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Ela ka i For:n .3747-1 't-A I CAun bh Fm3R2FRL TECHNICAL REPORT SUMMARY oD ayt5e /22/79 :. T HNtCAL REPORT SUMMARY. 5/22/79 ,..., TO: TECHNICAL COMMUNICATIONS CENTER -- 20120N TO: TECHNICAL COMMUNICATIONS CENTER - 201-2CN paras sport'spreton osts ts , ee) (Important - If report is printed on both sides ofpaper, send two copies to TCC.) Wt wel 2 L i . Division wo RT Project EEnnvviirroonnmmeennttaall LLaabboorraattoorryy ((EBEE && PPCC)) ~ ' '..~',.:' ozs kv j'Oept. Number Decatur, Alabama - Temessee River Fish Alor Decatur, Alabama - Tennessee River Fish Report Title ; Bioaccumulation of Fluorochemicals in Tenn. River Fish | [01 o..v' Bioaccumulation of Fluorochemicals in Tenn. River Fish I ~O01 ,~.,,~ To D. L. Bacon D. L. Bacon a ee Author(s) Employee Number{s) James E. Gagnon 213501 James E. Gagnon 213531 NO. of Png~s Incl~=dingCovorshoet S158 10 51568 10 I ~C Sp e I a Ba SECURITY ~, '~ Open (Company Confidential) Closed ecialAuthorization) 3M CHEMICAL REGISTRY New Chemicals Reported [] Yes [] No emonos, CURENTOBJECTIVE: Qualitative und quantitative determination of KEYWOROS; (Select terrr~ from 3M Tem Smmoer | yE#-3928, FM-3925, and FN-3422 in fish taken from the Thesaurus. Suggest other CURRENT OBJECTIVE; Qualitative and quantitative determination of , FM-3925, and FM-3422 in fish taken from the = Tennessee River Above and below Whceler Dam at Sis applicable terms.] Tennessee River above and below Wheeler Dam at 3M's Decatur plant. Analyze for organic and inorganic Decatur plant. Analyze for organic and inorganic _-- Tluoride in the same sunples. EE & PC 1uoride in the same samples. Decatur Decatur gph0 ort a- EE RT ea mm REPORT ABSTRACT: (200-250 words) Thi.~ abstract information is distributed by the Technical Communications Center to alert 3M'ers to Cnmpnny R&D. It is Comport\ confidential material. gel udyr Ke wPr A ~bTeioswacsounSuhloawtnedthat nd thro fluorochomicals of inorese oe CheC7] bat0ab.ado0v0te4a aWcphpomermbeeiplnreeordduDcamFmto-,ir3v9e0ew2ar3sse,yasdftiLoelHumy-n3d9oi2fnt0o;tthhceooanntdgcahaiasFnntHnr-eoOoli4nn5l%tyceacsCFttoHiin.scn3hoa9,n2lt5i.wtmhreaitcliteo,n 2s e | CcCohhomaambnnbinnineenelleddccatatottottffaaiillss,,hh 22((..ZI77o~44ttaa@lpluppurmmru~oaanndpdpuun1n1c..c1t1t3a3attupp~spp))mm,, hhaaooddff ttFFhh-~ee3-3990ll22aa33rr,,ggeesstt or M-1-33992255,, aanndd FFMM--33442222,, aass ddeetteerrmmiinneedd bbyy ggaass cchhrroommaattooggrraapphhyy.. t was shown that the three fluorochemicals of interest bioaccumulated more readily in the gastrointestinal tract, wnfnohaotitftellanuubdoourrsoroscechphere(momfidiocucaacamltlssisvewwoeehrrrseeyynsotoopebbnmss)ee,rrovvfeeLddtahkeeiinnn