Document 1n6DrVb10Q9Z65Jzqrnj9Q9a

c SaKaitfheVriisenePEr.esRideeent, PhD. : off FN Coen 3SaMfetEymiOpreornamteinotnsal Heath and ne Haze. 3SHE O5SEP-2 0:38 ne S79C000PBBaauxlsh3MA0Nv1e$ne5,13B3u.il3d1ing 4225.26 )ST a 258765 August 26,2005 Teh-otos-037 RDoocoumme6n4t28Processing Center (Mail Code 7407M) NO TSCA CBI OAtftfeincteioofnP:olTlSutCiAon8P(r)evCeonotridoinnaatnodrToxics US. Environmental Protection Agency K. etp--4o_-37 Cont W1a2s0h1iCnogntsotni,tuDt.ioCn.Av2e0n4u6e0, N. W. najin NO cp Re: TFlSuCorAocSheecmtiicoanls8,(D)oScukpepNtloesme[nStEaFlON-oTt[ice0:-3S7ul4fJoSnEatHeO--b0as3e8d1a-n0dC3a9r4b;oxSyElHiOc--0b5as9e8d:373 Dear Sir: T3uMorioscshuebmmiictatlisng this notice to supplement ts previous submissions on sulfonyl and carbonylic-based Lc3aoMbmomhreaarstcoirraeyclelanyntdlayvsaruieblcsaeebiqlveueendnottrlhmyeaeslnccrpleooeosnleeedddfaohnrualmeyatnnidcoasgleerrnueopmutorshtftwlhuwoiercrohechpperumeriscceahnltasss.eddaEtbaaycfhtrhosema3m3pM6lelEonwtvsaisorfoannmaelnytzaeld puuessriifnnlggulaoirpqouroiocdttecaihnnerporsmeuacltifpooingtaratatepio(hnyPtFteOacSnh)dnie(qmCuemFaa7sn5sd0ssp)cerceatenrndoemdpeeftrorfrylus(oiLxrCtoeo/ecMntSad/niMofSifc)er.aecnitMdfu(lcPuhoForOofAc)thhe(emiCdcaFatsaC,pOirOnecsHle)und,tiendgin the report was derived from extrapolated curves and should be consideraesd screening quality data conhleymaindcanaolrtsenoercewsesraerilpyroredpurceesdenbtyat3iMv.eofItnhaeddgietnieorna,lthpeopluelvaetlisoonfflelvuelosr.ocNheomtiaclallosftrehpeordteetdecatreed giennfeorramlaltyiocnorroborativeofpreviously reported values and/or do riot represent "substantial risk" 1you have any questions, please do not hesitate to contact Dale L. Bacon at (651) 778.4736. Sincerely, TF 5 ( Hithiune F l ie | ESKtanatvfhiferVroiincnmeeenDPt.raeRlseiTededec,nhtPnohlDogy and Safety Services ' BEST COPY AVAILABLE Sp------------------oe ---- i -- QuE id TSM iTiIt N14Y40 1 ---- aw EmROMME[NTAiL LBiORATiORY 3M NO TSCA CBI Analytical Report Revised August 12, 2005 Initial Quantitative Screening of Commercial Lots of Human Serum Obtained in 2004 for Endogenous Fluorochemicals Using Protein Precipitation and Liquid Chromatography/Tandem Mass Spectrometry Laboratory Request Number: E05-0120 Testing Laboratory 3M Environmental Health and Safety Operations 3M Environmental Laboratory 3M Environmental Laboratory Project Lead Mark E. Ellefson Building 2-3E-09 Saint PaPulO, BMoNx 353531133-3331 Phone: 651-778-5405 Testing Facility Management WilliBaumilKd.inRgea2-g3eEn-,0P9h.D. PO Box 3331 Saint Paul, MN 55133-3331 Phone: 651-778-6565 Requestor Dale Bacon BuPilOdiBngox2-333E3-109 Saint Paul, MN 55133-3331 Phone: 651-778-4736 1 Page 10018 -------------------------- aM EIROWER NTALe LwABoOERoc AmToOrResY 3M Eavironmental Laboratory Analytical Report ProjectNumber: E05-0120 `The following analytical report presents data from commercially available normal