeeal)iiIHdyoiIm--iCiM--t--tmnaniirlfIHel--OeiiilouaLicnam.--manfi^cmoufU. n(lrfraiiavybUa IM t i n t l l l ai 0 umtlm n ix a OwM i ionia ina 13 mL 11I1UM.7 ILI IW IOWCnPAnL--iMaecladeadd3bineiaalnaMeMpLe--aaiellatya.eda--planiaCOn*eiaaa--aenaVnrieMaE-Lal3--in0C--liO0aMMlwii3pCd03re(a-enf-(aIa3Itrio*-~MgOetatod--pn*annainLMnlOo))ool.iiabnDy--Oeaaeleaain&ncdJaai--nnnrlaalImhO^ibatata#euiinML--nidanla*ildik*md)ea31i IM na--pp))y--v I1 .M 11.11 BU--AeMde.Ipilall-e|0oi--e pnljLelneaeiTninoaalilinlndBnoala.pn*Cy1bl(OO0a--Mcl1O2--Un--LS. ad-e3lm-Lae).iea a pedeacd 113.1 12J tA^nO--leaCaeaaieja--*--dyba4a--dalMnnaanaaTadIaaanaa--daadOdjeed--aOafn--dniaOed.--nlAaami--iniAnciadaainTaaliyldnnindaeaeelllnaieil--ilidi--ailetl.mnun--m--htaMWabnaadd|>bib----lac--1ai--oadarldieaa-ancliaiidafbndi--eneMdha-----a--abdap-alMancailaidmBipal-ealdv>1aae^0eb: 1Ie--nld(alaamaamcncobMnaltmliaaaadtaoabctoyaondcdaeliilbaaiaai!uaaanaMiataBien--iadlmai--ea 13. 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PQ000760 ____ _ Ua4NM*wVWj7|j AWALYPCALM OTOP | Ma4tadc</tal)tatatafrriartata*af?wftta*jHutocAtad(PFOA)iaSiJ 1X.S StmuaaeMhmerpettalettauMeyt*--paeuniutti.ai'top*n4wU*e4a*n*rn*iwfUttodMWCirmawMMdfUMUdpaaowiaLdmym.*mJAl3y*y^(dru.anqpuia'tiaMiNim) 1X1 O f u4B13HtimtaoflWOTMt--o t4o1m1t#townwmp wypwmMXlotatntatOoaipmio^otfUocatuitotoeIitoItWWa tOaA. otua fieni ptram o t. wtai tto 131 M to ito t o OitOa K m rtft mbt oimtPo1FrMuMOMmIAmh*tl9UolWWtrdait*MaaibmtntiaytoatjMaMl*umiIiptTMttaDmitwtNrAxr-tltaatyaAwtoawtoftJMtoooO--imr ttpAiomo*faramitpytlartaanttttottataataoattiaraoUc(bcUrtmawar imtjiwtttaao-WtcaWio<Lkwn*rOatnl*cQaUMut.*B.pU?iftnocaf 1X4 1X3 1X4 ttAItXHaatodtmnoatotaajMdoariraartmMtdeittwdaovtthiadooniti*aatuiM.ua1ttorMadaMJtototaa0itfopWotal*Ji#o3MIatctt4&oatoiemHolntMjMoafattloenioditaotrtoftttlaootonMtrtattooootta(at.to#KnaaottoUoa)aUtnwtmttafaaaoepitmritottlotaUtoamrottaraotmcb*trauuaattlftottoatbaatioatpoatrM*tMiliottoaniatatItatwatooootsmdomiwoiontrhtttfoattelut*oodtiyttrraattotyoaobtpttty.wooooadtttrthtrataiaiAotttKtoobgtoovmaotwunankcmwd,CtHokiCtuaHttntmyttoojoom*ir. a o o a ly ita )n t ita to ta im m b on toa lycta. R I tUantoitaatffmlitkaitpatfamaa`ittofitoffatatlaattaaitoaMrraie(ibtooonfaPrfaOpAantao*top6uowatayUnL) PFA4tpowtato b o b t aytto Kaie LyL* a)eA--wMatattptaat--grraaatpi:ttDFtXque1ftoier BP ftta t b y to ta Ita fra ! ta n ti a m d fttt d.tfa tw ar y. tota ' PogeS?of6S Exygen Research Page 98 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen StudyNo.: P0000760 l&tygenProtooriNunbcr PQ00076 I .......r..t._.._._._.._..._.._._.