Document DvRrnVMnZgVmOadwDQ7mkZ1mO

_ ramon Analytical Report: LIMS E02-1053 = .- 3 Analytical Report LIMS E02-1053 MECH TL 226 -- [150 - Comparative AnalyAsnioaslfyFtiiucoarlocLhaebmoircaaltsoirnyHRuempaonrtSeTritulme Samples Obtained `Commercially - Data Requirement Not Applicable Author Lisa Stevenson Study Co1m1p3l0et2ion Date Performing Laboratory Extractioansd Anatyses BuiSkiMngEn2v9iEo-n0m9e,nt5a3l5 LBaubsohraAtvoreynue ) St.Paul MN 55108 i APnarloytjiecacltRIedpeonrtti:fEi0ca2t-i1o0n53 . Total Numbse2r of Pages OM EnvironmentalLaboratory 3M Environmental Laboratory CONTAIN NO CRI Page 000041 Page 1 - Analytical Report: LIMS E02-1053 Analytical Report: LIMS E02-1053 This page has been reserved for specific county requirements. 3M EnvironmentalLaboratory 3MEnvironmental Laboratory Page2 000042 Page2 Analytical Report: LIMS E02-1053 - EE Compliance Statement eAnraicaa rRopar:iLIpMS eE02n-10n53 - Analytical Laboratory Report Title: Comparative Analysis of Fluorochemicals in - Study donticaHtuonmaNnumSbeerru:m E02-1053 Samples Obtained`Commercially - `ThisstudywasnotconductedunderGoodLaboratory Practices. rri-- uhsfr - `William Reagen, Ph.D., Laboratory Management, SponsorRepresentative Date - (oYaiSntevAensonS,Ptrirneconal Anabical IvesTgaior \Biatsel2 WM Envronmontat Laboratory 3MEnvironmental Laboratory 000043 Pages Page3 _ Analytical Report: LIMS E02-1053 -- eeswses RmEeS s Quality Assurance Statement i - Analytical Laboratory Report Title: _ Comparative Analysis of Fluorochemicals in Sem Sombrapraof - Study Identification Number: 02-1053 Unk a es tot `This study has been Inspecbtytehde 3M Environmental Laboratory Quality Assurance e chow meraLabret ulyss = Principal Analytical Investigator (PAI) and laboratory management. - - " Sample spkng [Monsgomert[pa] Anais ora J] `QAU Representative A 13/02 Date PO 3M Environmental Laboratory 000044 aes Paged Table of Contents Analytical Report: LIMS E02-1053 Araya por: LS 02-1053 = Compliance Statement............................. rer-------------- ~ List of Tables.........cccccuerrrrnnenrs e ----------------------s----a----n - EXOCULVS SUMMAIY.....ccssssssssssm - `Specimen Receipt and Maintenance. ni ----------------------------------.) Chemical Characterization of the Reference SUDSLANCES.....ovoverecessssessnsrsmsrssssesn1n0s - incaCanons ATE Preparatoryand Analytical Method .................... terms ssssssesssssssenen1 Data Qulty Objectives anc Data logy occa Data Summary, Analyses, and Results ................. sss 13 - StSuamlmarMyetohfoQdusalaintydCCoAnGrUlRIAOnnsais Fos... 1183 `StatementofData Quality..................... sms 1 Appendix A: Characterizationof the ControlMBIccvrcorersserseensersicrssmmmmemsseesserss 16 AorpoemnBiB:cEoxtlraacttiionceasnd(A13naica Method. 13 } ETS-8231.1, Solid Phase ExtractionandAnalysis of Fluorochemical Compounds pages) eroom Compounds . Appendix C: QC Data Summary Tabls.......... esses --------------------------------ssssissss] `Appendix D: Data Spreadsheets 7 rr 38 ADP F: Inari ortcatas) of Analy (3 pagem 44 WEnionmanta Laborsiory 3M Environmental Laboratory Pages 000045 Pages Analytical Report: LIMS E02-1053 : 0 --- 0000000 `Analytic0 al Report0 : LIMS 0 02-1053 List of Tables . Table 1. PFOA Data SUMMAry of POOIEd SOM... Table 2. Pooled human serum samples received from commercial vendors in July and - Table 3. Characterization of the Analytical Reference Substances in Study E02-1063....10 `Table 4. Target lons Monitored in 3M Laboratory Analyses and Observed Retention Table 5. PFOA Data SUMMAry of POCIEd SOMUM..........covccernr1n3 Table 6.Limitof Peak Area Threshold in the Analyses of SeraEXIACIS ...........14 - Table 7. Characterization of the Control Matrix UsedforAnalyses in Study E02-1053....16 Table 8. Accoptance Criteria Summary of PFOA-NH4 QC samples Analyzed 11/01/02...87 - Table 9. Acceptance Criteria Summary of PFOA-Acid QC samples Analyzed 11/01/02...37 `aM EnvironmentalLaboratory 3M Environmental Laboratory 000046 Pages Page6 _ Analytical Report: LIMS E02-1053 _-- Study Personnel and Contributors Analytical Report: LIM 02-1053. 5 3ReMquEensvitroornmental Technology and Safety Services 3M Environmental Laboratory SBtuilPdaiunlg, 2M-N36-5059106 = Wiliam Reagen, Ph.D., Laboratory Management, Sponsor Representative Analytical Chemistry Laboratory - 3LEixMstarEaSnctvtaiivroeonnsnasmoennnd,tPaArlniaLnlcayibspeoaslrAanatl(oy3trMiycaLlaIbnv)estigator (PA) 3M Lab Contributing Personnel . MOagrnlieennekaM.KrHuepylianngi"n BRiocbhaWr.d WCy. nJnoen*es* | "Contactias pression sonic anion SSttuuddyyCIonmitpilateitoin:on1:0/1116//1032/02 . Location of Archives : LAalboorriagtionarly raacwcodradtiangantod 3anMalSyttiacnadlarredpoOrpterhaatviengbePernocaerdcuhrievse.datThtehean3alMytEincvalirroenfmeernetnacle standard reserve samples are archivedatthe 3M Environmental Laboratory according f`1ao0nna3glyMatisSctatlahnepdhqaarusdeaOyopfeortfhaittshiesntgpurdPeyrpoawcriealdtbuioreneasar.fcfhoRirevdmesdaeiavntail3nuMgatsiEopnnev.icriomnemnesntpaerltLaainbionrgattootryhefor as. 3M EnvironmentalLaboratory 3M Envviirroonnmmeennttal Laborattory 000047 Page? Page? _ i Executive Summary oreAnalytical Report: LIMS E02-1053 - A screening study was undertaken to compare branched and linear isomers of perflucrooctancate (PFOA - C;FsCOO)) in 4 lots of commercial pooled human sera with Enia Th - isomers of PFOA compared to the linear isoom fPe FOrA in the `commercial pooled populations (Table 1). Since this is a preliminary `screening study a larger sample size human sera samples. ~ AsshowninTable1, twoof thelots of commercialpooladsera showedthe presenceof branched Isomers of PFOA while the other two lots showed a much lower percentage (by at least 40x) of PFOA branched isomers. 3 Table 1. PFOADataSummaryofPooled Serum PRElE owerfo[oe [oon |sre | [ieee| Si mit | en] reIE P a FoAR = Eo wTe L nitreme 000045 ns os _ Analytical Report: LIMS E02-1053 _ --seweeruAs rane Fopore LS E0e z1053 Introduction and Purpose - rTETuCoeoEm.rp1o0u0c6r0h0p5a.oms5ieAcn6loafiItnnhhsgeamslsLttoufdPoysFfoOicrsAaot.onmdTaaerraetcrPaiFfnopOerAotdChornecsioaomvsgmaetoitsonomasemewawaairrnastcsioospnooaofePmnFmOAs ranging isshwas atiatyedom 16Omeroop were completed by the 3M Environmental Laboratory under `study number E02-1053, andthe results of these analyses are presented in this report. The analytical portion of - 00 lT`hiSoopneSscMicEmonmeimnoarrRmceeacnltevaielpntdLearabsonridsntuMoyayiraencrtetieAvneudagpnoceclee2d00h5u.mAaSnssprescisammepnlensecsoltecend rom _ Sorago a OMG3 10C, ad mines or moore ean canoelo, frozen in good condition on dry ice. All specimens were immediately transferred to fom he marl (anaca sanarsy so `extraction and analysis as described in the method. np The samples were kept isolated TRabnle,2. 