Document 2No0OX6Y3QDRGJwQRByLJ6NO7

[.. -I, ;>70> 4 Hasten |v i: ct<c>i tm ti *s I III). u*tei onlh sped- k MW-ioi >, -370 .i. i). n,, I V Ml. 9, .\tl.\C49, IIWMI). m*mcsi, t.UhW 40, lew Ml, N. .' ChfHI. IS, Sxivnlny, "M. Wraith >* A`. SO, -:.l l*l.,' !:, 07i, _ f'kr*i*lry, .don, 1050, e&'.vT AHMoi'ii A^fi iiuiikk RMPAHATJNti PCM FHOM OUT AND ANAf/WJM Method foiSei>ur;iting rolychWinnlc.d Hij>licnyls from DOT and Ils Analogs 701 lly JUDITH A. AHMOI'II mill .1 I'll!IIY A. IIHHKK (Division of IVsli. iilo Cliomistry nml Toxicqli>#;v, I'VmmI nml Drug ArlniinixlinLiiin, Wnalnnulon, IJ.C. 20204) Polyrhlorhtnlcil biphenyl* nrr separated from IM)T nml ils Riinlnga nml oilier rnmimm rlilnrliinlrtl iirnlirlilr* by column diminnlng* mphy on aitieie neid-CcHle. PCII nr rliilnl to depth of oa I" in open beaker and heal >7 hr in Ioven. After heating, plum Ireaher in dcsirral nr and let cool to room temjwrMurc. CJnitkly wciRh silicic Aritl into glans-Mloppcrcd bottle arid add .1% from (be tnhnmt wlilt petroleum ether prior water hy pi|*cl (07 g silicic arid + 3 ml water > 3% to elution of prnticiilrn will* n mixturo of nrc- water). Ktoppcr hot.tlc tightly and seal with (ape to tonltrile, brume, nml methylene chloride. He- litstiro that container w air-tight. Shake well until nil termination of TCII mid pesticide* can ho mnde water in adsorbed; make sure (hot no lumps remain. mi the nrjinrntc column elunien wiilimil cross Platte Hcnlod container in desiccator and nllow to Interference. The method in applicable to Min< equilibrate 15 hr. Kclurn container to desiccator pie* prepnrrd hy nmllipest table residue melle immediately after uac. Desired activity remains for ndnlnpy nml should !w nppiirnlde to sample rx- about 5 dityn. (tnct* prepnrrd for gas chrmuntogrnphy hy (b) CrlUc --Af.id-wnshcd (JohtiH-Mniiville usual procedure*. Itecnverirn of Aroclnr** 1251 Gup); must he dry and freo of clcciron.capluriiig ml I2<0 and of nevernl ciilorinotcd pesticide* suhttlanccs. through the separation method ranged from (t) Solvents.--Petroleum ether, licxane, ncetmn- 76 to 100% and 00 to 107%, res|*cetivly. trile, and methylene chloride, Miitnblc for use in pe.stieido rcfilduo analysis; diKliiU'd-in-gloM product i* Dcsuhtrs of polychlorinated biphenyls (1'CD) have. boon reported in wildlife s|>ccic\ notably fish and fitdi-catiiig birds, by invosti^ulnrs ex mining; these xjwcimctis for residues of chlorinated pesticide* (1-8). Theso comiwmd* arc exirnctod and isoluted along with the jxsstiridea, and dotreted by gas chromntogrnpiiin (GLC) nytem satisfoclory (available from Burdick anti Jnr.kxmi Laboratories Inc., 1053 S. Harvey St., Muskegon, Mich. 40442). (d) Muting mixture.--1% r.colcnitrilo, 10% hex ane, and 80% mclhylcno chlorido (v/v/v). Pipet 10 ml acetonitrile into 1 L volumetric flask, add 190 ml hexane, and make to volume with methylene chloride. normnlly employed in analyses for chlorinated pesticides. _ Apparatuo The muUi|>cxticido residue methods employed by the Food and Drug Administration (0) com pletely recover PCD. Tho presence of the multi- (a) Chromatographic column.-' 400 X 22 mm id with 24/40 T outer joint, coarse fritted plate, and Teflon stopcock (Koalas Claes Go. K-420550, C-4, eom|K)uent PCII in a samplo examined for jtesti- - or equivalent). cido residues could interfere with or prohibit, (b) Separator!/ Juhncl.