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Report No. SpiR 2-1 copy Yo. JA Distribution - Last Page FC-143 IN THE TEFLONe PROCESS HS.ALS. FSohretleburne, Edttor A.W. Mokhtar Perfod: March, 1981 - September, 1981 (Part Tine) Reference: SA-195 s Previous Reports: SpAR 79-3 Textile FSipbreurasncDeepartment Process Control Development -- E. I. DuPRoincthmdoendN,emoVuirrsgin&iaCo., Inc. March, 1982 Tsohteehceurriintdlyiovcioadftuiaoltnhse,toinwrfheoosrmpmoanttsihioibnsi.lmiattyFeorrioef)thotishsee Iosnsuetdhe1sdirsetsrpiobnustiibolne 1f1osrt thoee document will automatically mternatn,sferretutrwn tthoeirthesuacbcoevsesorasd.dresIsf. there fs no further use for the docu. Do rot leave exposed and unattended. 000083 EI$DP7R1O402023210 . INTRODUCTION [imnoni1u9n7_p,erftlhueoroMoctaCnoomaptae)ny notsioflidedtoDuDPuoPnotntthfatortuhsee FCin-1T4e3flsounrfapcotlaynmteri(zaam-TToevnel wiyn thTee TBeefrlsotnagePnrico.cessThaenrdefwoorrek. enIvtirvoansmennte.cessWaorryk tdooneteniinvo3r pr1e6-5 {|[levinimvoiuitsroorrfempeon5tr0toprp(bR.effn. sHi1o)nw,teevrseehrdo,wyebdaercntahuaastte aIontfwcaaosupfrnpoompteonstperde1sieTnnLitVtedeinitlhsoeiwrreroffnde0tt.hee5ctapwoobdrl,ke H{ietflhoansbpereoncensescewsistahryretsopemcotniftoorthitsheToFwCe-r14l3evTeelv.el througn the camplete OBJECTIVES FToC-1m4e3a.sure the extent, If any, of personnel exposure to TaonddbelvoeoldopatacTcLuVralteevemlest.hods for FC-L3 in air, water, yarn Tion tdheeteTrenifnleonthperorceeascst.ions and final disposition of FC-143 : Ttoreadtemteenrtnfntoe rtehmeovceondFiCt-i1o4n3 fforromadnidspbeyr-spiroonduacntds yoafrn.thermal SUMMARY AND CONCLUSIONS [sTfhoenhaarned tihneg oofnlycosptoteedntyiaarlnsaroerasdirtheactt pcoenrtsaocntelwitchan tbhe eTxepFolsoerd dtiospseirg--- [odieftfeccatnedt linevetlhseosfpFinCn-iLng41airTheenvpiroemerntf. launThooe llreeaveocliodoofcfpeFrCf-l1u4r3o waacsidnoitn athweeosupsinnsionlgutiwoanssh hwaavteernowtesbe1e-n4 cpopnms,idbeurtedno2 1piontietntihaals mbeeeannsdeoffinpeedrsoonn-d -- dneilspeerxspioosnurea.s inThtehe pcearsfeluoorfoyaarcnisd uwsaesd dfeotrecptaecdkinign eynadrnsusecso.atedLevwietlhs srapnignendingfrommac2h0i0n-e7,00 tphpem. leWvietlhs uonfcoapteerdflyuaorrnos tahcaitd cowneeredirneocntdleytecoftfablteh.e \wTnahosut's,ecxocntefheiedrmpe0od.t0e9nbtyipaptlah,e fwTohoriwcehlxepevoresluesrewoefolflpepbreefrllsoouwnonretohleaci0is.d4veipnrpymbli1oinomidit.t.ed,Levaenldstdhiids FrCe-as1o4n3s.4s Anpoptroxfiomuantdeliyn 1t0h8e isspiwnansihnegd oafrefa theenvyiarronmeonntthbeecwaausshe roefel twoor mroodlulls,e.givTihnegroefmfaiCnOd,eranddecatrhbeox7ylcaatrebso,n apsertfhleucyraornsongooehsydroivdeer. theThihseahtaesd . 2bd0ee0ecnaCu.sCeonf"tTihhreememodotnhoebhryydsIruKiracfneaaclftyoasrnmitssprroaeftsheFenCrt-,1t4hT3arniotftofhnegXa71s0c0,aasrbpoirntovpiiesdrefshleuatothreeod onulepecefsit-no sary hydrogen. 000034 SPRO00311 EID714223 N I3tT h dia SE-- en s-- n re I Bre ASa Yeiraetosetshi,ioessaepnmregensaotsewcatssr ndsedeprllSoorteods ftcoorn iWgahrrkisEnmgi,tttMoyhtGbeyby vweecihgaaransn ---- Yo tins scan set on 10s er Te amen 4%. rest asvicaron Thee ae camry ro shane 0 eto wf ts ek. -- ti amortm perivers ceronte, : preprL ed by: tr 2G ant Approved by: prTer 0000235 . TABLE OF CONTENTS I. Introduction 10. Environmental Analysis A In-Atr 8. Process Yash Water c. Yarn 0. Blood . Disposition in Process 111. Method Develoment. A TneAir . 