2P0o0o8ledhuman serumsamplesreceivedfromcommercialvendors InJulyand ) : Eoiendbienan |[VorsC s7.Sero mmins |mmm e| GS ST2EhrCpevoarmcroomennamtnroaldnParlmolascLtoouaidrbrcseoener.a1dt0io1swseirroabseaonenarleyedsdeisnaopnerpefoeirmnnedeAdusrSitnagpEoe0s2n1s0o5yH3aewasreobetaeined fom EnviarLasoo 3M EnvironmentalLaboratory 000049 [I Page9 Analytical Report: LIMS E02-1053 Analytical Report: LIM E02-1053. _-- 000000000 Chemical Characterization of the Reference Substances PerfluorooctCaAnoSstNeumAbmemro:n3i82u5m-2S6a-l1t (PFOA-NHE) } Chemical Formula: C-F1sCOZNH" Molecular Weight: 431 , `dTehties rcmhienmeidcably iNs MaR3,Maeplpercotxriomcahteemliyca2l0f%ucbrrianantcihoendp:r8o0d%ucltiinoenarloitsaonmedrcsobntyawienis,ghats.. : Perfluorooctanoste-Acld (PFOA-Acld) `CAS Number: 335-67-1 Chemical Formula: C;F(sCO:H Molecular Weight: 414 ``Tahpipsrocxhiemmaitceally i1s%a bcormamnecrhceida:l99p%roldiuncetaroibstoamienresd.from Oakwood Products and contains fTrhaegmmoelnetceudlfaurrtlhoenr4d1u3rwinagsasnealleyscitsedtoapsrtohdeucperilmoanrsy1i1o9n,fo1r69P,F2O1A9., aTnhdis3f6o9n.wTahse total fon current (TIC) was monitored for analysis. pCrheesmeinctaeldcihnatraabctuelrairzfaotiromnbienlfoowr.mation on the reference substances used in this study is Table 3. Characterizationofthe Analytical Reference Substances In Study E02-1053 PFOANHA| PFOAAGH ToRw1Iow| Tomer [[[oEroteonbe[ nT7 irSes||ctesw iroa| es| [mn | rors |menteven|n [pE EoyTT| waT |-- won| Corym3 `3M Environmental Laboratory 3MEnvironmental Laboratory 000050 Page 10 Page 10 Analytical Report: LIMS E02-1053 - T _--_ en Analyticale Report: LIM E02.1053 Sample Preparation and Analysis - Hebxeutgmriaancnntisnswgeerorunem1a7snaaOmlcyptzloeebdseruwse2ir0neg02ahniuagslhiy-nzpgeeadrfisonolrtimhdasnpchsatausldieyq.ueixdStcreahrcratoismoaanmt(poSlgPerEas)pwhpeyrr.oeceedxutrrea,cteSdample - emloedcetrVoesrpsruasy/etxatnrdaecmtemdarsasbbsiptescetrraomsteatnrdya(rdHsP.LC-ESIMSIMS) in the mulple reaction _ NbQurMaalRnictcaheteridtvfeainaenddaslltiynsaeinasdraoirfsdbosrmoaefrncaPhlFeidOneAaarnsditsafonnmdeeaarrrdPi(sFoPOmFAeOrAss-tNoaHfn,dP)aF.rOdIAt(PwwFaaOssAd-aeActcceoirm)mpialninesddhatehdmatiusxtiehnedg - fbrroamncthheedliPnFeaOrAPFisOoAmeirssomeelru.te within an approximate 0.2 minute retention time window - M_ethod Summaries FEloonclvalitorewodinnmigenniAstpaaplebnLrdiaabitoxrdaBe.tsocrryi.ptiAondoeftatihleedmdeetshcordiupsteiodfndutrhiengmetthhsoadnaulsyetdiailnstthiusdySbtyudtyhies 3M | 3M Environmental Laboratory PREPARANADATNALOYTRICYAL METHOD : + fErToSm-8B:i2o3l1o.gi1c,al"SMoaltirdiPcehsaTMse Extraction and Analysisof Fluorochemical Compounds : + gmHiruxatmduaernew.asteAercrea.twoaTnishterpirldeeipl(uatAreOedNds)euwrsauinsmgWaa2dt.d0eemrdLwaoasfsassnpeierkxutemrdawtcithtiehonntdshioleluavtepenpdtr,toopwr1hi0iactmheLaalnwsaioltyhStererevageednt tctouebnpetr,reicdfiiuplgiuetttaeotdecwltiahtrehitpwyraottteherei,nssau.pnedTrmhpaeatsassnatem.dptlThehrwoouasgsuhpcaearppnrpaeet-dac,notnmwdiiaxtesido,{nreaadnndsCfypesurStroPodEntotchaaertcrliedagne. saTenhldeacaatnneaadllyyfztreeod(ms.)aoAfsniainnlgtylesorpeerssitwmweaerrrysepleoelnruftcoehrdamrfeardcotmbeytrhmieosntSoiiPtfcoErPciaFnrgOtrAtiwduogseoirnwgimtHohrP2eL.G0p-rmoELdSuMcoftS/mfoeMntsSh..anoFlor Tw`ehaxesamtfporltaael,gmiteohnnetcmeuodrlrfeeucnruttlh(aeTrrICta)onipporenoadk4u1ac3re(ecCahsFara1ar;cetCetOrh0ios)ts,iucsmdealoeufcgtthhetederasisigotnnhsae 1fpo1rr9i,emaa1cr6yh9,fdo2an1u9fgo,hrtaaennrdalfy3o6sn0i.ast, `Dsapuagcihftcerreitoennstimonasytailmseosbfeorreeafecrhretdartgoetasanparloydtuocstoomnso.r that were monitored for analysis. `aMEnvironmentalLaboratory 3M Environmental Laboratory 000051 Page 11 Page 11 ] Analytical Report: LIMS E02-1053 Analytical Report: LIMS E02-1053 ANALYTICAL EQUIPMENT "sTthuedyf.ollowing is representativeof the settings used during the analytical phase of this . LAniaqluyitdicCalhrcoomluamtno:grKaeypsht:onHeewlBeettt-aPsaicTMkaCryds2Sxe1r0i0esm1m10(05Luimqu)id Chromatograph system Column temperature: 40C Mob`iCleompphoanseentcoAm:p2onmeMntasm:monium acetate FloCwormapteo:n3e0n0tyB:mmienthanol ISnojlevcetnitonGvroaldiuemnet:: 11-63.00umlinutes. Time (m0i0nutes) 4%08% : 11000 9800%% 11255 110000%% 116800 4400%% MQuaasdsruSppoelcetrsoymsetteemr:_ Micromass APl/Mass Spectrometer Quattro Ultima Triple SCoofntewaVroel:taMgaes:s20Ly-n6x"0 3.5 CMooldlois:ioEnleGcatsroEsnperraygyN:eg2a0t-i5v0e eV. SEloeucrtcreodBel:oZc-ksTpermapyerature: 150C 10C Analysis Type: Multiple Reaction Monitoring (MM) TRaebtleen4t,ioTnaTrigmeetlsonsMonktored In 3 LaboratoryAnalysesand Observed |[F= ron[[wromn|]mmemmes ||L rrnochme eedT|ur aniemse_|] 3M EnvironmentalLaboratory 3MEnvironmental Laboratory 000052 Page 12 Page 12 or si Analytical Report: LIMS E02-1053 Data Quality Objectives and Data Integrity SepoitontnLCoEmn osott o o, n ) Callbration: Calibration curves were not a component of this study. Isomer ratios of Limits of PeakAreaThreshold: Thelimitof peak area threshold was the lowest `standard point that had a signal to noiseratioof at le2atismets thofathte baseline noise. es omyestos. - Acceptance Criterla: The isomer ratio of branched:linear PFOA in the extracted continuing verification (QC) sample (labeled as RBS-date of extraction-QC- concentration) is required to meet +30%agreementversusthe extracted initial standard Demonstration of Specificity: Isomer identification will be substantiatedby . Data Summary, Analyses, and Results Data quality objectives for the analytical phase ofthisstudy outlined above were met with the exceptions noted in this report. `Summary of Data Results | [ron|Pusi Eemwna|[KreT[LeB [Toenm y]| Table5.PFOADataSummaryofPooledSerum a (E SEEeEmes [[m o=wroT[ewwm w[ |[o] | | r] ennenrmrsn 000053 os os Analytical Report: LIMS E02-1053 Analytical Report: LIMS EG2-1053 `Summary of Quality Control Analyses Results Calibration: Quantitation was not a component of this study. Conomtphaertiostaolnfoofn bcurrarnecnhted(T:IiCn)eaorf rpaetaiokianrtshaeseaxttrraectteentdioranbtbiitmemsatcroinxsissttaanndtaordrwtahestbaarsgead aAcniadl)y.te (.e. 7.9 and 8.1 minutes for PFOA-NH4, and 7.9 and 8.1 minutes for PFOAtLhiemietxstroafcPteedakPFAOrAe-aATchirde0s.h5o3l4d:ngT/hmeL spteaankdaarrde,autshirnegsthohledbwraasncdheetderimsionmeedr bTIaCsepdeaokn area at -2 times the basaline noise. Table6.LimitofPeakAreaThreshold intheAnalysesofSeraExtracts. `ConncgeinmtLr_a_tion|| BrTaInCcPheeadkiAsroemaer| Instrument [praosaosn casr|iedoPRsOMsASI0| 534ng soaecarrr[cQuatercoreunnima] 370mito TIC ok on re rnho. PFOAAck sarspcWhPFOAAG crric Binltaenreksst:. Al blanks were below the limit of peak area threshold for the compounds of cAocncteinputianngcveerCirfiitceartlioan: (TQhCe) lssaommpelrerwataiso owfitbhriannc+/h-ed1t0li%nefoarraPllFQOCA