cthtfhahreneonmemmluubssecclclloaeewtfiWllsahahyye,eeerrl..wehrilADAeam, white bass (Roce~+n ol~inol,~), taken ~rom below Wheeler Dam, had a combined FM-3923, FM-3925, and F~-3422 concentration ooff 00..4400 ppppmm.. AA w whhiittee ccrraappppiiee ((PPoom~oow~xies ~ anZ nu~ la riss)),, ffrroomm above Wheeler Dam, was found to contain only FM-3923, 0.004 pDm. Total organic fluoride ranged from 9.7 ppm, channel catfish, Total organic fluoride ranged ~rom 9.7 to 16.2 ppm, white crappie; Inorganic Fluoride ranged to 16.2 ppm, white crappie. Inorganic Irom 6.2 bpm, white bass, to 24.6 pon, channel catfish. from 6.2 ppm, white bass, to 24.6 ppm, ppm, channel catfish, fluoride ranged channel catfish. Future Studies: TLC on above Tish samples. Future Studies: . I BGaCc/kSgroonundchafnlnueolrocchatofniischalsaamnpalleyss.is c3c%: D Di.Rgihcekrer.-o2u36--22b A.Welter Allende] A,Mendel TLC on above fish samples. GC/MS on channel catfish samples. Booannckaagroccurranadppppifieleuoffrrrooom cmheaamM~iicinnannl eesasoonttaaalyLLsaiaskkee.. I r~fo rmation Initials: ZV L~.~. ~J smconmoeTIaL 3M CON FIDENTIAL WSMuaabcdjeeecAAtvvtaaoiilPaarbbollteeebbcyyiv33eMMOrffodorrerIrnsIsnppePecctatioonmn aavnn.ddSCCWo,oppyNyoii.nnggC2aa.ss0CC4o-on5nf3ifid0de5ennttiiaall IInnffoorrmmaattiioonn: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00000011 EExxhhiibbiitt otra] 11220088 State of Minnesota v. 3M Co., Court File No. 27-CV-10-28862 ors 3MA01409559 2 '`~feenmnn.. RRiivveerr FFiissnh//JJEEGG z= 5/22/79 5/22/79 INTRODUCTION INTRODUCTION oIItrtgaiisnsickknnoofwwlnnuotrthhiadatet 33lM ue'v'seslsDD,eecca1at0tu.ur9r,, pAA plmlaabb(aa1m)m(aa2)pp.llaanntItt eehffafflsluueeannltstohhbaaessenhhiiggShhhown that rofflolrugnuomaorenronoictcchheef(m lm3ui)ioc(c4ara)lild.sse ccaaWlennivthbbeiilosota,ahececsc1ueu0m m.9uculolampaptbtmeeine(iind1n )(fff2iiassc)hht. oriisnnI,t aahthallaesabbmooaerlrsxaaotttoorrbsyyeteenpeennwvsvhaiios--wn that rtptooolnamnssteceeenhtaiifdf(3dff)iei(s4tshhe)c. tccaaabW uulggiehhttht lteiihnnveesltthesheeocofTTm eenfnbnlnienuesoesdsrseoeecefhaecRRmitiiovvcereasrrl,snn.etehaaerr the Decatur next step was the Decatur plant had detectable levels of fluorochemicals, RREESSUULLTTSS AANNDD DDIISSCCUUSSSSITOONN wwToThfhaaiibbcclliehhente1hh1raaevvllseeiitssttttsshh(eeFUtt-hhss3eeaa9mm2eecc3oo,rnnrcceeeettFnneeNttn-nrr3ttaa9iit2too5iinn,oonntt,,aiinmmedeiinn FaaspspHpp-mm3tt,,4hh2ee2ii)nntt.hhrrffeeiieesshhffololffuuoorrccooooccmmhhppeeoommuuiinnccddaassllss of interest (FM-3923, FM-3925, and FM-3422). ASAannmaaplllyyessiiss34,ooffstthhhoewesrreetshsauutllttsstheffoorr{lttuhhoeeroddcihissessmeeiccctateeldds cbchhiacancnnonenelclenccatatrtfafiitssehh,,to a : Sgagnrardm eeaaptftleeeartr.3Aeex,xtIteetshnnotctwansiinnathltthahseeot