Document emR45Obod7dznmOym1R0r2BM4

- 226 US] ntTT - ANALYSIS OF ENDOGENOUS FLUORSOCtHEuMdICyALSTiINtNlOeRMAL POOLED HUMAN SERUM AND PLASIA - Data40RCeFqR uPairtr7e62ment - Author Mark E. Ellefson Study1C3 oNomvepmlbeer,t2i0o02n Date ' Revised Report 9 December, 2002 : PerfoSrM EmmiionnmgentaLlaLabboorlroray tory : 9B3u5iBdunsgh2A3v6e.n0u9e StPa, MN55106 Project Identification J 3M Environmental Laboratory Study Number E02-1039 Total Number of Pages 25 CONTAIN NC CBI 000093 - 3M ENVIRONMENTAL LABO0R2A-T1O0R3Y9 This page has been reserved for specific country requirements. 000094 Page 20225 - - GLP COMPLIANCE STATEMENT 3M EmvronwenTaL LasToorarTronoy kd - Study Te: APnlaalsymsais of Endogenous Fluorochemicals in Normal Pood Human Serum and Study Idenication Number: 3M Environmental Laboratorystuy Number E021039 - L"Tahbiosrsattuodryy Exceptions wParsaccoincdu(cGtLePd) to GLP complia iSntcanocmaprlciea,nc4e0 nce: wGitFhRT7o5x2i,c Swuiblsthaen cxecssCpoynotnrosl sAcets( TpSeCtAe) G ood - 40 GRFaRrc7c5o2p.y13p0r(ient)o:uTtshaerrs csonnostidaenreldec(hreoroiricgain)urroaldeonfscarections. The authenticated KE Eletoon,Sud=Didier yWehamR. Ragen, Tosing FacifyManagement T/a2t/e9 Joa /Daat/e fer/os Page 3 of 225 } - QUALITY ASSURANCE STATEMENT oeSena osgmnrony ee Study dontfcaison uamber: 9M Esai Laboratory Sy Nober E02.1058 - TpTliacssdeyenwtaaeuitge itehe EgneonnLahboeraetonryQSiultyyfAesaarn UUnnikt (GGAA)L,o6n [em meeTe] a sChoen) iad) _i2fefe 000096 Pa 4 ogf2e 25 _ 3M ENVIRONMENTAL LABORATORY 02.1039 - TABLE OF CONTENTS - `GLP Compliance Statement......... QUBIYASSULBIICE SIBBMENL ccc m-- ppd _ USEF TADIES css UOFFH IGUIBS.c.cco 6 wsms---- SEHXYECIUOOSMRUIOMNR. Y . ...cc ototcso ssssnssssememo 8 - SUIMRIY.ct sss - IUOGUGHON. TES SUDIANGS ce ss e n 1 . ROiOTEa SSUBIANCE.....cssssseesee oo 18 MEPrMepOarSatUoMryMaEnEdSAnac lytical Method ee is16 - AOBYHGE RESUS... DBR SUTIIRY ssn 48 20 SStatisH ticalE OMEftCNOEOMUOSUSN aIO0N CBo IGUIBIONS reses 31 82 : URISEEOfIAGBOTNTOIOMNSG.OS..c ...c.oco oossmsss ssmmsoee oo 83 3 SIGNIAIE PAGE cc g AUBRMEAN MONO... commer 36 AUETENB: DH TAOS... AUBCMENEC: CIOMBOGANS....ce 58 63 AANUEBcChmMeEnEDNt::PPrerp SOheBaItGsAOanMdCATFTOaICe!.ab.it.y INOMaNON............orroo 125 208 000097 Pa5ogr2e25 _ _--_-- - LisT OF TABLES 3M ENVIRONMENTAL Lago0R2a.1T0o3R9Y - Table1.2. Table 1.5. Endogenous levelsof Endogenouslevelsof testsubstancein test substancien normal normal pooled pooled human human serum nd Plasma..................o _ Table 2. Characterizaotfitohne Test Substances... " Table 3. CharacotfteherRefierezncaeStUDSiIAoNGnES emmmtmPl ovo 14 `Tabl4e. Descriptionof Test SystemsUsed inthis Study.. Table5.a. Endogenouslevelsof test substance in normal pooled hUMaNSerU -- ........... 20 - TaTbalbel56e..5.AcEcunrdaotgeenMoausss lDeetevromefinltaetssitonsoufbsEtnandcoegeinnoNoursmTaelsptooSlUebSdIhBuNmCaenS Plasma............................. 20 21 - Table7. Daughter 101of ENA0GENOUSTestSUBSIENCES....vcr.rroesrrrrorn 21 - LLiissttooFFFFlIGGuURREeSs = Figure 1: L NMRE CertifS ied 99.5R% Li--nea--r Is--omer PFOAhandaMixes d Brh anched and Linear Isomer Figur2e:C; lsomerDistributin.......... eT . FIQUI3E: CyISOMEFDISUIOUION ccc oenons25 FIGU4:TCEo ISOMETDISTBUION ......corrcess FIGUI5D: C1 1SOMETDISIIOUION...cccvnseson snd 27 Figur6e: Ci 1SOMBY DISIDULON ccc. mms 2 - Figur7e: FIQUI8: Cz 1somerDIStributo............. - PROS ISOMeNDISUOUION......o ------ ee 30 000098 Page 60225 _ TT ---------- - STUDY INFORMATION Sponsor 3M ENVIRONMENTAL LABORATORY 02-1039 3WiMllEinavmiKr.onRmeeangtaeln Laboratory _ Bidg. 2-36-09 S9t3.5PaBuuls,hMANve5n5u1e06 651-778-6565 - Study Director _ 3MaMrkEnEv.irEolnlemfesnotnal Laboratory 9Bl3d5g.Bu2s-3hEA-v0e9nue - St. Paul, MN 55106 851-778.5405 Study Location Testing Facilty . B3lMdg.En2v-i3r6o-n0m9ental Laboratory S9t3.5PaBuuls,hMANve5n5u1e06 . SWtialciyamR.K.A.RHeaangseonn,,LAanbaolryattiocrayl CMhaenmaigsetr 4 MCianrdlyenMe. MC.arHlesyoinn,g,AnAanlayltyitciaclaClhCehmeimsitst Ognjenka Krupljanin, Analytical Chemist Study Dates } ESxtpuedryiImneintitaatilonI:ni1ti0atOiocnt:o1b0erOc2t0o0b2er 2002 ] SEtxupedryiCmoemnptlaeltiCoonm:ple0t1ioNno:ve3m1bOecrto2b0e0r22002 Location of Archives. aaAlnclaclooyrrtidigiciannlaglptrhoaa3wsMedaoStftaatnhaidnsadsrtdtuhOdepyreweripaloltribtnehgaaPrvrceohcibevedeeudnreaastr.3chiRveEemndvaiiartnoitnnhmegen3stpMaelcEinLvmaiebronorsnapmteeornrttyaaiflnoriLnaagbsotrloaottnohgreya.s the quality of the preparation affords evaluation, 000093 Page 7 0f 225 _ _-- - EXECUTIVE SUMMARY 3M ENVIRONMENTAL LABO0R2A:T1O0R3Y9 - pAqsulacanrstemiefaynfiernnogdmoscgteeundntyroauolsfCthlheirvneeael,solaoftnsdpoeffrofculorumlomorteosrhcoefipatclaonmpcmoaeotrleceid(Cah7l)u,pmopaoelnnetpdaldhaeuscmmaaal,lnuoosnreeoroluoctmtoawfnacpsaotouelne(ddCe8rh)tua(mkPaeFnnOt)o, hpeerpftlaudoercoadfoldueocraonnooantaeno(aCt12e)(,CaS)n,dnpoenrafdleuocraofolcutoarneodseuclafonnoaatee ((CP1F0O)S,)p.erfluoroundecanoate (C11), - fwRreeosrmuel<tosb0s.fe0rr1ov0me--tdh0if.sor9sttnhuged/ymGLs7.ha(oTnwadebdlCe9qsu-a1Cna1ti2afnicdaoblm1ebp)lo.euvLnelodswsotfdoettnheeocnlt--iedndesat(reFicigtsuorlmeeevre1 sl--os fo1f0C)7b. r,aPCnFc9hO.eCSd1w2iasrsoamnpegrriesnsgent - oinfngtcihomemlmsaecnrrdceiewanalesdseplrortaessaoenfndtcopamlsmaebsrrmacanicainhlecsdoenracanednatnlrdiantepialoranisssmoramaenirgnsic.nognPfcerFnoOtmrAa0t.wi6ao5snspr5r.6aensgeningnt/gmiLnf.rtoahmends2c.w5rae-se2np7erdesleontst - as branched and linear isomers. 000100 Page 0225 : IM ENVIRONMENTAL LABO0R2A.T10O3R9Y = -_-- SUMMARY - pQpeuoanontltaeiddteahctauifvmieausnocrproeloecantsiamnnagosatotwedeer(tCe8e)rc,moinhndeeupctetanedddeocoganefnlfuooouurrsolnloeotvsneaolnfsopoaoftoeplee(rdGfSuh)o,urmnooahnneapdsteeacnracufamltueaon(rdCo7df),oeucranootastoef _ a((nCPa1Fl0y)O.tSi)cpaealrssfcdlreoesreconrdiienbcgeaddnaobtayatteihse(sG31u1Mm)m,EanrpvieirzrfeoldnumonernottdaabolldeeLscaab1n.o3or.aattaeonrd(yC11S2bt)u,dyan#dE0p2e-rf1l0u3o9roporcottaocnoel.sulTfhoneate - Table 1.2. Endogenous levelsoftes substanca in normal pooled human serum - SubTsetsatnce TCTRoem8aS (ng/mL) TAOpReE BiToCrReS&oSU7RCE Golem We: TCR$30 (ngml) __ (ngimt) (gmt_)| _ ICFFoS waor5e) ro24o5m]y [37202] [2720 cCon os) 10058) (<o0t0" 0031) 0295 327) 0320 0203 . lcs lcs 026s 1.80 oss) 0650 0605 295 0s00 560 lc 0013) 10025) 0010) 0.190 - 11Denotes values determined from concentrated spe method. `Value <LOQ. Table 1.6. Endogenous levelsoftest substance in normal pooled human Plasma. - |_Anayte TTOmR&74 (ngml) TCRiG8dS ReseaorvchaTtCeR683 TaTCmR-6W8e4st ___(ngimt) (ng/ml) (gm) _| ) [Pros lc lc <10 <o10! Tn 10038) 55 woz) 183 0024) <010" oss) 013s or lcC,o <<o0a120s!! 121 0.435 0170 oses 0160 os35 lcs lc: <0s2' 261 010" 0.100 a07 wore) ag7 02% {1 Denotes values determined from concentrated spe method. 'Value <L0Q ACc1c1u.raatned mPaFsOsSmferaosmuarecmoencnetnstraantdedelSePmeEnteaxltrcaocmtpoofsniotrimoanls wpoeorleeodbhtauimnaend fsoerreunmdo(sgeeenoTuabslCe76-). cChoanrcaecntterraitsetdicSdPaEugehxtterracitonosfwneorremaolbpsoeorlveeddhfuormeanndoplgaesnmoaus(sCe7e-CT1a2b,iea7n).d PFOS from a b`QarucaalcnioctmhapetlidivseahnaenddaliuysnsieinasgroiNfsMcohRmreorcmerPattFiofOgieArdamsptihaixncedadalrsytdasrnoedfsaaorldv.nedeIabt rrwaainsscohdmeeedtrearPnmFdiOnleAidnestathraaitnsdtoahrmedebrarsnaodnfcoPhfeFadOmPAiFxweOadsA. fisroommetrhseelliunteearwPitFhiOnAanisaopmeprr.oxiTmhiastefi0n.d2inmgionfutCe8rietseonmteironrettiemnetiwoinntdomw arensdolaurteiobnaswealsine resolved 000101 Page 9of225 - 3M ENVIRONMENTAL LABORATORY 02-1039 _ heixgthraeprohloatmeodlotogudeetseorfmiCn9e-Cq1ua2l,itaantidvePlyFtOhSe (psreeeseFnicgeuroers absence 1 - 8), of branched isomers for the. _ wfRereosrmuel<otsb0s.fe0rr1ov0me0tdh.ifso9rsttnuhged/ymCLs7.hoa(TnwadebdlCe9qsu-a1Cnat1i2afnicadbolm1ebp)l.oeuvLenlodswsodftoetthneeocnlt--iedndeeat(reFiicgstuolrmeeevsrels1os-fo8f)C.b7,raPnCFc9Oh-eSCd1w2iasrsoamnpegrriesnsgent - noinfg/tchomemLmsaecnrrcdeiewanalesdseplrortaessaeonnfdtcoapmslmabesrrmacanicainhlecsdoenracanendatnlrdiantepialoranisssmoramaenirgnsi.cnognPfcerFnoOtmrAa0t.wi6ao5sn-sp5rr.ea6snegningnt/gmiLnf.rtohamends2c.w5rae~se2np7erdesleontst as branched and linear isomers. 000102 Page 100f225 - IM ENVIRONMENTAL LagORATORY 02.1039 _ OO INTRODUCTION - `p(CTe1hn0et)a,pdueprceparoffsileuooorrfootdohecicstaasnntoouaadttyeei(s(CCt81o)1,p)e,hrepfpeotrrafmdlequucoaarnfotldiuotodatreicovanenoonsaactrneeoea(nlCie1n2(g)C,f9o)ar,npndeorpnfeairduefoclrauofhoelopuctoiaranonodeaestceuafn(oCon7a)at,tee - sT(uhPbeFsOtsSta)undciyen dntehosartimgainsldipsoosioneldceodomnhptluoimaaannscpeescewiirftiuhcmUcaoSnntdEroPpllAlaesTdmoatx.eisctTsShyuisbstssettmauncacysecspiedCronnaottrcoohlnavvAecenttai(o(TnySapClcAaG)lL{4Po0stsCtFudAy. Part 792. _-- TEST SUBSTANCE - Pmarteelriimailnairnynsocrrmeaelnipnogolienddihcuatmeadnthsaetrtuhme taensdt spulbassmtaa.nceIsnfloirsmteadtiboenlpoewrtaarienipnrgesteonttraacseabeinlditoyg,enous - sexoiusrtcien,bpihoylsoigciaclaldmeastcrriicpetsi.on, and storage conditions is not available for these compounds 2s they. Thonn Table 2. Charactorizationofthe Test Substancos - Test Sussrance Forma - [HeplR adecao fuorom nonansoated (1609))octon|c[eo crmw omoe ons o| - [[P[| oPoerrovuornddoesceacnsomsoaiteeCC8t))-- | corccoos || [Peromoctanesoborate @FGS) | orisor | The molecular structures are given below. - Name: C7 CMohleemciuclaalrNWaemiegh:t:Per36f3l,uoarsohsehpotwannoate v FlrF _F ]cr _o o elFrF lrF 000103 Page 11 0225 - 3MENVIRONMENTAL LagORATORY 02-1039 - Name: C8 _ CMohleemciuclaalrNWaemieg:ht:Pe4ntad1eacsas3fhlou,owrnooctanoate _ FFFoF FFFo _ F FOFFleeFrF 0 - Name: C9 Chemical Name: Heptadecafluorononanoate Molecular Weight: 463,asshown . FFF lrF [F_F F 0 - rleleler FF FF Name:C10 - Chemical Name: Nonadecafluorodecanoate Molecular Weight: 513, as shown - FlFrFrlr]FP |e_F r _o ) F FrFlrelF rleFrF 0 Name: C11 CMohleemciuclaalrNWaemiegh:t:Pe5r6f3l,uoarsousnhdoewcnanoate FFFlFee_rF_F ]rF _o F- rlelelrle 0a FF F FF 000104 Page 120225 _ 3MENVIRONMENTALLABORATORY 02-1039 - Name: C12 _ MoClheecmiuclaalrNWaemigeh:t:Pe6rfl1uaosrso3dhood,wecnanoate _ FlFror r|Fr r Fr EPF F og > _ F rlFeFlrlF rlF erF - Name: PFOS CMohleemciuclaalrNWaemiegh:t:Pe4r9f9l,uoarsooschtoawnensulfonate - F FoFrF p[FFF 05 _. - rlFeFlre]FrF 000105 Pa13gof2e25 } SE.. RR . - REFERENCE SUBSTANCE = Reference. B. SE k Er so | Traceabi pr # ae == Er ahiDescription Storage == Purity I : EE= L=n Ey [oe em [CoNw[J=e oBaaEr TfEol[eoenleLe fClCoaneoJToEeYr]] NE a= roo m0J, Jom [rem | 000106 Page 14 of 225 Sw Emmons usoessrsony . TEST SYSTEMS TE ---- ' REE ET ETS ROTEL : [PoHuomanlSee rumd __|SgmMe aukA ee,wd i ich,|[TCR se,Lotozzwosss | Foie mn sein : Seelicaton ofhe TestSyatem G55 on play Gang noma poo sre 370 CIodlolnCetcftoicoanriooafnToefosToSesysStayesmtmeem.TohSroamscpalmemesweeelrteenndtarose hyacn TCoRtrrube oer.of thfoutfs of nDPraaoueaungvcaenetnehadohUro3so{tmByoapw eASehoo hSaonerea sd beosAosepresocsrsiopsoslpeadeO uarapS sreosts,on, ramon om mame ana poi METHOD SUMMARIES P7r5e.CSp0o.atn2rso0aa1eit.ha1eoo,rnaySlWoaoealnfkddaiomPAcehnnaasseloeytnAtEAisx2ctSiar0TalucmtMTeieoaoetnmhaomnoSddapoAfrngsalyTeSsiosoor fFpluooaron caheecriceaerlinCtoemtp,ooupntdollsts foreaymr oCTFoeanmiFgeaoarrw3ae3an5ad0iB0bnaeorrvTthfoa ernS3o0res 5m0o0natsrSNovyoSs ampvesaveesroStti a oh35t00Lortg, oe a aks phe wari (57 Gonga ooaidractPehc adsSerPEEt Moe5tsheode ,oeAdma ir iaefoofrS PmpoefoahertSaoPEsmethod deE scerebyA T75S.31h. trere Teroamoanastma,envdev2ln0o0to.lawinmea%fo2y6bsBemtooamonhmNooargo sTooDnsoseasborad:AmsolSmFopnsrbSSnoOaar8msapaopiatndeerranfor SCoonmAieSssTt,oTonnsdemecewargiesposdepos5rs0ees)tor 30tcDeOonMcnan Senprp,gdr,ed wRFiNtl 000107 Page 15 of 225 = 3M ENVIRONMENTAL LABORATORY 02-1039 _ u(mesStePhdEa)ntooclac.ratlrFiiubdrrgaet.theertThsheeenrsuaintn.iavliyttyewsaosf ainctheireesvtedarbeyedlouutbeldifnrgotmhethienjSePctEiocnavrtorliudmgee uosfitnhge2.st0amndLarodfs - Analytical Method _ CALnoiaqlluuyitmdincCatlhercmooplemuramatnto:ugrerK:aepy4hs0t:oCnHeewlBeettta-sPialcTMkaCrgd"2Sxe1ri0e0smm11,050pLmiqpuairdtCihcerosmiazetograph system FCylcolweraTtiem:e:30107u.L0immiinnutes - MInojbeiclteiopnhvaosleumce:omp1o0nueLnt(s2:0 pL. for concentrated SPE method only) - S`Soollvveenntt A: B: M2.e0thmaMnolammonium acetate in water _ Solvent Gradient: Time (min. 0.00 %8 40% 1000 90% 1111.5000 90% 100% - 1132.5000 41000%% 16.00 40% = SMoafstwsarSep:ecMtarsosmieytnexrv:erMsiicorno3m.a5.ss Quatro Ultima triple quadrupole mass spectrometer Mass Spectrometer Acquisition Parameters: - () Channel P(amrezn)tion Daug(hitzerion EnCeolrlgiysio(enV) Cone (v) 1 3300 11900 2 2 . 2 00 16900 2 2 3 300 21900 = x . ` 38300 1000 2 2 () : Channel Pa(reeminzt)ion Da(ugmhzt)erlon EnCeolrlaiysio(enV) Cone (V) i ' 41300 11900 = El 2 4130 16300 Ed 3 300 21000 2 2 4 41300 300 2 = 000108 Page 16 0 225 2 _ IM ENVIRONMENTAL LABO0R2AT1O0R3Y Channel P(amrienn)tion Dau(gmhltze)rlon EnCeolrlgiysio(enV) Cone (V - ' "00 ry 2 = 2 w00 16000 = = - 5 8300 21000 2 2 _ ` 8200 "1000 = = [0] . Channel Parention {miz) Daughterion (mz) Colision Energy (6) Cone(V) ` 51200 om = = 2 S100 16000 = = } ) 51200 21000 2 . S100 46000 = = - ) Channel P(armeznt)ion Da(ugmhltze)rion EneCorlaiysio(enV) Cone(V) ' se300 om 2 3 2 300 18900 = = a S300 21000 2 2 ) ` sa00 S000 ) Clams! Pameston Dagherion galislon Cone) : ' e100 ry 0 2 2 61300 16900 = : a e100 2000 = 2 . 61300 sean 0 = 000109 Page 170225 _ IM ENVIRONMENTAL LABORATORY 02.1039 - Pros = Channel P(amrezn)tlon Da(umgihat)erion EnCoelrlaiysio(neV Cone (V ' 49900 0 " & - 2 9000 900 @ 3 "00 00 & CGaapiinl=ar1y.0VolEtMagVe: 4000 V - GMoadse:TemEpleercatrtousrper:ay25Ne0gatCive - DNerbyuilnigzGears:Pre8s.s0urLe/:mi3n0. psig Analysis Type: Mullple Reaction Monitoring (MRM) -_ ANALYTICAL RESULTS Data quality Appendix A). objectives outined in the 3M EnvironmentalLaboratory method were met (see ) Regrcaeatsiabsritaootnisiom.npcrQuourvavederqsauthainacidicaautricvooeenfffioitvcweiereintgthhoetfecddoent1ce/erxnmtwiranaasttiiaoopnnplroiafend0g.et99acp8aplorirobprgrariteiaaottneersotatnhdeacradtsa.anAdllsample ] CalifCbohrraietnnieodsnoegSpetlnaaonsdumasardlfesovr.elaslCoapfllitabesrsatmtasiuoanbnscdtuasrnevceresumiwneqtruheaentpCirhaeitpinaoernssee.dpflrRaoesmpmoearxttceradalcivbtarealdtuimeosan wrceuirrvesetnao(nltdeacverolrdsrseocifntaed : `creuegrnrvdeeossgsecinooonnusasinstatelesydtsoisfsubaussmtianignncitehmseuimpneotafhkeianCrheeian(s9e)sopfeotipnhltesa.asnmalaTyhtweee.reeqTudahetetioeanrcmcwiuanrseadcdyetotofebreemai<cnhLeOdlGeb)v.yel wTahse vcearlicfuilead.ted.AnyAlllelveevlelosutsshidoewe7d0%a r-e1s3p0on%soefgnroemaitnearlthwaanstdweiaccettihvaatteodf,haendblraengkression ro. : Contcliiamlniitubiornaftg2ioC5nal%cihbedrceavktiiwaotanisoVnearonifafltiyhczeaettidaornagt.elteFcaoosrntcqeeunvatenrrtayitaittoeinnsv.esadmeptleremsintoatmioonnist,oar iminds-tlreuvmeelntmaaltrriixt, with a Limicttuhraovnfe,Qtuwwaointtthiimtaeasetviteohlneo(rfLeOasQcp)co.unrsaTechoyefwaiLntOahliQyntw+ea3i0sn%e.tqhueaTblhleatonlketvhseealmlopoflweeasnsa.tlsytteanidnarthdeiLn OthQe wcaalsibaraltsioongreater Demo`canhnsrdtoirmsaaottmoiegorrniacpohpfriSocpperocerittfeiinoctniistoyn(.htieTmrheese,aicpdhpealnritcaiacfbitlceear)tii.sotnicofprainmaalyrtyeisonwsa,schsaurbascttaenrtisitaitceddabuyghter ons, ContrsreuocblosvtoeafrnyBcieaansa.dndtTobwerovaacllkeuevaletilnesgomtfehtmehiaondxtipcefiorprfatotirfeimdcaarntaiconeng.se, pIonrfestpheaerrumemedtsahtaomkdpnlwoeewsr,necPeoFvnOacleSunalatrneaddtitCoo1ns2deoetfxettrihmbeiintteeesdt maRneaaatlgiyetxensetf,faaencntdds mfdaoetrnratilxil iabenldaalnbykytsehswiegirhnep(lr>au1ns5m0wai%tshraeemcapoclvehesrs.ye)troeorcolevovewarli(ue<sat7re5at%nhgereedlceofvvarelormyo.f7b5aF%cokrtgoarll1ouo0tn%hd.er interferences. 