8. Yarn c. Blood IV. Thermal Treatment V. References VI. Appendix VIL Abstract VILL. Distribution Page 1 1 1 2 2 2 3 ` 4 4 5 5 ' Lstrage . E1SDP7R1O402023513 000088 . a1 . 1. INTRODUCTION Teflon ersburg, dispersion is West Virginia shipped to PPD Plant aSsprauan0c%esoflriomds/thveateDurPodnits,perPsairokn- tMh,atthceontFaCi-n1s43 5v%eTnrdoirt,onnoXt-1i0f0iedandDuP1o6n0t0 p$pnmMaFyC,-14L3978asthsautrfiatctwanatss.a pthoessiFbCl-e143telreavtoeglesn.in tThheerepfroorcee,ss iatndbewcoarmke ennevciersosnamreynt toto mdeeatseurr-e m1i)newatsheeqleuvieplmenotf pfemrsfotnendel ienxposseunrsei,tiviiftyanyt.o aIniltoiwaelr wodrektec(tRiefo.n Nneicneisesaorfy 5t0o peroe.deteMrmtihne 3itpsropToesveedls TwLiYthofin0c.r5easpepdb, `sietnsibteicvaimtye and out, todecdoeatpeorsmeisneor{tsremFaiinnals dinisptohseityiaornn.- whAeltshoe,r sfitncefs thwearsmhaeld pterresaitomne,nt twhaes co2ndpiotsisoinbleandrobuyteprotdoucFtCs-1o4f3 trheemromvaall tfrreoantmetnhte mduisst- be deternined. TI. ENVIRONMENTAL ANALYSIS A Inchir 2 Aspiirnnsianmgplmeaschiwneerse taken 2 and 3at(Feiigguhrte Il)o,caatnidonsat afroouurndlocTaetfiloonns maernoutnd1)the CFnilnyishoineng sAarmepaleindfurocmtioinnsdirdyeer.the (TianbdluectIi,onAttdarcyhe-r . sintsaicdke itnhleetduhcatd, athdeerteecwtaasblneo lpeevreslonn(e3l phpabz).ard Siinnvcoelvetdh.is Twhaes T1oswe0r.3deptpebc.t.ionThelaTiatck foorf idne-taeicrtiosnampplreesclubdaessed anoyn psetrasnodnanredls eduxepostoureairhabzoarrnde scionncteantfhneateixopno.sure problem reported by M is B. Water Tshaelt FaCf-t1e4r3 tihne Tfienfallonph daidsjpuesrtsmieonnt sistepchaatngPeadrketrosbtuhreg. sodTihiusm iJsEEcIoLnvTertheads stcohethweataecridsoflourbmiliitny.the Threegweansehrataitoenrbaftrha, bthuet reel machine Levels found (SK are 3) and wash wodule (SH 2) 1.3 ppm for SH-2 and 4.0 has ppm been analyzed. For SM-3. The ddiiffffeerreenntcesequriepfmleenctt ddeisfifgenr.encFeCs-14i3n iwnasrhegeenfefriactieedncyyardnuefrotom 3Te,vel.(0Copmpbmi)neadndseSwNe-r2 s(a4m5p0lepsomw)eresu2ppoprptm "ftoher SdHi-f2feraenndce1s ppinn for not SpMr-e2s.entFCan-14e3xpocsounrceenthrazaatrido.n in water at (Table 1) these levels does : SPRO00314, EID714226 000087 "de - c. yorn daSinidsnpteeKrresevdiloanyraranIndahnadddriTendop,nr-oddheuatcdetcsTt,eavbwalhleesrelreavtnehgleisnyga.orfnfrF1oCsm-LdE2i35p.0p-e7d0T0einfplotmoh.ne Tpexhrtiorsbaacbvtlaieroinaabdiswloiirttphytimo1en5thdaofneoltthoe`dtidFheC-n1uo6nt3evseTinegfniaipofpnilciacnIatttlsiyeolnff.panrdoSvoteox'birooen.ss covery (Ref. 2). 0. Blow TdfheretoencTtLeaVxbplofesoerlde7vCepl-es1r.4s3omMienelthboledoxocdTeoewdfeesrd 0d.e04.t0ep2cptmip.opnm.1MioaiMtboslsotowdahsads.