-.M_.A._w._g.u.U_.l._UL._.yw.n..w.c.^.b_ay..w_L.O_.g.W_n..SH_.T_.jMo_.S__ vUadQPOA)toS*I7 3 14.2 4wFoMamr p^tlatftaabBlpod*MnOki t2immm*bopmkb**iojifwPTiOwAy.pcior w tcnctio, w *m**rrW . (WiMiHlliWIWia) 14.3 +U$wW>f-cl<irtf ^MM>iPwW wMWfyFOAtow4mnf/mLw> w m fTOOA*a**t**-TAWal NhMTtLtt Exygen Research Page 58 o f65 Page 99 of 110 p. 100 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exyten Protocol Numbw: P0000760 AMKaAtei-dTmOCatMer. MvaEoToHinOeD lte*te MAteb* ter MSaidtae^Mlw*titfCPaddlteMeWaM * AdKPPOA)a Saw AuArclTteOMPlater AppatePB* IJJraOraUpCiRitlookojwnt,eePOlanIvSiMI fTwAoCtatkw*mlL*a!te. MCO,Jbyl|ML rUmnt Dt Sl//7? 4 ^ 'V um hm 4rn.0m Da*" S ? Exygen Research TiIFlt 1 P ttcW ofiS Page 100 of 110 p. 101 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 xy*n Pnxoeoi Nuoti-. M000760 [ wmBmmm* __________ M arnai S m tytO M & M S H im * VTOI7M AcidWAtmSwull fMSimpitmOMMrOMiMWtioiri(miiliOwjbnMfiUMh*rrQ*teQ)iawvalrefidmMi m*Hdy`q)mtiMuioiedi otofyawflwanideeercntfcMiwau* 2.0 MSD8 leferc k o rt ! yc&caMcal fdr properu fciy 3.0 H a if a - 33-J1 *'3 NA Mih MM lfolLprfMMMw|^tabaiMrHBiiMrmAi *a*r*t*** * *> l*,IaBU> H **wwp#fcaMij wmiB9eriliwMinat,htemH--a^mwpmrlaiont.i f a n mw> pboifairot wt ik. a 40 I f f d Snodarti 4444142J 4.M.W..M.i.m...Mr.i-IHrilrt-NtiH-/jKtCHopUCmrtCir-ytAretJeJ .t p m Onto 4-5 a r ta M m l iiiA o ii- ? p i A W rt 5.1 A hiph p r t n iM rtm l d n n m e ^ ft --path of puo pij* *p to > 12 .... ftfrN a a p tp rtv ta pvrtaM e r t w hiQ rs*aM i o f V ocimi 5*200 p i --a n rt o l ir t i llm Tpaatti Bi i i r (LC i^C /W )i d o ilu lta llw lMni n p a ii o fM ir ti 1.00001 g. 54 3 0 rt.< n oHi n ty pr epj Uoa com z i ha. 54 13r t . * n m ia patipupijl-- m m tfcpa nbao. 54 T% a rt la < ipipin (30-1001,100.200t). 55.47 2omLmStarHu flCn viHlidi. r t r t o 10 Di^oBrtppoK. 110 Am o^w O O W O O O pLew nO -lO O iiW .w iA^w W adpB. 1HL1IZ5l SVWePmdac8S.epfPoakrVtW t.a ( if) O l M iT riip M ^ogr60of6$ Exygen Research Page 101 of 110 p. 102 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Btygeit Protocol Number P000076 Moftodaf ^ riT a i wwoi ...M..nn*4W--MtVQWl* I M m t f Sm by Aad(PPOA)in Small 0 OraMHtnfMeSjM5i..1l4i CWmMhM1mDr*lUMtet .<tTir o l 13mL UOOOty <.l U T[N--mNlil:liiiaiml(S"ri4hU3r0U*-C() "' ------ . 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Lft PnpaabMdrSfiWoM 1.1 M a b ila fti aorta* 1000nL ofalar. 