000110 Page 18 of 225 - 3M ENVIRONMENTAL LABORATORY 02-1039 - Blan`kmse.thMoedtbhloadnkbslasnhkoswaenddnmoaterviixdbelnacneksofwbearcekgervaoluunadtecdonitnatmhienactoiuornseionfttrhoiduscsetdudiyn.theThseample. preparation stage. expected and such Tinhsetamnactersixwbelraenknsotdeidd sinhtohwe ernadwodgaetan.ous levels of the analytes. This was 000111 Page190f225 _ I ENVIRONMENTAL LABO0R2A.T1O0R3Y9 - DATA SUMMARY - o`pQfeurnafnoliuimotraatoihpveeopotslacenrdoeaehtnueimn(gaCs7n)w.peipraeesntmcaoadnfedocuracftthleeudodroeontoecfrtomauirnnoalatottiseono(fCof8n)oe,rnhmdeoapgtpeaondooelucesadfliheuuvoemrlasonnoofsneanrouamtean(dCS)f,our ots = pn1eo0rn3fa8ldupeorcroatoofacclotulao.nreoTdsheueclfasoncnoraaetteeen(i(PnCgF10Od)Sa,)tpaearsifdlseuusomcrmroaidbreeicdzabenyadattinehet(aCSb1iM1e)sE.n5v2p.ierroafnnlmdoern5.ot5ad.lodLMeacabaoirnactasoptriyk(eGS1tr2eu)cd,oyav#nerd0y2- information is contained in Appendix 8. Table 5.2. Endogenous levels of test substance in normalpooled human serum _ TCgR4m8a) TAmCpRi8r8e BoresouRE TCR687 olden We TCR690 _ Test Substance _(ngimb) [PFOS 3 ___ogiml) ____(ngimi) BE 70 (gm) _| 270 _ C. IC 0018) [2 EL) f<o0t0' [32 0205 os) 0320 Cu 058) fos fo3en 0203 lcs lcs 0265 [2] 160 0650 0605 295 0900 560 x lc: 0013 oz fcooto 0.1% 1 Denotes values determined from concentrated spe method. Value < LOG. - Table 5. Endoleveglsoeftenstsoubstuancsein normalpooled human Plasma ] TCRTGe7s4s TaCmRoEr8eS ResAeGaVrAcThITVCER683 STEW TCR.684 i |__ Analyte l[Pcros (ng/mL) (ng/mL) <<07100' 0T0a%) (ng/mL) fo1o5262) (ngimt) _| 163 c., Cio <010' 0049) 0135 [2] wor <010' 127) 0.170 0.160 c, ce <ozs' 0435 <0s2' 261 0585 307 0535 387 lc <0' 0.100 016) 02% Denotes values determined from concentrated spe method. 'Value < LOG. AwpoceocrlueerdoabthteauimMnaeandssfsoerDreeutnmedropmguirencnahtoaiusosendC,7fA-rcCoc1mu1rGaoatlneddmeanPsFWsOeSsmteianBsiauorlcooegnmiceceannlttssr(aaTtCneRdd-6eS9lP0eE)m.eenxtAtarclacccutormaopftoensomirtamisaolsns measurements are presented in Table 6 000112 Page 200225 _ 3M EnviRoNMENTAL LasoRATORY 02.1039 - Tabl5e. Accurate Mass DetermoifnEnadotgienoouns Test Substances - || Test Substance [| Accurate Mass || TheoMraestsical | DMevaisatsion ppm) ||| FProorbmaabtlse | oS - 362.9739 412.9637 362.9691 412.9659 C10:3F [5G 4 os| _ 462.9613 463.9627 PFOS | 498.9280 498.9297 C:0sF) Cs05F 1S cil 551622..99651452 556122..99556935 cDhaauragchtteerirstliocnrsetoefntEinodnotgiemensofuosr eTnedsotgSeunbosutsanCc7e-sC,'1SpaecnidfiPcFdOauSghintearcioonncsenwterraeteodbsSePrEveednaatct = fpofornenssoevrnemtraielfdiepidonoiTlnaeabdnlahelyu7tmicaanl pstlaansdmaardpsurocfhnaesaedr firsoommerGso.ldeAnsWuemsmtarBiyoolfogGiacaulgshi(eTCrRi-o6n8s4)o.bseDravuegshtiner Table 7. Daulongsoh fEnt doge enor usTest Substances Tost Substance c; Parent on (mis) 3% Daughter tons ais, 11s (mz) _ - cs c, 413 463 431699,,221690,,126199,, 116199, 119 = 513 469, 319, 269, 219, 169 - Css 563 519,319, 219, 169, 119 [Cprzos 6413 516390,.04199.,60319, 269, 219, 169, 119 : `eIcnsoodmmomegererscn,ioauTlshlefolspororefoscpehoneocmleiecdoarhlasubmwsaeenrnecseqeuroafulmdaiasitnvrdeilbpuytlidaoesntsmeaorfm(bFiinrgeaudnrceihsnec1do~nacn1ed0n).tlrianQetuaeardliiStsaoPtmEieevrexsaaoncafltyssoisfof : IaNsnMovoRmmearctePorgtFfrOiaepAdhisscttaaanlndldayardrr.edssooIltfvweadisnberdaeatnrecirhsmeoidmneaerdndPtFhliaOneAtahresitbsaronadmnaecrrdhseoadfndPPFFaOOmAAiixsweoadmsbearracsncceolhmoepdiaawnniedtdinnceainmng atihspeopmrpeorrx.eismeTanhtcieseo0ff.i2nbdrmiaingnnucothfeeCdretarenendtteinlotinineotanirmiiemswoeimneredrssoowlfuoatrinCod7n,awrtaehsebaehsxietglrhiaepnroelhraoetmseoodlltvooegddueeftsoeormfmitChn8eg-ICan1uea2ai.rtaaBtnuFduOlAy PROS. P2dLenFotdewOcnAtteeodaan.nrodniP-msdFioexOmteeSedrcatbdnirlsdaetvnrPeiclbFhusetOiodAofnabsw.nredarnFenciehgpauerrerdesiei1snsotocmmoieennrlrtsahPiwenFessOrcceArheroseobtnmsaeeandrtdvaooergtedsr.afomofrssotohfreaNCaM7nRdancpdoarCts9ta-eCds1nc2ebacrroamcpnooemusenrds ccceahnlrtirooamrlaatCtohonigncrauarmsvspoeifpkoetidhntewi(cteohxrt1rr0eascnptgoendodfciatnelgsltsrtsaautnbodsnatarcnducsroev/efmpLCo.7ino--tf CpCol1nz2ssimasatn)sd,FoPafinRpgdOouctSriheeri3sdees-hSoulovnmcegnometnnitpariinanstseexedtsrSapPcetEresd 000113 Page 21 of 225 - 3M ENVIRONMENTAL LABORATORY 02-1039 - wexatsraucstsedofacsotmhmeerbclainakl mpaoloilexdtohucomnasntruscetruamn. exPtoroalcetdedhcuamliabnraptiloanscmuarvceolbleecctaeudsien cpernetlriamlinCahriyna screening results indicated it did not contain quantifiable levels of endogenous test substances. 000114 Page 22 0f 225 _ 3M ENVIRONMENTAL LABEO0R2A.T10O3R9Y - Figur 1: NMRCartfiod 9.5% Linear omer PFOA and Mixed Branched and Linear Isomar PFOA Standards . 021106002 Sm (Mn, 1x1) 1 MRMof 4 ChanneElSs- 51824439] <= fnear (@.5%byNMR) nTeic Area . Uneisoamerr C8 standard % ached 05% oy my 419 - 0 021106001 Sm(Mn, 1x1) MRMof 4 ChanneElSs- : 100 152374137) <=linear 77.7% by NMR) 1.3T5i0c6 Area : Branched & near isomer PFOAstandard "5% 58018787 ranches 22.3% by vy => 1,88 0 250 500 7.50 1000 1250 | 1500 Time biSsruoammnemcrhaerPdyFaOonAfdPc9oE9nO.t5aAi%nSsntae2na2dr.a3ri%dssob:mreraNsn.MchReNdcMearRtnidfcie7erdt7i.sfi7tea%dndlsiatnraednadroafsrdtohmoefelsmiin.exaerdisbormaenrchPeFdOaAndconnetaairns 0.5% 000115 Page 23 0225 - - Figur2e Cr somar istration IM EvvrRoNMENTAL LAB`OE0R2A.T1O0R35Y _ p40o21025089 Sm (in, 1x1) 73 _ <= tinear 1 MRMof 4 Channelsri5a soventstndua30pps 26278 20a8o6n5 - "ew 116; . Branched=> - po021025091 Sm (Mn, 1x1) Chines plasma 109 276239_ tinea 1: MRMof 4Channe2l6s6TE6iSc5 Ares % . (ranched notobsarved 021025098 Sm (Mn, 1x1) 101 . Lamps rum 73 | coven 206d * 1] 1: MRMof 4Channels ES TIC Ltn 4021025100 Sm (Mn, 1x1) : 101 Sigma serum 1: MRMof 4Channels ES t 8.3T2I4C Area . * r (branched notobseA rve) 77A 225 <=uALinearnLa ) 021025102 Sm (Mn, 1x1) 1: MRM of 4Channels ES 100 Gotten West sem +h 49oT3iI4dC % 72, nen | Arrraancehdojoott shsend$'4hdl M ` e 250 5.00 750 10.00 12.50 15.00 `acSiudmwmearreyoobfsCe+rvAecdidin Cthhersoemalottosgofracmomsm:erLcoiwaltopnooonl-eddstheucmtalneveslesroufmtne branched isomersofCy 000116 Page 24 of 225 Figur3o:Cylsomer Distribution 3M ENVIRONMENTAL LABEOR02A.T1O0R3Y9 - 0121024012 Sm (Mn, 1x1) 645 4aa1 2 MRMof 4ChamelETSsi-c 3235 - Solentstandard 30 ppb <= Linear Area % 822 . n Branchea=> 984 6021024034 Sm (Mn, 1x1) 2 MRMof 4ChamelESs- - 100: Chineseplasma Opps 82 9023| cc linear 6.8T0i6C5 Area - Bancheds> 852314 ; 602o1024041 00 Sm (Mn, 1x1) 84s 2 MRMof 4ChameElTSsi-c Lampi"re serum 53805 | ex linear - % Sanche=s> S81188 63A0reea5 : 60o2102S4m0(4Mn3, 1x1) 2 MRMof 4 ChameElSs- 100: Sigma serum 75934600] <= near 81T3i5c % Bunches => 881144 Area 602o1024045 Sm (Mn, 1x1) 2 MRMof 4 CamelESs- 1"0%0 Goldenwestserum 148541020 x Linear 1.A2rT8ei6ac6 Branched => 780 o `Summary of C, 2Ch5r0omatogra5m0s0: Low to 7J50 non-detect lev1e0l0s0of branc1h2e5d0is|omers1o5f 0C0j Time were Observed in these lotsof commercial pooled human serum. 000117 Page 25 0225 - ENVIRONMENTAL LABO0R2A.T10O3R9Y Figure &: G somerDistribution 0210250S6m9 (Mn, 1x1) 2: MRMof 4 Channel5s - 10* Sowentstandard 30 ppb as3st <= near 40A1rT6eia5c - ranches not bzenved) 60201025091 Sm (Mn, 1x1) 2 MRM of4 ChannelESs |. 101* Chinese plasma 10pp0 "50ds <= Linear 48A1rT6eiac5 Gunched not oerved) - 002o1025098 Sm (Mn, 1x1) 2 MRM of4 ChanneElSs : 10 Lampie serum a0 i 8.1T2I0C4 wa fy, Area * eso| < Lingar Branched=> EA BAY \ 0210251S0m0 (Mn, 1x1) 10 2MRMof 4 ChannelsTEISC. ny Siomasenm oo <1near 15A6r0ea5 0 Branche=d> 01201025102 8m (Mn, 1x1) 2 MRMof 4 ChanneTlEISsC Gotten nests um aa 28A6r6ea5 * Branched >1888%3| cetinear `Summary of C, 2Ch5r0omatogr5am0s0: Low to 7io5n0-detect l1ev0e0ls0of bran1ch2e5d0isomers1o5f0C0 Time were observed n these los of commercial pooied human serum. 000118 Page 26 of 225 . Figure 5: Cio lsomr Distribution 3M ENVIRONMENTAL LagORATORY 02103 - 6021024012 Sm (Mn, 1x1) 3 MRMof 4 ChanneElSs. 100: 2% TIC - Soentstandxd 0 pop 26022] <= Linear 28A7ree5a Bunche => 93717 : o 021024034 Sm (Mn, 1x1) 3 MRMof 4 ChamneElSs- ) 100; Chinese plasma 1055 4289,147 ex Linear 4.9T7I0C5 Area ,* Bunche=d> 9S8633 0201024041 Sm (Mn, 1x1) : po 988 3 MRMof 4 ChanneElSs. TIC a-- 75 ce linear an 2.004 Area : * Banched=> S00 402o1024043 Sim (Mn, 11) 10 "5% Signaserum 22572] Branchad=> ahsge , 3 MRMof 4 ChamelESs. <x Linear 268T0I4C Area 021o024045 Sm (Mn, 1x1) 3 MRM of 4 ChanneElSs- 100 Soldenwest serum 2S2234 <= Linear 1.010625 Area * 0 suncned=> Sor| 180s816_s1i23g0 Time `Summary of 250 500 Co Chromatograms: Low 75 to non-detect 1000 levels of 1250 branched 1500 isomers of C.o were observed in these lotsofcommercial pooled human serum. 000119 Page 27 0225 . Figuro 6: Cut Isomer Distribution IM ENVIRONMENTAL LAB0O2R-A1T0O3R9Y - 0120100;25069 Sm (Mn, x1) fo 3 MRM of 4Chamels T5i.c Sowart snes 0 ps0 sat <e tiese 5725 Area : hi 1007 Brancnag ws 1021 : 021025081 Sm (i, 1x1) 100; woaszt 3 MRM of 4 Cranes ETSi.c 45405 China susma Oop esr Area - * Bunches > 1700035 : 0T2o1o625088 Sm (i, 1x1) 1031 3 MRM of Cramels i5.c Lampesem Brancnesn 2 tie"n Traea 0T2o1025100 Sm (in, 1x1) * Samazenm 102 3 MRMof 4 ChamelT5si.c El pe aroseyd Suneess 130%07 0120100,25102 Sm (i, 1x7) 102 3 MRMof 4 ChannelT5si.c Sottenwestsenm o3o] a7A1end * Brncnes > ray `Summary o2f0C0. Chr4o0m0atogr6a0m0s|: Lo8w00to |non1-0d0e0ect 1le7v0e0ls of 1b4r0a0nched Time isomersofCi, were observed n these lots of commercial pooled human serum. 000120 Page 28 0f225 3M ENVIRONMENTAL LagO0R2A-1T0O3R9Y Figur7o: C. lsomerDistribution 6T0o21025126 Sm (Mn, 1x1) 1075 2 MRM of 4 ChamelTEiSsC i "% Sovert standard 30 ppb. exe) <= near 8.A0r0eea5 ) (ranched notobserved) 40210251S4m8 (Mn, 1x1) , 10 2 MRMof 4ChamelEsS WoOmT near 6.6T9iec5 * Chineseplasma 10051 Area (ranchednot abserved) : p0o21025155 Sm (Mn, 1x1) 07s. 2 MRM of 4 ChamelSTEISC Lampire serum (branched net observes)371 near 6.A9r6e8a3 S0N21025157 Sm (Mn, 1x1) Sigmaserum 6o0o201025159 Sm (Mn, 1x1) oo] comuetsem 250 500 1072 Ja Branched => 1097704] 0m Branche=d> 1%, 750 1000 2: MRM of 4 ChamnelsTEiSC pr 101ed Area 2: MRM of 4 ChamelsTEiSc ea new 23584 Area 1250 | 1500 Time O`bSsuemrmvaerdyinofeCs.,eClhotrsoomfactoomgmrearmcsia:lLpoowolteodnhonu-mdaetnecsterluevmelsofbranched isomers of Cz were 000121 Page 29 of225 _ Figure : FOS lsomar Distribution IM ENviRoNMENTAL LAB0O2R.A1T0O3R9Y wmsiassnun, a) - To P---- EB ien oo vr rns. iis ores 8 cob Sm " THR, ks a) . * Crvese pas sss nan on sees } con FE Sm i THT, ) 7) . Lompre sem =bTy ene 12w50w8 ng5% X weooh eS Samson .6osno] TET,5 os i wy . aon,5%s wo FEET " Godenwestsenm so Pe an TR=% * ress a 200 a0 8% 800 1000 1250 1400. ha GSoummmmearrcyalofpoPoFleOdShCuhmraonmasteorugmr:ams: Branched isomers of PFOS wero observed in these ots of 000122 Page 30of 225 - - - IM EnviRONMENTAL LaBO0R2A-T1O0R3Y9 STATISTICAL METHODS AND CALCULATIONS = `Theoretical concentrationsof analyte in final eluate Concentration = (Concentration of Analytical Standard xAmount of standard added) / EV Observed result to original sample result: _ Original sample result = Observed resulxt DF Spike percent recoveries: ] oh Recovery = Observed Result -- Same Sample, Unspiked |0 Theoretical Concentration EV = Eluate volume: OF = Dilution factor Relative standard deviation: Relative Standard Deviation = SptanndadrdDDeveivatoionn x 100 ) Percent deviation: % Deviation -- Theoretical Cone. - Calculated Cone. Means and standard deviations wereTchaelocrueltatiecdalusCiongneExcel software. 000123 Page 310225 . 3M ENVIRONMENTAL LABORATORY 02.1039 .- STATEMENT OF CONCLUSION - fReosmul<ts0f.ro0m1-t0hs 0s.9 tnugd/ymsLho(Twaebdleqsua1natiafniadbl1eb)l.evLeloswoftothneonl--idneealreicstolmeevrelssooffCb7r,aCn9ch-eCd12isroamnegrisng wningeirthmee.osbacsnrederevwneaedsdfploorrtestsheoenftGco7amsmaenbrrdcaCin9aclh-eCsd1er2aancdaonlmdipnepoaluranisdsmosamedirenst.ceocntPceeFdnOt(rFAaitgwiuaorsnessprr1ae~ns1ge0in)n.tginfPotFhmOeSs2c.wr5ae.sen5pe7rdesleontst oafscbormamnecrhceidalansderlainaenardipsloamesrmsa. in concentrations ranging from 0.85 - 5.6 ngimi. and was present ACc1c1u,raatned mPaFsOsSmtehaastuarreemceonnstisstaenndt ewlitehmetnhteaorletciocmaplomsiatsisonasnwdeerleemoebnttaailnecdomfporoseintdioognenous C7- . Tmahteripxraerseenccoensoifstceonntfiwrimtahttohreyldianuegarhtiesromfeonrsaantalcyhtaircaacltesrtiasntdiacrrdest.ention times of target analytes in 000124 Page 320225 . 3M ENVIRONMENTAL LABO0R2A.T1O0R3Y9 REFERENCES - None - LIST OF ATTACHMENTS Attachment A: Extraction and Analytical Methods > Attachment B: Data Summary Tables. Attachment C: Sample Chromatograms Attachment D: Sample Prep Sheets, Test Substance Information and Notesto Fie Attachment E: Protocol, Protocol Amendments and Deviations REPORT REVISIONS - 5`Sbembie-cqauaunsteittahteivdeaetsatwimaasteisntfeonrdTedHPaFsOquSanainfdatTiHvePaFnDdSownelyrescrreemenoivnegdefsrtoimmattaebslecsou1la,d 1bbe, 5a, and otabbaliene2d(.paRgeef1e1r)e,nccheesmtiocaTlHsPtFruOctSuraensd(TpaHgPeF1D3S) wreefreerernecmeosvuebdsftraonmcetshetaibslteo3 t(epsatgseub14s)t,anmcaesss `spTeHcPtFrOoSmeatnerdaTcHquPisFiDtiSonweprareaamlesloerrsem(opvaegde f1r8)o,matnhde acocncturroaltoefmbaiasss(dpeatgeerm1i9n).atiRoenfdeirsecnucsessiotno ((ppaaggee 2201)) aanndd daacucgurhatteer moansdsadteattearbmliena7t(iopnagdeat2a1)t,abilseom6e(rpdaigsecu2s1s)i,odna(upgahgteer21o)n, adnisdcuisssoimoenr f9)i.guIrnetsro8duacntdio9n ((ppaaggees113)0,aanndd3S1t).ateWmoerndtinofgCionntchleusEixoecnu(lpiavgeeS3u4m)mwaarsym(opdaigfeie8d),toSruemflmeactrtyhe(.page errermoorvsawleorfetahlessoecmoir-rqeucatnetdi,tianicvleudeisntgimWaitleslaforK.THRePaFgOenS'sanpdhoTnHePFnDuSm.berSe(vpeargael 7t)y,pofgorrampuhliacsalfor tmhaesasnidoenviiactfioonr,mstaobfleT6HP(pFaOgSe2a1n)d. THPFDS in table 2 (page 11), and the unis designator for sAtpurdoyt.ocol amendment was written 0 address the removal of THPFOS and THPFDS from the 000125 Page 33 0 225 ) 3M ENVIROVMENTAL LagORATORY 02-1039 ere SIGNATURE PAGE ------------------------------ We certiy thet this report is a true and complete representation of the data for this study: ) MEKE. Eletson s Date 12/05/02 Study Director 2 --= , Wiliam K. Reagen Testing Facilty Management 2 25/6 Date 000126 Page 340225 i ATTACHMENT A: METHOD A---- Ernie 000127 Page 35 of 225 i IM EvronuEnTALLis0o2m.a1T0o3R9y } Record of Deviation T Tentiication Study Project No. i DeviaonType: 02-O1S0O3P9 (RMethod EquipmentProcedure (Checks) OPraicol 0Other: DocumentNumber: ETS-4231.1 Diet)ofocuinenc: 10 06 02 1025OxiG7 Ti. Description? Required Procedure/process: `methodfordetails. ETS-8-231.1 section 9.6, "Quality _ Control ert (QC) Sample" see eens msememoneereee . {Auhnud,ounuoghPtbrhyeorpreeedpuarr-einligprandoodcfijetsoTcncahultvesecapoomopnilninenst.oa eTdhaecnQiorCmae socarymeopftlhheaesncd10esaasmcprlleiisbcasuenhbrddevemwaetathhseomcidnowoniioroefehedn pitnrdeShppapr.eetdotoTmdnrioasndtideitinotgiruofein,sxhtobornecltytwor2enQeenCf,fshiaecmiceponlncety.isTnwuheeredeQpCeresapraaicyemoffopwtheelrcechleolmnblsraayttiesop.nick1euwdraavtesa3pnoesdviebhlel,e,0.5 exirctioneficiencyinexchmars tsi. SR aDluriibncgaitohneccouruvseewoefrehewsitthuidny2235o%fotfhcexQpCectseadmpvlaleusesp.reAplalrefeheSpspabspimkeastpeaxsassedt,hbeut n~l~y SofSlowspikespassed. rebels (schas amienAdcmtseaunnesdt,TaSkOePnr:evision, etc) Noadditionalscionwill beneeded. _ BE ---- RecordedBy: Oud (al god IV. ImonpStuady7c Preftect Date: J wire | 3g 4 s"uThdis.deviation does not adversely affectthe quality ofthe dat in he coof tnhecure rent 3i 3 AuthorizeBdyr: (Suedy Dlito) Prajecs Loft) Date: uf fox 1 Enon Labora onysy Oreooe istonnto.T|T ___R_ 000128 Page 36 of225 IM ENvRONMENTAL LABoOrRAtToORnY 3M Environmental Laboratory I Soll PhaCsoemEpxotruancdtisonoamndbAlnaosgiiscoWfaFtldocreoschamical Method Numba: ETS.8.231.1 po -- Revision Date: 3/52 Ente Dae:2/1/02 Amon TLsoireen Maerserr va5te oa 344 is '3 StepEoissew reanrttPoamf ni Pastors 000129 Page 37 of 225 : WM EnvmonmenTaL LasCoorraTtoorny - A1_ SeSr ocoptpeeaaannscdo Apspppnllieecaa0tt,cieoonntadpesfoSS e r,t00ro0r 0et0p0To0v00 frellnnt 2_Mathod Summary ) AS aamountoofr briolhogiecalmSatenreiaatlp,oesdeteenmeimoeedbOyatBehyemtanastlSy,aTdisapareoipargedp(eofdpeestihuteodansdisamsuesmph2oh ymo8ogecnirozt emd8)ebat 3 rmCea ryFoeeryaeenseae tyesIe ESNENS,m SAI 3 pefintions 24 DASiiuttia oncprt 50 Unf: ofmi ioGer 6 lscorbin, 22 e ScPhEecnarciodgie nveacoiso t hddtipescstane .nt Tm ----_re ee Ch ntam2m ie om 23 Retargeint gdradte wac ter efet) 5.4SQpauaritgyrecoini traesm ample ete reyo berytpe ely iyi. Warnings and Cautions 4:4 HAeralethgando Safetg y Warnoiwnegss edhighg hens ng ie Fi $3 42 Ucoiocmnsibeeicrep.Vincre peer lpia0. 