dianttah.e eRxetfrearcttoed Appendix C for detailed information regarding QC data. Precision: Precision was not a component of this study. Matrix Spikes: Matrix spikedatawerenot a component of this study. `veSrpiifkiecaRteiconosve(rGiCes)s.: Spike recoveries were not determined for the continuing Surrogates: Surrogates were not a component of this study. StatementofData Quality `rTehlieabrlaetiiodoefntiifsioemreorfstohebsseoruvrecdeipnrotdhuecst.tandards throughout this study were stable and a Statistical Methods and Calculations `pSetratciesntitcadlifmfeetrehnocdes. wSeerseAlpimpietnedditxo tEhefocraelcxualmaptlioencoaflcmuelaantiso,nsstuasneddaridn Ed0ev2i-a1t0i5on3s., and `3MEnvironmentalLaboratory 3M Environmental Laboratory 000054 Page 14 Page 14 Analytical Report: LIMS E02-1053 - a Analytical Report: LIMS E02-1053 Statement of Conclusion - IpRoseposuumlleatrtssifoornfosPm(FTtOahibAslesct1ou)d.mypSsaihrnoeewtedotdhtiasheiwsiliadnepeardreilsiitsmroiimbnueatrriyoonfscoPrfFeteOhneAinpigenrstctheuendtcyaoagmemleaorrfgcbeirraaslnacpmhopoelldeedsize - Whouumladnbseernaeesdaemdplteos.determine if a significant statistical ciferenca exists between pooled - Ab(sbryasnahtcohleweadnsitins4To0amxeb)rlosef1oP,fFtPwOFoAOoAbfrtwahhneicllheotetsdhoeifsocotmoheemrrmset.rwocilaotlspsoohloewdesderaamuschohwleodwtehrepperrecseenntcageeof _ _-- References ) 3M Environmental Laboratory Study # E02-1039,November2002 3MEnvironmentalLaboratory 3M Environmental Laboratory 000055 Page 15 Page 15 _ Analytical Report: LIMS E02-1053 Analytical Report: LIMS E02-1053. eee Appendix A: Characterization of the Control Matrix TEa0b2l:e170.53CharacterizationoftheControlMatrixUsedforAnalyseisn Study Rabbit = Control Matrix| TSoearudms SoTmSome a | (EE [aero] : ENE |Chom+i|casoirisoacot| Dwserdon Senm. `9M EnvironmentalLaboralory 3M EnvironmentalLaboratory 000056 Page 16 Page 16 _ Analytical Report: LIMS E02-1053 --_-- Analytical Report: LIMS E02-1053 Appendix B: Extraction and Analytical Method This appendix Includes the following method: - [ETS-8-231.1, Soiid Phase Extraction from Biological Matrices, (19 pages) and Analysis of FluorochemicaCl ompounds SMEnvironmentalLaboratory 3MEnvironmental Laboratory 000057 Page 17 Page 17 _ Analytical Report: LIMS E02-1053 Docu ina be sad, B caren foe a fron 10.16 200 3M Environmental Laboratory `Method - Solid Phase ExtractionandAnalysis ofFluorochemical Compounds from Biological Matrices Method Number: ETS-8-231.1 Adoption Date: //3/o1 - Revision Date: 3//5/oz. Effective Date: 2/13/62. Appeved By: . re LWaiblolriaatmorKy_MRaenaaggeenr TaDaLtes. 0 Exact Co ofOp rigiynal AL lotiex . Initial Dato 7 3M EnvironmentalLaborator Solid Phase ExtractioEnsrndsAanni bofyForsochirriscl Comproom Biologie Matrices Page 1015 000058 Roget _ Analytical Report: LIMS E02-1053 Drie ma Leumi, for 13 day soon 10 202 _ e1_BrSRecocpEeeanedIAepNplriIceaGtieSon eememssmmrmmmeteeeee - Soidypce x etc(SPE.Toi hn Sobeextn obpsBhy o ss --eso ea _ 22 MMeetthwoodSSoumwmearryy ee i} ALininaiGmooiunanntr,oofvolrreoabdgersphnheeeasivnlwe,hd1edpmeeiitnebbtybsyeatstrhe.ysTropeiegdle(oicudpsnpdp o isdeon psdAsnbn S oPrena nes) - P1Cr0ol maonbcl eedCupiSedPy toEichteu.nsiTm.ogsgFpylrycbeeos)ysnorfiehdierscpwheoscectoo(rdPLwSChPEEocSiSsnAht)mseno 3NE Definitions 3.4 Dilution - Aetoncmpreesssd 5 1fod 1mL ofsale + mi ofdctfo oof mL bio, , 3.2isApSecPGnoEthrocndacrittoorsiietdignencheroptae,nmoosvnesn ssofoccnec5s0scrdeorseadeocntdSciHhoeBondsendoincTsaseasneeeenne.lh ria hs owl 3.3 WReeeavgielnt gtrabdelwacteor nsnofmbeiaognssc) i 3.i4 QS iualnityncoenti (rol siampnler eifoin ceen(gl na,tieo dely i cond n eyofbil. AW 4_ Wao rninr gs andn Cautg ions eondC oeuens 41AHleaaylstwh aansdprSoapfiestlyvWa,miynegwssding hesworkingvil vents, nr io, : Uosecinwih lub g erpre.Whenrpg probecpl logofpityS00 4.2TCoCoaeuntcioirco,ntstlslohw sShPoEcSooliBne 0Loo 1 eseesafl hePmEeonnsdvt se. Af wading SoldPhaCseEaxntopnEooamsndBspsoialtmissorfPeseonic Piezarts " 3M Environmental Laborator 000059 Page 19 _ Analytical Report: LIMS E02-1053 Doc ment mas be wd ont for 1 aay fre 10 Ie 0) bDao,ntoet oHPpLeC wsiollivennttpeumsptsosmhaotvehcadpaocwit.yof400bar (800 ps) back pres. he Back press exceeds 400 - D0not unsolventpumps ody, _ 5_ Interfeenrecnecess Tcoonmtiacntimwiizteihhentesrafmeprloecosesx,Taecflto.nsouk tb uedfo samplesora o anypatofnsmenaion hatcomesin -- 6_ IT nstrume entatf ion,SSu uupppplliim eess,,aanno ddMMaattn eerrilaallst s ation, - iTnhsterfmleaoswtiinong, isunpsptlimeesnianidomna,ilpspse,ysbnedomdiseplaceaaorfstwhl eosdiwsshdi pecingthismethod. Exuvlet _ 6.1 Instrumentation Vortex mixer, VW, Vor Gere 2 Uli TuaT2x isehomogenize = Vacuum Pump SPE Buacion Manifold Contig,Misa 1000orEC Shaker, EvrbchorYWR Blane (40.1005) ] Micromass,Quateo IoUti tiplequadrpele MasSpectrometerequippedwih anclcrospray ization source HPHHOD orAgialowpussolventpumpsiynsg,solvesdegser,conn compatesn,d susp v 6.2 Supplies and Materials Eppendorfor disposablepiptes plasticorgas Dissectingsclels PVoolylpruompyelefnleasbkos,rgess, cyeaAofpholdiing 50.0 1. (Nalgene) 40m. lsvis (CHEN) Plasticsampulevials,Wheson, i. orlesppropesesie) Cenifge bes, polypropylene, 15m anSdO ml. . Lanes Graded pipetes, giass Syringes capableofmessing SL10 100. BoteTopDispenser (capableofdipensing SofoL vers) SPEcxtcion care, 5. Sep-Pak AnconaCy(Wate) 78mlsamplereserve (orth speopinesize) Crimpcp lasssutovilssndcaps 3M EnvironmentalLaboratory Sold PhaCsoemEpxoturaacdtEsioTfnrSao8nmd2BAi3ol1ong1icaaol fMlaltoryricoesssheimicsal Page3of1s Page 20 000060 B Analytical Report: LIMS E02-1053 Docent vy be aed. Lown oo 38 days fan 0 de 206 Crimpers _ HPLCaml columnspecific bedeterminedbyteamsanddocumented i herwdts. _ J7_ TReefaggeennttssaannddSSwtnanddeaerddss OO OOOOOO Reng radewae, MilQTM, Nope I,oreval AcHePLCgo rade cn e ai,l = MePaLCgrrad oe rcui, vae Ammonium sete, eae adeorsivas _ Bilgial tidorse,fenfomspp 7.4 Reagents preparation - `2od0leummveMteai.c cmoSnorvmeerooacoctneanieinspigleraeaiaegne.:nt Wreiieghvsaprprixisnuasnlyl03i00dssrreananivanda,cbeisn.10Pvouoriunos8g200a0gmied . Nnodtae: WrhenoprgepvaigpdreiefpfsSceiroavnalanetsdshacnrtshoidse. edinegersprarion areamtsandardpreaction, 7.2 Target analyte standard preparation - PrFeolplaorweintgare nxalcsoalydsad)mfaoyrtoemasyandterb ispvpee.opiMtefola scarosprlmepusrpiaonnso:snre aeceinte. The sWteaingdharsdlporgobsooiktolyab1er00spmpgroopfrirneetacataioyn. ino 100 mL.vlumeticfa an ecrdthe cual weighti he . Bing10 volume withmetarlfo sicksada ofspeoinsly 1505m(0ign0). ) cDillainth:eso1c0k00gomli.nxwSiLh/m10e0nmLo=f5r0 g3wlor.kingsandr 1 sainofspeusima5i0eploy. Earle Dcileeawna:kinSOgpgainmdaLrx 1|0wmilhlm/et1al0$i0OprmnoLLc.e workin standard2slat of spr. $0ppm. Example X Dcituteiwo:riOnpspoda 10wmithItan)05prgodmuc.e workinsade 3shinofspe. 