-am0rp.oln0e:2s pom. E. Disposttion in the Process yAtneaarmledysiinysarshnpa.isnnsihnPogrwenv(iRtoehufas.t "1)1.0% work oH(foRwetefhv.eer,4F)C-n1oh4na3es i1ssshowwfanosuhnetddhaootnffysatirhnne . mbhieencauattueesdes.at`FAC1-t7154230C0cahCna',s bt1eh0erreeexmtorivsaecdtnaonbtelheeramfFatCle-rl1y4310byrmeimdnaeuictnaeirsnb:goxaylTfhatitesiron3i.0s - ai(rsRnee"f.,ldaes4c,o"mp5pu)lo.lseidtiTioonntoctoonTfeCifOr,lhonastnhditsu,tbhien6pg ewfrheliectuhoorfwoass.Teepfutlsoeandmeo1nscahnaydid&rs c12o5l-u2m5n0.C. "T"hTehe analyzed by IR GtCubeovweans in a 10 cpnw.uarsgceedltlew.miptheTrrnaeittuNrrioecgoelnpertaongidr-at1mhmeeFdToIfRff-rvgaoasms siettseltfo warsun straebpleetiattivtehelse-mitneumtpeerastcuarness.. The Teflon tubing TttwheeompeGarCbastoturorbeatnhcveeasIpRpeaasckseseldla."pp`enadTrheeidtsh5ovlodmluiupnmuetveinwsea.safitner5tmhitehneuttu1be5i0sngCatofvr2eo0nn -- ascrmlea/almslieenrutieCn.FNspiDzeeaFkluonwta.itl = 4a1f2tt5ew0rin p0akweraet s2e3en0. 5 minutes at 2cu5lT0heCs,e(Ct0fh,ae)cytsabnedgiin.n w2th)o.icdhecwroeualsde.haveNoincdaircbaotneydl evpaepakosrataiton 1o7f00t-h1e750FC-c1m!43 (Faipgpueraer Aptrlootndhuocu-tgh`ovtcahcsuersse,thsetchaenoyslefdsiihndow m[ttpheartfschleoucwoarroWdhhoeexptythleenaret)itohneor-pentrohftelieovmraddproirbdaye-- ypo{foaptseetrnhfmteliiuxaoeblrdyaprhwoamidzotuanhcrotdhT,yrdfirratinoodmnee)xt.hc-ee1s0so0Sloeamfmaeionnud.nctopnoocTufeorrendtdheetwieanrFstmCoi-vn1ote4ih3ecteshd`eoTdeoiIfvuldemoernnsstitaGthlCye . htsyucdbaern.isdes.hTohwe'Thoetrepemepaieksranatgturee3v0i1wd0aesnccepmr,oofgrwtahhmieecdholeIffsrionninw1dhi5icc0ah-t2iwv2oe5ul.odf haTtvhheee - absorbed at 179 cn (Figure 3). : 1sDe7r1o402023715 000088 -3- : tIniono,rdeDrraetgoerdetteurbemsinevertehe ucsoemd.pleteTnheessgaosf etvhoelveddecafrrboomxyltah-e phaesasteidngthorfoutghhe tFhCe-1t4u3be.sodiTuhmis5at1utb/eTrgiatvoen aX-s1p0e0cimfiicxtucroelorwia-s emveotlruitciocnh.arge for 0,. It showed 04% of the theoretical C0, III. JETHOD DEVELOPIENT Tshiemilmaerthtood tuhsaetd uisnedthiisn ith methanol or freeze RreefseorrtencfeorI.deteTrhmeinsianmgplFeCs-1a4r3e dried, esterified to get the elexvterlascte1ds volatile ceesxottleruramctweipdtahciknitOnoFgY,ex(aOtnVh-ee20ar2ne)dacwtthaiesonheusxqeaudneencfhioendjegcewttietdhbeitnwtaeatreGrC,s.entshAietinveeisttyeG.r FfCe-d143isiosmenrost a(Repfu.re 6c)o.mpouTnhde aOnVd-2c0o2nsicsotlsumonf caotnsloelaisdtat5esfdtenhteis-e wdiitfhferaenNtig; compeoluecntdrsonintcoapotnuerepedaekt.ectAornewwasewulseetdt/Ptoackianrcrdea5s8e80tGhCe _ niesthsahdowsneirn tFiivgiutrye 4t.o the low ppb range. A typical chromstogram ' The following GC conditions were adopted for use: Carrier Gas Argon/Methane 53 20al Minute : Injection Temperature 180C Colum Temperature 100 Detector Teaperature 300 sample Size 2m tEhxetercnaallculsattainodnarodfs twheeresaumspelde icnonecaecnhtrartuinona.nd Ptrheeciirsipoenakwaasrg=a10f%n for any sample (Table 2). A. Air Analysts hAfofrurerezseaimnpdlr1ei0sedmwlearnoedf t1waakmtelenrBfFoiyrn/moaenntehainhmoopulirmaeadrtd.ead rOafnotere moelfsto3efrilwfiaittceearrtsiowpnae.sr Affsteqruenhcehaetdingwitihn wsaetaelredanBdott1leasl fhoerxaLnSe maidnduetde.s, Tthhee eSsotleurtioIns eTxittreractseadmpilnetso wtehree heuxseadr.e Tevel, which fs below the anMdetihnojdecwtaesd isnentshietiGvCe. 0.5 ppb proposed TLV. toTu0o.3mipcprob 000082 EISDs7PR1O4020238LE Cae . 