5dg Te itcomt ow 78cen 1 e dps hrmt ew.AES - Sot har s Exonenrdsr Peis ---- 000130 Page 38 of 225 ] IM ENVIRONMENTAL LAB0O2R-A1T0O3R9Y ) f Doto pesrteeprss hvee ve orcsi of 40i(59a0) t ckpcs ebetckprs ccs Doernerdees. ` 5 interferences cTomoinnannefierxTef.lon hdseidfesesss sypfneato oes 6_ Instrumentation, Supplies, and Materials ) TIhenSlonwin,gs gp,du ra rm bededi ricdsxofosn edWkpg ring 8, 3 edd. Exit 6.1 Instrumentation : Vor mise,VW,VoresGe VisTurseT25sehomegizce VasmPuy : $70 xmcion Musil Conf Mal 00aEC ---- Bice 4101000) J -- HEL100 Agofo pls ses arinsys, lve sets crane ssl 6.2 Supplies and Materials Eppendoron potslicchs Diseing wits P[ obrreb-- ore,cy pio id 91m | Ole) Jr------ CPicomnpbiesviieal,tWypersotgponn, 1m5kn.ie.anoe0pmp.pciei) tan 3{ [-- 3: Sige, cicmesSu i10c0A $ BoeTpDienerCapidepen Srfch.er) 5 7S5PtE sspciconsciodr,eoSerPee6 sb)rio Ca(Va) J1 Copepis aris nds Sod PChoenpEoxnadcstrEnsmnsdSeAinroinftarecsces Pg3ors 0001-1 Page 39 0f225 : IM ERVIRONMENTAL LAB`OR02A-T1O0R3Y9 [ee HPLCasim,seitobeerin bes ddr nerow i. 7_ ReagentsandStandards Reogews,MQ,Neon1,or silos AcPLi Cgeer, i Me HPLCgaarle Amor se,eg orile [ET -------- 7.1 Reagents preparation 2fl0ruoimia ie m em scaer eii sniena:e Wceitghwss,poitny0330 sGoeenl,seneg,Pvoosle e3le200gmeL. d Not: Wohepaianrieen,haeodeeh.ed astrion brsdpep, 7.2 rTaeorprgsiogtriaenaatllyytee sstanannddeayr)dfipry rdeepsaradtiocnrv.Mis p lroFnng.a spl. The Wneinghdpgroinesorte 100mgop frcia. 100m.vlan fk odsd hscdwih Srv Dies clstoonckisathionweihfmecskso3 fkipr,esainndly |0s0i0pomnGofnsdp.ray50penExar clini: 1000 dx mL Sop DciscwrsinS gsad10p | Lvi eoameo StoORi 8wokingsaid 2 hinofpor.50pp. Exrle Dituawto:Srokhasm x L J ih c0 hao013G pprLc wks 3 hon of pe. 050pp.Exar 7.3 Surrogate standard preparation Psrandpropgiosnst. o,The lin 30cleoly nd yaykepepe llse Weghrprocintty50.10gf regedd5316.vole kdreid ci igh. TieSnignvgo(heaenkenwilhimtegaonofetoresiome.sanTodoedsccgkoorfsapptrsitcaltly3r00 oT1op1g0e07mR7t.atevooastvrey: dd nr enor oatsSkot SS in 7.4 rInteerneal tstandard prTaoparaton i yt et fd sn pn Weigh primacy 1101 fers id 100.volarfkdc cadWES 83 |NTgF 5273 7 g SodPChatmEptoroenesnesdSralioefMFrossse Paesatiy 000132 Page 40 0225 . aM ERmmonenta LioscrratToon : iPgi ee on mmp staasrdeee coorgrdat.dTnttoastsekmtpiiaes|fs5o0.Hf0prgPdedoeIotm n A tn 5_Samplo Handing o he sw Seofere sd c bs n eieee. JTimtibumiasenttes rou chsr.Exc atsd. eeaesda Itii eecotsts asyseeco inn tony 5_Quaity Controt 9.1 Blanks 511 SP olventBlank RP 912 MnetthoaoBiank te, of pttToatm,aooTcatt waik.oForedwo Fy 913AMa natiBlm la1nkmn 10g wa seem dtsereaiodn sede.aPiso .Oebo eneost lye a es etmeyaatSea ore TotLIt SSonSTTe mBeey 9131mSturtdratmnc ityco a uid--:Be, 4 ics 913f2ro aConecurs he (emepaen i)e ceone.eoemithyo dems adeet _%3s 9133sfnSeo uipenrty bsestoeioaeemerei TfbeSrarresfo)alyitl rf 339? 9.1.3.8si ermom nbeaeroi bodne d ks eybeadede nd ilesdin i 8 92SSaemeplmeaRenplicapteepet tap Sd oa eEnerm sa fric Fassett 000133 Page 410225 3 `3MENVIRONMENTALLAB0O2RA1T0O3R9Y - 9.3 Surrmooggeatrkstanc dard rofsert ge dd corns SYorn be oe lin rv iOSinof tk gs1sdescribed. ) `Tpoarsryerreope9osbLtoraLllpyhadnw31e05mp.GoAirmheesrenealoeeenvoxftcmgs, Hoverer 9.4{InFtrerrnoalndstramnidaro dprotf eliyn,snldes ples im sresionssii x yJosiln resdpdb20mLof i15 mig bo, trig 9.5 Lab Control Sample . cto rp etscompton 9.P6QC ugalietqnyuciCt otenctcarrootolv(S(eQQ0C))yhSraimsmpoleee chre peipon fsimoo nd vyokhecotod ryBeaf i akces(12T) kqlmcocm mdGeoe(GtCAvro ia ro oes hrcdhgoef te ioic,fC5se osyy, As imnin QC epk e it contfa frmeosetcho eeass iiyn.Th ls ed kw my ednd LMoivoo cq05X030ie ofecb, Hr ToiGbCsrrhTeechLR1e a00L yCserr vr ieS r le sonesko tri ss e ebcs htrionsad QS C piL sxt it utrRreAImo beNmiEiSsre iyi nm.AyOCsrl S mp omm tpi crca i ys os ini,enQC rhsfossrs le S00 ccsraoomnw se ofoO7y r5129s4ofacti.e Aor HQtC,slf smst 9.7 SeaympplleeDiilhutnion ainf eh cs smdrs bedi i rgof ai tomcane. argsedane iebyri of covedogse od nhSr rans TTEo er idiemnp itcpeosn mpi iei sed i opartoS slsv is wo (i0s EE 5 72 Sod PCs cami rosnmadpnopipiefFarce Paseors 000134 Page 420f225 : 3M ERVIRONMENTALLABO0R2A-T1O0R3Y9 i S5o2r0nldcowiawirSsonnsopreefri ia)rhenrcodhnin(810g4oipnergocso.wrThhee 8niocptdroco)esoconcstoffdiSnbne dIebinreelwihvceheareni3fofre nokwriioin f15b%foreheeEtohsr:l aio ein willbereq 10_Callbration and Standardization 10.1 InstrumentCalibration Cnxemwiclcicootnucno,sfevmdiiimetpofyrbodw0faoemvniold.cAoedeimsi dlnsitosncianvess. yebiEasisrEl,sprAly. cTCrornlefr10sbneeki1easbdoeoppokpp:Gaorevpi,teo.fTtdhesdtVi beolvp0aecdoa4ieobpogGreeec+ohhroeawtsohp1e03Ss1ra5mni8s oe [A -------------- Foe Dm iit,recpropaso,ofcolmai ve ss ks. : Tredsrti asiovdeecrotsnoss nemiononTssshrdsssok,irnoufsrnrassbtas1ekd,iDnrardTkaoslreoy|m0dybertEceS,whSeon neepofi3eo4nselcGonCed UoseAmckmainnksCrcaocdieer. gps`, 15incon hecorenicnsof bevingsds. Reeteuion 210 be orhloss bteAbason en CATge. HToe ivcea , herr rybteskdm eLsdsaedyaiosiieFdiL eheo0mG.d idihowaoca desiheeodsrp cohsvameiinniee.dxci. ASyee one xeidgtiesatndrcofvspriteaxhe)tfi cas. Thscrhvtcioonwile rind AIeneeewvitiemeyk5ofd1te2l. dA5L eireseokb0ehdoweacgoi,esoolof,be rkteAeLLOmQwhoich ii SodPhaCs EosncopEosnmnesdBAerienteinnsofttisersohit psc 0t19 000135 Page 43 0 225 : 3M ENVIRONMENTAL LABO0R2A.T10O3R9Y 1JI.a .. . cSoRntcenlmpioionnartfsatm5i.e| _||ciannPAciepnmp2io0onimotn.fstatseyme E Eo --1S TS---- Z-- | [osmuwml 130" loomgormginl| 670egmt | : [[oossmtuogwnmli T 16 snaosmogrernnggnnlT t| | Ssooomogenr | [soo ouinl [80 | o 0mgsorngnl|-- 200mm] [sF-- O eT wnS --TS-- s2 oomio-- gel |1 -- soomer || Io5T o60mmo l T1s6o0||Tiompme7rio7gsel0| |orTmaiwgmeetar l|| To |e0mo| reWgega mt l 41 Procedures 14 Tissue Sample Preparation Onn re CCFut srparrbo0tv0pegiorfneya,(4010l0o,we Beerseproog sme,sing sigspl.THpat Weigh edly ko redpaipel Resort heweit: whoshc atc woke, oi. Rensibothez hrxinsmc vebec ne A125 mlof gnvar speilo ce uns decried i syoddosedna te Htoemamaphegsompelre.eot.he UeTors gdptein 0 rieodido peonymis, [oRTriis chcespropniierbmeciiningeteaemeeelcehhiiahe2v.se5s..of age de oeoe dined 535 roeemies 2ig4a cS3omassmiounnttioenmeeraiynns0iG00tghssdoto(w1i5eh1s0+51g0ea0ve orrocvoreacioornstnaisweigh,smars mtLorwanenvonre " 3Bg 8 Js Eg= Soka PaCsavxpmionsieornmdsBeA inpengernofiFniaescs il Pisolis 000136 Page 44 0225 : . 3MEnvRoNMENTAL LABO0R2A-T10O%R9Y 112 Fiuid SamplePreparation Obi snd lendshothw opto in em wt Le1h8e iPkphle eAcshceAieseviimetst nes,rsere D,rcisngo ds ndrh iis : Voor aisserlidvmatlaofbotpseppin o1sond le 0milo, erpropiaamet Renespcofr se ciososhvenenc A8c5m0mek.ofsassewnoe 10m. fo 1 ion, oeiin rind ist 1i03choumsnatersotvn.10min ov fr i ol,ctheve oka corny inh 1.3 Tissueand FuldSampleExtraction . Adfcnmo1m5iomgoernpcieeddmspeeespcofvoembpenoet.mg1u5mnnfscnion 1.10nd 1.2,ocreciooprsraevbey ,rd103 Remnsededbogesdponsoe ese schonsss ve bencmv. Resort oe omeremove cn xinorbs(ASCsAdesi vodka. SSppiikkeecohkc,lilen,dsardsm,iwheuprrenpaw:ishecgofsaderd ddescdribedn5scohdd.fobe Eicv rentxhGC le Vor iesrcovearp QC srspinysods. T= och ml nd nd 8 01m.ofserine,cp edvor io keby bdspeiraly 15 3P0o0emlongiamanestechnonp)npe for20 nos skali i: ofprin Riernogvosffsomphoesnhyoe1s0cpamiostonsapcpd assceieedn)1.0minis sicquscy el beprecios C8o3rr400smkp.orfmooby abeedvnowtvt0rc4rne.0,Tii.Scksifsgrrvheo.Rfeeoronnsnyiyoefhreoasheeo9si0snl0ds yAehhisiitoehneSgPbceord nd cwhris)i.ncre it 3 cm nd. NoOTwE1:3W.hmsni.gToeusvraey onySvrenrcescssupyAF my 5 KdAobioewnbegnsd coascnk or bn dndo. 53 sCaLs he ePoCcfatredbiyngshciarvitc iohwpteeoiu f5T0aBoofmceta,f BElXow gpcximacvyo 53. Aatroivehsteingchcoonicd,reunr. he le nereseedwi nd tw i of Wd pn E5 ENF Runevn igh proneSmesbosistydyccSPE igs. PSpaceicoitoton n1k3m spc, nd ndp a iailcor che rdorci enddcaiwig t2o0odofacl. SoldPhase Exes essndsAnayi of ischemic ConrpameBiagnsMcarsee reat Page45of 225 - IMENVIRONMENTALLAB0O2R-A1T0O3R9Y - Lrobarcnointgensedeootros IV5Sr.rsnrpr.i7ea,detthehess,yubbyerc,ovorlpsfe(stei dreveri,nsmoal Te roe gssan ldr. _ 14 ExtractAnalysis 144 Sofwaresetup - 1 deMasdeysidnse,rtopo leterih.bSvi hneendeosr ir2egssof CupSpeLi MDD 0AO - Il ofbem YY=Tatyey (= Al) rDD~oTexmion,ny - mmeFn)seii ufedo ee letini c - Aeieeranmvirng rimsdeterby, br 2Fsof et moth, nd 3-650 i cr: MMOD ATO! - 1 lof mes rn Weta MM Teton Do-Tenter Afo,ropptiiihemipoyit,sisn cea4) sicnig i.onrlhBe,9e01m) t cic los, - TRE CorEcor( e, ei oRi secipokrnooMbne aMa xnenoi)ESrnSsbfatfontaasiMkSosSybsEse oPlpasnes.dms5icMeiSTrRaeS72gsMossnRvpeione)tor BR Ror eteoni OL : - "Typically he anslyticalbatch unsequenceegins withsyste sabi,solventbanks,and seof exactedmati 5 - SortrcmdsecsbsirtithrvopQsCsSplae fceottseroveyhKtoseribccip,sSerbers hksy 23 $ So hsCuactarfneomrmdpsDaAiannspssdofaFstsrc [re 000138 Page 46of 225 - Erman iTorrs 1oa4LrCss2tpsitemkt ] SeE s rtet em rr } oCotrreasiaaonnams re st 3 Soman . : I I or --C C E I C 143S tesaETmtscepnm E rn mssQt Qeos : JOT mrer-- t-- y--e--I ts.pDeyee : Tra ereenCokpeimekttt Sf"vmaerermriryntriieer--mm--min------ i On dopenoricingattestse. Af ise S38 r Novs icciperle teevsirlpcmotiticouynmamsknistn aroumnd heip of probe.Resist 5 5 efves ntoas ttEro e nos 000139 Pa47gof2e25 : . 3M ENVIRONMENTAL LAB`O0R2A-T1O0R39Y HPLCcrt wtfoe 1-0 rare0 (Bi ptr 1 i ss8 [rr ---- `Smpoa nlykC Dhraobseseytseips ipciasC Bs Juieoseire gea.mbiel, inmd Ms sd 0 tyekwi 7 Ciianirrt piopees cnonsis.Fuh ston i onyvey rgMise } 12 DataAnalysis and Calculations 124odCearlcunlaotinones tan ct ywbedri i. i Cui hemateseantoi ni ll g ios FO weve) Cuteen cec sodsi in Blol ws io i eomenon) =SokeACoa nommeiponLonSp)t A"ros) 00105385. 0+ i obs1 100) i DWua~ tt ovon ia) ) } $A==SAurigedolte eernefrectmoyGy LO) 2 q8 OF Divs bc 2 FV=Fistvobre Js ) MSeAm=eMnatixaomfoumntahi sarcs,smth] 1 US mk c 31 role MA tidrie emfses vs) } [------ i heer O= ntRePr- MeoyBinkRest 0 : SoldhsCEaxoemntsamapArapietnafarseersc fern 000140 Pa48g0f2e25 3 . IM ENVIRONMENTALLas0o2R-A1TO0R3Y9 Cle tive edeon iobelovinyon RevsSandsDevin + SUDO 1 Cteec devin ing olwingcumin: Dison . DCoe ne-Cogttmt iCone 1 Cootssco cacmiyeonognt: ) Arn DFadmepalneaalldionl))"FVELLinCass * 0a 10078 = Go) i : [O------------ AR(rf) DF xd lpol)*EVEinCos * L048 =G60 rps el)FV(nlyiaMorix (000 } 13 Mothod Performance t eis co i eis 3 ) 131SpSymstoineicmilnSustdailbsihbeletdoyekedpgieobfodboE diet0)iceptaorf cdhSsyodasdnaiilbbee - eE7rt4tRSD,Arebo,dn fheo biekceosnpGeed som,tpecciyoa tiTeopcprikhonpr5ieiRSnnD,,at depalkosne0 ic ywi>l20b,e ems rin i)oe <A <1.0 wherAF 8 etyck asmneranfhtopptcoendvelepyesfelamybyc sitpcosm lertbienco0me sorn nF ei Sseen nd tof 132 Quantitation 3 . matebcee fscr i cli io eins mb ii24 cies oeohhexpi of8 LOG 5g . Cabrio sandRnswiRpesksSes snt antw trieosetsheiiere ari lankwillbedesiredto iu 8 2 Av cian vsme conic ive ihn lig LOG. ) Iicrecotmchci spemkbscss ened 133 Accuracy "Tao irsof leycosp3 2ofachqtycolsl chvla xedshwsn lasing - SeaPaCs EitacimofnEspmnsdBaoAlroiirgssonftFirscossh Pas13019 000141 Pa49gof2e25 _ WM EROMENTALLasaonrsrooRmy _ Suireoetndnfaiasns0teiOncBvesncotdrvp d<$4o.sD lbooo uiti ras Eg il 14_ Pollution Prvontion and Wasts Management Sfri-- cvee--pot-- a-- s-- t bto -- w in. - let atidpkgcee. 15 Rocords - Coania comon epio cem sdre v r ty 3 . Ee tpee redmfrt ta py tinomeett,evlsiSe eftownnfcoi:oetypehnmre otdreo , t egn . odfomMayobsct i ty ew i. Coy - Piposkndscgbrineyi,Seponegbades,dPeotsatfsoods dsri lyevs. 0 - SSokmpihc is ephet isssn0.cRLIcNd) sslesioteo yfm sionof cep Sa 3 16 Atachmonts - Attv. SEemainWetsesWee ` ern.CuberSmet tt Wes 3 17_Rofersncas 5 - n 3159925%OOpnensdm M Maoec TeMeGesireatQo Tigh Qopreci 3 - 18 Attacted Documents 3 Sd e aB ea sali uista ed is Ps toro 000142 i Page 5001225 } om Emons Luesomorosny 18 Revisions : eariBE n cguseitepeebsensobi aesn.cittscnmegstned [OaA--RS pm 1 3 iS98 . 5358 Ea rSsaaiFc esa 000143 - Compeunds from Biological Matrices. Page 51 of 225 . 4Eramormeren rogvuies Bfssunsie sina BwoitntpostToats I C= ---- -- 11 Tr 1 rr 1 ) rrr rr rrr , --rr r--r1 r1 - rrrrrr rrr ) C1 TT 1 TT1 rT1 TT1 --TT 1 1 - r CTT1r -- T r T 1 11 1 11 i} i I h C r fT rT y a r T e emenram1rawimvsot mnapsa1 sewarns 1] J } PFd EeRTm a a T lpe g 3 < 3g . EP E e rEr or aert eorma RRryygeuwiasso.ws i$}8&e ) J E C aI C S a e L n PTE SNG ... i TN 000144 _ Page 520225 : . aM Taras EnvironIMENTALLABORATORY A pp Voto ) pruotas -- 1 Er. ) oF EA rar l al = ) , ! A 1 -- -- ---- . - rr Tr ] r tT T ] - --1 . EI E I I S-- 1 r [ r rT - ) rr -- r -- -- 1 33s r -- T -- -- 3 a-- --r J-- I --E-- -- il i TT ce Gr Yr Eo pt iPs ron 000145 - Page 53 of 225 someasos eshrc vo : : p Ei-- a E,c r a B,E Em ons :i oElshE] EEee HH E B E E e r h i a : A re . T EEEEEEE E TE ; a 3 - EPiaglsae B30l0 P e I EEeEiTe P Topm C3b0 = 5cd 8 BE==y BBiHE FBHieE meE te EE Lro 000146 Pa54g0e 225 _ WMEfmmomenTacLisEomoszro1n0y SSsioueite Duara Mach: Dios Summary Wodshes Sf[oerrayammri smpteNumber [pate] orbeetoter |vTvTuTuTwTu[v |commens |veriteany:| - Tr r rr7 rrr - rrrrrrrr rrr [T rrr r - (r r rr r rr rrrr r rr [r rrrrr rr . rrrrrr rrrrr rrrrr rrr rrr rrr rT - rrr - - (rrr CToCre:-- rT TrTTTrT . Mhoision=___atsapier tubers 2 ERNE 3? ) 8i fomComino | Stdh[ErETiSSBLnIsokPseied Page 190719 000147 Page 55 0f225 . ATTACHMENT B: DATA TABLES IM ENVIRONMENTAL LABO0R2A-T1O0R3Y9 000148 Page 56 0f 225 - 28szze: FEEEE 28583228 2858328 E2358: } SEER | SEREER 585853 [e273 essary | jieeseses ) SELEEER &= 8g HR EEEEI THEE | Herenaag jleesieee | iBssazag Hilfesssay } :| Hsssesag 4i" fFi3iEsf 1 $efiiaiss 5 2888828 i SHEL | TT | 000149 Page 57 of 225 - HEssaszy : i Beaszsag - i fgsrsa fevisine i iEdezead essay EERE } i8z3113 : 398513 - ARES : Esrszas - 8EV8V8V3e2R8T 4 pieasaseg av vveee ) 8 [3 3 Has88aas| v oaf Egjifesesess i 335| fpr2e3s3e%sy gfg8 BSi+Hfsirsgsreer:ey i |s jeosseigos EBildlsdlhiesssazasneyy i $f|) fesseeey AF RE52E88H5E8E ase Silesian : E34 10055858 IHL 59 Co i H HEE I Bssosd) ) 000150 Pa58g0f2e25 ] TT : Hisanasg BT - tlie i rasa _ i oF SE o [HE EE IN: jee - bi[1 lls [EiE adte,e g| iforme . PFi H A flEeas2 22 oo gjeea | gf: i3 Ei EiiEfE5s5es2a8nsy Seb : 3 lgeisitisse #.p.r.ze5z i ig jie it (HEE AIHH HEAR 52 : g aa E3 3 F8E]OE) q IgE J gE oofgHhosserd 3iESH Hen |ErlaEsE } 3 EF id - < @ - < i} Pa59g 0f2e25 . Matrix Spike Recovery for Human Serum Data Quantitated with Chinese Plasma Calibration Curve _ TampAivreeraSgeerum [SigmAavSereargue m ECnodncoognternaotiuosn, LowSplke HighSpike| CEonncdoongreantoiuosn, Low Spike High Spike - Iavsiye gmL_ Recovery.' Recovery.