050pen.Earle 7.3 Surrogate standard preparation : sPtraenpdaarredspuroegsrattieosnas.ndr). The llowing san example lyad ayomayootbeapap forallsurge Weigh Bring pproxiatly 0vohame with 0-110 mg ofserogatesandr mea or og sand no sc 100.vue ofpposiily skan record 00 100pr. he cilweigh. : PcavroptleumenaRonsdkgsaanddsaarrnidndcgorndevwnororaktmionnswsianlhdreath,aannTodalarfrotreoswgpohprockksiinmoasetlasy |dpnolo.pfo0efs-u1ae,tsoRaensdoadshoeackta v10a. 7.4 Internal standard preparation Pseeapndaard prreaplrasitasn.dard). Toefollowin sanexampleonlya mayof mynobespreeforall ral Weighapprovimeely 0-10mgof ermalsda no 100i.vuesfa nd esr he ack weight. 3M EnvironmentalLaboratory SodPha`sCeomEpxorucntdisonEfsTonSmd4BA2ic3nlLoig1iscalofMaltorirccehsenical Pagesorts Page 21 000061 _ Analytical Report: LIMS E02-1053 PEE tay 6 WO ir, or 1 has Btn (0 22 _ PrBerpairge avnolmaneeawlitshtmaencdharadnwofrokrin rsealcs.nTrausstoscpkporfosspimeaolsyt|lmyl.3o0f-1r10l0psptma.d `volume Rsk1dbinfovohame wilhmethanolfo workinSard of30-1gpn.Resa seickt03av[ol0lom nse ndsada conrtiosine andar logo foeappreoan. - -- 8_ Sample Handling _____ Alamples ecsivd md stbeep oa il he tno peo. Allowspies1 hawtorompprceexscrion. _ copppiecda fviaslhsmoarlissytsd.s are preparedwihech lysis. Excsadarsandsalesaresed in m1a7 ysbeysorewdilaltbeodmelayeed,exmactep dsrrt e ncdonsas nepesamsadybereget t proximately4 nflor = 9_ Quality Control - 9.1 Blanks 944 SolventBlank - Alotof mean is ed svensk.Sle bss re ot exci 942 MethodBlank . Apxnianrliuotaondfa1l0ymzLeodfwwiahtee,cohr soelteFopllporwionpgeaheisPmrooucne, u(ewdo1& smpeiikoed viirthkS.Fooxaemtah vob1spsrte - 913 Matrix Blank A ucAsonenldeg1upaoptrooipfle1i.e0tem.i.vMda1ti.0ihoa8fskmasamapielp(erksea)dr3docfroohmommmooegeerniozferdec)shoiurnecedesss:up1ei4ombf yaca.oomoOlpmeiuatsmof3uorm0amsaycybye ifniiatailuweordd3)otrogheecorgee.esiatdsa,cuoesb12id CCCoVrsfmnreimlvsttolsy)T.TThemsiesobiesi sepyndrenston(a 91:31 siSg theycotnytrcoolmnraltmsacutrv(ewofheksdaywicosntarorleseri3diwsoiorspeiecd)u. ,prepuefous (6) iblanks : 91:3:2cuC,opmmeerfo won sped) b(i)mnaeti(saamke ssweiens)thsesiuxnicvoer-efrhe covmamelrle robita(inweodrhaerdiwihod foorgbe3nd : 81:3.3sthaemsemSceuormopmeiriemalaaltyhsaevacsiaoebdlyeaminaimaiaslsao(gdwuocc5ppmkrsdfsoiurhs(s)dmofao tebiiacldaanvkre,ippngrskcfdo)moe.uni)amllayivalklesmiag hoef 91.3.4beiftyipreotdocmoalroirieavwal,ush.eaneof method nd si bsmybe atedandwil be nodin 9.2 Sample Replicate `Samplesreplicas repreparedscorn1 sh dyprotoosrjc oud. Solid Pha`sCeomEpxtoruancdtsioEfnoTomsdsBAinonliosgyicsalofMaFtlioereoschrical Pugs sor19 3MEnvironmental Laboratory Page 22 000062 _ Analytical Report: LIMS E02-1053 Docent mag Be wi, rent, fo 14 dase rons 1016 2002 - 9.3 bSsuiarnrgogceoascteeanisctidaoinndisacr0adposniedaogfs oo ofsbeyClbslesuvepiidOithornogfekr irsooxeon _ SoTooptiaolryemroyvaibnpegsehsekaa0dnmidLnseslesd0obtbeoiae 11miLm.L.id1 Gadtihmowhnwvspebenreodfofremoxnomne,ntHoe ~ 9.4 c iInnteerno aslnsdtc andiamrica dodmgpoei ofocf esntry,ie ol c les sped ih rlsafcsh cioci _ apillner sad ide20mL.ofxtcine 5mL.cei he, bor ering 9.5 Lab Control Sample - `Labcontrolsamplesarenot a component ofthismethod. - 9.6PlQnruiaunalecimtqyulciCatovincetosrewonovld.T((oQQyCC)ph)seSl0ae1ms0ptloeioe cnvsesxcpi peffmioneeyosofd 0Svty theiss eohsPsep coeofotbe 3 SoTpFucGieeC(ir1l2l)iqtsyesccoenenpstepsrle(o(QkC)hywhilhnpyeoopkneQoCsdcorolfemrTatkldpoethoedcnoo(sceagoh1 f tolyoyf.cAis iina - eiare QiCyspatrerwsil clonsoinofifornsspdeied 5chbo nreg fvebs fbanyieo.nTohecls sedbelowmybeds. Lovie Xin SK0eLL0Q, . Hight Whore UL0Q Midlevel: equivalentto apointnearthemiddleofthecalibrationcurve, x ETSuiohnQCfosvrdipeirieneegswwhfrsOCsdnQCsl7teolviyyehSthceaarlin ccoingsreepstcblisnssordt CQomsCruosoapmnnpelredsoesnxmtrabacelteid wenittehtoxfoa pecadritictudleyaarssawmespeleseezt dmduistrnbesoasnalyizedmin,thesearmeQaCnaslytricaelrfuno. A ny he QC samples. ae le ) EiascheQrCiis,eatxpdoeceteid iossmhowofan2accoufracyGoCfs75-1r25%sofeoxphectveed. mess crn. a, es Aminimum of23 ofall QC samplesmustmeet 9.A7iSyoacmsplplecivDiilleouvti.on Poindion adn rmwelirc nprtionefio igFh snceaolf bbielce seaddowsilys otbce dogisdcbe s og of iTopiesfo dieddSuo ae lfin,1c0 gesnarRl wilfobesnpeuedmi,awospesmcoot sdailrt(5bytwoes10imL Sold PhaCsoemE poundsx EfousmdsBpc iaoclioypeoMfFacescal Paesoris 3MEnvironmentalLaboratory 000063 Pageee 23 _ Analytical Report: LIMS E02-1053 Doctiment in te ond, aurent, for 14d; frown 1 16 2002 - sh2a2em4cpxole icthwirsthisovninea3lnmcpoaesttii1pcirioeont1hex(n maaeeandlwx(i1ncgdbdsoiinpggrsaeidddes,iso.whsiTlmeoeeaisnsetcponrdvroeoc)cehceonsciosnofsGofirnigntgh d1e6tetremineelawihniechpevraclenutesfclomeetrirsepeorteswsiiboinnof1t5h%efsopthlesecwoonsavmpelens sonal sing will be eid fo 10_Callbration anddStaendarldizeation - 10.1 Instrument Calibration - `xiOnwaeicllnloesdaissn,fcaavmeeirwminliilnbmeeoprbfeyrpiaoreeesd(rf)rllovmelaxsna.dcAtdeddodmoaneti]dsiitnanrdoairdes, icfnueheessTmaeybmexanoheosnalseeps,peumdpyc 2 cTeavnes.eBreu10sbumeL,utsoiomngitbodrisaphpoaspkbrelotehelscsotnotpuolisme,arotf.iTchaiosenwdiiclocnbbeeetrweeiepndtouwohslrfTooepcugannnege nabosirmoosgfreooo1sh0es8s1pa5lnmdl8r. removed. - RFeocuorr1d.0smchsaalnidquot,vorooleeroanprhoepwrieniighooluusmtesofsoetlmexatinictsionewo3bmect,ibs aposp.rit. ssTaahmnpedlsaearsndaduanrvddetc.sAonpalleco.f Teshsanerdcuasmnprbikeisrnfgooufsa msatnxm dbstacndo dki,nbTarbks fsoeum1myetbaheyoadbbceavruekd3,0wdhpeetnersrmeinpepdeabyrtoheaoappnikalooOsnydCe docu ina ve fe ReUtfeAiusscecitnioens2,10ocrlobostsepsoc ncfoornm.c5e3r0toiof sfnoclblantinchtchaelcromnisonnsionnsrof2t0 eOwCokuilgseandr HTaryivpoeriarlr,eimthoemvuairynggbteeheasnp1ai0lkmeydLdssaianmepdlleoisseikmaeiit1so0mprlhie.ord1.io0medidi.baiorgtoegwdiethnhoawmeaodgees,npinolnodtrseeammdpiilnaedsrodehfmocomvxeeadpcsifoioroneexdtrsarctpiolne. - Fveaslieotniaeneaxlyascistuesdinmg aheipesaakndrerascofvegreottoscyacshs)tofsinegxtMraacts.Tshyecoevrcsataioenwslvlaberdermis by - {Amncytelbe5)ewlieatvsheilinsd2ae0y%5b%efdpeo2ci5.%idAuliIvinelcmousssttbserhdoewascivapioiedrl,oogdmreepiesnonnti<aat ,ofboexcepntk.theALoLOQuwhniocfh 3MEnvironmentalLaboratory Sold ha`CsomEpoxuniEs rfTaonScmdBAiimololyosgniisc)ofaFlcuroecherical Page7o19 Page 24 000064 ~ Analytical Report: LIMS E02-1053 Oca mgs fair ab Tenrent, for 14 days for 1076 1,00 Working on He | cornostire at |comaempermoinonetsme > Aonprerios ait) In eae Matrixdiluted 1:5 _| ee inFinal2.0mLvolume_ [osOugml NS | sO0nggoragml| 0375ngmi | _ [ost0uml 150 rsompansn | Soongal [----oso0ugmL I osoougmt 116 | s00nggoragml| 152 | o0ngigorngml| 4coagmi 800ngmL | | - |sSoob0uuggmmil"1778506| | 1iSeggorngmi| as0aggorngml| r40nymi 200mm | | [s00ugmL Tie | so0nggorngmL| 400ngmi | 2 I 1 S0s0soo0wouwgmimit n-- TT liao--[s5;05 t1u7iwg7anp1 gg7p/goo7rroanpgmncil.