-- Used for column eluant identification and measurement of some chlori nated pesticides bocauso of similarity of GLC retention times. The objective of this investigation was to develop a method to separate PCD from DDT end analogs so that residues of pesticides and PCD each could be determined without inter ference from the other. , reservoir; 250 ml with Teflon stopcock, 24/40 f" in side joint on stem, and 24/40 T outaidc joint *t top (Kontes Ginas Co. K-G33Q30, or equivalent). (e) Adapter.--IIosc connector type, 24/40 T inner joint at bottom, Teflon stopcock (Kontes Glass Co.` K-18.WOO, or equivalent). . (d) Kuticrna-Danish evaporative concentrator,-- With Snyder column and collection tube, 500 ml capacity (Kontes Glnss Co. K-570000, or equiv ftongrrtte METHOD alent). (e) Air repulalor.--Or pressure-reducing tlcvirc to deliver ea 1 lb pronsuro. Air must be dry and rlcan. (a) Silicic acid,--Mallinckrodt, 100 mesh powder;' (f) Gat chromatograph,^Equipped with electron ^specially prepared for chromatographic analyst* by capture detootor and 0* X 4 mm id glass column of the method of JUmeey and Psttorson," analytical either (/) 10% DC-200 on 80-100 mesh Chromo- leafsnt No. 2847. Treat as follows: Piaes siliele acid sorb W HP or (I) 111 mixture of 16% QF-I plus I i I i i i t i l ) ms|i uiwsq iiampu1 we* iwppr.,mrqw L wye* w*a\*TT",,wWWVWux;fw MONS 082740 JotlUNAI. TIIK A MAI' (Vn|. .VI, N\i. -I, M7fl> |l% |)(V?UO in NO-IMO mrsli Chmmnsiiih W HI'. voir, m|M*d alolN'Mi k, Klmvly i)|iply nir |ii i-Hutin-, <u,,| Oftrnth'nff ron'IihniiK: witri*i;rii |2 mt/miit, i-uliimti remliime elution unlil nil rliinut pnM>* llirmiuh nitil ilMerlor lenqHu alin e injection ti-m|>erA- umn. Cnnrcttlrnic clunto t, -uiUililc dcfuiito vnlutm. ture 22"r('.. ('onrnilrir design rlrrlmn rnphnc <|r- for analyMis for DDT and mining.;, trclnr operated at dr wlt-nge to poaluro J full amIo winder <lcflrrti''H (of I ng hcptarhlnr rjH>xi(ic when Iti'HidlH and Dinfttissiim fnl^Hrnle deflection I X 10"* amp. PCH are widely usril imlustrinl chrmiral'. It< this country a series of 1'CM cnllerl ArTs-fors'*' (J(i) .VffNirntimi /'rorn/rirr arc produced; each Aroelor is a mixture i| Weigh f> r nrhl-waidtcd Oolite, ffitm 20 g activated cbJorifinled biphenyls (1200 series), ddorm.'itn) ailirie nr.Ul and combine in 2,'rfl mi (realtor. Imme tcrphenyln (MOO series), or a combination of diately slurry with W ml |>clrlcum cl her, mixing well. l'uiir slurry into chromatographic rnlumn with stopcock open and ootnplote transfer nf ailiric AcidCeltic mixture, rinsing honker with small portion* of petroleum ether. Apply nir prewnirc os necessary to force enough polroloitm ether from column to nllnw spare for nil silicic ariH-Celite. Stir material in col chlorinated biphenyls and terplienyls (4100 series). The last 2 digits of the identifying number indionlo the weight |*er cent chlorine. AroHnrs 1254 and 1200, hiplrettyls containing 54 am) 60% chlorine, respectively, were chosen ns represent.!live TCI) for this study. umn with glass rod In remove nir bubbles. Apply nir pressure to top uf column to net l ie udwtrUonl nod to force petroleum ether from eolunm. Continue to apply nir pressure wntil petroleum etiicr level U nlMUit 3 mm above Mirfare of gel. (iVotr: Do not nllow column to go dry or t crock at nny time during the procedure. Close stopcock when air pressure in not 'being Applied. At (tits point column of mUorbent /Intilytirni IMinvior nf l*CII Aroeblor 1200 was used in tests to determine tire behavior of PCU in FDA multipcstiriilc residue analytical nrethodolojiy (0). The I'Cll were eluted from a Florisil column with 200 ml 0% ethyl cthcr-pctrolcum direr. Several common chloriimtfd pesticides, including DDT and ana should be firm and not lone its ahapo if tipped.) Plncf 2,'AJ ml voHifnelric receiver under column to collect rltiAic. Toko a suitable aliquot of droned up sample (0% lrlnri*il ohmic) (0) conioining I'Cll and ' (H>T and its nnnlopi dissolved in not more than 5 nrl petmlnun ether. (Afafc: Large atmnihU of PCO and petdieidm placed on eolunm may result in incom plete separation. Choose aliquot to contain amounts of I'CB and pesticide* required for determination.) Wowl)' anil carefully add sample to column; do nof logs, are. also found in this olunte. Hccnvcriev of the TCI! added to spinach and butU ifal tniiRed from 84 to 00%. Gas chromatography of An>clilors 1221, 1212, 1254, 12C0, 1202, 14fi5, M I2, and 5400 on columns of 10% DC-200 and 15% QIM/10% DC-200 with electron capture de tection showed tire Aroriors to )>c rnullieoiupouent mixtures with retention times throughout and beyond the retention time range of common disturb (op of adsorbent. Apply slight air pressure chlorinated pesticides. With a detector sensitivity unlilsolventlovel kcs3 mm above adsorbent. Com plete transfer of sample to column, using small porturns of petroleum ether, and apply slight nir pres sure until solvent level is ea 3 mm above altaorbent. Hiuse walls of column with small portion of polrokmm etlior and again apply slight air pressure until solvent love) is ea 3 mm above adnorlrent. Dace res ervoir containing 290 ml petroleum ether on top of column, open stopcock, and slowly apply air pressure to reservoir until an elution rate of ea S ml/min is producing full scale recorder response, to 1 ng hcptacidor epoxide, significant responses were ob tained with about 10-20 ng of tho various Arochv*. Initial attempts at separating PCH from DDT and its analogs included a nitration procedure, which gave poor results, consistent with those reported by Reynolds (!!) A method of separa ting PCR from DDT and its analogs was sought which would not alter these com|>ouiKls chemi established. Continue elution until eluate volume is cally but would Icavo them unchanged for exactly 2!>0 ml. Slop elution. Quantitatively transfer chiate to Kmlonm-Danwh conocntrntor and reduco volume to that neenwary for analysis for TCI). Plaee Kudcrna-IJanisli concentrator fitted with collectkm lube under column to oolleet second elnnto and any remaining petroleum ether oluant. Apply air pressure until petroleum ether eluant level is ea 3 . mm above adsorbent. Add 200 ml acetonitrilchexano-orethyieno chloride (1 + ) + 80) to reser individual analysis and which would be applicable to the G% ethyl otlrer-|>ctroleum ether Florisil chmlo in FDA's rmilli|X'*liridc residue method ology (0). Column chromatography met tlreso criteria and attempts nt separation were made using Florisil as the adsorbent with petroleum ethor eluant. Arochloi 1260 and p,p'-DDE were not separated and there was only a small margin ..r . . DDT. .. .iri C-.bim.i liirn ii*--1 Minlie "I ' tf .; i1 l"': : ' Ins'- i; * i-lutum ; nonhii'H in these ri ' nl silicon . chniiRC n vnr:e.*..*rh low' to alt but woui' rcmov.if i i fi IS MONS 082741 In KM <r w-t III) ilvr , I'. i'i'll > ImI . .v*l Ni>*> 11*.\ AND HI>IIKK?