5. tam SF1ii0vn-et15erae`ldaionyufatremnse,tahonadnneol1AlawnadwsasTadyrdeaesrdonvsteode,ornaeend aanraelnyzoefs ane m1 ySiaFdaernnteitcAahrletlyer.r WSeieansttttoveeerreftnyGhiuenesgnc6cmh.preledeg,s.e"neThxtetTrhsaidcsdtaearvddd.asw'iTtdThiyheairhsnefsxowaenehseaidtahhneecdarotneisudnineceefrporeeransbil1noepe3elMvifiaoenrssuittaiiensoscdn,e oeGrxetrrtaoct2a)id"osnorwpittihon noefthatrhael FCdidon ntohte rTeedfucleo.rsthsise.ssv.a"rianSioimlmtiyo.n c. 8lood sSap1ii0rk0edsdawmapbslleoason.dalyszaSem.dplieSdsteanfatfsiocradal,nly`o{tfnotePtrPhiDes.h"waptrceehrpeacrfker.odm atThehseetfraaipeiswnegrsefer sapniakleydzedblWoiotdh precision. saampplreescispiroenpaorfed1 at10%.ACD (wTearsete r2u)n wiAth.setgoosfs - Iv. MER TeeaneNT TTohterntahle tprreivsetenctandciadnateeffbeecctaiuvseelyofredmeolveetetrhieouFsC-aLf6f3e,ctsb.uton.ityar1ns . ahTpeormanotgpeeedrrhteiahoetatsev.deLfaSPrnrCoyemvei1fxo5otu0rrsac3wtt0ooarbkm2li5en(0uRteFCfeC.s-c1o&3o3n)r.fhi`aatsItRShse0hso0cwp0anrnpsstfehonaorctfe1I0oaffaf`nmd&igneTFurtldyueasfrrrenonrsem cthaerboCn0 gepseakbyotthe235a0bsconrpticoonnfpieramks aCt0, 12e6v0olcuationTs, decarbbxylating. There is no carbo) pesk at T1hse.pretsheencFeC. o1gF "J00-1750 cn fnriocmh1w50u-l2d00sChowfreavmapTorriattoinonK.-10F0u/rFtCh-eLrA3stSuoddyhiomf stahletgmaisesserveoltvnead pddcSoeen:sn!c1icajterriba(oootFnxffiyogla,upanrrtoedisauohl3cone)twf."i1nTt5hhie(TtshChepe=srhTpeorse,wierstnol1cntu7eho9a0rsotaufpmctpoahlam'eoi)hCsfy-lwdHutriohicraedobhecs.naoeirrscbbeoasanTnshcaepyerroayserpsniemb1aasi5kdvlreanoalontvdeeesde3c0vo1riiry0n cttfhhoraerogmugdgeethchtaeorbDlvoryordalyreuilgdmaeeet'rtiro(intRcueabwfela..lsy4ms,"aTedhaee5s1ut.brbyee,pAtanhsaeSslpiyCenOsc,giisfkiencvooofwlfnvoterhdae.mCoocupnoeZtminspuelseoestfsseonou3enrstFcsiogwleaoosnrf $o0ccu=rs10d%uroifngthethetrhmeaolrettirceaalt,hensth.owing tht no other major reaction 00003 e1s0p7R1o402023917 5. REFERENCES 1. Forte, M. A. - SpAR 79-3. 2. Forte, W. A., Mokhtar, A. K. - PCD Monthly, April, 1981. 3. Forte, M. A., Mokhtar, A. K. - 70 Monthly, Yay, 1981. 4. Lazerte, J. 0; ACS: 75, 4525 (1953). 5. Meschke, R. G. - PCRD-58-131. oFluroro,surfacStaSnt inuWaDter".MTEC] Motrod, "Deteraination of Gq 000091 E1sDP7R1o402O33018 sg APPENDIX Table 1 Table 2 Figure 1 Figure 2 Figure 3 Figure 4 Attachment I Attachment [1 FC-163 Semples GC Precision Teflon Spinning fn Afr Sampling Location IR Scans of 1aT OFF Gas FC-143 IR Scan GC Chronatogran Letter, S. S. Stafford to M. A. Forte, 12/17/81 GC Method FC-143 Analysts, 000092 $PRO00319. EID714231 : TABLE | 1. TEFLON SPLNING IN-AIR SAWLES Location LoS -Ron 6 2 92 Ron 28 3 We Rall 6 4 $2 -Roll 23 5. Operator's Desk 6. Between SM-2 and 3, Roll 12 7. SH2 - Between Sath and Kash Module we Non-Detectable (<0.3 ppb) Hon-Detectable (0.3 ppb) on-Detectabe (<0.3 pob) Non-Detectable (<0.3 ppb) Non-Detectable (<0.3 ppb) Non-Detectable (<0.3 ppb) Non-Detectable (<0.3 ppb) . 8. SM-3 - Between Bath and Wash Module Non-Detectable (<0.3 ppb) 5 WI - Rol 6 Non-Detectable (0.3 ppb) 0. 