%| ngimL __Recovery.% _Recovery.% l[cP.FO ) cn <<LLo0aQ <t0a --<alo0na <tToaa [| 4<% toa 104% on toa o2o% 7950%% 18% 100% ccu <<tlooaa 115286%% 1182%% oztroa 1s20e e1s0 - llcc. <0605 h1r50% a 12m 01610 1s0n0% 1i01s% . "Golden West Serum Bioresource Serum EnAdvoegreangoeus EnAdvoegreangoeus lanaiyte Concenngtirmla.tion, RLecoowvSeprly.ke% RHeicgohvSepriyk.e%|| ConcnegnrmaLton, RLeocwovSpeirkye%, _RHeicogvohy,Spike lcp.ros z"ztoa a2 T7o <7t00a T0w% E<ioza - llocn <0t%oa 112006% 2108%% <0t3o0a aoaen 1%6% ) lcc)r 0s9600 ao01n% TThiesss 208015 oaro s0e%n lc om aan oa <toa 2m 36% 000152 Page 60 of225 Matrix Spike Recovery for Human Serum Data Quantitated with Chinese Plasma Calibration Curve . Chi[neosaerioPsleasma CamepirPalasma Eniogonms Janae Concmomrhaion, ReLcoowsupnktes RaHtimgvhesppiiktei|| Concgonmrtaden, ReLcowoSvpeikres _HRiegthopviekye% - ccrnuok 5oa e Te yeox lhoaa S ox tyorn oa wo om loa a wo 3 cccrn preo]a dw oa awen pre] Soa ew oona owot Jaosoe 260 ww am Sica oe oz io ) CorEdnovdnrogaWeoenesotusPlasma ovaetreieResearch Plasma Endoguneus ls ConcTomiirmston. ReLcowosvpelkres RacHoivgehnsypikdei|| Concapemnradon, RecLoovwerSypikseh RHiegeh Svpeikse [FFos 18.26 840%. azn 15.58. 348% -- 121% - lcccnn <ooLowoQ w 8J8o%s om96% o<orLm0Q w o116e% own11m3e% : &ccrr oSosr Hoew - ososr wJorw ia 2% pr 2% va, ven 000153 Page 61 of 225 --_-- - aM ENvRONMENTAL Laso0r2a.T10O3R9Y - 3M PharmacePutFiOcSalTseAlnoamleytriAcnaallyRseisseaSrucmhmaanrdyDevelopment } (LFC/EM0S2-an1a0ly3ws9iass)opfaerpfooorlmeedd huusimnagnanseArgaislaemnptl1e1o0b0taqiunaetdemraormy HGoPlLdCensyWsetsetmBciooulpolgiecdaflosa MsuibcmriotmtaesdsusQi-ngTtohf2e fqoulaldorwuipnoglpeatriammee-toef-rfsliligshttemdaisnsTasbpleectr1:ometer. The sample was run as - Table 1 = TRiumne B;NH0.wC/H2,CmOM, MeOH (min) Inject: 204 - Analog wavoeultepnugtt:h NA 0 90 10 . PDReAcWoarvdeeldeMnagstsh RRaannggee:: 1109008.06000Dmam.|| 1275 00 110000 - ColuFmlnowTReamtpe:: am0b3imeinmtin | 11730 0 9%0 1100 Column: Beusil C15, - SSpom,m TonizRaetsioolnuMtoidoen:: E7,S0I0C0) . - AscucmumraartiezmeadsisnmTeaabsluer2:ements and elemental compositions obtained in this analysis are: | Table2 Time Mass Deviation Formula - [58min 5629739 [3629601 [133 | Gon | [63min T4129637 [4129659 [54 |CiOFis | - [65min [66min 5269603 5269610 [158 Tac20613 [4539627 [30 | CioHOyFiS | [Con | - 39 [68min Ta269734 [4269674 141 1 CuO CHiOF1S CuiOsFa 000154 Page 620225 _ 3M ENVIRONMENTAL LABORATORY E02-1039 ATTACHMENT C: CHROMATOGRAMS 000155 Page 63 of 225 _ - } 8 PE : i i . "i22e% oi NF aM Ennomenra Liseomoarosry ral v3 2g - i - gq . 5 |+ lo : Pe 5 bem tT 8 : 2 = - : S = 2 S g = % g 8 8 Y5o h & | 8 CE "ole 2 - zHe 2 2. 8 5 ls : git y |3 4 g3 SN E- z | i5 4 | 000156 Pa 64g 0f2e 25 ] odi22i03 i, id - 1a od 4 i2 wg Poff:g8 Es - NFle x 0i E8 sl 152s, BH } whom Lrsiomsiroiny : 5 0gos : 7~ f3 8 3i a 8: 3 2 5 gs 3 a TE - ] % : # f 8o 8 LE 83 5 iE Pa 65g of2e 25 } 3M or ERVIRONMENTALLABORATORY | 483 $27. 1 22% I - - aHiii: ai I Boi H N1I3 ES2] 8%: SHEM43 : bit : 3al8g | - CL -' Cd 2 i 12 :? A g gve 42 g 8 &: :i gg x 5 *3 3i2 le8| - 3 <3i = LOo i8 N+ HHe TTH. 3 FYE 3 :3 ; i - .ei& d : N3i -- ; n_ifa ~ 8og :5 3 Beiz : 2 gE % dos5m ry ed 33 E8 R9E oF 1Y | id SEL, eS 3 Pa 66g of2e 25 3MERVIRONMENTAL LABORATORY } ESieigl" #7 tl one 1 [EE i iiz: 23 g3 Hizs Az & 18 & & irs 1 ; ) 3 3 ' 58 : : . 5 25 $ 5 : tls 5 =2 ? 5 2 | =g Fa7 gd 8g 3lasf ig <$ 9 oF Ca 9 Beg = 3 : : = 5 BA, i518 z y 848 N|Eg 33 :i 5 Rh : 2; ; z; 2388 0 Cs fg I8] 53 5ls Ea4 Tn8 CC . 2% id rcs + C) Pa 67g of 2e 25 " i. EE 5: :3 - ' E-- : = 1 oq TEFF :: wo2 | Hee =o= s gd! TE 738 @ 21 8 } g g'o Te auLdg wd iE 3 | - iE +, a2 Chl CRE, i ie igif HE s 17 5 BE{ ds 3 TRE A 5 ih "iAlejE z= ila 2 Pa68g0f2e25 - i . | } | 4| T+ - Jj iE i % 312 IM EnviroeNTALLasoraTORY := 2i :: |: |i x g { Pod Eo 3:HSp0= Jb )o gs : 5 }| 3| s4f3 C"E3-d Pa 69g 0f2e 25 : Eu : | iI i f ) a& oRof 0d oe ge . 2Tg& sil Biie EEE i i \ :i Ha g 8 8 8! Hed g| = 8 A &| : 8 b : 8 sd 13 8 3 a Hl 13 * ha Pa 70g of 2e 25 _ } 3MExwvmonentaL Usomrony Ei 7 ea i HE f HaiEi R24i1g 3i | 0 3 83 [oo | i: yg i . 900% Q - J) EE 3 ) & i -- : 5 3 5 4g 11 H20is 2 =i y| Lo5 4 8x 22 g .} :t LPEA LT 2 Hn, a) lg Bele ee Pa71g0f2e25 3M ENVIRONMENTALLASORATORY - IiHE a4id HSai :i 5. i 3 of ol| ) 2: g ` g 3 . 23 ) a a, E fSib = ad Te ootf Be TE wa " . Hi . ii 3 . ne ;i : 2 23: ii0fa Iri=Et ii ir al sgl 3 51: Egy 311e8ly Fe " z Ri8 g i : gl ] } 8F| E3= i Ss 3| 1 || ch | ? .| 1 i i i g Pa 72g of2e 25 a | 28423 B3885% * aS i3 - a - 5 =Aq i - PS5s g : ""33 Cl CEi < 2288 } 3M EnvironvienTaL LasToRATrORY 42% - 1 a: rs3 fe| i !* ? g gl s a i--3 Z 3|8 | 3 g 3| 2 s: g oo, 1' F3e : ge * Pa73g0f2e25 i : i . g gsz - RE a. i 4 3 . a. i[EE : foEgBEGE EET iH . iS28 [238 ) 3M ENVIRONMENTAL fit LABORATORY 3 234 5% "le 3 3 8 8 3 i2: gg B8 Ey = i i Fn 52 3 5EsI1 a 13 iAe B8EL i Pa 74g of 2e 25 i SME` vmomenra. LisTomareony - Ee : i gt3 y nN Al os : 9I Se 49 2 HH ii : s Be g %5 5 2 i z 8g 8 ] -- n2 5 Ee 83 g "3|g 8g Ol l3 i Pg i 5h : 23}d BEH aifT ggE Fog --i v2e vc2 J Pa 75g of 2e 25 3MENVIRONMENTAL LABORATORY HH i 3 i | i} i 3 3 3 | g g g g 8 - i. ii <I ig g | Qo Hi ls W | Ss - CE . Cwg lgogi: 2 =< PiEg EO 3i giil ie . 8| A NE 3, 2 1 TR : d fly 1~ 3wy He eT ee 8g| Ee g 2 |8 ' gs 224g | in i iq Pa 76g of 2e 25 ] ons 3MENVIRONMENTALLagORATORY 8 - age - | - | fPEoo o E Fi |go To ~~. 3| --7 A -o I . Oo J 9 : : : 33 : IE Ff 5E i : Baie : ~ go| . i. g 2 g 3 || "i fl bog id . Pa 77g of 2e 25 } - rEyr : aiie | 3a - 8: : || ) | -| 3= Co | . |& |5 i3 & : I 22. F : 23g : EES 1553 : F&ife ) 3M we ENVIRONMENTALLABORATORY z IIei IIse! ig ; 3; 5 3 i3g) l| f Pg ; :g 3: :F g g : 8 gL z pk <i9 oe : |i Bidg ie _ = ! Pa78gof2e25 } IMEXIRONMENTALLagsoReATrOReY _ 82483 22% +33 oz 1 |g 82 2 5 2 e 33 3 3 3 } 4 : ) zyl 5 4 9 } | g i 1 g } o Pgos z ig 8 ; 8! :| | : : :2 lg TES ) 2 | i ai IBf o . Ef S iE | 1% [2B2g8 g2 EFo2 gwd og e8gg Eo | . Pa79gof 2e25 } SEE Emme acsarony iz i i : ou -A 8 i g 3 8. 3 SSIOo : i . |i , | | , s : em p23 a i 7 o 2 8 | ; A} -i . Poi dt log Pou Tr EE Ie I Bt : FL g i IH r e : Pa 80g of2e 25 i ) F5E3T8Ed - Bf - 8a3f2 . . ){ 8s . i | . ! aEumomenra. isoorartony 4i2d% 1]El 3 e ? X: :Ya : g&, g 3E.H 8E]E s% 7 == "5g & 5 - 5 R gg|l H3 . 8 ig . AH CE : 12 i38,.8 $25 1 : 5 3 2d 54 :5 |i 2 F = Pa 81g 0f2e25 3MERviRONMENTALLagORATORY - [r HdEaFNas-- see ---- i43533 2i5s3" F85%"]oy t: iH 3i ii ii ity - 17 oH 2 TF< F EZ S 5. E 5 gy 9 2 = :Ig: A, . 30 og z3 9Ia Hoo t 13i 3 : ii : TE ] 5 i8 4 y Pa 82g 0f2e 25 i sis ) 22432 - HSHa : 8 B= : : be i . i )i od i iE i "ooFffF2& C EEY iEis 223 [3:8 ) . a raromsenrn Luspomrsreonay - 8 2 i: : ; & :i 8! 3 N 3 $ 2 [Ey % ih Hp sf 3 n 8 58 i 18 8 ide | gig8 | <i ialki RE: aieg: 23ug toe Ny 24 Pa83g0f2e25 3M ENVIRONMENTAL pa LABORATORY HEfaeTd 85 i 87 i is 3 5 ) i 3 5 . :i &% .; .C-s 3 5 3 5 i 8 AI B= i 3 PoOfFf sf, 1Mhh CoCnflidi, TE ; #7 1 Bo s s 3 ` a af 3| sa e 2. b 'Ho 38 : 83 8| 5 3 sls LaI El oo da : if : Ha Hh. =| S353g i Lire e : Je R i Pa84gof2e25 i | : E3iH:: - ) . % A C8 o 0d ]5 ) z i 5 58 : is ) ean soe g g . 3 8 a 35, 3 a . 3 ToiuH ! : 2?| | 5 2 S | e o ! sl ; bod : * 32EdL EL | Pa85g0f2e25 i HH es: HH |E | | : | 4| 3 9 . JGlos ) eii o: . [I ge 5s i EBi3_L8 Emons ssponsirosns = i i 3 g g g 218 _ 8 i ?= 3 ; 3b i32R 8 8 1 A y o o 2 | 78 lk . a iE iE2 log a Pa86gof2e25 : Smo sFsmororn 55 EF, Rife" i [a ge 5 385 [5 3 8 2 - | 88 i i ids 3 } : . 4o g C \ | ) | 3 :3 3 HA i i elt Lal 2 s . 'g Ha 3 J } 5|L8] | 3 od s 4 ky i : 2 is 8 hire A8 8 i le Pa87gof2e25 ] } sm Enron. Ligomrony i i i TL - i xl i g ide - si" " " 5: | al - i Hi = 3 el : : Ho - &2es : 2& 4 i Sis 8 2a 5. 37 & a bd n = 3oHBe 3} 3 i ih0 = i T dyo! i 3 I! oh | FE : : | Lh Poa, THT - gif Hh 2 ! i Is H eds 5 g Ej 5 5 aie E eee ew eee ) Pa88g0f 2e25 3M ENVIRONMENTAL LABORATORY - bi 3 ag5e : g 3 " g } od z a 1a ] JE 1g "|g . "|g i Y i kh . iFR $3if i "if . : | 3 3 350 1E fg- 2 8 3 2 2 g g ~| s $938 ig 2 : ll Pa 89g of 2e 25 3MEXVIROMENTALLABORATORY | 8 - 2 iikb] | ; ; . ) Aq 4,8 | 3 Jd 8 S_ iN 2 82 C: E8 iE HH * 5 pd :a3 . 22 :i :: @ ol a1 8 3 Cd 4 Iq . 8 i 3g on g : bal HER & gl iig ik = =| : :ia i3 J 13 3 ) Pa90ogf2e25 sneer ares Efast 85% 2} 53 tl : ts i 4 >2 ? : Ss : ' s la ; ;ly 82 | . 2a PL 8 = Fl al 3 : $ | 3 hhh i 23 i : i . Gaff ET eT gE s 3 23 3 4 ig 3 3 | E52 gd ec Pa 91g of 2e 25 IM ENVIRONMENTAL LagORATORY } 3i8a8d2 2fz" zfz" sidiz 5% } 8 i 3 #3 8 if g 2 4 ol C Coh dw s BY ii Cllaa fi Pls al Ss i EE ) le L5 i C1E3RBF : id i Ik we iigf S388 5 1i ! ` 21 . ] 1 cgE 3 a s i"ih: pf TE i ah2 s 3! F egs 3 --=f 3 : @ nl . 8- ait ;{ ; b ; tf 2 #ei deg i3 : 3. 8 i Lb 3:9 LE 1d dE Pa92ogf2e25 ii } ag SM Emon: Luggmrony cot i. )| .: : 33 80 . :; | g 3k |8 ; yg 2 g 3 |4 ) 2 g <8 odii j_ id Ese : "54 : | i Pa93gof 2e25 } 1i32i3 : 3i 4 ) 5 - i 5: i J 1 - OE ) \3s3 } 2.55 [23% i igHz5 ) emi gpmied 5| 8 3! . yf 2 !; - g 8 ; 1 : 3 : 2g oa 3 5A 13s 8BossJ3 | 2 41 a esr) Pa94ogf2e25 WM EnvimONMENTALLABORATORY i : ) | & & = = a| 2 2 a g J L 2EF : B OR, i.G gBhy Bape 7 ois vig 7 ee 8 i ch %. 3 Hy | if Pa 95g 0f2e 25 3M ENVIRONMENTAL LABORATORY Saf 2 2 5 SE A EE | : -- PI . A :9 IC9 . i n . 3 CGE ' ge fF i Hl tL %i odRblo 15 8 8 a nL 3 g 2 .| : - 2 3g "Ig 3 i g Tg s i Hs fi if . Page 96 of 225  - [3TH i - Cd : CA3 BR=IS C8 |2 IM EvvmowenTas Lasorarory Fe i | 5 3 : g 8 | Hl &| I 5 ik Il gd ~5 Pa 97g of2e 25 . MEELaprieann - jSi83" iP3" iu #iz oon 3: HEH Hs 3 3 EH "lis _ z = &" = HH ] E ; g - Co I; e 3TEt H 4= i 9 3 18, 5 8d 17 fH23 a2t 3 TE HE:3 3rE 2oe : l22 g o g3 : iJ 2 58 \ L"lgg 5gs !8 "HE : hEi 5 +Hild i3n i:fs Sig! :3 82 s| ESFiJEl. idg e388 1 CE * s * gs Pa 98g of2e 25 _ EE - ---_-- Suds ia: -i 8= = : . * i . . . 'g [i = or i ES . |g & ' = 2 i i: piegie SM Envromens LasEomasrorny 3 2; a k 8 fTEeinfs jf 8 3 8 ' ? 3 q 8 g 8 : 3g F.: F 8 {o2f 2 & 2 T . g i 8 d ; ; Ea 8 sda 0 id 13 Pa99gof2e25 i|} Emon Lisoomsorony Hod om By ) Ii 5 PE 1 _ Ei i 5 ji : . if +B NIE | 3a Pe - o $ 55 = 5 33 o o"Z 8 ---- IE 7 8 ! :hE - 3: A 8 i= 2 3, - 5i , : [TE =| , i i J J"E iLid =1 EEioE h HE H| l =i |:; "1g-- dh s 3s :: 3: 5 TE . sie] 3~N Hh E = sE Eh ls Imi . Hig Ei5e4 g if g Page 100 of 225 WM ExmowmeNTALLscAToRY Ii - :E Pio | g 3s 4 'i || & i4 J Jd | 2 } | | I3iE . Lo | 1ifVR= ."i| : go . : CE g oai dS = 3 3 4 To L# oHd a | Page 101 of225 i} iE - EE: - 55%3 2g . - | - i . | 45J o= & 2 ls i 5 i if i $52 is :8 g z Tos 32 g IM EnvmonmenTaLLisaorartory I = i .& li 8 ' : : = - iE 3} 8 3 :5 ls 8 : | . g| : 14 2 g: jo le i Page 102 0f 225 : ES--e--es & i i i | JE ; [I " " I : | 2 8 3 =| Jf | ilg i FiiEs A AT3 g8 ] 3 lh :: 2 a = wn = = . 8 b - a i 8| A S EE iREE Page 103 of 225 i . IM EwRoNMENTALLasEorasToR i 3 3 3 " | Hy |g : A 2 24 5 iw g g 5, i: -- of a 2 ag 3: 3 =e ak Wy| SF s E 3 If ;EE dh liz g2 [E8H588 FFl :: i Fs3 5 5i CE FO } c5E 5i Fed 53g y Bo: 3 5Pdi L Fe Page104 0f225 i S887 25 i i i:- 2 k|e 3 3 | 3 NE 8 _ : y a 3 z EI 0a * .40 Lio 3i g: 3 N % g i z | i : 3 En hl] i3i = Ne i 2a iz f Page 105 of 225 a 8gd . HBaEtMy i iE 32 i ot1e. Po | SN - 2) 2| iJ a e Pf wg cz E : i5 1i35f5 [223 lBeigsge . IM EmvmomenraLasforaaTodry NE 38 is 2 i , ads . gi a o a2 g| 8a 27 3 :: 7 ', : g | # | 0 i? 2 | 8z 3lso Hi i 00]il Page 106 of 225 i . iii 3MExviRONMENTAL LABORATORY i Hi gi gf E 3! : i PoE =n oe 3: 8% g: FB g JBig ray ve Ty i 3 5 z a EE 4 =5 g = 2g ie8 8 a a a, i bal 3 55 :: A iHrE 8 - Ql EJ =3 1a0 %5 T 3go 3 Fle z : : 2 ~ 1 3 Ppoeq dp te wf C3: 22 i 8588 % 3 2 : 1 CRE ' | 3 3 ahl g<8 BE Yi sib Jd T % i Ean JA ig gE gE Page 107 of 225 } Emonisparaonts ) "3: 3 is 53 32 g 2 12 "ile : tele Cs :A 8 me Pe HE CD iF ! iCols2 s sd E3 : Bo, 8 id CEE JJ23 He f38f 7 2 i. 3 b% os 5d eay _soid | # s Tg = KE 3 2 gl 8 : v8 8. j 4H 4 ; . 5 RE 2] 8] Bos is pe I - zi ES b= 2 rAeh | [ 2~ J E Hiddbg | : " s 8. gl 4 gif 43 5 | gd gg Fog vo Page 108 of 225 # ' git - 1185i858 i| ] | | 3Al x . &| 9 :3 oi in = 53 IMEXvRONMENTALLABORATORY SEi CH 3ii 2){| #| ) 8 HI ly s i | ; gs | 2J | : |CEha iiS - i 21 | Page 109 of 225 a : H2Hs iLEE i . | ) | : Al gy| 3 35s 532 iEie 5I3E8: Fits i IM ERviROwENTALLaBoRpArToOiRoYd i ; 5 8 " 3 4# i g Sd g s: 3 5 Q * lig 8 S$ s |i )8. 8[I 4 B= L | 3s Page 110 0f 225 OFS E18R5E325 3=53 828 gia% we# SE ii i3 1i i1 s | d | Pk | 2 2 8 2 } | AZl :3 g 5 52 3f st | : i : t 1 3 5 Ig 5 fdr 3 3 Bagg 7 ig Tepe Tew In 3 z: 2 3 : LE] 8 8 8 23 8 ------ ge 8 Page 111 0f225 pi IMENVIROMENTAL LaBoRATORY : BBaEis 8FE5N% 4i23 4223" iist - HE : i 3 Ef"33 3: i3 3: 2 2 "a 4 0D 3 us 5 ] 4 Hie 4 9 thr ; Cd , c& oiil : i-- HiE u -- Pi Bi of Bh Beary mT fog 2: 8 g g a 5|ibd ho 1| Page 1120f225 i - 22 HH - . {| . -- 3 whoa soon iI i 8 . 2 F 3 2 N8 : S$ His 2 o"d5 3, i P Hk CE F 3H2E5% i mo 8:Be | Page 113 0f 225 i i : is 3s . 0 } : i || J J if, 8 8 iH aEI sd iss 35388 . Mmmm ucimroiny ag 3 ls 3 3 8 3 82 3: 83 85 8! t 3 f 3 b-- g8 . i id 8ol El13 3 +| Page 114 0f 225 IM EnvmonuEnTac LagoRATORY Hl -) EERkud Be i - To i i, o - - EL A id "|:gz3 CCELEE if 8 . Hh 2853 |3 3 3 8 r3 o 38 88 2 = 8 8 i1f8 ? 3" i gisld 4 =: F3 a R2 &E Page 115 of 225 esl ] "igia : +i i i : || ~8 5 :i Hrz : CeFel] 2853 3368 ow Emmons. Lisomrons . i .8 3 3 3 8 3 8 @ %8 S 8 < gif 3] gf) : If 3 8 i : a: Ho 3| ? Page 1160f225 ;_ H13E73 P1i5 a55 8 - gs z 32 g IM ENVIROMENTAL LagoraToRY #f5i1e Tl 3 : 5 z s = oo i i, - - g 8 3 - 1 Ch a Co hh i CE -3 : : 2 8| 8 EP = 8) = : . EhIo 3| o2f3f 8 Pa 117g0f2e25 i } EgRaalftl 3iF : 54 ] 28F2H 23 8%z g3 1. i ) oo 2 . =s >a z : :| a ; 1 i4 i : Fg 1 I ig aft : CE8 BEi 8 ' 3Tg + 3= : 3 z8i 8 1k"se 0% Emme aomsorosny i1 5 i & 23 z 83 3 2 & =. a 8 JE<< g ? id 3 i 8 "ggg 4| Page 118 0f 225 3 83 ) i) | 3 = : : ) )3 8 3ii ) i2i wien rns 3} 5 s : " .2 3 iE 1 Toe= 3 8 = | = | 8)lL . | :J 1i33 i. 1Hi Page 119 0f 225 ] 3 ExnamowEnTAL LABSORArTORY _ PY i g3a:ll S5ii1 ] .i i: 5?3 :: 8 TL 8: ] 3: i i3 08i 38 8g 8 i ki ' As 5 } 5 ER . T3 13.52 3 & ti Fed i i g 88 4 2g 8 i ke 2 &2 2 A & i 83: -- 1285, : o RE Page 1200225 ] . Be i 88% . 3c } o. - . od . (+ . [I :: _ le 2 el 3: ] 3: El H e SMEmmons usporosns y : 2 of 8 i $1 t ogl : 3 ! 13 a 5x i8 8 = 2g i fo | Ee gzm 18 Ss 2 s3 5 5 Page 121 0f225 : i. SW ErwmomenraLaaFoorza1r0o5n9 - i8 _ i zt - i i : : 3i : - | | | :5 : 3: 5oN | : , Po Ag } 5 i: ::| : } z3 3E -- :: ELE : i ) HINE :i - i : {4 1g 328 k: oo 888 * LE Page 122 of225 _ IM EwROwENTALLapjoraTooRY - [2B820u82t 42k53% 24 & - Bi:Y [i iy : : _ 32 g : i | : = || " . 8A - = a a elIeoN 3 == 2 5s =| 3 . A 3 . } :: Co 3 : ifaig @ ge Fo eg3 e . 1T8 o A %boo , be ~3 ! Page 123 0f 225 IW EvamoumenTaLLisnoRAeTORY sand - 82288 _ 155 5 A832 - i 1a i & #%8 4%% i. 5 3 53 ; 5i - |. i 3: i| - 3-- : } i =3 vy -A Hi sh ) Cgi 3: : I| i: gl 2| 8| =a 8 i= 8ti| i a. i . ig 3 * ) 2 ii tlh : - 1z iis J==p i iPlI Lr J g$ ,]iz38 fd : 5sg8 8s8 1 gg gs + g8E_s + Page 124 0f 225 _ aM EmronuenTaL LABEO0RA1T0OR5Y ATTACHMENT D: PREP SHEETS AND TRACEABILITY INFORMATION 000217 Page 125 0225 - aw Bivona.Lisoomearr0on%y [ee [Semao] o _ SPE ColumnsExtraction Worksheet prapas s xwma: 023o0r3 Methoda Revision:a E7582511 orton |g] sa | covered| "vaurs - loanara | soom Jomesraom| wa fame | | lampiosenm | ooo Jomo gm| wa fn how | _ lograsenn | soon Jomo rqem | wa pmo"howe | lporsoucoseum | zoom Jowers1960| wa foo hows | - langiopasma | zoom Jowers196m| wa fo hows | |ooenwestpesma |oom|waersigem| wa fen how | } | lonovaiveResoucesplasma|2000m[oer rgom | wa fan ow | ( 1 1 "11 Go ---- rT - + 11 } - [ 1 Zo1 pe | b= vr 1 I= [11 | [-- -- 1 1 [11 1 [-- 1 1 17 e1 rm L r T r - xcontoenncoeleivinrMeOH, 2s6wicsohiihsial ttr. 