>lil'AtMrrNa rcn 1H0M Din' AND anai/xih 7M ,4 M'jomliim Wtwwu Arnrlor 12C*n und |lDT. The *rp:trnlutu \\n* uni im(>rovrrl by variufimi of p,-mimrlcrN of the rhninmtogrnph.v. >ilirir Aritl Column eltiUMnfnmj4\y no mlific i* hI w iIh-u (`'Ido wn mixed wiLli Urn iwirl In m-hirve n fiisfer elation rale. from Ikrinlwwlictit enhrnm. litil.ini findings indicated A>i ini could lie elided from (lie column with p4rotrMn ether before elution of DDT and ntinV<v. However, there wak an incouwKUmcy in the rluliim pnlfrrn of Arnrlor 1200 and D!>T nud wings in Infer ex|>n intents. The only variable in tlw.w liial* was the lime of heating silicic acid at I30*(\ Silicic arid (si)icn gel) in a hydrated 4lron oxide (KiO/.nlU-O) whose activity will taugc a* Uie amount of physically bouml water Tlic l.10*C temperature of heating wan too low lo altar tlio structure of Kurfaco active aitoa M would have caused elimination or partial mnoviri of physically bound water (12-14). The effect of wafer wtilrnl of wlinc arid on elution and Ne|Kir:ifi<m of Arnrlor 12<*0 n'nd DDT analogs is shown in Kig. I. Silicic arid was heated n(. for several d,v before equilibrating willi 0 IH% (w/w) wilier. A mixture of Arnrlor ,/'- rim) )T, p,/i*-TI)K, ami /,/'- 1>I)1*J were, elided from column* of siUrin aeirl of various moisture content, using poUolrum ether ns the elunnt. The maximum margin of separation of PCI! from pesticides, with good reproducibility of elution pattern, wan obtained with silicic acid containing 3% wafer. A more polar eluant wnn required for complete elution of p,pM)DTnnd -TDK when water content was 6% or less. Aroclor 1200 was completely eluted with 200 ini petroleum ether; 250 mi eluant was required for complrto recovery of Aroclor 12M. When more than 6% watbr was ndded, activity was decreased to tho extent that rctcntivcncss was lost. In early experiments it appeared that the se|Mration of PCB and pesticides was affected by ml rmoutw rr*a iuuw t :. i, \\. \ vi !i *4- : ir 11 :ii I !. 1 ? ) | f#- 1-CSmI l ftlttclt icM wetor coolant on elution ind leparotlon |( Aroclor 12(0 ond POT ond onofogt. j' ** frocifSNO of potrotoum othor oluata tnciytcd by 6CC; utpttlMi tompound found procont In votumoc ' '"d by hoHxonui lino. Vonous poior oiuonts mod to oiuto poitleidss C, 0, ond C. A, Aroclor 12W; B, a^'.DOCi \ a.**'.OOT i C. p*'.TOE. ,, .,, X "--***?" v. MONS 082742 ^ l I' < i '4 physical variable* n 11 rnrlnot in tlu* prcpar.'ifion ami elution of the silicic ncbl-CcUli* column. It T*b 1. ReaVArl* and pftllon Arclor n4 sMwln*l*d patllclds* ddrd lo tilldc Add toluo.n wan possible In nliservc some imdesmihh* HTrcli* and llirir causative factors by eluting P&C Green No. 4 dvr from column* of silicic arid . fVtifr. I'neven adwirpliim nod widening of MiC Chemical Added, Found, No. MR % Tilde Duel* I* Rn"R<\ % Vtulion band orrurred whenever the column of Arfrarltent wan allowed to go dry or tn crack. Similar effects on the elution Kami wrro noted when water was not first added to the silicic acid. Aror.lor 1264 Aroclor 1260 Aldrin 40 20-40 1 100* OS 100* 101 Etude r 10 It 4 9VIf 90 100s 100 101 It wax aasumed Hint elution of POR and pesti cide* wax nlao adversely affected by these con ditions. I Experiments with time of heating showed that . silicic acid should Ire braird a minimum of 7 hr at 130C Ixifore re-establishing the water content to 3%. Silicic acid remained satisfactory for uae Llndono HC(itcMor Hoplochlor epoilde Dleldrln Endrin p.p'-DDE cji'oor pjd-DDT S^'TDC 0.9 1 1 1 1 5 io 10 9 96 9) 100 104 94 99 91 9B 97 4 94 ICO 4 #H ->8 4 90104 2 102 106 4 9) 90 II 10-106 14 9110) IS 