93 - rol 23 Non-Detectable (0.3 ppb) Samples taken at estinated position of operator's head during wor.k TH. TEFLOKE SPINNING FC-143WATER ARN LEVEL Mz Hash Mater 1.2 pom Sever 1pm Regenerated Yarn 49 ppm Sintered Yarn S13 Mash Mater 4.0 om seer 2.0 9m Regenerated Yorn 60 ppm - Sintared Yarn w . ersoe7r1o402033220 000023 : TABLE 11 GC PRECISION SweLE 5 ppm FC-143 10pm FC-143 0.5 ppm 0.25 pom GC COUNTSTHOUSANDS 232.5, 261.0, 234.1 63.2, 62.3, 65.2, 6.6, $9.0 31.4, 34.3, 38.8, 39.5 12.5, 15.5, 19.1, 18.4. BLOOD SAWPLES ILC with PROS. Stafford ; SWPLE SPIKED LEVEL (ppm F) VEASURED LEVEL (ppm F) 1 50 4 56 : 2 15 19 3 Blank 0 4 L027 0.026 5 on ous 6 Lo . 12 hal 7 Blank 009 8 L058 L047 3 EN Et 10 054 L059 000094 EI$DP7R1O402033321 srw mane N | Barn cis ine 3 same | oe Wasn iaWASH 28; fls OO QR- SuroJd. SONICISwre=eng - orERaTORS 2 Sample = 00002 . . : . uy z A. - x =-5 . 58S . z 66001 Figse 2 o TEFL 18itOFGTCIcvoAOuHmEaVAkTsED 10 OHCELL - KRS~5WINDS Y 9 5i0F% "8 | 8i ! 8 f |t Q i Q 44 m aT ou 2Lgx2 &gZ| ~ | - 38 8 | o 8 | ao 00sL | i 0c" 0% 0652 FONYLLIWSNGHL % 000096 Q8 oC'G? - 7s0p7r1o4o0233z3 conmcmomnsccuaurreomn om pediEE aes ETH HHH Se oH EE el When rH Eh FC-143 SDI SALT & TRITON X100 1:5 RATIO SENET TE OERFLUORGADNOHYORIOE ABSORBANCE PEAK Tem nAhAaRRR THN he. HRS HH He HH =H . - -- := 3 OB = == a SE TRH t OTH Ee eeeeee Er EE == SeeFER eee op ree He ee S S E e h Es e e s s.=S eee ee ee eeee a "ert --tr--rr--It_trtt rarerret ---------- T Eee ere e =ee=0t" e= e 3 Ee eee te = ee == =] Er h--r ----r-- = ee eee - E eeS re EE I REEe ee fume = edEE ee m ee r e = = Ss EEe p r e eee ng = b See= =p =ee p e e=e Ee e =e i Heae . IOHSLLTWSNYE: % _ . 00009277 . ol : FIGURE 4 : - STGCANDRUANRDO0F.2C0-518o34 | + | 1205ppm r-------- -- | So ~T J -- pcm3 peRk Gas Aafs 20k: - owl Zuzesr Temp [10% Pe ie DeTEETAE sample 5128 3a 2d ee n- Et ToS TTI EE L205PPT EEE SORTER: in 000095 EE TTT 10s7er1o402033725 :Ya an ATTACHMENIT oc Lpgi.adamnt lSmi f= E. I. ow Pon oe Nemours & Company WILMINGTON. DELAWARE 19098 TK A Pa File - 32 apc seoR December 17, 1981 <SrPmRrUCoER,ETAEX.ITIE FIBERS RICHARD, VA. DST(ElRoUbINIoA.TIO51N1-G6P01P;ERFELTIAOLROYGeCaT.AN8O1A-T2E0.32I:N20A3Q5U:EOUNSotAsIsRookDITPoT.NGE6R1S6K7PLES 4/61 were 4anaxlayptoerstafdorbyperpfhluesro7o/c2t/u8n1,iuttehe(fC3o)uruasqiunigoutshesBiursisahprionmgesriossraamgphliees sseuibrmeidtted BRITA emits and sample Laenvification are as Foliove . Saemilseo. 1-23 Leomiticnsion SADCantaelmyaslytzses Stack at owier 6/29-1/2/81 is pe-liy/al (3) ae. (3) a311--a2s833 (w28) #132,, oStuatcekratof IDnrlyeter "" az #4, IsnabluesettioonTedfriyoenr " a0.d032 ado = (8) Cin-d14C3g (co1nceanmtarcanttiuomnpecraflleuaciraotoacdtaan8oatthee)svaalts.useTdheasLovcearliblriasittionforstgaunadamridi,letion was 0.007 ug/al. (b) ChohrercoyDm.laatnokgaryamas lfoorngesramapilre f3lezdpilfifnegrteidmeslmigghtrlyhaivneapfpiveeasranscedetfercosman#t3,s #L4e,veland jon Key voredesr:fiuorooctancate eels MrRlrsts S Seffner : 5. 5. stactord onal ingswit dinami sue 00009% 1s0e7r1o4o2033026 . ATATTTAACGHHEENT L1L1 WWwEETeHOD T31H6-/0048028-627 OU FONT FIBERS PRODUCTS : TEFLON FC-143 AALISTS Spru5.ancS.e FSihbeetrbsurnPelant Cee = E. L._Tedxutpiolnet FdeibeNresmouDrespar8tmCeo.n,t Inc. Richmond, Virginia. 2321 . 