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J BactCopy of Original GE ele ) 000218 Page 126 0f 225 I Nor(GLPSPE ColumnsExtacon Workshost me e ereae] J Prepate PEP onaonz iono2 HotodRevision:36.251 lomcmtar | wom fwwesrgem| ow foe [0] - osnicmta | wom wwesgem| wa fume || [osstsenmpane | som wwe igen| wa BEST lowe | _ [asstsonmauneotops |som|waten.19.6m | uotososorefimo forw | lassencurvensopp | oom [waar 19,6m |rouiotoaoso4[EB henme | - lsbitssnmeuneorspn |som |waten,19.6 |tsuotoaosora[ime bonw | } | fosbtsonm ouvorsopn | oom waters,1g.6m |souotozosoreERE fone | |abtseumcunetoppr - * lssanmanesopmn | oom |watrs,196m [onactozoeovf fone | |som [waa 106m [sonuotorosorafone fem | - lamp sovmusosop | som [waar 19.0m |rouotorosorefr bom | llamosenmussoos |soom [wna 19.0 [100 otozoso-refe bon | - foamsonmboncs |wom [westgom| wa foe foe lsamasonmborsz | wom[wm tgom| wa forfoes | looenvestseumpinict | soon |waws igen| wa foon lowe | _ loosen westsorumiancs | oom [warssg om| wa fro foe | |osenwestserumits050p0 | sonm {wer 19,6 | ouotozosotsfrm fone | loosenwestsarumis-sos |so0m ws 0.6m[ouctorosorsfrii fone | } womfw sgom| wa fo few | oom wer rgom| ta fre ow | com wats10,001|sousoaosre[im fer | . [oorssoes esemonsums ao_| 00m[srs10,0m [sooustonomnwere feran | omen POT ie rAor 7 _ Additionalcomments: ACh I AGI cima? SRRERE ce cx LC fale tal psy 000219 Page 127 0f 225 } IW EinrONENTAL LASEOoRzAT1O0R3Y I Cr = oFByorLaonSePnE ColuemenssExtractionWorkahetvsssn rt: TS pr Sy No2.r10% pa loco looskmirgz sores | used py Conmans | wom weston| wa fooe || | womIewmigom| wa Pome | | lcninesopasmacuvesppp | stom_[watas156m| touotoaosorefe honme | . [crnese plasmacuvoarsoon |doom [waters 1g.6m|tsuotozospe[ie heres | { Jormesopusmocunezsess |som mas.1g.om| sototozosoafre berm | - lctneseplasmacurvespp |soom[ates15,0 |soouoroposo-reice lene | | |conesepasmacurvosoppn |soomt_|eers15,6m [soouororoso ule lowe | . 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[avovtueResearch smaincr | stom_|wnesspo | ma fom lon i ovat Researpasmaiance | doom [woestgon| wa frm fon | | - "morse Resescnpasmatisspp| s00m [wats150m toooongnreff | Susacton tsa (ater con - _x_conditon column with MeOH;_x_wmasohwiwthnmilsowsaoter;_x_fitersample; LBoacrteCopoe yf Orgij nal Wa Da } Additionsalacoammhenttsmsom, somprtsoiessTA1oHn.Sdcnarbse:dte7wR3 Soi wk05G,CnSEed19 @ TA Tn 000220 Page 128 0f225 3 } | W Emowena,Lisoormrroonsy 3M ENVIRONMENTAL LABORATORY NototFie le Asocated Study Number: forsmpts at irprepped 1011, tareBrees Reser SerumMS 5g 1nd `5ppb,labelsonvialswere accidentallyswitched. -------- arm ooo 1{ . ] 1 - - EE -- om- mmm -- =- ee hA om e ue Ao Ho - cd RSAS pFhi fLorley . Form ETS4-15.0 000221 Page 129 of 225 i RARBiEen Test Control and Rfaren Substance Log A C Ese o TO " E m o F pe oa w] Ma rr [por 1 pre fee 1 . (Siae: ra Oo K f fo: - =ar2si200. 3 wr rr fos ew ArchiedSbstanceNotAvaiabie] - E c Bo T a Tae | i| - ) sEaara 1dLocatonSiorage: Frozen F19_ e cronToTtc s SAETeA oRrE RE RR Ror By be EctCopy ofOrga - Loe 4 wren 000222 Page 130 of 225 i . am Eimmomena LasEomsroony : mw) ind : sraTmoyee,||| Cpwome||| aiCiaRrsSe |Eo FoRTrmTPhTl sES | wo . EF[Ee ppPe ee `ExactCoofp Origy inal - a Loac| wiilex 000223 Page 131 0f 225 i } E---- oes } Se TestControl and Retro Substance Log oo - i feaSBa oerr p eweearsor o[n orvme pr frm - (mfairsr:se Gfihk oe i co -- [a[terorozrz002 F1 omAerhivedomsanse Not valle osedmesn | - - O (e fPuttoy: N refoo BLor {rrr - i Cal ey BactCopyof Original 000224 - Page 132 of 225 . IM EAVRONMENTAL LABO0R2A-T10O3R9Y - ete ) ccorleedssmanpam SSOeloLr | winarmen| Gsohomr a Prnsa eroat rs ow)are [F0as|[Gas| Tews [03% - ESaae reat1e | Baancei0?|Gmarnecrai1Dewww Ft 1 jk fowme] Exact CopyofOrginal Ln gen : bid Data 000225 - Page 133 0225 `3M ENVIRONMENTALLABORATORY ) . 02-1039 X ooTloeddFhaurmmaannpPlraessmaa ross USELOG. wiBnordoow || (mwaissdorovowl)|| winadtaerval otreason orem) E|REwm - ance D1 | Balance 02| Salance1 ExactCoofpOrgiynal - Line urisen tal Dan 000226 - Page 134 0f 225 : WMEmnronenTaL LsoFroa1T0o%R9Y Test Control and Reference Substance Log Sr E ell ala oorrreroea ovbaichF: TGoTe00T ME 1 i [prime [oom 5 foRaalrsberszo s wJk ioomT Rate - Toaw 7 TAA-- 0032002 - Cra ea osm Re)mAnrc--hi-- ved1 iSubstance Not Avaliable Toweoimesn | 1] prTE ee | ) e[oaartoyenrsein [Fre ar Far - : ECxoancetCopyorfOreiginnal wt "Daa 0002<7 Page 135 of 225 - 3MENVIRONMENTALLABO0R2A.T1O03R9Y _ FcaoeiuenrdnaCmraanspPaossisHuman Pass USETOG - E viGtuW ail ||rowsisnGcee)|| Gwiraeanwasal | Pu a ossnnSfoarrdemaoava)e Bianca | Some102| aancatd Sa0v s FT]7] bbw wwe fe Jokwm Bact CopyofOrga . 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Exact Copy of Original oie spor Ce 000229 Page 1370225 - IM EnvRommeNTAL Las`o0m2a:T1o0R39Y _ Tost Control and Reference Substance Log _ [srvSaamemveenaemgaepPoesed aP aesFamaR Pas FoaR CRS TORT caw ass are [5 _ B(REsrara RET T FT rc rg ox Se Toa - Ki oamaomenrs i 0 a ES ven - ) ArchivedsabstanceNotAviano Po . 3 [ae[sencscataaornow.rseyedveossms--a--in CDamtpsSe Si Locsiovsiongs [Fromme - SCaocmeimsoeenntgsFeoyrmas: 1 -- ExactCopy ofOriginal - LanC_ \W/ifo3- Initial Dats 000230 Page 138 of 225 - Bi 3MEivRONMENTALLug0o2r.A1T0o3R9Y ~ sie Turan Piss FrCo ie SEL ons CC a Ee Cra Er - Svlii= ncoev0al1|| G(ummnacoers5s2||Bwoiasrecsatt Tem TT -- www T ve E TS -- 2c | y ExCacntCoofppOrvgiynael a Deo } 000231 Page 139of225 - 3M ENVIRONMENTALLaBo0r2a.T1O03R9Y - ores Taman PF Corie _ Chsas USETE = eiwnW ia ieinanL E a1t || rol Rsasrcrvs)a | wGirnodvesr| Paru easarnsfor arnemom ae ) SCTal [eBe ee | Ws TO : BactCoofpOrigynat LTitoa wpuse 000232 Page 1400225 siomagra n e EerE (Roe m ew t m =iiw fRe rL:En ox e oOne rer f sri] E-- e ------------ ) ArchivediSubstance Not Avaliabia] . B Cx a DYe -- R ------] . | . ExCopa y ofc Orgit nal Luc wove ital Dato 000233 ) Page 141 0f225 - IMENMIROWMENTAL LaB0O2R-A1T0O3R9Y - ed aman Sou From Bowsounes USEToS RaaHuman Serum [CRs Gros| Pors oersan [Ba 5a - CSlwii% nahcnicoowiaeDt'||F mGasasomrve2e)||awsiane dnmca1la| em e E m 7 E je oc fon : ExCoapyofcrgt ane wor Wi Oa 000234 Page 142 0f225 -- -- mr Em Emomveieien tT ok Jiomma BactCopy ofOrginal en wngen lntal Date 000235 Page 143 of225 - IM EnvRoNMENTAL La0B2o.RA1T0O3R9Y Tost Control and Reference Substanco Log Scireanliar i foe tos:r pr% e fs Jomeri ilwir - [Err or fr Is #3 TRS oT rir _ [[r CoElveerEy T = ef Sos Yes w ---------- Ew oArchivediSubstance a Not Avallatle e] - PRoeco [Coco coer asysvess-- Camas - FfaC bericsationofcomatoL n - C[lCooemmmaaesryy |e S ___i _ TRAE TTe T ] . BaacntCeoofypOrgeiyesn ta uy 000236 Page 144 0225 _ IM ENVIRONMENTALLago0R2A-T1O03R9Y - : Fooslerd e HHuammaan sruom rm oa SELO0 [Com Ta || rossvenal| Pipe orrd arr = Cs - E BsaEnucenla0'[||robsosnove2)||| onwaeamelatdeB sowiemesl a T ijoc fms] . act CopyofOrigin LaWca wayy, 000237 Page 145 0f225 _ IM ERvIRONMENTALLABO0R2A:T1O0R3Y9 - oa Rama soa am Cae me _ conelsdsHumansei - CewSievWreeTs || avsRisrenses)| wGie[gonan | Peoransan Staennoer er SianeoiD)s| Evancarp3|saa1 So ? ) Ect CopyofOi PC ra r C0Z38 Page 146of225 eomses mr: a : em rr : frFa:a e go rea Oat | : oa frre Tm - I I| E H B= E me m =-- e [WiiecurForma: -- ELETE -- Ga ae ExactGu, . - lal" Dagp. 000239 Page 147 of 225 _ SM EmonLaseoroaTosry _ Tooo oeee],r V(i mm2r||||ei,a| i A rae EB3sag c%Bo | -- i eGicocny Ctot vec i 000240 Page 148 of 225 2 IM EMIRONMENTAL La`gEoorza-T1O03R9Y - i Haman Seri or Siam ae Human serum USETOS 0 [CoBvtsiaBsnndicUiooowVsia0la1|||E (mwasoasmriol tmv||Gm rwoisdasrwmew] iavl | poosrsTeesroSrananaovam)er SaCva7 l] [Bn iss| ee EE] : Exact CopyofOriginal are wien CC) 000241 Page 149 07225 WM ENVIRONMENTAL LABORATORY aa -- i Srre waFe oPa er ewEE E a Si r tL a m i e a r Eg E RT ree oren esreee r ei) i I Termme EaE m m ---- r e - rage Ba CopyocfOrgt inal 000242 Page 150of 225 - IM ENVIROMENTALLABO0R2A.T1O0R39Y - olieed HHaurmmaann SSearrumrFor GolemWeak USELOG _ 550 TG| Re Gromer| Pearsp ande eres [anes is| Da - Bvairvciaaind||(Groasssocva2)|| owniandcoalwd (I EfeFm jo Ja] . ExCopay ofcOrgitnal abnec uve om : 000243 Page 151 of225 - IMEvRONMENTALLas0o2r.a1T0OR3Y9 = i oada Hmonaan SSeervr a GRR GEOG - TSwehBaoinores||rwaorrenr||| wCsesiren|a| Ppress amon) | BTe ES[Tor|| bm TT emewemm jr fwwma----] - BaaW cntCeoo osfOpruigiynaal 000244 Page 1520225 _-- i mm CT|fpee esca . . ] [EeEn| :: C1E|(fet ; RN iia 3 EEEREERARR Page 153 of 225 ] 3M ENviRONMENTAL LasFoRATrORY } } -, :! |I . ana -- qn ER Smeecnn ST a R RSegtuomur TtaIrs aE I osbsvy en Stancardnumberforthe mec 02002-63 y E o C p E iel : S e E mr| mt| fo omiousTame | 0 sr] Beemer Bros 1 mms1 ew ww tSoniy n Cg efilele : ae iyCabos 1o131 0x Ect CopyofOrgy "a gen 000246 Page 154 0225 - aMEimonmena, LiEsoozmrroonsr - SINGLE COMPONENT PREPARATION L0G owe_lo:10: 02 - Ara oKJ P[ a--g--ano. -- _ ows ___toopph super pix rom SP e Stock Numper_0202 -63 ) Wattarvom Sul ] enn score ) -- NA J NA on JI --N--orma HeOl /[2A - ; 510 x Fravonme____ 28wl roscasmisr oop srgtomston___ aol L Exim oa: 13 OR / : L Ect Coo nyct rgale Initial Data. rossi b2a LY ofuloz 000247 Page 155 0225 3 SR aMEmmons LisToemarToorny = SINGLE COMPONENT PREPARATION L0G = _o--un:_J02/C 5 ) Bboaike. _0z050 | suc 075ppls see sooner (2002 - (2 - were 37.544 sro MA ) Cy tpl OO WA omensAJA______ ENE peOH /AAE310 J - rasmne 35460 aime 075776 ) sunnier R06 L commom__[1/BOR/ - ne cla Ex Copa yofc Origt inal - Initial Dats i A Lohr : 000248 _ Page 156 of 225 -_ --_-- waMeENvironmENTAL LaBsoermarToonRsY sro - --e-- et _ ---- omur__IC ICC, nam BookNo. _02050 } Dosctpten: cas ph sunrnix `Stock Number: 0202-6 | - hint 12.5 4d Sameer NA i pe ! 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[ome Tm[oR[ie [ore] en rb | | [espJJpmalend] 1[51 0 | | Co ACD Fero l|rb15e3 apdl[e1nTtoSInT]| JaCa nAcni Pr0e-12m6? lelyoigenl] wednd][1] Tesoor?| fen Prvaca llmk fe[e10a lfis TTTeooss| al | | | ) Cr Acid en| + St . oF Flows] [|[= Ca ACD Fiore gagenss )ul sip [rms [2g ipeel[s1 ] [Tota 14 EA IERIE| :E ECPEDO 5A|ATr TaE 25 AE sol |FIE E TeE =lop ) (oekez -- i sass LheA SHY L3ffoufe - 000251 Page 159 0f225 momaawgrr | EcEep Tenantpeeerernes | [re fer i prep ovbaie: 0 ATIED ad em Teer Wa |A A-- EE ALa a A : BE ES=EEaemse TiEED r ) Archived/Substance Not Available| : a _---- R = e RPe coD pT = OamsOsee.cyon . a ExCopa yofc Origt inal Lac wae - 00052 _ Page 160 of225 5025200009148 FR AORN oc CERTIFICATE Epon uoTvssnoaeoTa om EOraremaTsOesRrOoMsTORoYs OF ANALYSIS RrRe-mMaIi--a2cS5 va vam PPRROODDUUCCTT NKUAMYBEE!R:TR3I4D2E0C4A-T1LURFEMEPTAIGEE ACESL,OT59NU%MBER: OT249CU : ronan: Gein [ET------ wrens ovr see ite cvTALLINE 80110 cLfonTrorTi1Et0 SOETeRTR E0TTSoTe nAIaNkDAyRRBDlFG06gFin Sa Fu vem cowoms To sTRUGTIRE. : DarigorLiiioiuraoi ax aTirLeEcomToN, ane 1990 ExactCopyof Original : LINC 10/3/02 ital" Dats. : he ALDRICH CHEMICAL COMPANY. : ------ in-- s -- ra --r--ie--e ----h ---- ny --B--y I aSEt B00 t ei a) tatld.rticnh cLhtemicHaElAcTo. S5rmmismr : a TOTAL Pec0.4 me 000253 . oT Page 161 0f225 - `3M ENVIRONMENTALLAB0O2R-A1T0O3R5Y - i . rCriadas1c3a1t.u0c2r5onapianAocitca USELoG wWiBnodmoevsal |||rwosoRsmceervn || Gwraietavte| Pro aeneos raow)eer a5"s ow[ICn8 s| | - am | ee TEE ) a`BenactcCoowfiOphriagaijynael:n 000254 Page 1620225 . . WM EnvronmenTL Ls[ oaroy ) oue_g/amba SINGLE COMPONENT PREPARATION LOG Psraicekto.. _o5z80t0 poe Auta) . cusses 710 lydcr ca hopBounse dod (rain) Stoktunter__95)-25 - __2oezs, sass 975) 99.50% on ____N ) `Comectod Weight 2.0472, St --. Lleol)- TNA 2204. FoalVole: So.) Fratcuscaesior:__/ 1443pBoer. rr) sengotocaton__2 Af flog +My [ong ewamnvun_2/25/70 a Etof Oorgy Revived by:ModSuter polo 000255 Page 163 of225 i . WM ERvroENTAL LuooRaArToOsRnY . i oe._g/amba SINGLE COMPONENT PREPARATION LOG [Proomt 8 saneAwad ) oecrpson Tr lycsfceca heptane Lond Crone) sooner 9815/2285 : I__ 2025, soca 974/ 28.52% coma 2.0L70, NM etMol) TH= 20 FoalVoue: So.) Foatcocstnton__/ J 9p2EsDrefs sunsotomion__2, 4 fhge Su Lop. Comtnvn_2/5/07 Etoyof Orgs ge rooms (fy|Slovtnen yoloor 000256 Page 163 of 225 swimmergs Subject an CharacterizationofTCR99131-025 by 'H-NVIR and "F-NMRSpectroscopy SAMPLEDESCRIPTION: ee Thuan es -------- v a r `OBJECTIVE: . `This sample was subjected to a combination of 'H-NMR and '*F-NMR spectral analyses to determine the B `puroiftthye nominal product. Special emphasis was also placed on attempting to identify and quantify any a - EXPERIMENTAL: Tt Ho IEA methyl)benzene (p-HFX), and then totally dissolved in a CFCly/deuterated acetone (acetone-dg) solvent y `mixture for subsequent analysis by NMR. Initial one-dimensional (1D) 400 MHz "H-NMR and 376 MHz "F-NMR spectra were acquired at room temperature using a Varian UNITYplus 400 FT-NMR spectrometer. A two-dimensional (2D) 'F-NMR correlatedspectroscopy (COSY) experiment was also acquired using a Varian UNITY INOVA 500 FT-NMR spectrometteor facilitate assignment of "F signals ini used s either 1) a 'HJ/F-NMR intemal standard to allow the calculation ofthe sbsolute weight percent. `concentrationsofspecific components, or 2) a 'H/'*F-NMR cross integration standard to permitthe cross ) `correlationof the relative 'H and "F signal intensitiesforevaluationofthe overall sample composition. "~The "H-NMR and "F-NMR spectral data indicated this sample was arelatively high purity formofthe `components, including probable isomers, were also assigned. A 'H/F-NMR cross integration analysis 'H/F-NMR cross integration analysis are summarized below in TABLE-1. The relative weight percent ext=orsioms `concentrations shown in TABLE-1 should be very close to their respective absolute weight percent values Paget of2 oCk Cy)zigpr 000257 Page 164of225 3 aM EimronwenTALLisEcoraaTtooRny } Oconer 30,2002 T3CMRSIAMLD43A5na,lyLtoicPLOibIRSeEs:t TGoIDe716r3s8 t . aCnopigeuseotfitohnesaNbMouRttssepeacsela,ttpslcsheesd iettmhethkeipoawp.e copy of is earforyou fence, you have ) TomKester 3 NfVaaalrlree rtATA A143SPT)Tm 200 Sample TCR-99131.025, LotTPAUIBOLT2E19BUfom he Telomerprojec. - CvoemaploneCnotmpSosiintcinoan!esesl by "0"F-NMR Cros grWanEAAnyR x . RelaiveinWgleeigvhital%eCoanceentrations CCE.Co Sa : Probab(lwehTereeranvesrabgrea0nc=h5e.d05h)omers Tw i (hePerob0abl`eCtFse3r(miCynFa2)sop-=rCoF2p0(y5ClEob}rr(aSnCCcFth:Oe)dnM,hompeorsses TE (asAsumper(onCbFae3b)l.2e-sCfoFhr-e(crClFdals)ihp-oCnaO:Hpsueps TT OICR.CFCOM 1X 1 CincHonsaltPraoolobpadhbalepc|"homapFoneFntsr,ocCa rXn,d = where Xan be posible shandests fncogal rugs. .. Tr EPsossesmhieborleenCaovFeb(nCgeFesrne-=C5O.0C5Ho,r C7 RT BTR ] Bact apyot Org Lon a S iy,e rezor2 000258 Page 165 of 225 | os IM ENVIROMENTAL LABORATORY Certificate of Analysis = 3 "The sampleofTCR-99131-025, Lot PUOT219E was snalyzed using a combinatiofn "E-NMR and "H-NMR spectral analysis techniques. The overall qualitativeand quantitative compositional results that || = fos ar Overall CompositionalResults by Combined '*F/'H-NMR Spectral Analyses CF(CF2)x-CF(CE;{CE2y-COH. (CF3)x-CF-(CF2)y-COH :gay } Probable rr ea Cuan saturated aliphatic hydrocarbons and Possible CF(CF2)-CO:CHy "Tom Kestner 0.021% `BactCopyof Original Intel' Dats 00259 Page 166 of 225 IM ENVIRONMENTAL LAB0O2R-A1T0O3R9Y Test Control and Referenco Substance Log or raancns : SEE aw a TL . [Ermtenae orSe [c=oonmaemeerrs:szssr [ok-1omTsgmaoeVArT S0 o prer - Comor Jusoste m VOW - For Archived/Substance5N5o7t%,ApvaiisltabeleT'USGOT OR FAR econ ecamad: CSooSrtocfAantsyes LAS anzsivz . . f(oCunocaeiosn,oafrsmiveas t [Owwoodpeodues . (lSioLoccstoFSiazmaag:e: [Comers c[oRonormiaToosm, TCREOT Caress Sold LAS TTHATE