0.15a | of papj-r* Pagt 61 o f 6S Exygen Research Page 102 of 110 p. 103 Interim Report #23 - Analysis of Sediment Samples Exygen StudyNo.: P0000760 Exyfm Protocol Ninber: POO0T6O UdwdtfAM>)<MfcrfcilA>OJUTimi<Ci Af oLfyMTl<TrU(WOriDnrt>i)or vNOim Aod(PyOA)iiiS^rF 9.1 i9999M4...1U.U.14WoAAI*^rItfwp1eAa1^*L2LfqtJIide9lli>to*ffiMMmfifefNtifMacekLc*Al*MteiUiMLell*HJl4Olo..dlDyOt*ToIf1eihtC&M*f^ol2RJHWihW*C9MoHomio9MBtW--teimiLL(t.rtMMe*itflteiC.tLii*ehnfwetDtthHeiNeoMPtwMefe*Bt.-Mteo1ueMt9oiCreJMttlo*ettt9aeoeediMptikatieefytpoirPPamloaLFiFnwnOlOwio>eoAAkf<unbMP>ottaefetOpewt*itRAuneor^lffpmhiftMyrw1ei*i0i1ei0iho*mhwyAItyoklCbbiifhhwii04MtNwntiHoy1Moptc*rrM(f1ho1r0 9J2..I: aLTfWCtef*tteCalfiftttteyHgdlitel.wtetotfeBHyittetettweeiif*teitHermiloprtywtJ taewH wh**teriti--Steyttbeen lonhatNei*11l0aN0HotMetfiJ mM2199 VM12t11e4999)w 10 DiWUitm1UMOWm0k9tIW12S-*L finte LOtuT/29s1AimE...2l19lLoanow^iMite betta * re ?*teIhBoatti. lofMaterteMytepn^WM 100 B19o.1tet 102 SmEiAt*eiaewU4^wtthweiMehMweOi*Mloteoti-tfa(eU^mM*btinBetceets#woeilO^eoelml<wwtie*thetMwiotltieoemv9pHy<uwt9jeeotmo^ie9MtMtpi.ymroaioOnooooaoertneleolwtre*>tWeJwbrfrtwayilcMitueteehdtotweitpieotKniiotOhwc.ounii F o g t6 2 c f6 S Exygen Research Page 103 o fl 10 p. 104 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygea Protocol Number. P0000760 MmM Hmrnkmvm pit Mm m I ky LC/MS/MS C Acid<PP0A) UD^atftll HO l --fli tewed-- 1U LLLUUU mAhIdadtJg--dMf--cdhaMMd1,raewiaLmy*eliidwaM40Upaotvomal*eddirnrat|fe--lktMSUwOim*U*oM>!t..apHaN4Moy*patetrN2fyruMkeXac*N-enCemwafpiidrk'gheeMfmety.nunbcoi f(fmctcuv*fy Tamdm I mL ft M d| dtopo-H pipo-- Me * 15 *0. )IlU.s i L7 fljr Dm t lnl nf i dM n --g*--nn i mt-3'Mt0i0Mo#fd5i0tt*o *"n-r* Ld T--n--rMi -.----------------- h p rin h lt -- if t p M b* - d add H i fM--ow^ airOO" TrS"aiLi *a--OntCwwrf-Tl*dInp*N-ac})'*T 1-- " I ,w - 1 dry-- ^-- 1 t>d.foHfwoy<n Bi fcptBb*(--Iw>N--^"lam.IUL.tlt UBUaMdtwinif--e -n2h^----f hdhMia--d.CwCgogQeoMctU2idnaL.oDf ndcunmdenb--ne. p4w** ll.ll A--b-- -- ilaan ailn O ip nyLC/WOAdS. 110 CN--i--p^hy l i t IhCjoMctSMmS m trnrnmAofft--twcdfnt--ndtafN-,dniNnp--k udpta-ttUed ainodopMte iom dd*l of111 113 aAd--wi na--td'tddo--io--MmfMtff--dafawfOd<pAihlUio----lpnM--*rti----at atSMpv--t--d,cNtamad-todu--a|odiNo.im--o---tkmamfbal0utt<--oifmifvaedwddoukrdbn--wyouod--oieainatbMb--*Ow--nufdmi------wh--teruanmyn--ldey5evon-elttlxooss *iat-ipor--d--o iy M d a --pi--(Naa--uN fe r n -- -- fit--tends) In M W tin ft-- --4 t--t i--*ci)M n nMowLLA*ywtUnghtio(eftocf^pwenaokriacnaO* norm. iM--.dnd filwoMnaoftaaoneid--bdtmabaodrarddihfratdp----d --. Ailn)yiicla.mpin t hpttf* Page 6) 0/65 Exygen Research Page 104 of 110 p. 105 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Sxyio ProtocolNumber: PO0OCT6O 1ton * J - AMALVnCALH_C__aO__O___ MMN^tavaaoiTM MaMJtawntrljC/M&MS