10so7R1o402033927 000100 MOETTEHOD T3/H1-60/48025-821 . PAGE 2'0F 10 Lo scope 1.1 TFhCi-s14m3etihnodairi,s wuasteedr,tobldoeosdcriabned sonamypalren.preparation and GC analysis for 2. PRINCIPLE OF METHOD 2.1 sdraymipnlge.s fYraormn fsnamapilre,swaatreersooarkebdlooind maertehafniorlsttocoenxcternatcrtatetdhebFyC-f1r4e3e.ze Tvhoelnatitlhee mFeCt-h1y8l3 1e5steers.terified by heating witn BFy/methanol to forn the . CF3{0F,)000uNat" + CHy--O3K CF3(CF,)g COOH, Thheexanree.actiThoen hfsexaqnueencshoeldutiwointhiswatsehrotanidntothea GeCstewrithextanracetleedctrionnto cpaepakturaereadetceocmtpoarr.isonThetoFCs-t1a4n3darcdosn.centration is determined based on 3. SIGNIFICANCE MD USE : 3.1 Tahnidsimnetbtlooodd.is uThseedaptpolidceatbelreminreanFgeCs-14a3reT:eflonyarn, in air, in water YAafrrn--0.530 p-pb100-01pppmpm WBaltoeord -- 00..0022 ppppmm -- 2255 ppppmm 4. INTERFERENCES 41 aestteerrfyuisntg abgeenrte.moved fron the samples to preventreaction with the 5. APPARATUS 5.1 GdaestecCthorromaantodgr5a8p8h0 -teHremwinlee]ttHePwalcektatrdPaSc68k0arwditChomNpi,as.electron capture 5.2 Argon/Methane Carrier Gas 96/57 - Burdett. 5.3 Syringe - Hamilton - 701 - 10 u1 - Supelco Co. 5.4 T1e58l.ematic Air Sampler - Taylor Parker Co., Norfolk, Virginia, Cat. No. 3 5.5 Bsaattat.eries, nickel-codmiun, 8.4 volts - Taylor 2arker Co., Cat. No. 5.6 Vicils - Sal, glass - Fisher Cat. 403-3388. | spRo00328 EID714240 000501 METHOD TH-0405-82T : PDAAGTEE 33/0176/8120 : 5.7 Erlenmeyer Flask - 250 w) Glass Stoppered - Fisher Cat. No. 10-047C. 5.8 GSCupeClocluomnCo.10 glass, packed with OV-202 on 100/120 Supelco port = 5.5 Heater - Fischer #11495-50 or eauivalent. 5.10 Sand Bath with copper tubes - Spruance Process Control Development. S01 Pipers L ml - Fister Cat. #13-6508; 5 al - Fisher Cat. f13-650F. 5.02 Manometer - Fisher Cat. #11-292 or eautvatent. 5.13 LyopiTizer - Fisher Cat. 71026941 or equivalent. 5.18 Freeze Ory Flasks (4), 360 m1 - Fisher Cat. 10-269-53. 5.05 VeqauciuvmalePnutn.p - Tuo Stage Kode] 0-25 - Fisher Cat. ho. 01-183-31 or 5.16 Piper Aspirator Bulb - Fisher Cat. #14-0708. ) 517 Imptrger Tube - LG-6850-100 - Scfentific Glass Co., Vineland, N.J. 5.08 Teflon cap liners - Supelco. - 5.19 Dewar Flask, 1 quart size - Fisher Cat. #10-1958. 5:20 facum system trap - LO-HI25-102 - Scientific Glass co., Vineland, 6. REAGENTS AND MATERIALS 6.1 5JoMeelt.hanol - Pesticide grade in glass ampoules - Supeelnco Cat. No. 6.2 Methanol - Fisher Cat. #2A-S36. 6.3 Hexane - Fisher Cat. #H-301. 6.4 Dry Ice - Richmond Ory Ice Company. 6.5 Acetone - Fisher Cat. KA-L7-5. 7. mecaUTIONS 7.1 BaFnyf/oMuelteh.anoWlear- WreuabrberTesgt)ohveersgwlhoevnespowuherninginoirtiapilpleytibnrge.aking the glass } 7:2 Year rubber gloves when handing methane] or hexane. Keep ova from 7.3 Wear leatner gloves when handling vials or heater and sand bath. 000102 E1sDe7r10402043120 MNETTEHOD T2/H1-60/48025-82T . PAGE 4 0F 10 - 7.4 Wear leather gloves when handing dry ice. 7.5 Bwliotohd.blooRdu,bbehreatglwoivtehs mcuosntcebnetrawtoerdn wbhleenachhanidnli2nghotblooovde.n aht e-n0fiCnisfhoerd oonveertobulro,gd.thenRinfsleushalldowpnipedtrsa,inbewictkherwaatnedr.otheUrseeqblueiapcmhentfnwi"t1h0:1bleraacthf.o 5 SweLNG 81 Ini 8.1.1 Psletacetur1n0ernlfoOIr woaneterhouirn. anFliomwpisnhgoeurldtubbee.setSetatt3ub1eteinrsT/emliennuattei.c anSdet Telenatic in area to be sampled. 