oShieppsinpgorcoim.meLrA:SN1o0032U0028 -must ship ground small quant sxcepion. (30 mg EctCopy of Orgoal CTMaC wGean n 000260 Page 167 of225 : -- ee EE, - 1O7a61k0w1doDoadnPiroRdouacdts, Inc. West Colombia, 5C 29172 o :i : PFahxon(e8009030)967335337500 :} : CERTIFICATE OF ANALYSIS ~ : ; Date: 15-Jul-02 z Material: ~~ Pentadecafluorooctanoic acid Tg CatNo: 1319 CasNo: 1355671) : TotNo: 210002 : i; Assay: 97+% by NaOH titration JS ---- Melting Point: 59-61C : Co wood .: : 5 Co Lo 3 wd Eateoyaorg LC n a wage: i : 3 /QC Manags Cd 000261 Page 168of225 _ 3M ENVIRONMENTALLAB0OR2A1T0O3R9Y - _ cd ihsecrhcC aoraos sanSacied USELOG - Shviia nreRismteEss E | ornm are)| Gteatm| onSeano) 3 = ee EE] [ssdey oostrg [isaBesg emnaaraveowoss pia| Jeww [owisaeE ) Bact apyofOrga Lox oie Inital Dats 000262 Page 169 of 225 WM EwROmENTAL LisEooRarTooR%Y ] owe_p/ir/} moi Aa SINGLE COMPONENT PREPARATION LOG SPoaoskeeo.. _o4z5010 oosctvin: Ls by lies Mooto echronre Bed shoe 2 mr5poon stockNumser__J (R= /) 27 + WoghtarvoCtunme 2oz/sy saucers 5// Concenvatanar Pury: HA oer Corcton _ Pos NA | oenoon 0015 SoventanNogmkTere_( 2 01) S00) 243 Foavoume:___ Sp] resto: __/2.7 0 somgotossion Jud [ur = Len I } : eimenvun__3 [15/03 EctCoof oryginal vc olan Initial Dats. Rovewebsy:(Ya \. Skeveron orlicoy 000263 Page 170 of 225 ) IM Emm ENTAL Las`oEorza.T1O0R39Y : 3M SPECIALTY MATERIALS MANUFACTURING DIVISION ANALYTICAL LABORATORY Tn Lisa Stevenson -(-5568) - ET&SS - 236.09 Request # GIDITIEN : Eom Tom Kester (15633) SMMD Amlyical Lib- 2362811 Subject: Characterization of TCR-617 by "H-NMR, "F-NMR, and LC/MS Asalyses i Date October25,2002: Updated Report ~ LC/MS Analysis or Impurities i SA MPTCLR-E6D17E,SlCotR2I1P00T0I2OrNo:m the Telomesprojec. Nominal prod=ucCFt(CF,)CO;H, where average.6(white powder), [Semple_T Specwa#'s [ EupenmentDesopios | . TCR617__| H71638.IDS01|500MizH-NMRinaceione-dsolve + p-HFXcrossintegration/internalsid__| TCR617 UPDATE: QAuafleitatthiveiniLtiOalMNSMaRnalcyosmipsotsoiatisosnt!natnahleyssiss greupmoretnwtaosf isssuoedom0fyheoeuiomnpur1i0t-2y4c-o0m2p,oJnoeenltMsilinletphesrafmoprlmeedofa ; TCR-617. This updated reported summarizes the new information regarding the identities nd 4i cStornuccetnutrreatfiroonmstfhoerosrogmienoalftrhepeoirtmpiusrniotywcroempploanceedatwsi.thYaopurowbialblleno(tiCceFthOat)thCeOtentaettihveerlyseaisd.signed olefin OBJECTIVE: `piTumhrpistuycstaoymfptclhoeempwnooanmseinsntuasbl.jepcrTtoheddeuctstoa.amSpcploeemcbiwiaanlsaetamilposhonaogsfiivs"enHwa-tosNJaMoleR!oaMpnldialc"eedFfoo-nNaMsRtqsiupeaelmicptttairtnaiglve0anLadCl/yesMenSsytaonnadldeytseqirsumtaionnaeststihasetny - iinsthLeOaMssSignanmaelnytsoisfiinmptuirsicuypcdoamtpeodnreenpotrst.. Jos] asked that | ncorprate th qualiaive information for : ET-NMREXPERIMENTAL: : { IAnpiortihoenonfzethne (sarmHpl)e.waasnadcscuhreatoelaylwyeidgihsesdo,lvsepdikineddweishiraekdnoswensoanmsou(nstioonfs.1-bisf(ovrisfluuobros-et aonoalmysitsembpyerNaMtRur.e uAsin5g00aMVHizan'HU-NNIMTRYsIpNecOtVrAum5a0n0dF2T47N0MMRzspec"tFro.mNeMteRr.spTehcitsrusmamwpelreeparceqpuairraetdioant 4 `method permitted the p-HFX to be used as cither 1) a 'H/"*F-NMR internal standard to allow the ___ cieavnlatclguurlaaatttiiiooonnnoosfftttahhnedeaoravdbesr0oaplluletserawmtepiltgehhetcoepmreproocsseinottmicoeonln.cteontnraotfiotnesorfelsapteicviefiHc caonmdp'oFnesnitgsn,alori2e)nsai"tHes/Ffo-rNMR cross ' uy : 3 "hTehencoommibnialnepdro"dHuc-tN,MCRF,o("CFF-oNJ-MRC,Oa,ndwLhCe/rMStheanaavleyrsaegseivndailcuatoedfthi=s6s.a02m.pleSmwaalsl aamhoiugnhtpsuroitfyafoowrm of nimapusriity tceocmhpnoinqeunetwsa,sihncelnuduisnegdpr(0obcalblcelitsoemetrhs,rewleartievealwseoigahsstigpneerdc.entAcoFnce"mFe-aNtMonRs corfotshseiindteengtriaftiieodn Components. The qualaindaqtuainiavive compositional els that wer deivd fom the combined bs10ienltgolhweitirneiaTslAp'eBHcLi/Ev-e1Fs,-hNsTMohRleucereowlsesiiivgnhettewgpreeairtgciheotnntpavenarallcyuesenists,caoansncdesntthureamtqmuioaoilnwisnatasttgheiovewwnaLsCin/pTMreASsBeaLnnaEliyn.stihsse,hasorauemdspbluemmvaerriyzleodse Fogel of2 BactCopy of Original LnC a "ofa0 jq 000264 Page 1710225 ) aM EvonuenTA LisEoorraTiooR%y ) Outer 28, 2002 USnMoDorAtnyiLE)NLSiARneaulysorGIIDTpI3s8 2 TCR.617,Lo 240002 ) RESULTS cont Trace amouns ofa fw ler signedcomponents wer so decd ni NVI sec, but `additional work would be needed in an effort to ideornquatnti ifyftheyse other components. : `CopiqesuoiftrheeNhMoRtspteecstsraaarpadttaechseldw,itphltehseepapercoKpnyoo.f thisreportforyoureference.Ifyouhave. Tom Keser "EE . William Reagen FileReference: W71638.GID.UpdatedResuls_TCR617_Lok 10002TelomerProct.DOC/IO1 - Sample: TCR-617,LotT21a0B00L2Ef1om he Teloreeprojet. 3i OverallCCoompmopneonstiStiiReosrunlstaslby 'H/'*F-NMRCrossVIR RInteegratliongialvneediWaelLiCmg/ehMatSseCronAn nenedntaons amon | wm| = LMSwhesrheowaevderaag6e n(=r6o.0,2 bnyc,"Fn-eNtMR(.oor). Frobsaublmee(neCIoroFlosso0hn)epaCoseeOrssMcd | we ! as posible GHiCEOCOPACRCTL COM i: i where 1P2os,asFiysboltsaesanCbdFln(seeCsFu(f2mC)oFe.s-eCyCaF(iCCsF4yo)cFn-(plCCFe2op),e-nCOH pros T 0.019% om TFoe st Ca tie esm apad oshpam wsrosasn TB REE DE Bact Coofrpty fe Qae gGaasin 00265 ) Page 172 0 225 - IMErvROwENTALLag`oEm0A2.T1O0R3Y9 _ . } :1 2: _ 1: . - :i i . 3i Certificate of Analysis "NominalProduct;CF(CFa)COsH, where average nw6. Pentadecaflvoroocaancciid ProductCode: TCR-617,Lot210002 October 28,2002 "Tom KesandtJoeelMilrler `dLTeChre/isvMaeSdmpfalnraeolomysftihTssCteRec-ch6on1imq7bu,ielsno.etdT2ah1n0ea0loyv0se2erwsalaaseaqunsaaullmiytmazateridivuezseaidnndbgeqaulaocnwotiminbtaiTtniAavtBeiLcoEonm-opLfos"iFti-oNnMalR,res"uHlt-sNMthRa,t waenrde Sample: TTCABRLE6Lo1t21700,02 Quantitativeand `QCuaolmiptoanteivnetCoSmtrpuocstiutreisonal Resuls byCom"Hb-NMHiRaNnndMLRC/eMSAdnaly Relativ(etsiWangelleiegthrtiatClloasnnacleyisnitsr)gations where avCerFa{ge(CF=-6.C0O2 Rby,"F-NMR. DPaoristyt LOMS Psrhoboawbelde1C6FC(Fm-aj(oC5r,F)nC=a,O w(miner) Probaasbsluem(eCnu-F14f2o0)rCcaOl.culaactyciloincchpuerprosseseid E53 2P5ospsosisbilbleeCCFF(,CCFF2-)Oe-CCFF(ICCF,})(-CCFFs,),CFC,O-COt To% Wher x20, y20snd sume xy = 4forclofation urge aPosssib=lse (fCoFru)cya-Clm-e(uClFte2o)ne-COSHpurposes 0.013% Tac ProsoiitbsleoCf,oHlessasganteudaceomdponaleipnhtatsicwhiurocGubeoenel 55NVR en i - : Fasc tof } ile Referee: othTCR-617_Lox210002dos 000266 tttonn QWao ygapn Page 173 0225 . `SM EXVIRONMENTALLABEOR0A1TO0R3Y E icese |" Tost Control and Reference Substance Log a . o fSiosara ar FeoPs | 5Se fREs imosomrszso sokom paste Teowop aJorao . C(-- Crontin men W-- eeGn ---- VOW -- - PyArchivedSubstariSceENOot AvalrfdablTe ATWAORsOs eco eave [GE |shCooosotdPottrAodreuycne as ors . ce55acnCooon,moodroevs,ion RoTor aTORmEAT . CFoasasrrForm oCa xaicroa:3pimognra sspor ia. 1A3 160202 . og EWatrCopyof Oriwnaga } 000267 Page 1740f225 - me - 1; | ww mew oo Fr me py W7Oe8ar0tk0CwdoolDouudnmbbParrCo2Rdo9uac7dt2s, Inc, Phone 609 Rssr Fax (803) 739-6957 Cg ood; iA i - ; . CERTIFICATE OFANALYSIS Date: 27:Novay Matesinh Hieptadecafiuorononanie acid CatNo: 2m CasNo: (arses) SV ASSAY 994% by NaOH titcation SE i : Gso g Sl : So Appennce Oofnfwhitesoti)a Melting Point: s57.620C. Pr.1 nC i/ajn % at i . 0 i Py 7 i JcomMeanYaas 3 God Ei fo } 000268 Page 175 0f225 - IM ExwmonnENTALLusEroazr'o1R0y% - USET0G napaancecalutonapancadt - CwiSRenednTs ||| rvievra || wGooneom | resin ear r ree o GPllr t s |B EG - `Exact CopyofOriginal ae Ble 000269 Page 176 of 225 - . IM ERVIRONMENTAL LABEOoRaATtOoRsY 2 SINGLE COMPONENT PREPARATION L0G oue__5/idl ) BPeacgkeinee,, _o4z8ot0 - snays__ fo) --_ _ ossciton_Lopts ores Nieneoannauose Aud Hoel (5 Frocond sosrumver_ TCA -) 3 arvoine vent uses: O43 2 -------- A 3 Corrected Weight __/5, 26. 171 Balance 10: 98 OtoreFceciono__n_ NS soventang iA Numver,_/ ep fTpl-d) lo292. ) Foovome___ 0] FontConcriaton_/268 ppm ) swsgotocaton_Lu// Ther = Loew Temp oronvoe_2 f5/6.3 ) CnC ne ExactCopyofOriginal . Initial [) overt Ya ou A Sleseece__opl3islon. 000270 Page 17 of27 25 . . IM EXVRONMENTAL LABEOoRA1T0OR%Y - 334 SPECIALTY MATERIALS MANUFACTURING DIVISION ANALYTICAL LABORATORY EY Lisa Stevenson (35568) - ET&SS 235.09 Request GID:TI638 - Eom Tom Kestner- (5639) SMD Anlyical Lab 2362811 - Subject: Dae OCchtaroabcetre2r8i,za2t0i0o2n of TCR-61by8 "H-NMR and "F-NMR Spectroscopy _ =S" AMTCPRL-E61D8,ESloCtRHI7P5T6I8OfNr:om teTelomerproject Nominal product = FCF). COL, where average nie 7 (white sli). i} [[[Sm( TiCmeRpAlTeeSC |T_--_7T1S3S3s1 5pe8GeIm6cDtm440wh5 00s47| 5|| 1_5007_M6iMe_3_P_Eiin_eiRsnEdEyxpsesenlmsevabt+pDoemsHFcgrilpEroioowsXaioeod OBIECTIVE: . p"Tuhristysoamfptlhee wnaomsisnuabljepcrtoedductto.aScpoemcbiianlaetimopn ohfa'wHa-sNsMlRoapnldac"eFd-oNnMaRtcsmpepcitrnagl0anaelnystelsyto0ddetqeuramniiythsery impurity components EXPERIMENTAL: amAneaptloyhrstyiiseoonnyzofeNtnMheRe.(saHmAEpXl4e)0.0waMnsidsectchHuernNsetMoltyaRlwleysispgeohceltdvr,oesmdpiaknineddd3ew7ui6tteMhraaitkzedn7oswFcn-iNaoVnmRo(usspncoetficoi-nbw)iesrf(ourfslruoberseodq-utentroom p{eemrpmeirtseutteheuspi-nHgFXVatroibaenuUsNdTTasYcphlesr401)0 FFTU-N"MFR-NsMpeRctiommeatelr.stTahnidsarsda1m0plaellroewpnaeseisolnulmaettiohnodofthe absolut weight percent concentrations ofspecif component, o 2a PF-NMR eros tegration - osvtearnadlalrdsatmoppleermciotmpthoesiciroons.s correlationofthe relative 'H and "F signal intensities for evaluationofthe RESULTS: TCphrooemdpu'ocnH,e-nCNtFMssRw(CeanFrdai"sCoFO-asN,sMiRgwnsepde.hctArtaeh'leHadvJarteParFaei.gndNeiMcvaaRltecdrotohfsistsc=agm6pa.l9i5eo5w.nasSnmaaalhlligsmhopcuuhrninttsiy qfofouramwooafswthsiemhpnuourmsiitenydatlo +... qCanuaaalnylsiiaestaihevesceuoammpmtoaisrinitziweoendiagblhetcluaolwctisntThaActBawLeEnr-ec1dierToihvneedorfefelraotmivteeewesiidgnhtglpercraoclemnptFocorFntc.eNntMrTaRhteiaognrsussashntoiewngnreaitn2i2don TM TRprAMeBsRLeEns-pie1ncttsrhhae,osublaudmtpbaleedvdeTrorynaccsleoswaeomrtookuntwhtoesiuorlfrdeasbpefeocntievtdehaedbssonulanuantsessiwgoenitegdh0Ctoepmenrpciaenrytevosarlwqueeussaanasssduomhdisnegemeoiodwnaeiterwas. components a(CnoypiqeusesotfitohnesNabMouRtsthepse reeasrueclasa,tcplease wlittrithknpoawp.ercopy ofthis reportforyourefernce. you have ) Bact Co ofOp rigiy nal- Loe iofson Initia) Dats | Paget of2 000271 Page 178 0f 225 i ran 3M ENVIRONMENTAL LABORATORY SSDD A ilRBeennGER rJamR . "TomKestner AAAs i Samp TCE618,LorTbARBBRLsEo Terr fe. : ee OvCeriaCllCoEmpoOsitRieosunltaslby| 'H/F-G NMRCSroo ssaIntew grwatiaonreAn n:aelycsims seei" o| . `Probable H-(CF2)s-COH ae e ms eaae `Probable CF(CF2),-CO;CH;| 0.65% h: g To aspossible To_o* t*s Te oe otsimilar So ee PossiblCeHy,.;saturatedaliphatichydrocarbons srr |_______0014%| `ExactCopy ofOriginal lnc oi3)m Intel "pgp pact ] co0Z72 Page 179 of 225 : aM Emote.LiEsooerioorsys Certificateof Analysis . Nominal ProdHucet:ptCFi;e(cCFo)r,o-CoOnH,awnhaiecrciedaveragen=7 : ProductCodes TCR.S18, LotH1568 Outer28,2002 TomKester : "ThsheesysecasommpglbeiuonafedTasCnRa.-ly6s1Te8os,soleotvsHue7m5c6m8uawlarasitabnzeealelooyddwzeQidnuTsuiAngBaiLcE1omcboimnaptoisoinoonflFe-nNtMsRdhawnd "eH-ANMsRspectral . Sample:TaCRSn1Se,Lo 756s CQuoamnptointeanttivSeevCoemprossitional Resultsby CombinedRe'lFi/v'eHW-eNiMHgRhEtSpRecCVtroaEnlcAennalayisoenss bb ee wheHremCerEagrC6o9n5e 5 ae nRgPiuarllassei sFoiPnrtobeeabfleCoC{aCcEtF)iCoCnOOCMp,ups Ew : hereaheaeaygelnen6th5er5 L# G+ : Toaashpeoocsshridbileneg Tsmeo* pooTsoeertsHtiEmilsar ST i "ProbableC,H. saturatedaliphatichydrocarbons -- ECRoCca,pCo rE y tsar Dis | Page ofl } FileReference: CofA_TCR-618_Lot H7568.doc. 000273 Page 180 of225 IM ElmmoumenTa:Lag`oEroaztT1O0R3Y9 Tost Control and Reference Substance Log - [ToooTsmvennaasmimesom Reese ESE TER SETRO TCR wo - f[iomaA n TRTose Reco Garnd ProduTce4t80s. oT 5 ST - fis v Toor TY } ECaosaene So WERT OSGT vow -. ArchivediSubstance Not Avaliable | aPords ee SSODTS,,Cp orOofw TAerEtliOsK Nd ARGs eacont ootasyo mneon-- Unk - [58 eesvovsirge-- TFFagan - [Commas SSTtIiaAnaZdaArrSdthwaepssebsroosrnTmsotvDreodo1JmCFtPraeEmpsraTsu19r1niroorm 4o71o0.08L0AG8.0124900 ] sdb3omsdspe sages pot : EatCony ofoo CC E r sel2ifon 000274 Page 181 of 225 i 3M ERVIRONMENTAL LAB0O2R.A1T0O3R9Y - 3MSPECIALTY MATERIALS MANUFACTURING DIVISION ANALYTICAL LABORATORY To Lisa Stevenson -(-5569) - ETRSS -236.09 Request # GID:71638 - From TomKestner- (+5633) - SMMD AnalyticalLab - 236.28-11 Sublect; CharacterizationofSDU36 by 'H-NVIR and "F-NMR Spectroscopy - Dae: Octo28b, 2e00r2 - S= AMDP03L6E,DlEotSRCIRIIKPfToImONt:heTelopmroejecrt. feNe ominal |proSd=eu7 CceFt(mCsFy).-E E CO.H, wherew average n (e whiteT powder)n . -- ] - [SDT | TIGR IDE|400VtFIRi eon solvent HE cr gm | OBJECTIVE: - `pTuhriistysaompUflhe wnoamsisnuabljepcrtoedductto.aScpoemcbiianlaetmipohnaosfis"Hwa-sNaMiRsoalnadcFed-oNnMaRttesmpepcttirnagl tanaildyensteisftyo0ddetqeuramnitniefytahney. impurity components. - EXPERIMENTAL: Ameptohrytliooenonfzetnhee s(a5m-pHle),waasndactchuernatteoltyalwleyidgihsesdo,lvsepdikienddewuittehraatkendoawcentoanmeo(uanctetoofn1e,d-eb)ifso(risfulbvsreoq-uent _ a"noaolymsitsembpyeNstMuRr.e uAsing00aMVaHrzian'UHN-INTMYRpisupesc4t0r0umFaTn-dNaMI3R76spMeHctzromPeFte.rN.MTRhisspseacmtprluempwreerpearoaqtuiiornemdeatthod pabesromliuttiecdwetiheghpt-pHeFrXce1n0t bceonucesndtraasticotnshoef1s)peac`iFfiJccFo-mNpoMnRenitnst,eronral2s)tanHd/ar'd Fto-NaMllRowctrhoesscailnctuelgartaitoinonofthe - sotvaenrdaalrdsa0mppleermciotmptohsitciroons.s correlationofthe relative 'H and "UF signal intensities or evaluationofthe RESULTS: : "nTohmein'aHl:NprMoRd.uactn,dC1FyN(CMFaR) CspOe3ctHr,alwdhaetreitnhdeicaavteedratgiesvaslaumeploefs=sa7.8r5e.latSimveallyhiamgohupunrtistyoforfmeowfitmphuerity 2 `tceocmhpnoinqeunetws,asinhceiunduisneg ptroobacballeciulsaotmeetrhse,rewlartievealwseoiagshstigpneerdc.entAc'onHceFnt-rNatMioRnscorfotshseinitdeegnrtaitfiioendanalysis . +... `"oRmpUonEeNniMs.R rThoesquialritaativne anndaquayntiatartiuvemcmoamproesidtiboenallowreisnulTtAstBhLaEtw-eLre Tdheerilveadtifvreomwetiheghstinpgleentital . caosnscuemnitnragtnioownastserhowawsinpTreAsBeLnE-in1thsehosaumlpdleb.e veTrryaceosameotuonttseiofraesnpuemcteirvoeuasbooltuhetreuwneaisgshitgpneerdccenotmpvoalnueensts worerqeuasnliofdyetseocmteeodfitnhtehsee "otFh-erNMcoRmpsopnecetnrtusm, but additional work would be needed in an effort 0 identify (aCnopyiqeuseosfttiohnesNabMoRu sthespe reaseueltsc,alcethsesd wleitthmethekapawp.er copy oftis reptfoyour efecence. Ifyou have. } ExCopay ofcrgitna WaC lag pay : Pass of2 0027S } Page 1820225 Sw Emons iswamsrsony P---- AT aaems4 ROS : Tons - g2r. er ARR FOREN.T.oe.sSETA teti eames - OveralClompositionalResults by 'H/'"F-NMRCross IntegrationAnalysis - CF3(CFaw-COzH 98.01% Ro `Probable CFy(CF2),-CF(CF;HCF2),COH 141% , fa roe 1| w= Probable (CFo)-CF-(CFa)eCO:H T 036% smemf3 8rrctnionopues So A aN . su eo28r5 lcon upon r TT r EYS-- rT TE atcopa . Liga [>] [) | Page2of2 : 000276 . Page 183 0f 225 i COD FRONTS Faxis03-TI-E8T en BH REOURT VESoI-N0S3t o - } ) . ~ . O1WFea7s6ktr0wC18oo4lo0oDuumdbrEmiPb3ara8eoS0dB0uoCcadtIs, Inc. ferry CERTIFICATE OF ANALYSIS Date: TE Material: CasNos LotNo: Nonadecafluorodecanaocicd [35762] RIK Assay: Products morevolatilethanPerfluorodecancicsicd <1% Perfluorodecaonic acid 98% min. Products lessvolatilethan Perfluorodecanaccicd <% Appearance: White solid Melting Point: 83.85C : Ur`EuxactCopyogfaOrigtinael a Dato Vo - (YuumteiyYz fart || 27 Page 183467225 mein --- S ETEEEE iE = Sa XT EctCoof Oryginal 2 A i/o ital' Dats 000278 Page 186 0f 225 aM EwamcmenTasLasTcmraiToomsy i Fete 50 . SINGLE COMPONENT PREPARATION LOG oue_2lelos Bote, _oz0z2 says Mu4) . omarion __LLEPA 5 foc sean SD 274 : voeuss __[02 ng Cnn" 0 5, . comenawoire [01:n0y sano 2/5/ [r-- We [--_-- Wonbor AteMoca[=THEA 205 reve [00] resconnton__[ 000pan sontoJocrd fsltoron__ someone 116 lb i 5 Bact Car . ne. offen wrplod glo lo- 179 Page J#70225 IM EmviRoNmENTAL LABoOzRA1T0OR9Y Tost Control and Reference Substanca Log [ Em pro -------- o] a ree ww foirmeer i0i)) Sr Rest owo e n i fre as IE ox E aoies ram Se ---- i -------- YL ---- a) ArchivediSubstanceSNoot ARvSallabla oe Co sry oCwsawreiedsoofdnianiLAS01502 f[aecCvo:aon aeesan [aam Trp, TOREoT iar Fomets--TGTWFEIOFCor Tal Sa 03 5 G53 rh ay cin| = ct coofpOryga : a a" y 00280 Page 188 of 225 I EnviRONMENTAL Las`oE0Rza.T1O0R39Y . 