spuobosleeqduheuntmlaynscsreereunmedthfaotrweenrdeogpeurncohuassfeldbuoyrtochheem3icMalEsn.vironmental Laboratory and `Thirty-six separate loofptoolsed normal human serumwereextractedusing a `protein precipitation technique and screened for sixteen different fluorochemicals `using liquid chromatography/tandem massspectrometry(LC/MS/MS). Serum `samples were received from various suppliers between 9/9/04 and 12/2/04. Samples `were analyzed between 02/03/05 and 02/09/05. `This range-finding study was designed to provide lower limitsof quantitation t(haLtLmOaQn)yooffatphpertoaxrigmeattaenallyy1t0e0sw-e3r0e0pprpets.enUtpaotncroenv ocfi ethnee dmatutw car,hilatowwtaesirtdhoiasncnotvhseered ca10n0b-e3c0o0mpplpettteadr,gsetiglnevaell.tonAosiasne rianttieorsimwesorleuteionvandauantnlidlaaulmiomraietodftefdienteietcitvdeiosntudy (LOD) was defined for cach analyte. As a result, calibration curves were extrapolated bettwhe eLeLOnQandthenewly defined LOD, allowing screening q`umaulsittbyedaetmapthoasbiezdedetthaet mrimcfhioornfstoehmededaatnaaplryetseesnatseldionwtahsis1r9e.9poprptt.waTshedreerfiovreed,firt om `extrapolated curves and should be considered as screening quality data only. `Sample results are summarized in Table 1. The average values reported represct `samples in which there was detectable analyte. Sample values that were fess than the limitofdetection were not included in the average value calculations. Please refer to Section for individual sample results. Page 2018 3 -- mip------------------ esto-- sim--pr--imeirs. seEoTrL o Table1. Summary of Peforinatad Acid Resuts ke TEx Pe Th EC a = io LS An ItKG GUL [| diwn e {[5o5w[[2e5os|we[Toowmss| aosro|1m2m[|owwe[ooesmo|<aicooo)] [ [f ti oStann w ds poviaton TI|ov2se1os7r[[|2s64ss2||Nwww7E[|1o[am0gm2ess[[]3osu5er0sy[oz|moesarir[[|wwawww TTToososeaz||<<0iloomoo|]] Nambeorotf Saampaosewilh OT No eed.TSws oTwy STE i ee NR?= NotReported. Thisanalytewasdetectedinoneof the 36 Tl samplesbutappearstobe 2contaminantor Table 2. Summary of thor esuiati sn igly Fluorivated Anata Ross EeT e T a e reas NE Sra [ [ | m We ean wn edan --<t|0< <t0oo oJ]o0pp1a0or8o [[aomoo srsosem "|s3sa2s r7o|||[ 1s166a03o|||<0 tLtooobpa o.T||oo8 0e0ws8[ sm||| [| to FrSacthainow ndaofrSdabmopviisetsiowni T|<onooo"uJsotota[tzoooostizoe[]ruemzs||627711|| ntoon' |nooozmee]| [tnt |asoor|osaoo |zovy sEe[soene |son| aso |!sone| iPseoamkesrwsefroer PobRsOeSrvaenddinPtFhOeAc.hrRoemlaattoigverabmrsanccohrerdesapnodndliinnegartoilsionmeearr arantdiobsrwaenrcehed determinedforbothanalytesandarepresentedbelow (thehumanserumvalue represents an averageof % branched isomers for allofthe human serum samples that icnodnitvaiidnueadl dseatmepcltaebslaerleevperlessoefnteeadcihnaTnaablyltee)1.2."TIhne%addibtriaonn,chweedlli-scohmaerracrteesruilztesdfloorts of 'PFOS (Lot 171)and PFOA (Lot 332) were analyzedtogetheras a matrix spike (QC050203-004) in rabbit serum. Data from that analysis was evaluated for `branched and linear isomer distribution and agrees well with previously obtained NMR data. ---- 4 SuBnROWES TALE LASORS ATORY Table 3. SummoafPrFOyA and PFOS lsomer Ratios heaoa t Smale e CEa eLs r E a BIT dT Cle ee Er [ HummnSer| uma 6%ve|rs sog n e| Watrix Spike (QC050203-00 [2 |w% w | LoTtC3R3-3(1N2oM3rR.