82 Yam 8.2.1 No special sampling reauired. 83 Blo 8.3.1 Orbetfariingertahteorneucnetsislaryrebaldyoodforsaumspel.es fSereom7M.e5difcoarl.dispSotsoarle. fn : 5. CALIBRATION AND STANDARDIZATION . 9.1 FC-143 Standards 9.1.1 WVoeliugnhe0.w1it0h00megthoafnoFlC.-143Thiisntois2th1e0010ml00voplmumesttraincdarfdl.ask. Make to 9.1.2 Take 1 nl of 9.1.1 and dilute to 50 ml with methanol. This is the 50 pm standard. 9.1.3 Tsatkaenda5rdm.1 of 9.1.2 and dilute to 10 with methanol. This ds the 25-ppn 9.1.4 T10akeppm19s1tanodfar9d..1.1 and dilute to 1000 ml with methanol. This is the 9.1.5 Tpamkes5tanmdarodf.9.1.4 and dilute to 10 Al with methanol. This is the 9.1.6 pTamkest1a#n1darodf.9.1.4 and dflute to 10 ml with meethanol. This fs the 9.1.7 Tppamkest1amnldarodf.9.1.5 and dilute to 10 ml with methanol. This is the 0.5 9.1.8 Tppamkest1amn)darodf.9.1.6 and dilute to 10 ml with methanol. This is the 0.1 0004102 $PRO00330 E1D714242 . MEITEHOD T3/H1-60/48025-821 me 507 10 10. TLPRTOyCEoDUpREn(fRefzereenrcesOAptertaatcihomne)nt I, GC Conditions and Attachment I, 10.1 Yarn - Sintered and 181. 10.1.1 FAodrd {sinnlte`rmeedthyaanroln., w"eFiogrh108.15ya9rnt,o 0we.i0g0h010a.n0d5 putyarinntoto0.g0l0a0s1s v4,ial2.46 ta glass vial and add L 1 mechani+ 10.1.2 Atdedmp1eraaltuBrFa'Moefth6a5n.7o0l.C. Heat in sand bath for 15-20 minutes at sand 10.1.3 Rheemxaonvee. frTohnenbatshhakaendfaorllo3w0 stoecocnodosl.. Then add L ml DI Hy and 1 el 10.1.4 AFCl-l1o4w3TapyeearsATtofsse2pa.r9atmeinauntdess.hoot sample on GC (See Attachment 11. 10.1.5 SShionotteresdta-nda0.r5d,s (1.90.,1) 5t.h0a.tppbnracket the expected sample level. BT 16, 25, 30 pon 10.16 See 11.1 for calculation. 10.2 Inchir Somples : 10.2.1 vPiiaple.t on"Cearmelfuolflytphleacweateirt finroma FtrheeezienpOirnygerFlatsukb,e pIunttoona ctlheeanr,ushgelrasstop aUnydopnhoiolkize1r% utnotitlheLalylopthhie1iwzaetrer(iAsttgaocnhemen(t2-[31).rs.le)ave on the 10.2.2 Rgeivmeotrvh,ee tsPahnuedt'vsibaalTtherflrfaoonrre1tg5ha.es2k0feltmasikninutaentsdheaatvdida6lo5n-eT7op0a,l% osfcBreFw,'Mitethtaomennneotl enbdy place 10.2.3 HReexmaonvee. fraTnhentheshbaakethfaorrd30allsoewcontdos.cool. Then add 1 ml OI Hy0 and 1 51 10.2.4 A(lSleoewActtheachlmaeyenrts1t)o. separate and soot: the hexane layer on the GC. 10.2.5 Shoot the standards that bracket the sample (0.1, 0.5, 1.0 pp). 10.2.6 See 11.2 for calculation. 10.3 Hater 10.3.1 Bipet 1a) of vater nto a clean, glass vial. Then follow 10.2.1 - 000104 1s0e7R10402043331 MAETTEHOD T3/H1-60/48028-27 PAGE 80F 10 | 10.4 lose (See 7.5 for handling) 10.0.1 pi1)pofebltood into clean, glass ial, freeze ery ard ru 5 in 1. caLovATon na yam Ri pm ABre A = Sample & peak area 5 = Standard GC peak ares = Standard concentration, ppm 0 = Heftt of sample 112 Ale, tater, Blood Fetes pom b, A = Semple GC peak area 8 = Standard KC peak area = Standard concentration, pn 12. PRECISION AND ACCURACY 12.0 prectston 4s t 10%. i 13. REFERENCE - = BEB paeielsetad - Detention of Gg Flurssrfacan in ter 16. KEY S080 DioEX 16.1 FC-L63 - in yarn, water, air and blood. 