3M SPECIALTY MATERIALS MANUFACTURING DIVISION ANALYTICAL LABORATORY T Lisa Stevenson - (8-5568) ETASS ~2.36.09 Request # GID:TI638 Fom Tom Kestner- (35635) - SMMD Analytical Lib- 2362811 Subst CharacterizationofTCR-61by9 "H-NMR and "F-NMR Spectroscopy - Dae October 29,2002 - `+SAMTPLECRDE.Sl6CRt1IU9PLIT,NIfOoNm:the Telomeeprojet. Nominal prod=uct CF(CFy)- COS, where average n 9 (whitpowder). - [[CTeReIT| TP7O1T63 OGIIDD.A0G1S|30760Mt"APNERineetsne.mednh+pHeFFcosapgaairl | : , Op"TuBhriJstEysoCafmTpIhlVeewEna:osmisnuabljepcrtoedductto. &cSopmecbiianlaetmipohnaosfHis -wasNalMsaonRpdlac"eFd-oNnMiR spee ctraltm aonadleysnpeisftyoadlnedtqerumi ainnteittn yhaeny impurity companents. : EApXoPrtEiRoInoMfEtNheTAsaLm:ple was accurately weighed, spiked with aknow amountof 1-bis(ifuoro- - oliyonsmyiltsebmeopnyzrNeanMteRur.(eHuAE4Xs0)0&i,MVaniHndagtnh"eUHnN-tINotTMaYRlpylsudsisps4o0le0veFdcnTidn-tdNa3eMrv7Ri6ussMpeiHmdrozsmec"toEen-r.eNMaTRehlsiopnesceat-mr4pul)mepfwroeerrpsearuaacbtqisuoenimraeeatdthod . pSShesruamluinttcetwdtoephiagehprtr-apHeFrtXcheen0ctbrcoesosuncocms3eelnaetititordhneoaofft1)sihpe3oreFneUcslacFt-ioNvHMemIaRnpidnotUeFsomrasl,2i)gsntaaalnJdiar"dn10taFlelofwnc-orrhosvesacNshiaialntttuMielgoiarniaoRioefonntsohfethe ovecll sample composition. _ "RTEheSU"LHTNSM:R and FNM special data indice tis siwmas paeatliveely Nigh purtyformofhe - nCcoamhminpaaalinperwo,dsuicnttc,hleuCndFui(snCgFp.rfo)ob-caCbaOlle3Hslo,emtwerhhse,rewlteahrieevaeavlWesreoalaggsehitvgapaleeurdce.eonftAnc.'o=n/c$e3nFt.-raNtSMimoRanlsclorfaostmshoeuinnittdesegnrotaitfaiioeffndeawnailmypsuirsity . +. ccSooUnmcpPeoRnntRernAattMsi.RonrsThsoehsoqwumanleiitnaaTtiAvteBaaLndmEqyusahnotsuileadibsveeovcoetmypaolsoidtsiboonealtlohweeiilnrTssApBteLhaiEt.vw1e,aebTsdoeelruritveetwdefeiogmhweptiehrgechsetinnptgelvrecaetlniatsl wSeerteuaiinsg ndeotweactteedwistepisFNentMiRn thspescatmrpulme,.bTurtaacedmoduiwnoorifknwouomunelrdolbues noetehdreduinnasasnigenefd cfo0mpooennretnfttys } or quantify soofmtheese ober components SCorpyiqeuseostfitohnesNabMouRt tshespe raeerels,ctspcliheaesdeweithmethkpaawp.ercopy of is reportfo your refer. Ifyou have . - ECa oyofOt inal AX json _ pet oz intel pate } 000281 Page 189 0225 ; October 20,2002 IM EmvROMMENTAL Las`oEoRzA:T1O0R39Y TIMCSRM,MLDoAt rUa1l:]TeLalboRsequPreosjtectGIDTI638 : Tom Kestner - prwRoakneon Vimhgn Fe mek GITOTrR esPI re - Sample: TCR.619,LotTUALIBNLfEomtheTelomerproject Overall CompositReisotns!by Hy *F-NMR CrossIntegration Analysis Component Structures NMR Re(slingaleivetaWleimegahsutreCmoenncte)nraions I PE - : Probable internal branched isomers. 26% (wher xP2r0osbCnaFdbyla(estCsrFuan3msxe)--yolCe=Ff6n(.s6C)ofFfygoeHnaCecrCFuaalOa)ft,Hoiromn: purposes 0H F(osssssbtulrmcaentexsry-mCiF=n6(a.lC6Fi3ssf)opyor-ocCpaFyll=cCublrEaa-tn(icCohFneC2dO)pui,rsp-oosemse)rs oT - (sssume(nC=F6.s6))-CfoFr-c{aClFual)ai-oCnOHpurposes) FrobabCulHelye saturatedaliphatic hydrocarbons |__0_ 0%__| - Tac i Svar cht sodone re 100Ged FRpecR - actCopyof ogeat oh sip Ital Date Pisco - - vids Page 190 0225 ) 3M EXVIROMENTALLABO0R2A-T1O0R3Y9 Certificate of Analysis - Nominal Product, CF(CFah OSH, whereaverage n= Perluoroundscanacicd `Product Code: TOR.G19, Lot ULIN, October 29,2002 "aTnhaelyssaimsptleechonfiqTuCeRs.-6T1h9e,olvoetrUaIlIqNuawlaitsaatnivaelyazneddquusainntgitaaticvoemcboimnpaotsiiotnioonfa"lFr-esNuVltIsRtahntdw'eHre-NdMerRisvpeedctfrraolm these combined analyses arc summarized belowinTABLE-L. . . . Sample: TTACBRL.E6Lot1U9LI,N OverallCompositReisuoltnssby ComFb/iHNnMReSpedctralAnalyses "ComponentStructures Relative WeHighNt?MCoRncentrations single tialana Proba(bwlheeirneteravnearlagberanc=h8e.d63fsomers Pari . - (whe xs CnFd,a(sCsF.u)mx-eyCF=(6C.F63;f)o-r(cCClFOae)sa, n purposes) Prraonbsa.bClFeytr(aCnsE-:ol)ef-iCasFo-fCgeFn-er(aCl FfOo)sr,m: 05% > assume xy =6.63forcalculation purpo Possible terminal isopropyl branched isomers oi assum(eCnF=)6.-6CfFo{r cCaFlculaCtiOonMpurposes) - "Tota Inorganic Nworide 300017% Toc ein sumer chrvn gnd ponents we10God ENRspeci *-. TomKester - _ BactCoofpOrigyin Qe lotta paty - Paseo Fl Refase: Co TCRL6otU11No9e 000283 Page 191 0225 IM ENOARONMENTAL LABORATORY Oakwood Products, Inc. : - WP1e7h4sa1tneOClo(dl30uD3m)ub7ni3ba3,a5rS5C0R0o9a1d72 f i]5 - Fax (803) 739-6957 * i - CERTIFICATE OF ANALYSIS .. - Date: 15Jul02 } Material: Perfluoroundecancic acid i 5d CatNo: 2265 i : CasNo: [4234235] - LotNo: UMN - Assay: 994% by NaOH titration i =1 ad - Appesmances | White solid - Melting Point: 92.98C hy. | atcmrooge me wale - :3 QC Managr 00284 o i : Page 192 of 225 - IM ENVIRONMENTALLAB`OERA0T2O1R0Y - 1 AGRE | Ri ats --- = |E wSieinss||ravssiormvo)|| HE iaiort rosin ono BTe R[5 |=] . dctCoofOprgiynal QU ga) - Initia) Dato. - 000285 _ Page 193 0f 225 } IM EiwmonmENTALLagBoReATiORsY ) ou 9/33/01 SINGLE COMPONENT PREPARATION LOG [ Pusan.--88 sours Lurn). - Description: Lee Aliecsundecrea: c did Sooktmonr__ TLR =C1D - 2 0220 aaca0__979) | ey Sonceatration or NA _ Comcswagn__0:0670 `Other ComTecotcioon NF [-- Noroolal[TrHM-,A_LbTd Y FovompeuJ____ FelConanTLtpaorenr_/2 soo2unnd[turolmleTiinny Ooincwn_24a/07 `ECoxpyoafOrcigitnal - Lue i/o tal ) nemmsor (OyB, Slutnion folks - 000286 Page 194 of 225 ) IM EvvROMMENTALLas`cEroazT.1O0R3Y9 Test Control and Reference Substance Log [me Sarncce veas me Farmar RSET id wr wa Sir E [CrIieOrV Fae Fr Joaood Prodac oe [a So frmssor1i22 pe bo 4 x LL-- -- - CL) I) Tow 10) ArchivediSubstance Not Available | - Cr ---- -- - [eercsono amon . or . | SSliaCnacar8rawhaoissSboeoornemGov9oeod1mJEtFP rmepOsUeaRaru1r9 nproiorm 1078044D050.6L0A8C01241900 SPipint gcomments: tanonspi,n form-ashtipai3somanllquayaxcpdon. rr] sd3Tmadpsdf s0037cofpaot NMRSDOST ot . Brat CopyofOgos MtCa dDaona 000287 Page 195 0f225 ) . SH EvvmomenaL LasEoomaarroom%y . 3M SPECIALTY MATERIALS MANUFACTURING DIVISION ANALYTICAL LABORATORY To Lisa Stevenson - (8-- E5T&S6S 2835.)09 Request GID:TIER8 Erom: "Tom Ke-s(3-t 5633n ) -e SMMrD Analytical Lab - 236-2B-11 Subject: Characterizationof SDO37 by "H-NMR and "F-NMR Spectroscopy . Du Ocaber2s, 202 . SA= M5PNDoL-m0iE3n7Da,lEbSpotCrRRo2I4dP=KuTIcfrOtoNmt:(hCFe)TCeoOme,rpwrohjeercte.average 10 (wit powder). 3 [S007 TeOD 20 le NE ete g ve o rs at| tioe/internalsud. . O"pTBhuiJsrEsoiCafmTtpIlyeVeEwn:aomsisnuabljepcrtoedductto.aScpoemcbiisnlaetmipohnaosfHis-wNasMR50apnldic"eFd:oNnMtRemsppetcitnrga anadlyesnesyoadndeqturainte thney Spuriycomponents, : EXPERIMENTAL: mAeptoyrpioennozfenthse (saHmFpl)e,waasnsdcctuhrnateoltaylwleyidgihsesdo,lvsepdikineddweittherksnoswecntaomno(unsttoofn1e-di(fiorfsluubrseoq-uent anbyy NMsR. A 400Miz H-NMRspecu snd 376Miz NMI spermwereacquiredat coom temperature usaiVanrigan UNITYplus 400 FT-NMR spectrometer. This sample preparation method. permitted the p-HFX to be usedaseither 1) a 'H/'*F-NMR intemal standard to allow the calculaotfitohne - S`oavtbeasrnoadllaulrtedsaw0mepiplgeehtrcpomemirphcoteesnicttrcioosonsncceontnrlaattiioonsnofospfreecilfiac cvompeone4nntdsF, or2si)gnaal'nH/e''sF-sNMRfocrreosvsailntuegarotatfiioohnne RESULTS: " The "H-NMR and "F-NMR spectral data indicated this sample was a high purity formofthe nominal p{Crooomdphuocnnte,enCtFws3,e(siCnFh2ce)h,i-wnCgOa;pHrt,oobwcahbaellreceslotthmeehraesv,errweaeglreievvaeallWsueeiaogshsftnigp=neerd1c.0e.n0tA4c2.oFnSmFsa-lelNnaMtmRosuconrftotsshosfenaedgefrieafwtiiioemndpusriyty s components. Th qualitativesndquiniaive compositional results het were derived from he single ial co"nHce/nFtr-aNtMioRnscrsohssawinnteignrTatAiBoLnEan-a1lyssihsoaudebsumvmearryilzeod bteoltohweeineTsApBeLcEt-i1v.baTohleterelwaetiigvhetwepiegrhctepevracleunets - `h1aeassseudmeoittnehgsetrneocdowimanpttoehrneewNnatMssRpresspeenctti,n tbhuetsaadmdplieo.nsTlrwaocerkamwoouunltdsboeafnefeewdotnhaernunsafsstig0need ncotmpionoernQtusanwietrye . aConpyiqeuseosftitohnesNsbMouRt stphescetrraeasruelta,ttpalcehsedeweitthmetheknpaopwer copyofthis reportforyourreference.Ifyou have - Exact Co ofOp rigiynal Lal tal - Pagel of2 000288 Page 196 of 225 IM ENVIRONMENTAL LABORATORY i `Sample: SD037, Lot R24K fromthe Telomerproject. = nae - Overall Compositional Results by 'H/\"F-NMR Cross IntegrationAnalysis Possible CF;(CF2)-CF(CF:)-(CF2),-COH Probable chlorinated impurity, CI-CF:CFx-Ry, E onE CC Tole Too - ExCopay ofcrgital nl lun _ Inltal Dats Page20f2 000289 Page 197 0f 225 IM ENVIRONMENTAL LasoraTORY Certificate of Analysis SS - ProductCode:SD037, Lot R24K. i re "The sampleof SDO37, lot R2 was4 analyKzed usaciombinnatgionof"F-NMR and "H-NMR spectral EC a ae 4 Quantitative Compositional Results by Combined "'F/'H-NMRSpectral Ana Possible CF(CF2)-CF(CF)-(CCFaO)H, 0.088% eeen oo - CC Toeme 1 _oois% | one - taldle - Page of} File Reference: CofA_SD037_LotR24Kdoc: 000290 Page 198 0f225 CRED PRODUCTS FRR0TTISEE? re mss Ligon 3 O7a4l1w0o4aDudnbParrodBuocntds,Inc. - WPFehaoxtn4Ce0a09tu7)m3b55.i6n09,547C0172 '- . CERTIFICATE OF ANALYSIS i Date 1LFeb00 Material: Perfluorododecanaoiled i CatNo: 2266 LotNo: R2K Assay: PPerloudourcotdsomdoercevaonliactilceitdhanPecfluorododecanaoci9cd6%m<i2n%, . Productslessvolatile thinPerluorododecanacicd <2% o. Appesance: Whitesolid MeltingPoin: 107-108C . fuumaelliYtsy Clitol BatConyof Orgad coonwraaioees e 000291 Page 19907225 ) . aw Eivmomenna.LisEoomearroosnsy - 5hCoRmeEsrca wwe - siaTrveeonrms|||iewnvmsn|| dine|aestss ra HHEE [@57s2g_Jooreeg lazassey wnsadozososs Bie FJRWw Josmsmooz | ExactCopyofOriginal 3 QCon ain 000292 Page 200 0225 ) IW EnvroMENTALLoREoArT1O0R0Y0 . SINGLECOMPONENT PREPARATION LOG . ome B/29/p2. wae fwn) BPoaogkaeo.. _0525040 - Description: Load, pce doidhcies o Ae - Cobozlootd ~~ Socktumsoe__S) 0 77 - gorVe. 2 O%Fs `Balance 1D: 904 . po Concentration or Np To, OtherComction NA Commas O IZSy SovanNtoraonotr LT;oll=THK ttyy Feavoume:____s. FoalConsaton__// 20 yo pun Sogotocaton: Zug) [lo=ofnu Teg Exmtoncun__R fio [0.7 . act opy ofOat Cone wpe ntl Date. Reviewedby Ya. A Shoe jol)s2 00293 Page 201 of225 ) . IW EvmoneNTAL LasEoomra1T0o5n%y Tost Control and Referance Substance Log r iE ss s cv hores pros Fama Pause crs [TOR FEl . ffraome: r Soroon ras ec Ew iv srr ff RIraSormemsep rs3egas co e Soa eskoaones . ion ip WORE JOS vow - F(a ArchivediSubatancewNoTtAvaiolabie | esas [OrwoRoiRnfoet aaprrromC?esFaEnSCSrNeGtOSeFIoDfACnRisE.LAC 42501 - ae doen ws - (WSoetrocFsorsmess Coens FCEaF vrrioesnCooYCaenTay Tora TET PUR TRS Sovheiiarirowcaoes bsstooornraegdevah(er0od2o)mFoarmep5e1ar6r51u00rLoAroCim0r2014G67S00H0E0R00:00L6A3C0 1243150 } |SRihnEignGECCRooOTmsm:oAaes:SS0O0ah0regMuEaoSuSmsogso3o3ds0o0n0naesreoy9pfcaoadmLpaAlCeCGonAooYfmCyyise.8 NLGAOCS.ONGO2 | + psa I 7 sdOiBmsdssl| sc0tEnMIES00p scOTBAMTECEIS5T0 - 0.1682 ItaBorpros es . ECoc py Ot rgy wx lag tal" Dety 000294 Page 202 of 225 ) IM EinamowEnTAL LisEooreaT1o0R%Y Ce30n6tRerseeAarnDailoytSiacteaCollogLe,aPAboT9r80a1 torviaemsca.naIanbcic.o - e Phone: (614)201.8032 Far(014)2o3r(131.4)12321-515380 ) INTERIM CERTIRFosIiCsiAo3TnE OFANALYSIS Centre Analytica3lMLaPbroordautcotr:iePsFCOOS,ALRoetfe2r1e7nce #: 023-0184 Reference #: SD-018 - Purity: 86.9% (1 oir ] Ew TeenueaNtMoRn - VE 1 CCPalSu)m 1 000mm . 23.. MSoadginuemsium 23 0L040319wweinmt 45&.. PNtiooctnkaeslsium' 456.. 6<0..0800400951wwiwtr/twti%h - 7. Manganese 7._<0.001 whe : Zz | jam . "Twaomrs.)fray NoreDeed Gos) - |PRFOeAsdAvarSolvem (IGA)|| [oNe03nm3cwDienwmseed s|| . [PorpgbaTrnyicCDhAlSonriCiodne_s (C) | | Nouphmbe | 1 001s wna 25.. FBlruoomriiddee 23. C00590wwtwm% 5. NPihovpehae || 7. Safe 55 o wosrun|| 353] 7 sist| S - [[om Orga2nicpArciedsa" (IC) 2Lo0r1wmaann | 33 1 J 3 NFERPAA | +3 0o2l8owweanan | 8 Them1eraClarArbaoln 1 TheorVaeluei=e1a7.6l% L 124swins - | | 233. HNaiyrdorgoegnen 23 TThhTeeooerreoettwiicciaalllVVVaallauueee ==o00s%%om | 243. 0BL24a4hwaiems% - 5. Fluorine 5. Theowtal Valvemath | 5. Shlwim% conmoita 600295 Page tof3 Page 203 of 225 i aM EfvmonmenTaL Las0o2r-a1T0o3n9y Ce30n98tRreseeaArcnh aOlveytiScaalColLEge,aPbA oT0r80a1 torWiwceonsio,labIneca.r : fe Phone. 814)231.8032 Fa (814) 201o-(6116)2201512380 INTERIM CERTIRFevIisCioAnT3E OFANALYSIS Centre Analytical Laboratories COA Referenc#e: 023-0184 Dateof Last Analysis: 0831/00 Expiration Date: 08131106 : Storage Conditions:Frozen 10C Re-assessment Date: 08/31/06 "Purity = 100% - (sumofmetal impurities, 1.45% +LC/MS impurities, 8.41%+Inorganic Fluoride, 0.59% +NMR impurities, 1.905% organic acid impurities, 0.38%+POAA, : 033%) Purity = 100% 13.=0876.9%% `Total impurity from all tests = 13.07% Potassium is expected in this salt form and is therefore not considered an impurity. . oPbusreirtvyebdyfoDrStChisissagmepnleer.ally not applicable to materialsof lowpurity. No endotherm was. - "iSnuolrfguarniicnatnhieosnammeptlheoadpcpoenadristitoonbse. cTohnveesriteodntoreSsuOltaangrdeheesnwceelldewtietchtehdeussiunlfgutrhe - odnettehremriensautlito,n tihnethSe eOliesmneonttcaloananlyssisi,adleienmdpirungreictodyn.fidence to this interpretation. Based "EA Trflorosceic cid . HFBA Heptafluorobutyric acid z &d NPFFPPAA NPeonntaafflluvoorrooppernotpaannociicc acciidd 32g - Theoretical value calculations based on the empirical formula, CyF17SO;K (MW=538) 3 if "This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). conomasa . 000296 Paezor3 Page 204 0225 : aM Efvmonwena, LoCraoTroiroY C5e57n8tRerseearchAnOavalytSiiceaCollegLe,aPbA oT6r80a1 tor--i_veinsic,eniaIlnabcio.om ' Phone: (614) 201-8032 Fax (814) 201-1or2(85143) 231-1580 INTERIM CERTIRFevIiCsiAo3TnE OFANALYSIS Centre Analytical Laboratories COA Reference #: 023-0184 ) LC/MS Purity Profile: CC a epmy [ wewwmem e ew w am oa mw fem [mat CNio0rt0vee:OsF,TrsheaesnpCedciatriadvnelcduyr.Cv6esT.vhaelLuCiek5sewwviaeslreu,ectwahlaecsuClc7aatlvecadullsuaeitenwdagsutshicenagCltu#hleaaatnveddeCru6asgisentgarentsdhuaelrtadvfcerarolaimgbertahrteeisCounl4t {rom the C5 and CS standard curves, Prepared By: LCharhles Si Som sDoatfeter 28J Scientist, Centre Analytical Laboratories g Je 29 | iI - Reviewed By: 7 lth Flaherty Date `Laboratory Manager, Centre Analytical Laboratories. } connotea 000297 Page3or3 Page 205 0f 225 : IM EmvRonwENTALLis0o2R.A1T0o3R9Y Fcoasss Patorcacane Sulonte FG33 wwe i Sore . gm | |oownircdoaodw0s ||Iasanscoc0)2||swhidaonwsa oe [I ass oh vz[5 LECoprygo - aCn7e] gan oa } 10298 Page 206 of225 _ aM EwvmonmenTALLaesrooos SINGLE COMPONENT PREPARATION L0G owe: __ ps BackNo. _02022 - soose__ Lag) PageNo. -- 56 - ouster LE05 sheild Socktunsne_ 50.015 [r-- Uses: -- Purty: ZS 2 20.9 Pe - Cormected Weight 52. 