(96c99h063a0Pr-0ra3Oc0S)oPrFivOazAleued) po Lot171(NMR charactrvzalaued) ER RE RR ER Table4,Reference Substances iikin i aw ee m best e ie e aC] = ER ETME SeSE CE |totodwcrss | proacende| wwis [ ronan [man[om | | emtuepmmiens |Neracsr | aw [ronson[ses | ome | ||_Petsotemicssd | prin irc)| Ouvosiprivs| rove |sion| om | |e ait|aac | aa tia |oa | om | |_redsmocsss |rroncore[aw [renmssony|ssn| om | |Eepatvoomicnss| Conia |obvi | Toren [mon[om | [[ooiemtvontecmoi sia| clones |outros| monde [sain[em | |retmicamienie| ciiaia |ouvoipraen| rove |wan| om | E Chr |E en | mer [o[ann oomn ] |remote| ro | torsion [moma| oom] [retomocmmtonmsse | vos | | roamooisiain[sex| om | [rotons [wos | ow |roromosisiom[oe| ows [rotenone vem | ow | rosemsg[ower| om | [rotons wos| aw _ | ten [wee| om | [omrnsit vomon |rem | vam [am] em | Faedoris < _-- WU ENVIRONMPERNOTEACLTLNABOOERSAT0O1R2Y0 The samples for this study were prepared as follows: 1. Theserum sampleswereallowed tothawandwartmo room temperature. 2. One milllteofserum (or water in the case ofmethod blanks) wes added to 2 15mLscrew-capped polypropylene centrifuge tube. 3. Matrixspikesandmethodblankswerepreparedbyspiking heserum (or water)withthe Surrogate to all saernumaslaomfypilnettse,reecsastl:ibIrnataidodnisttiaondna",r*dCs,PmFaOtrAixwabslaandksd,eadnads a `method blanks at a concentrationof3.01 ng/mL 10 evalua extraction `method performance 4. Ttwuboemsilwleirleitcearspopfedacaentodnviotrrtileexwmeirxeeda,ddaeldlotwoitnhgetsheersuemraunmdptrohteeciennsttroifuge precipitate. 5. The tubes were centrifuged at approximately 3000foffor 20 minutes to pellet the precipitate. 6. Afterremovalfromthecentrifuge,thesupematantwastransferred to an autovial for analysis. tQuaanndteimfimcaatsisonspweacstraomcectroym.pTlhieshfboeyldlohwiignhgppearrfaomremtaenrcsewleirqeuiudsecdh:romatography Liquid Chromatograph:HewletPackard Series 1100 Liquid Chromatograph system A`nCaollytuimcatlemcpoelruamtnu:reK:e3y0stoCne BetasilTM Cyy2x100mm, Sum particle size Stop Time; 20.0 mines Flow rate: 300 wLmin Injection volume: 5 kL M`SooblivleentpAh:as2e.0commMpoanmenmtosn:iumacetateinASTMType I water Solvent B HPLCGrade Methanol - Solvent Gradicats - T0me0 x28% a10s 2so%n 5B5500 9200%% 2000 2% Page Sof 18 6 --------------------------------e--a--m-- es--im-- p t WENVIROMEPNTRALLOANSOOUR0A8TTO1R2Y0 Mass Spectrometer: MDX Sciex API 4000.Q-Trap MassSpectrometer Detector Software: AnalystTM Version 1.4 TIoenmipzeartaitounrMeo:d4e5:0ElCectrospray Negative Gs1:35 EGnSt2r:an4c5e Potential: 10 `Analysis Type: Multiple Reaction Monitoring (MRM) Table 5. Acquisition Parameters 2629 [PPHAGeaca)| 5130 --| 1689. 