M w c fr > tlin m irfn it M tt (PFOX) in Sae -- 111 Cm _ a fa -- . H r e p o k a f it la if m e * a l) ie h a a n tp a rte ! -- I i nea na ih a f a w q a m oo. aic a M . tMeiUkiiJnMhfhaMifatpiratoPt tnnOA)Mm a1oarMtae*itmll aWfeaO>t i*awmfaailfeawatfIihaata|nfaaPtaunanrl,iOamlm.iexa LMOQUinrke U j fa a a e M a fa e a h o l fa h a e i -- l i a -- t a t a ra aro 7 0 -IM H o t .OaWtrah eWa Hlahaaafalntiatfill hhjraaaaataaiajatat ilaAifyamaatkwi( iteanaMctioene UA Uk IX i ' 1A q r a ilf a M a f a f a if a f h a a m iliiiilo a d f a h y iie ^ f a H m t In a Te. ha m w O c l a ra k a h an a a f t a in a carat. l io n . f a m n f a r i a l a i -- m a i a c a c i he c a d a ti* I w i i a a ilW i a i f a m i ! r o t e a f f i e i a fa m a * H a o eo eM ea e r t iv i (k ) f a t ifa li c a ra f o n i a m he f i t t a p t1 h fiJ O ). I f lit r o h i f a i e n tre e ha In a , thea a tm m lmH f U i l M > ha h ia a B if fa ii n i o pecaliae. ^ r e fa * f a a i m m M he n a a a ly z c i. Xereaneo d a w h a la n l u i * e h i ta n fa M aM d n f aore than t l t l c n fa a fa a a a lj l i i l l lf a . I f .la m ica rare d rift e rrer hit h e ifl rrthid HO CMcsttcm PPQAfcmdMtaL)14.1 |kUMa*aMd*mdfcbjlm)lpTcwtmilMfu)wrmtLia)gaM8rillnarMftaenpiN*u|Wimvm(riiimrfaPrPraOeAnwfaemedp(aui>awafwmwL. xOPirijqmtfrcar 1~ --------- -- f jfn r ttia q T tO AM J Far M tfia Jm* * v i* fa m a i m m prier R>exw cuor. u k *eemey(K)* s fcttow g fn iw a m mkialwa f t r pareva ncevwy. _[_0l_e_m_)__W__(MoaUM-eeeitle>aeffacnaUa_d_i.a_n_a_l(_0f_O_J_.)_)|_mN_e_r_let'1 PagtiAtfes Exygen Research Page 105 of 110 p. 106 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygen Protocol Nwribcr P0000160 h p t -- r> 1 ANALYTICAL m it h o d MmmmI Sanaa LQMVMS f 14J W*- feOMriagt*ltMntDMnvart th* anontofFPQA found m tfftnL io ewp*in k rw **L) Exygen Research flag* 65 o f65 Page 106 of 110 p. 107 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 EwgeIT 'r e s e a r c h 3058 Research Drtv* Phone: 81*-272-103 sute College, Pa 16801 Fax: 814-231-1580 PROTOCOL AMENDMENT Amendment Number: 1 E B to M D Ir OVWQS 1 M "Exygan Study Number: P0Q01131 CofcnlStudyNumber Jjgps ____________ _ asaPTlgNPFWfflOepCTK?N 1)AnalyticalProcedureSummaryV0001780:Sect)on8.1 2)VerificationofAnalyticalProcedure 1) AddtoSection8.J:SectionB.IAMMMtoawipitearatandaKtemaybeusadto prepewattametecnnoerXiultaned toefcaoluBonaa neceaaary. Alternatelvalaof fortMeatlonaotubon*mayaln baprepared. 