90 100 IS 17107 . after heating for periods up to 30 days nt 130*C. However, low recoveries of pesticide* were ob- tainod from adsorbent heated for 40-80 days. . J.T. Baker, Merck, and Mallmckrodt, "ana . lyltcal grnde," 100 mesh, silicic ncirls, witli similar * 260 ml petroleum ether. * Rocovtrlee estimated; no Arocior preeenl in eecond eiuete. * 200 ml cetonllrlle-heKene-methylene chloride <1 + 19 + 10). statements of imiwritics, were found to perform satisfactorily after treatment ns described under Method. Mallinckrodt silicic acid (a) was the samples and various techniques ore available for adsorbent of choirc, since *pcoinl testing by the determining aldrin. Recoveries of Aroclnrs 1251 ' manufacturer insures a 8|>ccifc performance and and 12G0 and jKwltcidcs arc given in Table I. sliould lessen lot-to-h>t variation. Six lots of this, Arudors 1221, 1232, 1202, 6442, and 54GO woro material manufactured over a 2-year period have also completely separated from itcslirides by the been evaluated; all were satisfactory and re petroleum ether elution. The multicomitoncnl producible in their performance. pesticides, chlordanc and toxnplicnc, were eluted by the polar eluant and did not interfere with tmr/armtmce of Svpora (ion PCB. An adsorbent column of 20 g silicic acid (con There is only a small margin of separatum taining 3% added water) plus 5 g Olile was between PCB and p.p'-DDE. The elution of PCIi determined to be the best for sctMirnting 1*011 with petroleum ether should he stopped just as from DDT and analogs. The separation was the eluate volume renehos 250 ml. A trace of -accomplished by eluting PCB with 250 ml polar solvent in tho sample placed on the column petroleum ether followed by elution of DDT and will result in elution of tome p,p-DDE with I'CH. - analogs with 200 ml eluant of acetonitrile-hexane Samples should be in |>ctrolcum ether solution ' mcthylcno chloride (1 4- 10 -f 80). DDT and and placed on the column in a volume not greater ' analogs are eluted by the first 100-126 ml of tho than 5 ml. Separation of PCB nnd pesticides may . second eluant. In addition to o,p'- and p,p'-DDT, not bo eomplctc if excessive amounts of these , pji'-DDF., and p.p'-TDE, complete recovery of compound* tire present in the wimple placed on ' lindane, heplnchlor, hcptachlor epoxido, dicldrin, the silicic acid column. Estimation of the nmnunl - and endrin was obtained by the second elution. of PCR present erm he made from gas chroma Aldrin was eluted with PCB. With the exception tography before separation. The wimple aliquot * of dicldrin and rndrin, all these pesticides and should bo chosen to contain only the amounts of PCB am found in (lie 6% ethyl ether-petroleum pcstioido and PCB required for determination. i ether Fioritil eluate. The inability to separate For example, with tho QLC sensitivity described / aldrin from PCB is not a problem, as aldrin it earlier, we would choooo an aliquot containing : lardy proaent as a residue in environmental about 20 ms PCD. If the eluate from the silicic I t I I i * - No I. i * Tinui acid rob Ire :i mu tion. /t/ifilir* renr. oi A i :iud : : hrnv i. pr-lid.. tnin (*nl tht rr. column fortifi."'! mlii>. 12:.;, * (2Ie\W tr-i. licuiiot. were pi into 21 CI.C t giv.