2| 2190 [0] erties | 45 | [PFOA(C AGH) | 4130 |s8e2ie0f6s0 | 40 | [Goad |""sso |sierzeszies | so | [Codd | "se |sesazieszeei | 0 | 187,2689,2188 |CaAdd | 6130 | 5687.1689.3187 | 50 | [resaToes| 70 | ss | [Fosa[ars 7s | eo | [pres "ose | ees7es | 5 | [Peis | see 1 esesmo | es | | Pros | Tasso |eowa2fw00 | eo | [TPFos |"azo | aege0s | 0 | [--mweros~~ see | seezeto | 0 | [ProaraTM | wes 1-- wes | 40 | `When multiple transitions were monitored, the total ion curcent (TIC) was used to ``qmueaanstuifryemeeancsh.analyte, thereby providing greatersensitivitythan individual Q3 fon 4.1 Calibration 411 Calibration Curve An extracted calibration curve was formed by spiking rabbit serum at prescribed levels and extracting the curve in the same manner as the samples. Stock solutions `were individually preparedfromneat fluorochemicals and diluted in methanol (except PFBA, which was prepared in Milli-Q water to prevent esterification from occurring). Samples were quantified versus an 8-point extracted calibration curve. `The regression analysis was performed using 2 quadratic curve fit weighted 1/x. Page6of18 7 SWENVIRONMPERNOTIAELCLTANBGOER0AT5O1R2Y Calibration standards were within + 20% (+25% for the Lower LimitofQuantitation (LLOQ) with a coefficientofdetermination >0.995. Low-level calibration standards, which were not within 25%,werenotincluded inthecalibration curve. Calibration standards that were not greater than twice the method blanks were not included in the calibration curve. 412 ContinuingCalibration Verification (CCV) A Continuing Calibration Verification (CCV) was run atleast once every 10 samples, bracketing the samples with the calibration curve. The CCVrecoverywas within 25% for all analytes. 413 SystemSuitability Five system suitability standards were analyzed before the initial calibration curve andaferthelastCCV.Thesesampleshadareacountswith a %RSDof<5%anda retention time %RSD of2% when evaluated independently exceptforthe following instances: Several individual transitions monitored for the Cio Acid failed the retention time system suitability criteria. However, the data reported was derivedfromthe quantitation ofthe TIC, which passed system suitability requirements. Allofthe system suitability setsforFBSA area counts failed. The %RSDs were 6.2%, 7.5%and 8.4%. However, nosampleshad area counts above the LLOQ for this analyte therefore the data was accepted. 414 Lower LimitofQuantitation (LLOQ) `TheLLOQforeachanalytewasequaltothe loweststandardinthe calibrationcurve that metaccuracyrequirementsof 75% -125%. 415 LimitofDetection (LOD) t`hTahtewLeOrDe2f-o3rtciamcehsaanbaolyvteetwhaesmeeqtuhaoldtboltahnek.area counts (converted to a concentration) 416 Blanks Method Blanks All ofthe method blanks in this study had area counts < 50%ofthe LLOQ. Matrix Blanks `Two matrix blankswereprepianrraebbdit serumand analyzed with the samples. One matrix blank contained endogenous levelsof PFOS that were above the LLOQ. An average endogenous value for PFOS was determinbeyd substituting a number equal to the LLOQ for BLK050203-003. g PagTe f18 ee awEnvOmENTA ASOeReArTOrReYs Table 6. Average Endogenous PFOS Value Dstermination SE ea |__ uoapgmy 5050205 00 |o<0i.i3m 0o6a | Average: ows| Theaverageendogenous PFOSvaluewasused{ocorrectthematrixspike. `responsefor endogenous levels of PFOS in rabbitserum. 