2oIn)nthLenaotwauapamnadpeiehheieg.htMetpUlkMkeigEleawrelextorafc(htioenanaantdy/toaratofooroewacarhamnaaltyrtixemcoanycebnetaraltteiorendsdategpieecntdetdna _____________H___ B&nOBALE IHJgharcoooanlratlona o#standarda need to ba praparad In ordarto pika tha tampia 2d)oTohmaaaatmnigpnlaearliamavia.iatilforamallmammaltw andaarunaaa malarIhai aopadad. SpBdng at the pra-rMarmlnedlavela In the protocol pula the eofced " 2 ^ 7 Pw ^m lnedapW ngl^SSdhthaconcantrfcmlmMirthan the detection Jirtt Alao.lheaniyietoval'kithtgnuidvM tar protocol. When 8 levels Intha aamplaagreatfraxoaad tha apWno levels. an accurate raciM ^value cannot be cakajMad for tfteQC sample. rtghar spiking lewlaJn tha oottaatM cover the analyte concentrateis expected In tie welar aarryleo. im pact on ~* 10n0 ^ far> 0-1 B*TMple of mat mammal IVer and Is 1000 noyfnLfnra oat mL*ampte ofmaftmammaltarum. fortha water tamptoawtflerwure that nxxaCK: recovery data 4 ! i - * z t" U---------- t: LIBRARYKr.W 0M 122M - E. ExyganQAURavtaw I n s f i n i r ADUIRWTRATTVEFORM Exygen Research Page 107 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 3 0 Research Drive Phone: 814-272-1039 State College, PA 16191 Tvc 814-231-1580 Amendment Number. EExffyegcetinveSDtuadtye:Number PROTOCOL AMENDMENT 2 P0030/0071/10351 Client Study Number. DESCRIPTIONOF AMEMjeu SECTION page1) Report page 11 of85 2) Test Materiata, 8 o( 65: PF08 transttionmonitored 499 -> 99. PagelcM Nona 1) Irwtoadafone(Inallepori,Intatn reportsvrtlbeissued. 2) PFOSbanaMon monitored may also be499> 80. 1} Due to 8w excessive ateaaof toe RATIONALE data aete, Interim reports wM be toaued to Bow the client to receive data In a timelier manan w r *M tr - n f 2) The API 4000 LC/MSAIS ayatema detect the 499 -> 80 PROS transWon with greater aensJIMtytu n 49 9-9 9 transition. ______ 1) The dent writ be able to receive and review Vw data more qutakb. 2) The 499 -> 80 bensWon can be delected vrith greater aenaitMty, therefore, giving bettor chromatography. y y v c p m UMMQMOraipMM* SudDwirl/hnegeiw*aeree* ExygaaUsings arweBrScngurtRisqiarsd) o LBRfflf kV000122S4 5S ---------- Exygen CALI Review h j e d n h ADUramUTTVE FORM Exygen Research Page 108 of 110 Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 Exygen \ \ / C ^ R E SEARCH 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fa*: 814-231 -1580 DEVIATION FORM _______________________________ ;_____________________________________________ Pw>1 (42 General: X Project Specific Deviation ___ Fadiily Deviation Date of Occurence: 04/28/06 Exygen Project#: P780/P1131 Deviation U 5 Client Project#: MA Reference#: 06-076 RecuUtorv Driven Djviation Typg: (include VH h r methods end SOPa) X _____ GMP GLP Other None Samde Descrlotlon: X Protocol VfcNA Notebook reference: MA Method SOP Login# : L0008191 Container#: HA Lot: ________ NA Summery of pevtttten; The three sediment samples In L8191 (C0172892 - C0172894) were originally extracted using the sedsnent method V0001782. Poor recoveries were obtained for PFOS, PFOA and MC PFOA. Because of this, the study sponsor requested the use of an alternative extraction for these compounds, es foiows: Direct Injection Method: Before the samples were weighed for the extraction, they were mixed thoroughly by vigorously shaking the container. A one-gram portion of sediment was weighed into a 15-m*itrter cantrifuge lube h r the extraction. Ten m#*itefs of 1% acetic acid In methanol was added to each sample. The samples were then shaken by hand, vorlexed, and sonicated for thirty minutes. The samples were then centrifuged for -10 minutes at -3000 rpm. Each sample was analyzed by LC/MS/MS etodroepray. Using this method acceptable data was obtainedfor PFOS. but the recoveries for PFOA and UC PFOA were sdl poor. Another atomattve method sms then used for PFOA and C PFOA as foSows. Alternative SPE Method: The samples thatwere prepared in 1% acetic acid tor the direct injection method were used tar Vtssextraction. Fwe m iMere of each sample woe atquoted Info a 50-rnL polypropylene centrifuge tube and the volumewas taken to 40 mLwfth water. The samples were lltan ' canthfoged for-10 minutes a t-3000 rpm. The supernatant was Stan loaded onto a C ,, SPE cartridge conditioned wRh 10 mL of methanol and 5.mL of water. The ekiata wee diecardod. Approximately five mllMters of methanol was added to the cartridge. Five mflliitars of efoete was collected into a graduated 15 mL potypropytena cantrifuge tube. Each sample waa analyzed by LC/MS/MS etectrospray. Causa: ___ Preparation ___Analysis____ Instrument___ Cttent Request X Other Impact: ' More usable date was obtained. " LIBRARY ID: V0001840-6 hxygen Research ADMINISTRATIVE FORM Rage lUb>ol IIU Interim Report #23 - Analysis of Sediment Samples Exygen Study No.: P0000760 tt-CnH-EnH EHS'.*236 F1BraHEnmstv6r5i1cn733 195 0+5/01 '06 13:6 HWOM.106M 0m3/t0! 3 MW SNtsSWMCaanfaicithaD,MilHv>1 f w 14W 'U Id, MMtrfRMWMa 1 .. . . * . .. ** **:'. ; ,* . * *. ' f; . ' N'':<t f . 1 . v. **<*'**,vf/**-!.*v.:..*.**;>VV. \...*,**<* \i'* ' \ ;.: - V . ' ' . >V . v v.' *' ' '*.* **'s*s'***:. *.`** `.'-i . i4: >. t.r. *. \t" .>V. .-.S.%,,*v.* *%<*\' . ' . ...' *.. i . * . '-*.*'*V.*..*. .*v1*.. . v/ .* 4 . '*. , <..if '**,-y:'<Yy--*v>' i '' .. ' *. "sJ'.r ?/- 'V^o.. **.'` . `*'..*j.*.';**. Exygen Research Page 110 of 110