142 a analysts. 0002.05 10s7vm1o802043432 METHOD TH-0405-827 ApaTcEe 377'10F6/8T2o Carrer Gas Injection Temperature Oven Temperature Detector Temperature Semple Size Coun Packing ATTACHYENT | HP_5680 GC CONDITIONS ArgonfMethane 95/5 20 ml/minute 180C 100% 00% 2m 6' Glass 1/8" 0 0V-202 on 100/120 Supelcoport. : GC Terntnal Conditions a - . - Run tine - 0.1 minutes Tan Skin. - Attenuation 2 (adjust as necessary for peak size) 000208 $PR000333 E1D714245 MTETEHOD T3/H1-80/48025-82T PAGE 80F 10 FREEZE DRYING SAVPLES Eautprent Setup 1. Put "500 ml of acetone in the lyophilizer tank. 2. Carefully acd erough dry fce to keep it as a solid. Replace 11d. 3. A36ddd "dr5y0fimcle taoceptaocnke atroouvnadcuuimt. trap Dewar. Set the vacuum trap in the Dewar and 4. Wook up heavy pup. Tee in wtahlelmarruobnbeetrertubbeitnwgeefnromthethetralpyoapnhdilipuzmepr. to the trap to the vacuum sample Setup 1. Tfackee/actehetonseammpilxetsurfen. theKeegplastshenviailmserasnedddliopngtheemnoufgnh thfeorIyCoopmnpil1eftzeerfrederzying. 2. oPflacTehetrheushferrozeonp,viapllasceinononetheofMtahsek farnedezceodmreyctflaskst.re 1Puyt0pahffiztelrerwiitnhtthehetop metal neck. : 3. Ovpaecnumt.he cAlolmnoetchtefrosn mtuostvacbuewmo.n veOnntl.y those ports being used can be open to : 4. Cut on the pump, open the manometer conenctions. Yacwm must be 0.1 m. 5. After freezing, shut off manometer, carefully open sample 1yopilizer port and cut off port. 000107 SPRO00334 EID714246 -- RE i Is 0 | 3 ; y IN fT 1. "3gif11 iIs TreI 5% ER = > & 4 Ei #4 Fg id i TRXN > 23 NC 000208 | ! TEST vETHOD APPROVAL "Teflone"-- 0F4C0-s1-88321Analysis" "m5.o5, Srhetburne site Authorizedsy For (Organization! Spruance Sir wos J5 PbreoecleossmeCnotntrol Tp evetome ent - spruce Process Control Lab Supervisor smoot. OMRKEIETEHOD 3THM/-880/480%25-82T --Soh rusnc--e nate L3/aat/e2 itr 000100 s1seor7o1o4023436 . ES . rasTmacT PTShooetbav7.i6n-1ss4ra3eti(vocinmsmopenrtvouecme]spsemerwafaslsuuroerad.o.Scuicsntpeaacmtioerad.t.ew)atteserurar.tfoagSceltnoa.ondt uaMsneeatchoyidansrnt.wheereiTneFdaleiovrne.e aabreers Jaonrgn,bloSgust tra terere: "IS aYTovHerhgsewaner'retwhhawiteelhlFC-bT1se4l3ocwodaitTceUad1r'b5vo:irtynlaadtnieesspewsrehsseinopnre,eastehenatds o5tn0o0.S7i0n0 S005 a1 off Cy and periuoroseptamononiydae.r IOEXING SUBJECTS 1. Measurement of perfiuorosctanotc acid (FE-143) tn air, water, yarn. 2. emontun perfloroactaraate dicarboxylation of. 3. Sodtum perfluorsoctanoate dfcarboxylation of. ) 1se0m7o104023437 000150 DISTRIBUTION copy No. LocATION 1 6.RBC..FaiHgalrepe,r,Jr.dr.-,R.- P0.CDDFeimlaerest Spruance 2 R. 7FD. JFainlies, Jr. W. T. Varoblak - Spruance 3 6.3.L7.L.WatHtesDan-teJl. H. Fischer - Spruance 4 E.2S0. FBirlienton - E. K. Koffenberger - Nesours-H11mington 5 0. 6. 0'ell - Nemours-K11aington 6 3. P. Yuk = 76D File Sprugnce 788 Research Library Sorunce . 94810 Central Report Index Centre Road ~ naz Patent Liaison File Centre Road 13 As,.sW.. VShoeklhbtuarrne-,7MD. FA.ilFeorte, Soruance 055001.27 000131 ES1PDR7O1040235038