|0 | o--isss8mt0a7 o0v0 nnlggam_--ri --|)]| - SurrogateSid 100 ug/ml 10 6500ng/gor og [S00mgmt| 1RPrOoceIdureSs ------ em 11.1ObTtiinsoszue ue apis SamplePreparation - CuatbsepperoaicnalySs00p0egrmfeedy(1,-0t10w00ig ebrpeeriBaamo,win discocpl. Tis - Reeciogrhdthhescuihetdonihee emihtrsodlupmssihecak,criimtviolnwrk ood spoprock. i Ret sed Ao3h25 lof se ere reagent tr xanansavebes ved rl il te las dinedby he nyt nd docu te Htoems ogtehel isamaplpeeo.s gPoa he Ui Taras idesprensa ed godfo pposiely 2ie,ox ) byemitand document in mis le ong ppt. Rinsetheprobe intothetubecontaining thesarplewith2.5mLofreagentgradewater,orothervolumeasdetermined. s1Tca3ka0reiolguynovmrsaptiaarnna 0c05 0dsiga(nis.t(mwi5le0r+-3s0't.sr0e0x0 hgdsipflor.oeRnxedcfeoi,sETndSi:9l5w21efiog1,33rd s fooFrhvo etiaeotneoe eolin: visdmind y o ytand dd 3MEnvironmentalLaboratory Sold Pr`as CExotomnEosspmdsBoaAiliiougsinloVfridreecsehsenicsl Passos 000065 Page25 _ Analytical Report: LIMS E02-1053 Document be sied. Faeentfor TEL from 10 16 20202 112 Fluid Sample Preparation - `Obianfrozen lidsample andallow tothaw 1roomtemperature or ilukewarmwater, LSaebeealtcah1e5mdwlorpkoslhyepreotp(yAlteancehcmnernituAgoertsuimbielwairtwhorthkesshteaed)foumdboecrum,esnatmipnlgeIthDer,eemxariancitnigonSdteapts.eandanalyst nals. - 10Vo4rtpelaxmstiicstahmpfullueivdsialm,poleotfohearpapprporxoiprmiaatteelcyoo1t5sienceorn.ds,thenwansfer 1.0 iL of uid,orotherappropriateamount Retumunusedsamples ofreezerafrextractionamour avebeen removed. = Aadnddd5.o0mcLuofmrieena:gennnottweaet0tfdiloethe1.0mi oflidfor a 116 dilution,oroberdilutionas Geerinedbythe nly - 1s7amevdoliumleoutathseiarbtoohvanen.1.0mi. iremovedfocsninitialvohume,adjustthewatervolume cordingly to maintainthe 11.3 Tissue and Fluid Sample Extraction - clAlfeutatenertd1i5hmsomeLoogpelnoiilzdesydaspmapmrlpelocseephnfatoyrvriebalfpuegpeeertnonxpbireeme.apiaerleyd1ac5csoorcdoinndgst0sheecntitornasnsf1e1r.1a1.n0mdL1,1.o2,fvootrhteerxmapipxrooprrsihaatkeevbokyamhea,dt0h.e3. - R`eRetcuomrdutnhuevsoelddumleeredmhoovmeogdeonnitzheeexptornaicotinosntwootrhkesfheecezt,e (atfatecrhemxetrnatcAtioofnasmiomuileairswhoarvksehbeeet).removed. - `Spikebanks,samples,andstands,readyforextractionwithsurogaestandard adescribedinthismethod. Spikeeachcalibrationstandard mateixwith thesppropeiat amountofsndadssdescribedinthismethodfor he calibrationcurvestandardsand chQCsample. `Vortexmixthe standardcurvesamplesandQCsamplesforapproximately seconds. - "sTeoccoandcsh.sampleandsundard,add $0mL of cetoitil,cap,andvortexmi orshakebyhandapproximately15 . 3P0l0apcamleosnamtphelemsoodenltsheitseadkienrasetc3inonap6.p1r)o.prissspeedfor 20minutestoadequatelymix (sseting ofapproximately sRteimnogvoeffarpopmrotxhiemsahtaekleyr2a0n0d0cpemioinftgheeamtoadnelppsrlosprdiaitessecpteiodnf6o.r1).10minestoadequatelypellettheprecipitate (3 : Adsedoclduatn4iot0nt.h0eCmSauLppeaornfndarmteaaingtxenbntygoirtnavhedervetwiaangtcesentvoehre4lct5li0emamenLs.$.It0unmbeLh,icasseknietnpgitfchiaergoeerdobeter.ofRieardmdlouivfceoesnmaamanpyylobefestfchhreaomnmagtterhidex(csLoee.lnettsheishfaoumapghnleede maybeputintothe enuifge ubeandten hewateradded). - Anachthe reservoir 0the SPEcarvidgeandtachthi resrvoiartidgewit oa vacuummanifold. - mfoNlOsoTwtEho:afvWeh7beemneLrniudnnriian.nwgnFtdlhooewwvnsa.mcuauymv.asreyttthhrevoaugchucuamrctrhiadmgbesearnadtthapepKroPxAimmaateylby e1r5uKsPeA f-oorgsilvoewatnuabpepsraonxdimdaetyeicguaifoenr Pr0epmarealtiheqSuoPtsEocfawrattiedrg,etbakyiwngaschairnegntowtictoewailltohw atphperocxoilmuatmenlytor5u0mntLodorfymentehsasnaoflt,efreolalcohwwedabsyh approximatelytwo t Afterhwastthreincgoiolsucmounmtpoldgerty,npehsosu.rthesampleintothereservicaridgeuitandallow all ofth liquid fo pass Runthevacuum onhighforspproximatly minutesto adequatelydryeach SPEcanridge. Plaacollcestieon15mLpolypropylenecentifietubeunde eachcardand tewith20mLofmethanol. `Spike exactedblarks, samples, andsandardswithinternalstandard adescribed i hismethod. 3MEnvironmental Laboratory `Solid Phase ExtractioEnTaSn8d2A3n1al.y1sisof Fuorochemicsl Page9or1y. `Compounds from Biological Matrices 000066 Page 26 ) Analytical Report: LIMS E02-1053 Docu at may be wed, ourent, for 1 days fons 160 2002 . cLaxamabecblieorcnaidcaghee,gdnesdcntailuimyooveir)plL,opIeiMr3f5tSorammiipnmrgboeprhre,seme,cxicw,iit.hnlhseolvserosd,yaunmybecr,ompvoanlesfse(1anceheidveed),umexbcearc,ionsiympuel, Trane sch cnt03glassati idcsp. : 114 ExtractAnalysis 1141 Softwareset-up i OensttyheearMmaosnsdyaym,aaidpages,eer aptwilsl uclrsftdroaueg.hShaevlethhelestwnithssrchmadeiinontl tdoeestartiosgyt.n2 aigosorf ExampleSampleLis:IYYMcMeADD2D020a4: : ital feinsane ame (A = Ai) YY =Test0y0) MM =Testmont0h2) : DD Tesda08y) =Firs sample is (un)ofeda (henetspe is willendwith, ee, wmdsoon) Ssoiqguneallleenanmuemubseirnag heariswsitnh t|addesigseslbeyec,oheoraex:ch2dliecsamoef.eetyeamont ay, nd 83g Example lename: TYYMMceDALDZOW20GY01 ital of sentve YY =Tey MM =Testmonth DD=Tesdy t= digitseco le ambersarinwih rough599 001) Anid,sa2mpeatdeosfctrihpetsioanms.ple,ssign method(MS)foracing.a let le, abodeamber, a ctovolar, "TMoRcMis(elmiepthoRde,sccliicoknoMnoMneithnogd)E.dSotrbTuooinaiinotnhMeoMdSeS4asnsePoane and1nsdelmeactsSIR0(4S9igeo coan Rrecaoprdrionng)or DminaapslAsopv)e.id,sAidldoinoi"oefnotarlatpdredoadocntscon uFfaogsrinaieitnosanatnoadniniMnoRoMot.iunmsn. Smaavybeeacouilsltiioen.mSebehMod iIfcMSrMMSosinmysesearGrtsisd s're "Tsyupnidcaarlldy.thesnlytical bth sequencebeginswihsysem sab,seven lank,and setof exraced trix SbaemaplseaexdipesriaodeiacnalallyytzoedmowntihotrwpooQssCisblaelaaelyicjceacmieydoveeravnedraye otthcsonpsiedeirnejedcmtilon.eSeexnectbsbatssshybled inclaudsiechd. SoldPhaseExracionEaTndSAan1s1ysofFucrocheical Page 100719 3MEnvironmentalLaboratory `ComfompBioologuicanlMadtrisces Page 27 000067 _ Analytical Report: LIMS E02-1053 frosts ay ov wel, Teun, fr Mssfom 0774 2002 1142 HPLCsetup - Setupsap ryscoring hesample st raedabove, RSeetcuoprdtshecHaPcLCotnes lnlb ncnonniongshooak,coofodoenssrheoraycsaoe:sappropriatefo apimalrepose - P Tiect-- ampl-- e1 -- Cyce=10t0riinsees ---- Mobi ps:SolventA. 2m Anni Act,Solves B Mecano. - PR---- Ce -- - ow [we [|= = } [>[=] LA .. 