417 solventBlanks Acetonitrile blankswere analyzed throughout the analytical run.`Analyteresponsewas less than % the LLOQinall cases. 418 Surogate 13CPFOAwes addedas asurrogate toallserumsamples,calibration standards, `matrix blanks,andmethodblanks at aconcentration 0f3.01 ng/mtLoevaluate the. `extraction method performance. All surrogate recoveries were: within 20%. 42 Laboratory Control Spikes (LCS) wSiitxhLtahbeorsaatmoprlyeCs.ontRroel Spswiekeurse(clLoCrSrte)cwtseerdfeoprreepnadroegdeinnoruasblbeivteslesroufmanaanldytaenianlytzheed `matrix (where appropriate), and arepresented below. Table 7. Matrix Spike Recovarie in Rabbit Serum TE a eWargs e e | emp ee e Reateina PRD a en] TE on [ocsmmmss| 30 | euoa [mn | I nm|[Focomnotmoeansoss||| srvessee1 | m mmas[||wws1nws||.| 1] Loom Cees[mr Ror Ar wm | ww | q Pages ors EE Sw BoTyT Til. Man SpeRecon RabiSemont) Fm Th Gn Eee [EEE cE fcoY 08 ERS lal NekEeeRu 1 i |= e aooscaosoo|T sowsn|e r C <uon a |T wa || Lotaatnonmi |OomGOSo | 76s | ee em] |oovsoaosoos | ves | m2 | om | [Tocosoaosoos| 768 | sz | am | IT [ocosaosoo| 30s | <toa | wa | Qcosa0s 002 38 | cuca | wa | PHAITacd ooossons| ses | <uoa| mA | uoq=a0ingm |Qcosowsoos | ves | eee | ew | | `ocosoaoso0s Tes[eo | ds ow | rw [ooosoapsoos | 765 | esa | ew | Cs [aco|so sia z w|s<ouooa n| . [Cacosomsoz[312 |<uoa| wa SW, ["ocosoaoso0s | "ate |<uoa| wa | LoQea1zngm |OCOSZS00 | 78s | ese | ew | [[c[comosooaossoos|| vaese | |_m7iis || woomw || [ocosozoso0r | 2x | 28 | tom | |ocoso20002| 267 | zm | em| 51% ion |Goosazo0ps|Tzer [zes | eax | [ 1100207ng. | QOO0203004| 753 | vss | vom | ["acosoaoso0s 1 7s3| ves | dow | [acosozosooe | 753 "| ez | vo | RR Emre a | |Qcosmassot2| 300 | saa | woe% | IAL. [acosooso0s | 300 | a2 | tom | 1L0Q=0747ngimt. |QCOS|G72560|307602 4| tote |ocos|ez vsso | soso ez| s ioo% [acosaosoos| 756 | 7a | tex | Fagesotis 10 eee --------_Tpeer eeeeee ------t le Tale 7. Ma Spike RecinRoabivSnecronss) auEnROmEe TALUBo OUTORY [B airs e UNi,meSnet opbise CJo R MGalEsg [ocosoaosoor| aor | _zer | ew | Qoosomsooz | sor | ses | x | "ceroa Qcosomsoos| ser | ae | ew | | Qooseaosdos| aor | aes | ew | [ocosoaosoos | sor | ae | em | [Toomsomsoos | aor | 21s |ex| TT1 [Toowsoaaoor | ses | am | wre | [Tocosoaaooz | aaa | aot | wow | am Sods [Cocosoamzoos [aay | ae |ww | 1L0Q=0.303 ngiml. [Tocosoamaoos| 754 | ms | vom | [Tocosomaoos| 754 | ees |wm | [ocososoot| __2 or LLoa=0208ngm.