15mg `Balance ID: gry Or oracton Fackors: _0, $225 [--. Numoer. _/2, ok, 7 WA-otory Foavane___ 5.) FoCornion__J lf gn `Storage Location: Rie - `ExpirationDate: les [or toorfroyt waCine "G Reviewedby: ah Sletten LIPTAY 000299 Page 207 of 225 - `3M ENVIRONMENTAL LABO0R2A-T10O3R9Y ees---------------- ATTACHMENT E: PROTOCOLAND AMENDMENT 000300 Page 208 of 225 - IM ENVIRONMENTAL LaB`OER0AT2O1R0Y - . - ~-. - . STUDY PROTOCOL STUDY TITLE AnalysisofEndogenous Fuorocheicals in Normal PooledHumanSerum and Plasma SPONSOR William K. Reagen, PhD DATA REQUIREMENT "0CrRPa 702 TESTING FACILITY 3M EnvBiuriolndimnegnt2a.l35L.a0b9oratory S9t3P5auBlu,sMh NAv5e5n10e6 LABORATORY STUDY IDENTIFICATION 3M Environmenial Study Number E02-1039 NUMBER OF PAGES 0 Ect Cooyf Orginal ntec daGegn , 000301 Page 209 0 225 - - Jos ttn Parnas aM Enron LiAsomrYony waren - Anta of Eadagons soSTcUiDYaIlDENTNIoFrmIaClAFTIlOdN Huma Sern 1d Plas - sronson Wiliam Rese, Ph.D. - S533Mp5 aEBulnshMaANmve5en5e1l,06BLaubolranto3ry.95.09 Ess - SruorDmecron Marke. Bion 3M Enionmental Laborsory } - ES53s5PtBuAashsNAivoesn$u5e1,0B8ulding 2.35.09 TestFacury . S5SUPM5MEBmuihNonAmveen5t5ea1,l0B8Laalbdorisntgo2ry.05:09 : ProrasesSrv Twerasis - EExxppeerriimmeennttaall TSueamniDnaaieon Date 0110 NOsotvears1022002 [-- 00302 BtCopy ofOrga Loc, fa. Page 2100f225 . _ Anofs Endy ogens cus Flucrochamicais Emcee ispomorodny : 0210 40 ootiwtePteripeors - 11 JTPihrienpsotosbaefebteinsmund LiitoiCamhidtoypnreotceancioetneeedC10, oehasyri(pnHPshFos,soatCs1fl0,mipsrnliCerHadsEoFdssSteneor(1pPl0a5Cp)1e2mu)arssdacapneeed a Pee ng pm ty foc oe pESe 20 Reguistory Compliance - : 2.1 e Te Rtens This study will be conducted in accordance with the United End States Environmental . 50 Tousubmsmee } 31 ePreltirmionaorynsameriaio)iinosumsnahpgotoeoepccopomripootessatgcgdnleo.wcorrnetpnore ores company nn ) [oTossw ubstancee s Tm] - i: . - ) . rons reign ExactCopy of Original Initial [5] pnsato ] 000303 Page 211 0225 _ _ Si tttPrams aM ExmmomwEnTAL LsoERoeAeTrOoRsY cen 40 ReferenceSubstances [Em Tow [oolon [mao] om Roforanc Substances - [TFoerShesrtaan| v enor|renon| ig [chCeorrn[vor| ca, rome| - [[EFFTmaeomatiraneare[|oorrooor[[ornoann [|Gaoooen|| Gdwv8ie,[[mooomn[[roronrmt|| |Eaoe rpsE ietces: [EwEon[rRE oEnon|GEE5re TommE saa|Eany| ivonn| - |eCPu, tTeri [|enccmoonm[|enreonoroemornm||||gSSGoootomne||[c0o0o[ooonm|[ advpo sis| - Tana " } |SsTupEairnEtee|| vor [rome curios | Toner [orT aze [o [osour|| ogree:| ) Partoamoca=ns | Cu5s0nC = Ju, eaTR TR TT : 50 TetSysen - TestSystems "Sigma Alarch,MiwaukoeW,I : a; ren| bg po aR, ean Cofor Emir ty J 00304 Page212 of225 - ~ oatEr ncsenon Pctencss IM ENVIRONMENTAL LAB0O2R.A1T0O3R9Y cave i TestSvsres Ex Tracessiure : rer[ e [FE E||E ]| EC E C $1 SJuesrtuimfiacantdipolnasomfatchoentteasitnseynstdeomg.enoBuassleedveolsnopfrtehleimtiesntaraynaleystteisn.g, normal pooled - 52 dHadteentofficinaittiiaolnoprfeTpeasrtatSiyosnteems.t sSuambpsletsaosrnltclesebtesyidsetnetmi,fiseadmbpylethneusmtbuedry,nruempbliecra,te number iF applicable), analya(s),andproject leader, 60 Surrogate Matrix . Surrogate Matrix Susmocare tar Source Trucssaury (roms | onesie | wore | = 61 pJuosoilfeidcartaibobni sofertuhmecSounrtraiongsatveerMyalrorwi.endBoagseendouosnlepvreellsiomfintahreytetsetstainnagl,ytneosrmaanld {s hereby suitablefo use 2 surrogate mat. 62 `Idaemnbteirfi,cadtaieonooffnSituiralropgraetpearMaattiroinx,.esStasmupbslteasnscheaolrbesudrreongastiefmiabetydit,hessatmupdlye - number, replicate umber(ifspplicable), analys(s), and projoct leader ) Re 70 Analytical Methods 7.1 EAnnavliyrsoinsmeonfttahleLeasbtoraantdorrye.ferTehneceansaulbyssteasncweisllwiblelcboencdouncdtuecdtaesddienstchreib3edMby 3M ) `EAanvailryosinsmeonftFalluoLraobcohreamtiocraylMCeotmhpodouEnTdS.s5.f2r3o1m,Bi"oSloolgiidcaPlhamsaterEixcetsr"cton and ExactCopy of Orginal i} x lita plpaaion. | Wemcnmenar soy Presario : 000305 Page 213 0f225 . _ Aroratna Perna 3M ENVIRONMENTAL LAB0O2R.A1T0O3R9Y envem 8.0 Data Quality Objectives 81 Absolue Recovery: - S11 Thhuemaanbssoelurtuemraencdovpelraysomfatahnedmreatthsoedruwmi.llFboervcaaclhumeadtis,ephareatsealmypilnes wil bexetrfaocrtiefdiehdoatuwghotlheevemlestohfod(,50a0npdptanaanldyzpepdb)b.ycAolmpaarmipsosn wwiitlhbeextemal ccaalliibbrraattiioonnocfurnvoens-ewixlltbeapctreedpsaarndeadrdisn.meTthhaenrooln,-aexntdiwscitledcosntsainsdtaordf3. - `pmpirnoipmruimneofrnegirenss(i9o)nlweivlellb,einucsleuddinogdeasmcertihbaenohlisblaannkv. (Tfhrebebesstt Sceursacty all eves ofth standard). . 8.12 Tdheeteancicnuerdacay (a9%chrelceovveelr,yn)danfodrparelcilsivoens(cAoCmbYoinfedh.eTsheecroeviesienso)cwoinltloble limi oraccuracy; precision mus be beter than 15% at cah eve, 82 CianlCihbrianteisone:plCaalsimbaraatnidonracburivtessewiul.l beThperceuprvaesfwriolml ceoxntssicstteodfmamtiinismtuanmdaorfds, nanianley(s9i)slseivenlgs tahnedpaeamkaatrieasbolafntkh.e Tahnaelyetqe.uatTihonewaiclclubreacdyoetfeeramcinhedlebvyelrewgirlesbseion - Vreergirfeisesdi.onArneycallecvuellaotuetds,iedexc7e5p %t-he1L2L5%OQofnwohmiicnhamlusmtusbte bweitdiecnt3va0t%edof,noamnidnal. `oAfllfoluerve(l4s)mluesvtelsshaowyabeesdpeoanctsievarteedseirn atnhyanotewisceet,tohattohftshte bwlialnlk.beAreamnaaxlyizmeud.m 83 LdiemtietrsmoifneQduaonrtictaacthiaonna(lyLtOe):TThhelelvoewledreitietrmofiqnuseandstittheatLioLnO(QLmLuOsQt)swhiolwbae chaonvetrwiycewithlaitnof7t5h%e -bl1a2k5.%Tfhoresteheliamniatlsytweisllabneddmeutsetrmsihnoewd durreisnpgotnhsecgoreuartseerof - tdheeacsttiuvdaytaenddidn oacpuamretinctueladr ientt,htehreapwradcattiac.alSlhiomuitldof qthueaLnLiOaQtolnevoelrctaliisbrsaettiwoinlble i bseetawieldbetrtehaenanleyxztedacucelptaqbulaentlietvaetledSianmplsetsibneclluodwintghethperavcatliicdalatLedOLQoLOfQt.hat . `TThhee ulepvpeelrdleitmeirtmoifnqeudan5tittahteiUonL(OUQLOmQs)twsilhlobweadreetceorvmeirnyedwiitnhisner7u5m%an-d1p2l5a%smfao.r ~ tdhoecanuamleynttese.dTinhethseealwimidtastwa.illSbhoeudledtetrhmeiUnLedOdQurlienvgetlhceaclioburrasteioonfsttahensdatruddybeandde-. alcotwievraetdedtion taepearxtticuhliagrhesestt,atchceepprtaacbtliecaelvlelitofquantitation fo his set will be : | Awinllynsaemeple bweitdhilaunteadrenatgretahteerratnhgaeno1f1h0e%ocfaltihbreathiiognhecsutrvaec.ce[p{tsaablmeplsetsand=ard Ey diluted into therangeofthe curve during analyses and enough sample remainsa, Copyof Origa . post-run dilution validation will beperformed to verify sample values. To a rela ntl Data : Ersoy Frmsatro 000306 Page 214 of 225 ) ) J-- IMEnvimonmENTAL Laso0r2a.T10O3R9Y erie : preeprrfeosrenmttathivdeilsutaimonpvlaelisda.titon, n| emLsaamlpilqueowtsilfobresueipdarsataedmipnotlortwewoos 1 gram 2 aprmoocuendtusrefcoonississutesosfamiptlien) gthtehnedsialmutpeldeuwsiitnhg atdwdoitpornoaceldmuraets.iTphrieorfirfsot. eexxttrraaccttiwoint(hssroalvaedndtionsgts-exrta)r,acwhtiiloen t(hmeetsheacnoonldepxrroaccetduardediconngsiasdtdsioofdniallutmientghatnhoel solvent). Itoftdheetevramliuense awrheircohtvwailtuheinis135c%ororfeectacrheportesheenrtaadtdiiotnioofntahl etesstaimnpglweiclolncbeenrterqautiiroend. > 84 UseofConfimnatoryMethods `Confimatorymethods ae typically not needed with LC/MS/MS analysis. ) : 85 DemonstrationofSpecificity 85.1 Trehteenitdieonntitfiimcea,tiboyntohfeancahlayratcetserwiisltlicbepsmuabsrtyantoina,tetdhebychcahrracotmeartiostgircapprhoidcuct i fon, and isomeric proportions (where applicable). 76 Controlof Bias ) Tsuwbostlancee vaonfdembalrtarsicxkfertiitfnihcgataontnisc,ipparteepdarraendagetoKfntohwenmecotnhcoednwtirlatliboenseovfatlhueatfeedstto dbleatnekrsmiwnielrbeecouvenrywintdh c0acehvsaelua(t0eemvaeltuhaotdetpherfloervmelaonfceb.acRkegargoeunntdainndtemrafterreinxces. 9.0 Statistical Methods and Calculations 9.1 Sctaatnisst,icsatlamnedatrhdoddesvifaoriotnhse,anaanlydtrieclaaltirveessutsanwdialrldbdeevliiamtiitoendso(tshsespcparlocpurlsaitci)o.ns of 100 Report ..~ "AThreeproerptorotftwhiel rienscullutdseo,fbuthtensotubdeylwiimliltbeed ptor,etpharefdolblyow3iMng,EnwvhiernonampepnlticaalblLea:boratory. 10.1.1 Name and address ofthe ali performing the study, 10.1.2 Dates upon whichth study ws initised andcompleted - 10.1.3 AexcsteaptteimoennttoofGcooompdlLiiabnocreatboyrythPeraScttuidceySDtiarnedcatrodrsa.ddressing any. Bact CopyofOrginal 10.1.4 A copyofthe protocol, and any amendments and deviations. Qa iofa/n : 10.1.5 Adescriptionofthe methods usetdo conduct the tet(s). The report will ltal pata i Enso tay -- 000307 Page 215 0225 ] rst memo cnn or - `contain updated methods incorporating any changes or improvements. ]} p e olobts TSA SonommepmmermTDk Tr e,R e emn potteis - 10.1.10Statistical methods used to evaluate the data,ifapplicable. - : BE i i Apms etyegyA rwo esnam 10.1.12The locationwhererawdataandthefinalreap reto ober stort ed. i L oSspee em lss obi eef 410. p DsMoEEnnere gLoi iorn aQutlyyirl r Us t ee : fD Tee CRE e i, 20 Leotbisrortsrngmtepr . " 12.1 tpslamntbmie dh e E En Original data or copies thereof, will be available at 3M Environmental 182 THbeebmtdnpdt--erei--wi --t--n 0 Gast,eaaa.e | mri re 000308 03 Page 216 of 225 Ans tng Pssancss IM EvRommENTAL Lag`oEoRzA.T1O0R39Y enon 12:22 Sudy comespondence - 1223 Shipping records 1224 Rawdaa _ 12:25 Approved finalreport original signed copy) 12:26 Electronic copes ofdaa . 12.3 Tinhtehefaorlclhoiwivnegsscupcpoortrindgfiroenc3oMgrdsEnwviilrobnemetnitanldLasbeopraaroatreylySOfPosm: the study oder 12:31 Trainingrecoris 1232 Calbraton records - 1233 Instrumentmaintenancelogs . 12.3.4Standardoperating proceduces, equipment procedurne,d methods. 43.0 Sample Retention 13.1 lAabpoorrattioornyofforthaepreerfieodrenocfepsoutbestsancheasnus2yeedairnstahefserudryewpiolrtbse srueteadi.ned inthe - 132 Smaomnpthlse erxotrmactthsewiimleboefenaalns.and refigeratdforapei ofnot essthanthree ) 14.0 Protocol Amendments and Deviations 14.1 AammeennddmmeennttssasingdneddebvyitahteiSotnusdyothDeiprreocttoocroalnwdillhebeSpiontnhseoroRremproefwsrcitattevne . {`iAnmlenpdromteoncotls. wAllll bhecoansid1neceghdepasreoptaostcolof wthiellpbreotioncdoilcaatneddwiillhebesfintalaredpor(t0.the `DAinryeoctohrerncdhafnlgeedswwiitlhltbheiernotwhedsfso.rmofwriten deviations, signedby the Study 150_ Attachments Nore Sensors samy 000309 `LExacitCeooffOprigiynal ital" Doty fen Page 217 of 225 - 3M EnvRoNvEnTAL La`gEo0RzA.T1O03R9Y AristraPcericss eoaiom . ProtocolSignature Study Director: - Niack E iets . 3M Environmental Laboratory IY Dai: poo Protocol Approval Sponsor: . m Willan K ReageE n, PD--. phd Dai: 3M Environment) Laboratory } i Memon sone act Copy of Orginal LTim ta wO/ a e [er 000310 Page 218 0f 225 - IM ENVIRONMENTAL LAB`cOoRzA.T1O0R39Y AnalysisofEndogenous FuorochemicSatlusdiyn NTiotrlmeal Pooled Human SearndPulasmma - PROTOCOL AMENDMENT NO.1 AOmcteonbdemre3n1t,20D0a2te: 3PMeErnfvoirrmonimnegntLaalbLoarbaotroatroyry . SUP5B3u,5ilBdMuinNsgh2A5-v53e18n-4u049e1000 3M EnviLraonbmoernattaolLraybPorroajtoercytSItduednytiLfIicVaStiAoEn02-1039 - ExactCopy of Origin aaa 5 00311 . Page 219 of 225 ; IM EmvROMENTAL LaB0oR2A1TO0R3Y } Protoc"oAlmHeEn0d-m1en3t111 ) This amendment modifies the following portion(s) of the protocol: . 1ProRpii sowiREthAeaDv cSn:adcSccice oBnoouF1go.h1aL:cThheceshtso,lsae ucsoviyeresydwfibelGlo sotuhir niwlibwhese vxvrstoAfs(bps0rs0tl5yodhf Sna rmi cmsvfe opaindbans, (sT)ihesiml ,s txev ads+oaedfl tbeescdoains Dadgrik.nTcoSve ws ilbePepa EeSmSil,aid icntof : ACtoemnpTaonpnai:edThesiwletirec.ovey fetidwiltbcated erifs der isyeof . Beason;A pledhcg ne sysdition. . 2ij.oPneycRh OiChTAeDeO:PSCaECOT5OdLR: CSavri.n:ThCGoltwbicacraovreswoiileoPprrepna fofoinx9)tceat0ic : "lSiaAmn.iMtT7E0encNhu3DeosnCwiasllletconnno:fCoaaframtiooonnnicvaeufsiewiollp0)opvrelp.dRsefoomnoefxbtecmmactgiorsdaa wnimldes GaooCchsaimoeasi:d erwin, ) Bea aton:r Tosaamr pelceosvwee:eWstsiyexccuesaneidedriaosdba0k,tGootloof hsssandswes. } E2TESPnr3ovr3io5coholsS,RdeabbPosm:eiSEaECyTxTIihOnNscissoAnsndnAwysiiliohsfehonfedteCrdotc3osdemercbsydaIsHeEfwvoiimlbnBercoonngLltabdmoardseory.M3eMhl : i e t2l0ReeEBAesAorisnsdAl a heyctotuosf dPreoctSteocrrsnCobycmapCowEilenoomBvdelodLbmbesIeMEvESieEnTdS!i2o0n1, i oofwrteaeismidwyimvllrhivyeldogdrttrrr fo resys. Teots ors wi beGamera2 : nhauronrwidaeRiepnt1n :beSecaeods dnc83onhynsauglpeoefeinhCs, eborkselis on11s0%lofaarbedsweithldleptticco bpentge0 - e Ealnydre tseove alelos.tT(noLpe.vf3ootTnehelfoioonprvdoecienr,coorree solE etwiolg o surrsedwioiosteivon les) - 5Fviekenvtippestokstec wim(do t1ah lfieonsst7c)ie,twnhldBooercmoeidepnonF kesshg ecnr).itofdeirni5WAxGcvaiisl ma prsaiohe npaeconcnnion BactCopy forges : FV aEnicnmentl Lavotery Pogozors EI Dan <0oes Page 220 0f225 i prasid 3M ENVIRONMENTAL LABORATORY i --"--amo--n 1 } F oeS J Bt Te poplin of pt -- ne i a e noc,Ror s SHCCULL TLT, etete 0sty ayloyni rires 1s snp Cte eeee TS i D D eS memee e, t CE e mei fe ia .eBrhas.ly - AMENDTOREAD:Thepurposeofthisstudyisto quantify perfluorobepatciadn(oC7i)c, pentadecafluorooctanaic protocsseconss . - Comm om e Test Substances - e [ r mm ant s r o eCTne] n -- i| : e emmaee rarToe ne]| . -- an ) -- sEv-- ---- [ Pomsieco| tomocoeiwooonire| s Bactoypyotorgng LC w/usea Initial" [) 000313 Page 221 of 225 - aMEmmownenTeL LsorriaTeorsy - Protoc"olam#o0n0d.1n3o1n11 - [[r mrem e nsm saT nc em nr ce - [ I [Cm om i -- me ||e -- n t c tcoe re -- aa os rn ] s e To -- r -- - REASON:TheC,compoundwas eliminatedfromthestudy. - Z.PROTOCOLREADS:SECTION49. Retaronce substances - [ERETTree [oo| g Toe [oorm [om|o=m | [im [ooTow oro ; [ETorEi]S Pes | creo |ov | wSeos| StGieprf [e[owon|[rroom]| aT oJ] : [ETSteeirveeiys EE || eveonrm [oworeno[GSuGoommess a x= | a|me,[om |iim ee el prem | - ean ts --TSPosenair|me,[eee |=, [iets|ormmor|one | Gost | M0 |wn| ron| er re Te en[oe [mm] = petTsosnascane [rene | Tere =m Las E32 me = r-s - reiriyamne | eso| tenoorn ao| fon[ue oem : RetSoeaenrcese Substances Te| ceTo | EE [ Tee[|s =a o [ Ty am| Sono 5| * | conamymonges epiat |ooo[ron | Samer |oie, [om|dt| CauCarwaoy n 3M EnvironmentalLaboratory Page 4of6 000314 Page 222 of 225 immovers g i P[tEtwe mry[oooem[e[[[ooowenn[[iE[TmE[|EoT2onTToom[[iAi] : C[EtiZmE=reh,T[Tooo[oermm[[J[roooownmn[[Bi=J[oe|m|To2m [[ommn|||oooomeee|| FFEEEEE [em [oe [om| 2 22 - rl ll ms t sse i t n t ee Sot S m ir ne nn , o . 64 JustificationoftheSurrogateMatrix. Baons prele imind ary testing, normal pooled rabbit serum contains ERT . g[ma-- inital Date rms ss 000315 Page 223 of 225 . WM Evvmowwenta: asoSmoaeTroor%s i Protocaoml#en0d0-m1e3n1t11 } Eifie100o 8mTonxe neeowt n oe deeelet i SA C A simon ASAT Reh : Amendment Approval } e EE TostonS- parsRepraains e ohB--ae : "ZThFiln SA i2ftere gfuee / J Su Eman ssotoy EctCopy of gy Ln wpe Initial Data Pagosars 00316 Page 224 of225 = Protocol E02-1039 `Amendment #2 Analysis of Endogenous Fiorochamicsltsud1yNToirtmoal Pocied Human Serum and Plasma - _ PROTOACDmOeeLcnedAmmMbeEenNrtDDM2a0E0tN3eT NO. 2 - aM EnviaInMEmPneainrtofanormTmeeicnnhgtnoaLllaobgLoyraab&tooSrarafyettoy Services St5.3P5auBlu,sNhNAv5e5n1t08 - "his amendmentLmaoborraetsoEr7hy4eP5r6foojl0elc2otw-Iidn1egn0tpiofirciaotnio(n)ofthe protocol; - ppPeeArnGfaEudoe3r,coaSdleEucCoaTrnIocOsoNcaa1c.n1dc,c(PCsRe1OdT)O(pCCehOf,LuRohteEopAdrDoa:ddeTechaaeTnuapoiumrcapordsaen(oCof1i2h)ci,siesst(tu0dy)yr,somp0sedrqeuTaconartmiotinyocpraeonfdsseosarnaothsiep.ctak(nTi(AcCP1aEc0Oi)dS)(,7), SSeeuirsuhmmyaianosdppleerraTauc,oornvoTedhnictsaioohnesdslGoLdm?otcsend(t.ThHveF4)eanyd peerttuartanecasnctlitontdeo(ePoFOv) inoopri:lSpocoedthion ) pSAeMdfEoN(rCDoE)d7,o0edRpeEcaAadDne:ocTihaevcoiprduor(pnCo1os2ne)n,oofaknidsspcdeu(yCn9r)oi ooc0naqamudcnealciornoptedecei(ccPraEonhOoe).ptincanniiorc(mCaa1cl0i)dp.o(nCpi7re)s,ephoeunrmtoaaednesssnsoeersoanocdtps1s1c). . Chi onmyedoGrcLPnossk pt!ayve pil eh stance hr dosed oo sec. cntoled tt sym as poo i TiRneEtmAeonSvdeOeddNo3sTmHquPahFnteOiSttaotafinv3 de TanHdPuoFbnDsySaecweersee,rSneimoosvneud3m.r0,ospmaogheue3lsabsnofohdheaireld,oyfeirInnetshneicroeenvis,suebdTsrHteapFnoOrcteSbeeaecnuaduosTneH4t.Ph0eF,DdptSsgnw<ese AmendmentApproval i Ppt rg WhomK Roagen, Sponsor Representative So brn ote ) Za = A / 7/, Mark E. Etefson, Study Oroctor ~) 2 Date 000317 Page 225 of 225