1143Instrumentset-up i FRiefertwoit5hi5n:2A4s,pOhpeerrornssandMoaianiaonnSoofuth'eMoirdoealsssQua ITreQusdpoleMassSecon Chockthesolventlvlin HPL reservesadrofl fs. (hjoacehesdgeess. ishte capifl odt0hewofethrepr,obeA,UssmaneAeioebecchnecekpathecioep.hTehSeiossdelecapitlwit Tamontesitugen. OOppeenntteenenspEasge.Click onoper blockso nd deson lationes sters Dovnlosd he HPLCmethodsonae ovo low beg sym alin. Setheflowto 10-50uLsispmeineo SeuHPLC pupa On" Observedope istcoin outof epof hepa. Afoemisshouldbe peed vilhnoivogn einaed pofthe probe, Resist he pothepobe oomistscbseed lowtoporslpoiils10mtin. Typicnmsnamesprsetens nts: Dryingga 250-40 ersons ES ebgs10e -1 n rsh Sold Phase ExicioEnransdaA nnl nofFui ruchs aial Page 1torts 3M Environmental Laboratory Compounds fom Bice Matrices Pag2e8 000068 Analytical Report: LIMS E02-1053 Saucier may be wed, fou bday fom 1015 3003 } HPLCconstfw ode,flow 10-500 pin Pree<40)ba tisracer oi ds ons HPLCi cpeingcot) . Soebosktrpenepeony 150C Despehnneapetini24n0C : ietdihpe teapgsn, serlLs, A -- scion thdfom Mas andsor in dy bineih oy CelnkoannseaettbusonpipheAWcyooConGluPdoee (he cainoftesteon ayvaysong Mas 12 Data Analysis and Calculations 121 Calculations teclon ed nosii,ty illbedoce inecow Cue cesao coinedi ein dion ine lowingein: : MavixAron (moemnLt))"=W--Vig@WoGr VreGVm eBYlG)D Cakecncoceilnionssaoda fwofeflelowinigsantin Coneneniosinon (WrorBn)y ===SPASColowoinainoAinnmSopduAmmiromuDn)t) 10T0u0gs IV weigh wh LO LOL) DV =Diia tvhvunoele(sg devi) ARSV.ASamrplye llasnetrfeomovMeafoyxssoaypial LOL) DF Disonfcr [i MA =Matixmoun 26am = MAofseidsand evesmtioe | gr | LSmlve 3ample=MAofiedspl_ger aLofai' el.vat) uote ikepret cove inbs ligsation: ery berveelReo -MMoasiiBBlkakpReeet Soi PhCeomEpxoturnscdtsioErnossmndeiAlonofMFatoi tersshsee Page 20119 3M EnvironmentalLaboratory Page29 000069 } Analytical Report: LIMS E02-1053 Do mag ren, or 1 dag fs 102002 Clin tv tei hicn et - ReveSotsDeri + SeoADTln i Cl rs eon ng loi ci: oe no EpiScHClasico, | wo [I g AR (ng/mL) * DF Sdrcuevee(Lmeitmi)) *EFV(emldiinCu)ve * 1L000urgg = Giglp) } : AR DF i stm nbinGo Calculateactualconcentrationofanalyte intissue (g/g): --Ls = 690) 13 Method Performance 13.1mSmSoysstia 1embSa ueivtpialbblelob idtTyesctdTeirco oix,esi)T biecionrernpeeofdicnhcok aebeissni.yti wlle nIaontSeeksmeiynnrosiete yii tRiess LgmSPresrhbecRri,ireeyneig ed 35 tf T ly ro e Scab i eg Hin, Fsoy 13.2 Quantitation A`T[m lheicovefsefs iccienotrofm ndettnermi: npationvalue bein 94 dic forthecalibation curve, plodied i cif byregressionusing the peak LOG, areasofthe CA lasna ntcoviehi eskpofsmdeiveropisosevceosdsssdSki10e0dei ll 133c Accuracye dsrc beei u betm cree Tm aioa l lycess2h ly i ie hvcidnd 3MEnvironmentalLaboratory SoldrCosmpEaxntnseonroslngyaf scin rae arts 000070 Page 30 ) Analytical Report: LIMS E02-1053 Dement eben "rent, for 1 day froin 1016 2002 - 1`r0Suerosnpecsaocnd1lasncdyolinesfad.lsIwahineiasretc0so%nm,dhsse iHhasevsecoc3npfeirvcentet dorvligipo,ancbe<ebSdeUec.rvgiiDanl ivel ebevGouiosidnre iidsraotngewwoilsbe 124 PPoolllluuttiioonnPPrroevveennttiioonnaannddWWaassttoeMMaannaaggeemmeenntt ~~~ Sulevaste disposedof i soins board assconioes. Flammable sentwatsdiposdof inhigh STUconsiner. laspipewasti disposed finbroke ascontin oad he bors . 1=5 RReeccoorrddss `anComtphelxieactioenwekhectached 0 hiseho,otherpplewoah,ndsrwith esdrw ) Emaixmlcbhyepr.a,gOcebigesoriarofonrmmafeiotorhnosdm,anyyebgemaatsitdocdnomnifeaabnpohidec,saalllpolveinmghef,yorearicoinoinfdaupl,cbltet)esouoe(1 tPoIsCnAa)mend - Phriepheesuenpdageesn ample r nd asoig,n ahdfomMay oldewith hesy rwcha. Copy Pothcalnioncveby he peanreso.Pri eegapsaodsrswithsy ow i. Pai dink sua, negationmod, ndhoo fomMas, nd se with hesy `Sena ota ing sable bare cel70ocLIVS) ds hesyle, Bdacekcupocdlson data 0apprompedriuim.Record istd notebookte le ameadlocationofbac 16 Attachments AsschmerAt: Extraction Wort AsahmenBs: Surpl WeightVohume Wore . AcheC,CleanSundar Caen Workshes ArcDihlionsmSuemyWDor,st 17 References iETdS--24A,m"sppehreitoPr1ensdnMe aoraaneSoofuhse"Micormss Quo I Te Qudpol Mass Spectrometer Fi ET5:9.52 Operonand MaiofnTseeGrinsder" 18_Affected Documents None Solid PhaCsoemEpxosucniEsonTro2SmdB2A i3ol1og0incalofMPsatairceoyschisal Page 140119 3MEnvironmental Laboratory Page 31 000071 i Analytical Report: LIMS E02-1053 Document iiay tc +d Ceurrent, for 1 days ino. 101 2002 19 Revisions RNeuvmisbieorn RevisionDescription ReDviuseion : 1 eMxiancoirfonporrocmhacnsageaestdiAdsudiepdrrndoeesagle,e,d nfdocrmlautiloon nosl.lAsedcdtieodnssctocnhcmeenmsibn15ged 01802 py SolidPhaseEsaciEoTnaSnd8A2s3s11is ofFlsorocherical Page 150119 3MEnvironmental Laboratory `ComfopmBiocoguicna Madtrisc . Page 22 000072 =e _ DUM Analytical Report: LIMS E02-1053 Ew fer Fo edang t foe 10 16 5002 - spbhteelepisr ine BonWet rotsT epneer TE e com | e ME2E sE e Fpgsn em . C Tr T o Tr T r ---- s Tr T T - -- T F TT r - F T br T r -T E m e aEmo m m TT T - m em awRs rn ILER mS am r etE teT e R e orn EESTI eehe aeee momen EeRtBceesar NE rem ne 3MEnvironmentalLaboratory ts RrIsa rn ratcas 000073 Page 33 _ Analytical Report: LIMS E02-1053 FRIment= Ee ad, enn ar 13 Gan fron STs 2602 tachment B.- Sample WeightVolume Worksheet - PrAneaplyDsaete:s: _ M`eSatmhploedMRaetvriisxo:n: EqSutiupdymeNunmtbeNru:mber: Fina Sol&vTNeNumabetr: LF WVol| EEOE T mbt, added | Removed (@) eT _ 1 I [TT [ r7 T 1 TT 1] eT I . T [TT [TT 1 [-- ----7T - rr [--] T/ --7T TT ----F----F+-- r EE rr TT ] t ---- r T r , TT rT 7 [1 I I [1] Fo Completion VriodBy_________ Solid PhaCse otracmtiofnBpraonmTBodiSAolnuossgyiaesoMfdaFturcisrcoecsheical Page 170119 3M Environmental Laboratory Page34 000074 _ Analytical Report: LIMS E02-1053 Dries be wad, Fn dafo5n 102 - Prepdat AnachmenCt: Calibration Standard Concenration Worksheet Standard umber: - ASnamtplae lma:tes: Methoareiion: EFqiuaitprmenot nauvnmbdeTtrNs: BlaakTsueor Flddendir: _ `AAnnaallyytte mmiixs ssdd aapppprroox.. 50..05000iunlg ASnaulyreterramiolsstcdgsadapopptrroeon.s.0oc00f.u0sgeavg:nnat:inoeansysix = Saaicoe pt AnimisLpied || voFlAmuTmte|| aPa iidl||AToiie } wl | Dion | Densy _ [ICov oCsmmo 1I oom 1 |EsoToTA ier sie] d [s1 oooo T Tom1e 1s t aswwToJioo aL ier--Todiiaes|| - EI aoo m -- re w 031Ce Y Ea EH 3 01 [Fran] me]S| . Caliconcentions ofsaat ei teon 2.0mL. sven od il aid i nFoaowtuee||| SSawcriroonlpei||| Am"sFinie|| ow | SSuwarocgakis| wel | A[nAaeis|| ame | SSerraagmaie we : Et 2 | oraIP E | nJ iso Tas dm o hes e-- [iio] == Cam : = Fo] Fo] is Tarr | Solid Pha`se CExcoctimoEnrorspmnsBdiaoAonlaaoluygsiiesnoMfFaitlruioscresschsial Page itor 3M EnvironmentalLaboratory 000075 Page35 _ Analytical Report: LIMS E02-1053 FRI ry sent, for Es tron 116 Tu AtachmenDt: DilutionsSummaryWorksheet _ DiBSltouuxtdiyNo:unmbDaetre:/Analyst EMSxartaTcvitmoTenNpe DNoauitmoabAa tea:ari:ynts _ cSreomepcetNeotmebrer[[ v Tv To Tu [T wouoJmv commT ons |vena:| - I rrr rrTr T - T rrr r T rr1 . I Fe I rrr r rT rr - N rrE r] , --F rrr] -- i e rr T r ] ] Fom Compton Ved By: Sold h`eBCerotomnrpopmBioolioguicantlMadtritcses i 1 3M EnvironmentalLaboratory Page 36 000076 Analytical Report: LIMS E02-1053 - a eweeeisArm an Aopo or: LMs E02-1089 Appendix C: QC Data Summary Tables } Table8. AccSeapmtpalneceoCrtrtecaatSounmmary of PXEeoOaArnNeHhoSeQdCsamplesAnalyzed 1/0102 Sum Sean nar - |Restoretomb [RBStotTeeaC toni |e |] | ass [5 | (%oOm ftCe eF:OS TNh i So rendca em 3S| aaveoSnaz hrorsaoata lc yci m i03a0do tFte] knavweg iiincmef5 foi bvooerrrtchtzs - Table9. AcceptanceCriterlaSummaryof Sample entcaton PBFPOrAr-aAmociamdnQCsamplos Analyzed 1101/02 Sum Banca ese . [Restoretong [RBStoITEaC omg | op] | 25s | 7 | [RLS L esDioe a Hee:acm TTtoRotmegarmrieeiseGzSbFaT| evaer abriotBon2 sn4 crrcmett tpre ss|vno e nitoo e of5p rmaergia WEniorments Laboratory 3M Environmental Laborator> 000077 Pages? Tugge 37 --_-- Appendix D: Data Spreadsheets Analytical Report: LIMS E02-1053 Analytical Report: LIMS 02-1053 3MEnvironmentalLaboratory 3M EnvironmentalLaboratory 000078 Page 38 Page 38 - E02-1053 Analytical Report: LIMS E02-1053 we Jr-- _ FRraiTtnioneeFtasr GRreiinee?r TRoacmmePseik|| Bacchi. Bristle DToiraionn |SBunolIboinRcoctTion _ FReOrAtN PRTOoAnNRA PPEORONE BraschedLiser RESRaISO1I01ES7Q0r2C oaDgnain111 RBSL00802GC 10ngm 11 000 Gwoiims zoesuus||| obponortlnooos E520A02 RRBDSViOoni:zoSGeCOonogatMngT 13a 28510320 en S12 oo - SS3a5sw5s oj3au5nmne|| booantniiootlneosg o ows | conioios F3Tie3a ow f--OSmwmll TChaatFBrLraumepiet Toe em panos|e] 0 waa nas|| oonoioon olseze - "BelovTimCio3hfP0aeGtkolAdSreinsBoTaeeE oo aSo iSoius|| oDoontaonioen a1n3e0 = Bch 7:mitsore sy inFROMM sandscocnions 25 ld. Not ded sm coat Ersaznn 3MEnvironmentalLaborator 4 [-------- 000079 Peed - E02-1053 Pr Analytical Report: LIMS E02-1053 FATAOLAY-SAICS P1oolmeddaawer otlcuddi teHmeopeofthe dy sndwre ot eporied _ Menttaton TrReBetrTiidnnecFh7o9 RTeitLTniianneeea1k|Dianeosne||SBuamsohBaciRhyaiTninc75s7 FROMAG PRO AS pean ey BruschdLinear - RBSIRSO1T0O1S270i03Cd1r0Onanagl 22 1 RBSIOATL QC onal 21 mosm smaoesos flooooo om] aamm iw RBRSBsIWiOon1NiDz0EQ0GCE 1ll3on0oganBgEaT 3a2n RES102803Se Bais w5e0 almosw Pf|opooamitnooiorowaes]e odamr oa ola F-- oSewmbz TCTRCR68G7PtoDsLieudempsiees iam Joonniooss] asn ueuse ffoooimow]s 53] oesss - "owLTiCnR"koGTf0PeCeknaAveteswTesse m3n esmasr Dfoooooonn| oamae erst 3MEnvironmentalLaboratory ContimSoaatotons 000080 Page 40 - E02.1053 by Analytical Report: LIMS E02-1053 - RRAmir Menton TRraTonieemFros F Ratme ers RTameTcht FROANA PRONE FORA RetTioe79 _ a Am Am Sma EoT BraSsHaimaaettLi loom . rS eRsEoSg IoncGEo1o0mmsmnt i1 || o 5 RSIoC oats| sawioisssi Sw aDwawese [|[pooamieooonns]| wn [ounoos| kuammee ffb w ae |i - *DRDotrscthdppsscii7:.6vmiNanoicnsx c|hroor5yTPPO eNIsisTaEts1 cao hoenncen |pBpiT oyon| es maixdnay cl|r in erseastt 3M EnvironmentalLaboratory Horan SorQCveSdRate 000081 Page a1 - E02-1053 Analytical Report: LIMS E02-1053 - [007Rs BrarcnhecdPeak CinearPk Ldentteston PReOTAiAmeG?Hd RPeRTOiAmAeGsEi RetTae791 - Area Arn BrancShaemd:aLtinear - RRBBSSSItIOanIOda0Ir2ds01&1020nC0g.g/CaQVL.C22-1| wson22 aaussssos ||ppooaarntootroosnts "00 |x a2 ffon < RRRBBSE1S0I8SO02N0I0C2SQ01C0n0gg10m0tg2L2122+2||| d71t3s3 ios 22mss tows || bboaaztitnoottoosns pono | 2100 __oos Dataot edeporc. Noktclnthesoedt hesumesnd thereto T ffas 57 ied BEST. 3M EEnrvsiraoznmaennstalLaboratory HumanSera QCveStdRatios 000082 Page 42 _ Analytical Report: LIMS E02-1053 = 0 rAnae lyicae l Reporrt: LIMS E02-1053 Appendix E: Example Calculations - Calculations usedfor AnalysesinStudy E02-1053 - Percentage of Branched:Linear Isomer (also referred to s ratio nthe report) - Percantage = (Branched TBIrCaPnecahkeAdrTeIaC+PLaiskarArTeIaC Pak Ares) "100 `ASmapmplleeTTOORR-669888PPOFOAAPPoorrccoennttaaggee:: ((0BS0a5/8(/8(0850599s+d411d466e6N)"*110000== 1166%% % Difoence =(ExpectedTIC%BrancEhxepdec/tSeudmTnIi%lSBirdan=cOhbosdarSvuemdiTnCal%StBaranched/Sum GC)* 100 Sum = Branched peak area +Linewrpos area 5 OMfrencoefPFOA RES102202-0C-10 nin:-1 sample analyzed 1072202 OItCal=SRBdS1=0R2B2S0120-1G7C0-21:010ngnigm/Lm-1L-11TTICC % % BBraanncchheeddiiSSuumm = = 22 26 ' e ifo=r12o-- 2-n26c)12e6 = -- re~---- 3MEnvironmental Laboratory 3MEnvironmental Laboratory 000083 Pago 4s Page 43 Analytical Report: LIMS E02-1053 - tee meat merge Anaytcal Roport: LIMSEE02O:10E53 Appendix F: Interim Certificate(s)of Analysis SM EnvironmentalLaboratory 3M EnvironmentalLaboratory 000084 Page4 Pagedd _ Analvical Report LIMS02-1053 fe PCheonne:tesr5s1e4a231.5052 LFa;acb(8o16r)a2t2or1i0-e(5s11,9)221I-5n1c5R3.3E0E Centre AInaNlyTtiEcaRlILaMboCraEtoRriTeIs FCOIACAReTteEreOacFe #A:N0A23L-0Y33S(IReSvision 1) - 3MProduct: AmmoniumPerfluorooctanoate `Test Control Reference #: TCR-99131-37, Lot #: 332 _ foams 7Purity: S9p5T e.2l%aton aw) _ aenication - eT1." CCaPlMum 2 Magnesiam 43. PSooadsuimom 56. Niiocnkel 7. Nunginese [rae] 21 5 00000000011swwwiimsn +5 <00000011wwiitsn 76 .000.00011wwiisntss - [[TToomlT%eTfmmppuurriittyyC(GMOSA))| || w NoneGn umniie] d | roams ChloArniidoen - 52.. BFlruoomriiddee 21. <00000isswwims 54. NNiiee 6 Phosphate +5 o20g090wwiismn 5 o06wann - 5: Suma 65 S0oo0t0wimrme X "Orga2InicPTFEPAAAcids (I 5 HBA 2L llamss 5 01win lem4eraNl PAAny + asm i : 521... HCNayirdnbrooognge'enn 3 Sulfa TThhTeehoeororereteiticaallVVVaaallluuee +=023232.355%%% Thcoedial Valo =0% 321 3118793wmm/iiw nn% 43min mo5.a_FltuoArnianel TheoreiaVale = 66.1% 5. 62min Ton Seicetive Electrode Theoreia Val=e 418% 49mm CONO2I03337REVI doe 3MEnvironmental Laboratory 000085 Fuge tor2 Pageds _ -- Amavlvical Report LIMSEO0:.1050 _ oe CentreAnalytical Phone: (314)231.8002 LFaaxb(5o14r)a2t3owr1iow-e(s511,4)223I15n-1co83.5n0 INTERIM CERTIFICATE OF ANALYSIS - Centre Analytical Laboratories COA Reference #: 023-033 (Revision 1) 3M Product: Ammonium Perfluorcoctanoate Test Control Reference #: TCR-99131-37, Lot #: 332 _ DaoftLaest Analysis: 12/15/00 Expiration Date: 12/15/06 - StorageConditions: <-10C Reassessment Date: 12/15/06 i} T"oPtuarlitLy C=/1M0S0i%mp-u(rTiottiaels,Me4t.a4l9%i)mpurities, 0.006% + Total NMR impurities, 0.34% + `Total impurity from all tests = 4.84% Purity = 10-0 4.8% 4% =95.2% TFA Trifluoroacetic acid HFBA Heptafluorobutyric acid - NFPA Nonafluoropentanic acid PFPA Pentafluoropropanoic acid MThWe=o4re3t1i.ca1l)value calculations based on the empirical formula, CoF:s0ONH,) ) LC/MS Purity Profile: [Peak T Retin Tie ala) | fais)|Wesily--|| ArAersa Cre 1 rwwwww `This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). Prepared By: Scientist, Centre Ana alytical Laboratories DueIA Reviewed By: ", wo LaboFraltaohreyrtMyanager, Centre Analytical LaboratoriesDate COAGZIO-ITREVLdoc 331M EnvivriornomennmteanltalLabLoarboaratory 000086 Pugez0r2 Page`age d46. _ --_-- AnAanallyyttiiccaallRReeppoorrt:tLLIIMMSSE0E20.2-11005533 S3VMLEENNVIRONMENNTTAALLLABORATTOORRYY ~~~ _ Note to File . TheexpdiesrfxnPPOilootsHnU [401DU1d332 (TCR.99131-018wadTCR.99131037)mybe - eimoded 5youn(12/15/06) a abilitywas densidad EOO-1851(yey)B00.2193 7 -- FeEan] a -- en -- Recorded By Ba Bi FomBTS4150 - etomonn se toler 3MEnvironmental Laboratory 000087 Bl uy of copy cull Page 47 Analytical Report: LIMS E02-1053 _ 3M SPECIALTY MATERIALS & MANUFACTURING DIVISION ANALYTICAL LABORATORY RequestNo, 62631 - To: William Reagen - (8-~E6nvi5ron6men)tal Lab- 2-38-09 StudyNo. FACT-TCR-005 Etom: Tom Kestae-r (3-5633) - SMMD Analytical Lab - 236-2B-11 - Subject; ICRheSmpieccatlroCshcaorpaycterizationof PFOA, Lot 332, TCR-99131.37 by "H-NMR, F-NMR, and Datei December 11,2000 -_ - S*AMPPFLOAE,DEloSt 3C3R2,IPTCTRI-9O9N1:31-37; Nominal product =CyFis-CO;*) NH. (white powder). The sample was stored in a 20 C freezer at all times except when aliquots were removed for analysis. _ OBJECTIVE: . ``aTlnhsoiomsianscaaqlmuppilrroeeddwufacotsr astnuhbedjpteuocrtcpehodasrteaooctf"ecHroi-nzNefaMisrRmmiaannngdyt"hi*emFpn-uoNrmiMitRnyasclpoepmcetprrofalnlueoanrntiasnlayatsseedspoctsaosridbbeoletx.yelramAtinenesFatTlht-eIfpuRunrcsitptieyocontfarltughmrewouaps. EXPERIMENTAL: EL-NMR bAisp(orritfiolnuoorfomtheethtyhla)wbeendzseanem,p(lpe-HwFaXs),acacnurdattheelny wtoetiaglhlyedd,issspoilkveeddwiintahcaetkonnoe-wdne faomrosuunbtseoqfu1e,n4t- analysis by - N6M2R63.1.A40n1)inwiteirale 400MHz acquired u"sHin-gNaMVRarsipaencUtrNuImT(Y# phl6u2s63410.040F1T)-aNMnaR3sd7p6ectMrHomzet"er*.FA-NMsRecsopnedctporrutmio(n# of - tdhiesssoalmvpedleinwdaesutaelrsaotaecdcturriaftleuloyrowaeciegtihceda,cisdpi(kCeFd;wCiOt,hDa =knToFAwDn)a.moAunntaodfdpit-iHonFaXl,40an0dMtHhezn "toHta-lNlyMR `saosslpsveoeccntitra.utmeTd(h#weiht6ph2r6ib3mr1ao.ra4yd0pN2u)rapHnodseraeo3sf7ou6nsaMinncHgeztthhe*atTFhF-aANdDMbReseosnlpvoeebcnstterwruavmes(d#tiofn6h2e"6lH3p1-m.Ni4M0n2iR)msiwpzeeercetthrceuolmilnoetfcetrtefhdeerieannccteehtseonTe-FdAsD sasolautnioinn.teTmahlesstaamnpdlaredpfroerpaarbastoilountemewetihgohdtdpeesrccreinbtedmeaabsouvreewmaenstisntinenedietdhetrospoelurtmiiotn.the useofthe p-HFX | E-R i AtrapnosrmtiisosnioofnthFeT-sIaRmsppleecwtarusmp(repAaGr2e6d31fo)rwFaTs-ItRhesnpeacctqrualiraendaluyssiinsguasiDniggitlhaebKFBTrS-d4is0kFtTe-cIhnRique. A spectrophotometer RESULTS: ThihgehcpoumribtiynfeodrNm VofRthsepencotmrialnadlatiesoimnedriciactperdotdhuectsammipxlteuoref,PCFyFOaAn,s1l-oCtO323"2),NTHCLR"-9,9w1h3e1r-e37`nc'ownsaisstmeadinolfya 7. the A few NMR tsrpaeccet-rlaelvedaltai.mpurity components were also observed, tentatively assigned, and quantified from Page 113 3M Environmental Laboratory Page 43 000088 _ December 11,2000 Analytical Report: LIMS E02-1053 33MMSSMMMMDDAAnnaallyyttiiccaalLLaabb:ReBqiude,st23#66.2286-3111 RESULTS(cont): - Tanhde "guFa-lNiaMiRvespaencdtrqaulaanntiatlaytsievseacroemspousmimtairoinzaeldeisnlTtAsBtLhEat-1w.ereAdneyvwaetefrrtohmatthmeasyihnagveetbiaelen`pHr-esNeMnRt in - sthheoswanmpinleTAwBaLsEi-g1norsehdouflodr cbaelcvuelraytcilonospeurtpootsheesir. rTeshpeec"t'ivFe-aNbMsRolruetleatwieviegwhetigphertcpeenrtcveanltuceosncweintthrtahteions stated assumptions. fluorocarbon chains In ordertoperform contained 8carbon the relative weight percent atoms except where noted. calculations, Iassumedall of the In general, the "'F-NMR technique - iismpnuortiptayrtciocmuplaornleynwtesllunslueistestdhfeocrhcahianrasctaerreivzeirnyg sshmoarltl. aAmomuonrtes coofmppolteentteiaclhafrlaucotreorcizhaetmiiocnaolfahonmyoloothger - `iomtphuerriutnyidheonmtioflioegdsimwpouurlitdieresqaurierealasnoaldyestiesctbeydeilnetchteroNspMraRysMpeSctorraa,sbiumtilaadrditteicohnnailquweo.rkTrwaocueldamboe.unts of required in an effort to identify or quantify theseother materials. `The FT-IR spectrum was used to verify the nominal perfluorinated carboxylate salt functional group. - rCeospulitess,oorfitfahenNyfMuRrthaenrdwIoRrkspeicstnreaeadreed,atptlaecahseedlfeotrmyeoukrnroewf.erence. If you have any questions about these Tom Kestner | L`iTsanayCalReomdeen--QEATI S - 2.38.09 Rick Payer- SARC Anaya Lab -236.2C-1 Fle Rel: 263104)PACTTCRO03dct Stady Protocol #FACT-TCR-005 Pager 3MEnvironmentalLaboratory 000089 Page 49 December 1, 2000 Analytical Report: LIMS E02-1053 33MM SSMMMMDDAnAanlyatiycaalLLaabb:ReBqiude,st23#6622683-11 TABLE-1 Sample: PFOA, lot 332, TCR-99131-37 | Overall CompositionalResultsby 'F-NMR Analysis & "H-NMR Internal Standardization Analysis Structural Assignments F-NMR Relative Wt. % : _ Normal chain s-- omer -- CoCnocnecTenntrtrraaettiioonnss | : (wher x asCsFu3m(eCdFt2ob):e-CfOo;r"c)seNulHat,on prpo (where CIFn3t(eCrnFa2l)m,o-nCoFm(eCFt5h)y-l(bCrFa2n)c,h-eCdOi"sNomHe.rs" xy as1sbeufomrcaeleudion purp0odsxe4.,0, 0) =12.5% Tsopropyl branch isomer (uhere(x CaEsssu)mCeFd-o(bCoF2f)o,c-aClOc"laNonHpup t-butyl branch isomer (where x(sCuF)m,eCd-t(obCeFy3)f,r-cCaOlc"ulNatiHon,purpos FF . =X % Possible F FF F + 0CT Internal gem-dimethy] branch isomers. (wheCrxFe3y~a(sCsFumae)dxto-bCe(3CfFor3c)-a(lCFc2u)p,ulp-NoaCsHOets,:i"xo20n) o v J. PCI n Fch Possible ' Ng (heeCPaoFsasaiubuls-eCtaRosl(bpCehFai3fb)or-mcaCanlOcceShulaiNtsdiooHnme,rpurposes Probable F-SFy-Ry, (whpeoessibalsysuamsedF-tSbFey-7 CfaoFazcxu-aCiOo,nNpurHposes 0.085% =0.029% Concentration 1)Trace amountsofother unidentifiedcomponeats ce isodetected intheNMRspectra. Study Protocol #FACT-TCR005 3MEnviwriroonnmmeennttal Laboratory Page3of3 000090 Page 50 } -_-- AAmnaallvytiiccaallRReoppoorrt::LLIIMMSSEE02R-1O05R3 Certificate of Analysis ' `NominalProduPcentt;aCdFecya(lCuFo)rxooCcOtSaHn,iwchceirdeaverage nx 6 - `Product Code: TCR-L6ot121700,02 Tom KOcetosbetra2on8d,eJ2oe0o02Miller : LC/MS analysistehaiques. Theoven qualanidaquaintitvatieve compositions ess ate The sampleofTCR-617, lot 210002 was analyzed using a combinatioon f F-NMR, "H-NMR, and derivedfromthesecombined analysesare summarized beinl TABo LE-w 1. v TABLE-1 Quantitativeand Qualit ative ComposSiatmipolnea:l TCR-617, Results by Lot 210002 Combined "*F/s'nHdL-C/NMSMR Analyses i} `Component Structures H/PF-NMR| Relative Weight% Concentrations | (single trial analysis . `CF3(CFa-COH. <99.51% whereaversge n- 6.02by "F-NME. Purity LC/MS showedn=6 (major), n=5, n=4 (minors). assume net for calelation purposes g Probable (CF3);-CF-(CF2)e-CO:H Probable (CeF130)-CO;H acyclic ether acid aspossible CF;CF;-O-CF(CF, ,CF,-CO; her Pos0,14 sibleanCFd(sCuFam)ey-rCyF(=C4Fso)r-c(aCl2ef)u,i-oCnOHpurposes aPosssi1bls3e (fCouFrc;)a;mt-Ci-eoCFn2)sp-gCoOsHe Tinwotsofoh ksigndcompen ws 0danced HeNTRFo 0.057% Dhomaec Socte-- (0-250 Ll Crofisfod fe 3M EnvironmentalLaboratory FileRefs Cofh_TLCok2R1100702_0 000091 Page 51 _ Analytical Report: LIMS E02-1053 e Appeendo ix G: r Report Signae ture Page n Analytical Reeport te: LIrMS E02-10t53r _ pr P22 `William Reagen, Ph.D., Laboratory Management, Sponsor Representative Date Fs A Slovgngen - Lisa Stevenson,Principal Analytical Investigator loa Date 3MEnvironmentalLaboratory 3MEnvironmental Laboratory 000092 Page 52 Page 52