|[CQocOoOsOm2a0n2z0o0n4s|| 7766 | ze | ww | [as ox | aes | wx | | |__7t5e2a | | wtomm || Icoummmom[rss[ms ow| rr I TT mmmww| [2 1 s ew| FaSA, [Cocosoaosoos | sas | aes | om | (L=o03a03mgmt|OCOSI0004| 7s | cosomons| as | mse | ex | ma | vex | 14% [ocosmooos| es | m1 |ww| rt 1 rr 1 Cocosomsoor| 300 | 274 | ox | Loahxoisaonom[[o"cooosmoopssaonms|| ar0 s | | amree | | owomw| | il Page toes -- SWENRONERNTACL LNABOERAsTOsRY Table 7. Matrix Spike Recoveries in Rabbit Serum (continued) 5FEEhe {uwna lek EEE TY ! iT . ibn eee Te "PS [To|o3mmm|maes oo [ooeesn]| uoa=o3snomi|[_ocoCscso ose||cov7ss 85t 1|1m 0i5sa e ||swexs n|| | oocosamsoos | es | ma | om | 7 ad Tooecmseomseoosn |[ sw a || ssemesw |]wsexx ||. osx Loa~oasnom [C _oowmmsooo s || 7o m0a8 | |s 79e0e |a a0m0x|] [o|cro oa m | rea e |e een] T (-- Cosme | 3T " se |om] Loa=TomRoSnomi. [ |_ooc||cw oamep sm"| o o |s e s eso o o ||oeen mxs||Ea [Cosmas T78s00 0 | 1 tom] consweosoos | ee | es | ew | e ooomsoo | amo s T |r ep | ee | 1T0R36S3na omi |Co _ocwoo mmaotseso|||esasrsmeeosesmso I ||an 3ame0ou0s s]|oon | [Cecamemsans TreeTro Toe m] [oc|om res m|sveo z |owes en | Page11f18 12 i SM EROENR TALLBOE RATORY TLaovleee8. PFOS Matrix Spike Recovary in Rabbit Serum, Corrected for Endogenous FoR EE EE FP ie eaiee s m me e me eEseeCe e [acosozoz001|306|sur | oats | 286 |om| ae737003snom[[.Taaoccmooseosszsoaaotoenosez|| a3707o48| | s7o| 2s| | ooaarstsse [|ma2a7m2T||w weoeow||| 25% RC 2 TY [acosoz0zoos| ra |7a1| sts | vse | ew| 4.3 Accuracy Theaccuracyforeachanalytereported wascalculatedby takingtheaverageofthe. `matrix spike recoveries for that analyte. The results are presented below. Table. Method AccuforrInadivciduyal Analytes wo Try [prea |em | | cizhce| ae | [nee ox | | FBSA | =m | [era| azw | | rosa | sex | [Crace | sox | | pres | =m | [pro | wax [| [pens | vox | [condd| =m | [| Pros | sex | [CloaciaTM|=m [| | THeros| eax | -- esee a [e CFEitRhi cTd|=mB ||ntherDsS|r = ETSA |eocin 4.4 Sample Related Comments `Theextraacndtanialoysinsofthe samples wasperformed utilizing anon-validated `method. The matrixspike results, C PFOAsurrogate recoveries, andthe `Wehxetrnapeovlaaltueadtcianlgibtrhaetiaocncucruarcvye a(nbdetpwreeceinstihoenoLfLtOheQsaanmdplLeOrDe)sulsths.ould be considered Tables 10 and 11 summrize individual sample data. Pegs 12018 13 EES--, Ergo -------- Tabla 10. Perfuorinated Acid Rosuits rr esbmmaroregeermeee aw emmoNMEiNeTAgL rLArsOiRATaORdY Elhee de: ocr dPEe eaeE WE CSRSsHRae (ihESBe E SR] SER i H ia a ere] Re | rr [sso[e57l 0[a 2%[a ao] oo[T aise | 1n 22|s ooo[H~Eaoo[ [ss om [00 | 00 |<0[asst| me[woo | woo | woooo|| [[smsseis[|o"<so0|| oonp|[w<ooo0|[w<oooo||7e8s0[|o2wsn ||swoooo|| woooo || wtoooo|] [mI esa 700[EcoCoTooTE'aToo 798 tas0| woo0|YwoTo |EwTon| [[rmaeesmso | aa3m:[|a<oon0[[cwoooo"[sotooo[|3418s0 || v24is || woooo|| ooreoo || wtoooo]] [[mmeesms[T4e0r0[[asoenT|oooo[[waosos|ess3s0|[t1o&s2|| woooo|| swoooo || wiooo]] [essTze [won[woo[op[sez|11 | oo | oo | woo] 1% Page 30f18 eee etereeneee Table 10. Perfucrinated Acid Results (continued) SUENVIRR OMENTRALLABOERAaTrORsY [WEPIOERESeSereiea JB (naim hEnS (sReeEen(,oTgi iL} Baiean ssLefol R eaglmi)iFaguinit [mO Feroarn r| eoE s[FFoaoeof| hwoo[ai 4o00 e|oalr o| [bawooo|e Baeco |msoo|oo<rnoo||| [[wTaocooste[oeerso ||2o6o||c<ioooo[|d0o0o||4#3s2 ||be12rss|| wdoooo|| <ooo0||<<oooo|| [[nnaastes [eos ||io0e0[[S<o0o[|f<aioeo[arioor |sso | 00[ 00|doo ||1a1sss[|o2ar||=soooo | sas|2s|=o || o<woso || <<oo00|| |ose| <oo| [[[imnFaiareoroosso|T |sstso 9||<o iooo0[||T aoo0no0o [||s<ooiooooo |z4"oem [||oo1wme0s|||swoooooo|||<<w0oo00o||e<sooooo||| [[nkosost[ssstoon[|wo0o0|| woooo|| o0o0[[zswe| t[aesei|| soooo ||e emo||m <soo0o|| [[naooss [To0ez0t|| [acess | coo| 0000 ||stoooo|[oao0 || asmare [|oorrss|| oo[too|woo|zss |ose | wwaooo~|| <<oo0o|| <<oo00|| oo|<00 | woo| [[F[riviaeeoosms||<0c000 ||<000||<<tioooo|| oooo|4eesr||o1ssti|| oooo||<<0oo0||==oooo|| f[e[iFnmiaens:erso[||s<<cc00o0 ||<a0a00n[|[s0<o00o0|[[sddoooooo[[|we4imoe[|113t4is2s |T| owooooo|||swwooooo|||wswoooowo||| [[uoeTeomnsecronez| s0o0o00||<u0im00n0||s<s0oo0bo|||esciooooo|||a<1i4mosn|[eo<mteois5|||<woo0oo|||awwooonoo|||ss<ooooon||| [[[wimavacecoomsms[s<<ei00w0||e<c0000mT||e<ioioono||[aodompo[|oz[2en57 T|oo[msosssTs||iwooooo[||w a<oooo ||s<mo oooooo||| [Hew [0[am[wn[ome[dor[im| mw | om | ma | [[oioonw[[roosoo[|s26ss[Twwn |otsoer|[omaor [|ozaer|[ wa ese|Twxw| [a[ao oor[om son[or om[0[on| we| [sToermmrise|t=e | 5|o |= | ow LLOQ hr0100. | | o [ & || OApliNo tillwabaesrGeeaoleytensonoohfeeehlr3s6wihlplplbesporappeafrnshoedbef contSmyia.ntoansnl; oC ROA ep me,oveei 3 Is Page 140118 0ENVIROME ENTALR LANBOOERoC ATsORY Table 11. Sample ResfourAdldittionsal Peruorinatod and Highly Fluorinated Analytes =i TE iy 3 Sa Pil io fina [_(Em508wi(esEsoPS10dhoieo[|o<oD o|<oo|"4 |H23b 0 |soToo[ioae| [[rmeessssT|o<ooo|[o<oomo||eamoer||oaoems ||smarz|| wwoooo[[aaurs|| [[e wesssT[soono||s<oooo[[wwesrw|I aztate|| svaess||soooo||oooosmor || [[wmeAss [ [o oo o || acoooo|[Toooroos[|aarms|| 2w0a4s||dwoobo||oososeeo || [eso | oo|<oo|emer[am | tes|soo |oowi | [ [a ae essTTooop|[T<oomos|[Todsosber1[sazs||2210ss|| sdoooo||aooessr || [[a reess || coopo||<<oooo[|owoomws||aamm ||tsoora||soopo||oaocmer|| [ness Top[mtr|oowe| im | ra|ao0|ower| [[amsesmsze T|oooo|[wooop||o<oowos[|iendns || t3ess|| wwoooo||ocooemws|| [meses Tao |<ioo aos [am[161|aon | aoe | [Naess |"<oo| 400|ooere [der |12| doo | conor | [[w--mo ATos00T[woooo||<<ioono||ooosuers|| s4ems||z22a0[|w<ooob ||oomeesr|| [esse | oo| woo|ems|am | sme| oo |omer | [[wmweesmte |"w<oooo[|T<aoo0p[|oomoe|| atmree||maa||woooo||oooosersr|| [meso [oo[woo|aob |sav| tas| <ioo |ome | [[mmaaewessss[TwT ao0o0 [|o<opo|[eaeoe | s3a20"||2r2er1|| woooo||ocoosmo|| [[mmewseessz "oaioo0[[Tooop[e"aomnmezr||ooasszs {|avness|| wdoooo||ooorroors || [a|e_Twraesoes || <woooo|| dwooob[ooomp || 44c||wmso|| woooo||aneoerr|| [ [x aesmm[o<ioob ||<<toooo[|oagoese[|stooeos ||ara1r||"w<ioooo||naceesesr|| [[mwee sess || <otooo|o<eoso|[ooomo||"aimns ||staerr||<woooo||oowoer|| [[mwweessssT|oooo|[w<oooo|| woopo|| twamr ||sweies||aoooo||oooonmr|| Page 15018 ie Seowuem osoRnTORY Table 1. Sample Rest for Addons Pruorinatd and Highly Floriatod `Analytes (continued) fo 18 Hele dn ff fs ol 7 i f a aa F[ 0 re we on[o<ooro"[oamoca {|suaor110vess 1|n TsoaMn[[ooTmmeerr|] [ieer | Jeovmer Toeomso[|wsao{saensT| mToome|] [T i oumwar omassa in|oz[oo | vs |EanS[ wm |oom | P aeeinS teL100itoar e0,t abl 12. Isomer RaftoriIndiovidsual Samples ET EEE : ETE Eleelotell na [ mwewo | cwema . | wx | wx | [ese | wan | x[wx | [ower | Powmten | am |ew | [wes | reopens | oes| sex | NewYork ENE IE [we rms s 1 Newchiagan [Tmeanw [ |we x | mee we [oem]ow] [meee Teoma] [ax| [owes | wowsowees |aa% | ex | [aes | wewesowwes | ao% | ex | [mes |wewsowsss |cuoo| ww | [owes | tems | am | ex | [oweess T | cac ma |eaeexee | awww]| [owes |owns | ao | em | [ mwmw |cms | wx[em | [owes | hewvex |ew | wx | mwas | Newvex | ox | wx | Fae 16018 " IMENVIRONMR ENTALI LWAOSOER0C A8T1O2R0Y Table 12. Isomer Ratios for Individual Samples (continued) Er ERE PIEl Gr] [meso wegen]ox | sx | [wes Te| e ox[n sw | [wes To | son x | ee | [wee TT ves | eax | aw | [wees Te| e sex |s ex | [wesTe| m tex |e ew | [weso Tha | en m |a sx | [were TT ayes |e | ew | [were TT wescwsers |<uoo | aw | [mes |wesmowsets | tex | sow | [wee tem | em | ew | [owes Teewa | ew | [owesTe| w om | s ew | [noes | ems | as | aw | ------ rr rr Awww [ow | | +SanLplLe valewas <TL0Q | rosin|ow | ow | TNA697 andTN-A-6978a rom thesame lotofpooled serucn. Aloriginalrawdataaiidthe alyticalreporthavebeen archivedatthe 3M Environmental Laboratory. The test materials and analyticalreference standard reservesamples,aswellasthesamplespertainingtothisprojectarearchivedatthe 3M Environmental Laboratory. Reservesampls,digitalcopies oforiginaldataandalloriginalpaperdatawillbe retainiendthearchivesof 3MEnvironmentalLaboratoryforaperiodofat least 10 years following report signing. `Under the conditionsofthe study, endogenous fuorochemicals were found fo be psreersuemntwhinilaellPsFamOpAlews.asPpFrHeSse,ntPiFnOd,etaenctdaTble lHevelPsiweFraelldbeDuttecoStneedsianmepvleer.y lot of Conversely, FBSA, THPFOS, and the Ci acid were not detected in anyofthe w`siatmhpilnes2u0si%n.g the present methodology. C PFOA surrogate recoveries were all 12 Page 170618 rio piemeeteeemees gtr moseseres ----eeeeerrii aMEWIROWER NTALEASORE ATORY ZLLz -- oeLe -- Wip ka Rep agan,s Labora--toryMaren 28/Ba2e /05" The 3MEnvironmentalLaboratory'sQualityAssuranceUnithasauditedthedataand `rfeorp thio s prr ojet ct. Ca ayFosrance Representing = Page180615 1" ------------------ # BAUG.12.2005 5:71PM QUALITY ASSOCIATES 28 U1 N0.07 B1/" WEVIROWI`SPNRTOAELCTLMABEORSAT0O12R0Y Gm hdtesc zLzaborsieyMa-- na. ger d2a8d1a/k0r5 `The3M BaviroamentalLabortory'sQualityAssursnceUritbasauditedthedataand `Tfoerthpisproojerct. olo"C N - QtyAssurance Raper gus Tae RECEIVED TIME AUG. 12. 448d Page 1sor1s PRINT TINE AUG. 12. 4:49PM 20