-H i tun* U Fig. 2. lyi'stPW rasgra MONS 08*743  aaiI nliinin SVtOO^ o> too* 1mi ir ' v* MMOt *) fc. 00106 ' 1M0) 10)06 Mor . IMM Ift iftCOAO Mti0(l 4-. .v .ilnMt* lor . I..rv 1251 ''/`*nblc I. i^/'iti wore t.li-4 try the : .!nm,vHH*it mmp rliitfil '.i.Vre with - H'jwiTttioii iimii of PCI) ,;mI just RN . A tnire of * the column im i.i*r wtlutimt not greater . tiriilim mn.v hum of these |4urcvl nil llif Amount . ci" clironifl* *nt|4d nlii|oot .f amount* nf .rtcrminntwHi. | uly drxrilwd .-t containing rnm the ailirio MtMOim AND I^KKK: HIvPAIlATINO ITU I'UOM 1I*T AND AMAMHiH 755 Tt>l 2. Rutvtfltl ind p#ftlon o< AroMors unri cMtrlnMei) pAitlciftv* adrfod to fru) tilricl and put tlwot'iiti Ilia aillelc acid column , % Recovery ^ Chemical Eluale 1" Added, --------------- --------------------------- ppm Trial 1 Tflnl 2 Trial 9 Eluate 2* Trial 1 Trial 2 Trial i levrf J Ator.lor l?M Aiorloi 1260 p.p'-DDt pji'-tDC p.i.'DDT 7.0 2.0 0.15' 0. IS 0.M 100 .0 0 0 - 76 , 0 0 0 95 - 0 0 0 0-0 - 0-- 100 100 96 96 19 . 90 100 90 06 Aroclnr IISI Aioclor 1260 pp'-OOt PJ.-TOC p^j'.ODT 20.0 20.0 2.5' 2.5 6.0 -- 100 0 0 0 . 76 1-- 0 0 0 --0 o --. 10 102 90 101 II too * 250 ml patrelaum ether. 200 ml ecolonltrllo-heKene-methyleno chloride (1 +19 +10). ,. * No fortification. 4 Trout contained 0.19 ppm p,p'.ODE. Recovery determined on amount added plut residue. -- -- -- -- ariil rnlnnm wo* concentrated to 5 ml this would hr a mutable concentration for CLC determina tion. /Ip/rlirnfi'oo rtf Methoil ftpnrntiuit of 1'CH from DDT and analogs nnd rrfuvcry determinations were made on mixtures nfArwInr 1251 or 1200 and p,p'-DDT, p,p'-TD10, ami p,//-DDI5 odded to cleaned up extracts of hrowii trout. The trout was analyzed by multiIVHliciric residue methods (0) and found to con tain only p,p'*DDJ5 at 0.10 ppm. Five portions of the 0% ethyl ctlior-|>ctroleum ether Florisil column cluatc, each equivalent to 20 g fish, were fortified with a PCB-pcaticido mixture. Fortifi- ralion was at 2 levels: (/) 40 pg (2.0 ppm) Aroclor 1254,0 pg (0.30 ppm) p.p'-DDT, 3 pg (0.15 ppm) p.p'-TD)5, and 3 pg (0.15 ppm) p,p'-l)D15; () 400 pg (20.0 ppm) Aroclor 1254,100 pg (5.0 ppm) y.p'-DDT, 60 pg (2.5 ppm) p,p'-TDE, and 50 pg (2.5 ppm) p,p'-l)DE. In a second trial at each level Aroclor 1200 wun substituted for Aroclor 1254. Three trials were made at the lower forti fication level. The fortified Flori.sil column cluntcn ere placed on the silicic acid column, separated into 2 fractions, and analysed by electron capture f*l as described under Method. Results are riven in Table 2. Gaa chromatograms of the mix- Uw before and after separation are .shown in ti2. .. Lake Michigan coho nalmon with residues of PCI) nnd pesticide* resulting from environmental exjiosnrc was extracted and denned up by multi pesticide residue methodology (9) prior to separa tion and measurement of l'CH and |>ostieidrs. A 1 mi aliquot of the concentrated 6% ethyl etherl>clroicum ether Florisil column cluatc, equiva lent to 5.4 g fish, was placed on the silicic acid column, separated into 2 fractions, and analyzed by electron capture GLC as described. The gns chromatograms in Fig. 3 show u good separation of PCB from DDT and analogs. Determination by electron capture GLC showed the salmon to contain 14.6 ppm PCB, 3.2 ppm p,p'-DDT, 1.3 ppm o,p'-DDT, 10.4 ppm p,p'-DDE, and 0.4 ppm o.p'-DDK. PCB rcsiduo was measured in terms of Aroclor 1254, using total area of the gns chromatographic response. "GLC retention times, a positive microcoulomctric halogen rc*|K>hHC for all GLC peaks, and iwlmvior on the silicic acid column showed the residue in the first cluatc to bo PCB. Retention times nnd a positive microcoulomctric halogen rcs|>onsc indicated the identity of DDT nnd analogs. Thin layer chroma tography and dchydrohnlogcnation with alkali confirmed the identity of the DDT isomera. Most pectrometry identified p,p'-DDE. |UNwi Min) 9,1970. "'ll.!.