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* ire Industrial Medicine CENTRAL RESEARCH & DEVELOPMENT DEPARTMENT Haskell Laboratory for Toxicology AR226-1614 cc: P. C. R. F. mening tan Resnick, PPD, E-269/411 Reinhardt/J. G. Aftosmis, wate.) o-#a vay 12, 1982 son: MEMO TO: bc. G. L. KHEeNRNOESDIYCRS Blerthand* ANALYSIS oF BLoOD SERUM FOR FC-143 aieEeAaEttach SE aEea SeproceSmEdIuNerEIeEn(fOoTrHneetThheiItirealidbiutonrmveeae.entyaJhnoeaLrleayx)steirxsatS.crotaecdtThcewoiisntcsheeenvrtaurpmoarti-sion S LeTO e neTeeeeLT mLincmaerniicvhosrienerecnaelertdisfshoemeecvhaapnoer.atioAnL,L of wrheiccehntsioiytshastutehge5e0nwsCo..rkthoeft Tbalvoecss sFe-ve1r4alLiyeamrasinlaygoasasnodcitahtaetdowfitHhasktehlel anesIthesneememsete,e o emeANtMhaSactiEaR ttnhhiaessea})n bilbioPtnydesTtoShoEeiixnnterstaschtthaoetfFnC-rcC1ore4ve3eaaltdemfnertnootxmbobsnnioedcrushunmd 2.4N HCL at room temperature seems inadequate to hydrolyze an amide or ester of FC-143. fosrtahcerrerTheeearaEciiodostoCtiFi,aa0nn(oCiFeR,0l)A,eaCFd,CSOS,HECsareiE nsophsyismiicli aalr taondFCc-hb1ie4m3icaalnd sxcumse : 000194 $ g EIDO72179 : ANALYSIS OF SERUM FOR FC-143 INTRODUCTION CFoCn-v1e4r3te1ds weixtthracdtieadzomfertohmanaen a(cDiAMd)ifiteodthseermuenthsyalmpleestweirthforheGxCa.ne/ether and PREPARATION OF DIAZOMETHANE USsoeluttihoenAlofdriDcihazoCmheemtihcaanleCformopamnyD'IsAZApLrDocaesdurdeetafiorled"Pbreelpoawr.ation of Etheral-Alcoholic 1. Preparation of etheral-alcoholic solutions of diazomethane: Einthawnaotler(9(58%,m1)25fmn1)a i1s00amdldeddistotilalisnoglutfiloanskoffitptoetdaswsiituhm hdryodprpoixnigdefu(n5n9e)l an3dcoannneecftfeidcietnottcwoondreencseeirvinsgetfdloawsnkswaridn fseorriedsi,stitlhleatsieocno.nd Tohfewhcioncdhencsoenrttahienssur2f0a-c3e0 molf etthheere.therT,heanidnlebtothtubreecoeifvetrhse asreeconcdoolreedceitvoer0.dips below Tahned aflassokluctioonntaionfin2g1.5t9he(a0.l1kalmioles)oluotfioDniaziasldheatiendabionuta w2a0t0emr boatfhettoher65i,s aTdadteidonthsrhoouuglhd atbhoeutdroeqpupailngtfhuennrealteinofabaodudtiti2o5n.minuWtheesn. thTehedrroaptpeingoffduinnsetlilcisonteimnptuye,d aunntoitlherth4e0dmilstoifllienthgerethiesradidsedcolsolrolwelsys.andThtehecodmibsitnieldlateitohnerails dfirseteizlelratceomcpoanrttamiennst aofbouatre3gfroifgerdaitaozrome(tshhaenlef 1anidfemuisstabboeutst2orweedekisn otrhe until weakly