* >fsssw|e*iw'**' 1 i i . ......... HONS 082744 I iI i Wfl \ JOUIINAb OK TIIK AOAC (Vol. .VI, No. I, 1070) 1 j I I. I i i l ' FlO. t-?6l.C Gn)M Of krawn Irout tttnd (orUliid with 2.0 ppm Araclor 1254, 0.2 ppm ,p'-ODT. 0.29 ppm p.p'- | . TOC, and 0.25 ppm p.p'.OOE (pint 0.10 ppm rotldua) before and after teparatlon on allicle acid column; A, botora > eeparatloni 0. pdnlwiw ether alvate from alilele add column containing PCOt C, polar aluolo tram alllclo acid ; . ealumn containing (1) p.pVDDE, (2) p.p'-TOC, and (3> p.p'-OOT. 10 mg aamplt Injected for aach curve. ClC ; . tenditlana given under Method. ric. ' b-.'.'U'. act* <22 Cfor ............................... vi.iniiiui^iaiptw.i HONS 082745 iip . i, |H7O/ |flMor>l A^l) UVIlKISi 8H1AIIAT1N0 PCH KIlOM OUT AND ANAMXlft OT, All pm m'> flO. 1 mr twwi if Uhl MicMfan coho salmon aatroct containing ratldua* of PCS ml DOT ami analogs boloro end aflor separation on athlete add eotumnr A, before separations O, petroleum etber eluate Irom aitkie ttH COMMM epnlabltr* 14.* ppm PC (at Areder 1234)| C. polar elude Irom tlllclc acid column centelnln* m 0.40 ppm o*'-DDE. (2) 10.4 ppm p.p'-OOC. (3) 1.3 ppm a.p'-DDT, <4) 3.2 ppm P.p'-ODT. 2.7 m aimplo Injected tm curvet A. O, and C* 0.10 mg tamplo Injected for curve C, utod for Pf'-OOt euarHNatton. OkC cendWeno .- (Ivon undor Method. . 7 M0NS 082746 7SK joniiNAi. ok mi; aoai: (Vi*I. .VI, i (tmtrltiNM.it Tin* mrlhod drvHi|>rd for nrpninlin;; P(!ll O'U , \'i,h,r, ?U>, Ttl T2't (I'lr.V) (5) Untdm, A. V., Mini Mnrwlrn, K., V 210, from chlorinated jnvdiridrs is routinely 1274 12711 (11107). ' apidirtddc to samplra |rr|mrr<l for (MX! |K\slindi* (0) llhiphrinigh, It, W.,Itrh'hli', l'.f fl<-i * . i;, . ivkuIuc nnnly.w. Its uxr hy l; I h>r;itoi i<'s analysing I'eukntl, I), II., mul Kirvrt:, M. N . ' I00K.II02 (WfH). ??0, ' fr pesticide mklur.s should I'liininnU' any doubt (7) JConninn, J. H., ten Nrvnr lie Min \t C( or the validity of residue data, particularly Ihosc mil He Vns, 11. II., iXnlurr 221, I! Jr". | !'.* ' data for DDT mwl nonions. The separation of PCU from chlorinated |>cs1indcs will also permit (H) Ilwrbrmigli, H. W., Hrirhlr, P., ami (* ' <t, ri. no accurate nssrwoncnt of the PCI) contribution R., Hull, linviron. Contain. Torirnl. 4, f2 20| to environmental pollution. The coho mlmon (I0GH). r example pmented here is additional evidence of (0) /V.ificirfe Anahjlir/il Manual, Vol. 1, F'.nl aihI Uio presence of FCU in some parts of the aquatic. Drug Administration, Washington, D C,. I0GK. environment in this country. (10) Aroelor Platiciteri, Tcrhmcnl Bulletin D/)Mr 300, Monsanto Co., fit. leuii, Mo. ItermiKNCBs (11) Hoynoids, L. M-, Hull. Environ. Contam. Toxicol. 4, 125-143 (1000). (1) Rotiurn, i^Anal\& 90, 467-475 (1055). (12) Rnydor, L. R., Sopor, Set. 1, 101-219 (I0GC). (2) Holden, A. V., J. Appi. BcU. J(flappl.), 45 (13) Snyder, L. R., J. Chromatog, 11, ]9;V2i7 (1066). (1003). Mr. MU l,-nr * 0) Wtdmark, 0., JAOAC SO, 1000 (1007). (14) Snyder, L. R., V. CKrotnotog. 25, 274-203 . (4) Holms*, D. ., Simmon*, J. H., and TaUon, J. (1000). . M ! m)i MM- I. rn.; N If,a eni: rh'.i lilll' CM (i.> a e\;> Him. n\i eld. (0), hyd aim I**'..i I CS. y*!"; '''`'"Wffi*}vyiiyjiTi;;'^M'1 1 iw- MONS 062 747