yellow). DKnioawznome0thaenxeplo1sdenoqtuitoenlyuneaxcccoeuendtianbgllyy. toHxeicn,ce,butALLitsWORsKoluWtIiToHnsDIAhZaOvMeETbHeAeNnE, rSeHgIaErLdDleIsNs EoFfFIChIoEwNTit HOiOs DSg.enerUasteedT,EFSLOHNOULsDleeBEvesCARonRIEalDl OUgTrouBnEdHINgDlasSsAFEjToYints. EXTRACTION oP3fl1a1c92e-000um5lp0)ta:oque2oA0udsmdl) aobifonutsa er55u0mmlml(ioffpollryeespasrgoepnttyhlanegnre2a0desmclrH,Celwadcfdaopllwoacwteeendrtritbofyugm1ea5ketmluabeofto(t9Na0al%lgevhnoeelxuamnee/ 7an0d% ettrhaenrs,ferShtahkeeh2exmainneu/teetsh,rhpighhasespeteodacegnlatsrsifuvgiael (1(2K,i0m0b0lerp6n0)357f)o.r 2 minutes RtSo2e1p5eb7ar5te)a]ke.xturpaEccvteainpotonrriafttuewgicevedi,als'eosalcihdcsontwtiiemtenhtswiatahtsta15i00nmlClesusnhdeexstraeneeal/esttshrpeearatuml[aiotf (mNS,acyietobnet2i0fniepcclesPsoraforduyCcitos, oifntNye:rn rsitnagndaurpdto(1 afallvoCldonPd\oCwOiOtNh itnheme9t0hahneoxla)n.e/10AddetDhetr uanndtifinujnedcetr5a1strienatoh the . g S 000195 EID072180 - Sz. GAS CHROMATOGRAPHY coLm m12e'sh(f1i/8t"ted0.4w.ith55)on-2c0o%luDmCn-20i0njeacntdio1n0.% Bentone 34 on Anakrom ABS, 100/110 PROGRAM Atnhenini1t0ia/lmint.emptoeraatufrinealoft5e0mpCeraisturperoogfra1m5e0d watit4h/ami6n.minf.orh9o.ld2.miInn.,jection 2t8emmpe/rmaitnu.reofis9520A0rC/,5 CelHe.ctron capture detector is 340C with a flow of DIscusson aTnhde ptehaekpceaokrrefosrpontdhiengmetthoyltheesmteetrhyolf etshteerCoofiFnCte-r1n4a3lwisltlandoacrcdurwialtl 11o.c1cumrin. 3613.9 min 8U5sin+g130%exotfraFcCt-i1o4n3s,asondeetcearnmineexdpec(tbot(hatGCthmeet2h-o1d0 yagndTewvietlh)ratodior-elcaobveelred/ pslcaisnmtaillsaatmiploens.counting standards) by adding known FC-143 to Red Cross wTihlel abboevethmeetshuobdjecctanofalsaoSbeeparuasteed wfroirttheunranproucreidnuerea.nalysis. That analysis Tthhee dientteercntaolr rsetsapnodnasred asnedrveesffitcheienpcuyrpoofsetohfe mDoAnMitroeraictnigont.he 6ICt iisnjaescstiuorne,d tthhaetref2o0re1 aonfy vtaheriaCy,tfonstainndarredsulctanantbeGCaccpuerakatearleyasaddfeodr ttohetCheatreset assasmuplmee,d T0izebde arnedspoannysenefcaecstosrasryapfpalcitcoarblaeppltioedFC-t1o43t.he FThCu-s143allarCeydo'pearlmaisttianrge onnoermato obtain an accurate FC-143 analysis. CALIBRATION mAetsthaanndoa,lrdthsioslutisionequoifvaFlEe-n1t43to1s1 pprge/pya1r.ed Absy adispsroelcvaiuntgion100priaogritno10D0AM,m1 aciddropconodfitpi-otnasl.uenesulfonic acid (15 in methanol) 1s added to assure 9r.afW. Belisle ce: BD..FW..NiHapgpeonldt- 2- 0210-11-15 000196 Sz 2 EIDO72181 =