btggheaaessstterfrleoouniionnrtttoehecasshttteiinm ntahaiellcamttlrusrasacccbtlti,oe, crroleeanppycerreoronddtwuuracacsttteiivvfeetoounssyydassttneeommt,, tatronoedsbbuilifotoaasatcc.ccauugm mrIuetulelacatwateneithtathhlseeeoatrthbhlrerieeeeerseerffnlelupuooothrrrotaocscthheet(hm m3ei)ic(c4ama)llu.ssscooleff interest. layer was interest. These found not These ! results agree with earlier reports (3)(4). W Wthwheoennwhccooolmmeppaarfriiinnsghg tsthahemepltteoostt,aalltfhfelluuoolrraoorccghheeerm micichcaaalnlneccloonntcteaentntftis((ThTFFCCc)o) ntffoaoirrnetthdheemore StSttewhihxiannoapnnccleew antthwawbbotiooilcictethoeehnfittfTshihfihseeoshrhsffalw wtl~mheueoiroprrseelrQ -o~ccmccsahaah, yuueegmm gthhibhietcetcaaliirilannercclgoaottehnthn~eteetedensesnta~attm ,,moaeen2t2n.haa.e77errl44eeaahc,,ippapgptmhafamisvrvrphesaes.ara. stscoio11ont.n.n1i1aat3o3babnlilneeppeppcdm mo.e. m ffoirceients aeafflonnxouddrrporlcsascoihihncnnaaahccnnteeiennoneeinlm mlcooarcfcrloeaeastrtffffiwaiatshstothhttuiy.syl. dmttibiFFasesyllsusuubuoeoeeexrropoeccriisceshh.telepaempmrdtiree.icecdsasaelelnsnstottbbitiiihononaeacctthcchhueeuigm mhullualalarpragtgtaeeeerrrtiiintnffiiiossfPnhhaa,,ttttcyymmoooerttrfieeifssisscuuieee,n, ts ; fluoroehemicals would be expected. TctFcihHhMo-aa-n3nn39n9n2er2e3l3altecciisassattfphpfiirarsseevh hses,ee, nnntosstatam maatpbtpleleeehhniigg33AA hhd,ee, rtretthrcchaanoonninnncceeooednttnhhtterefrraoratrtiissoaoaFnm nmNpss-pl3le9iiesn2ns.3.,tthheeSSnioinnddccieieessxsspeebblccaiiottnceaeaudcdtccicuoum nmsiullaa-- fortion for the higher rates have the higher conceatrations can be not been determined concentrations Can be offered for FM-3923, offered no explanations rTtTrihhihgaegeotorrttw ootwuouhoessllffyyicissohhrcceoom smsapaspm amaarpmrpelpelddleeesssttoww ohmhiw awicyhchhhoolnleeohhtaaddffihiscacshvooherreessassarm mepttppalarklekeeseess.nn.entffraTTrohtohmemie vetrtrheheeaceamsmosoonnnww cieilnffllotol rrr anntootth tiht oiisnbsbseo iiss Stoohfif nacTftlelutuohocrerooorcecchhoeesrm emaimicpscaalam lelsssplwe((w eswrhhem oolaleeytaknffeioisnsthh,hfvavravaolemluueetrssehepm mraeaayypsepbbrnoeotxahihtimiivggaehhteeercr soaoonrmrceellnooltw worecaeratr)ti)oi. n ons, the results can be Since core samples the results can be rigorously were taken rigorously compared. from the qompared. approximate same location, TTfhihese h Dfaism,h wwhhTiiIttCeeobfbaas0sss.40ffrroopmpmm,bbeelwlohowwilWeWhheteehel% eeerwq.hDDiatamme,,~ TsFaCmploef 024.4, 0happdm,& w whhoillee tfhieshwThFiCteo cssraaam mpppplileee fcra0p.0p0ie4 fI1rBBo,, m pfrpomm . hhaaaddbovaaew wWhhhooelleeeler aWbiotvhe such Wheeler soDsllam fmaam raraglgh,leelilrrgsahssm TeTttrFa FapCCttleiifssiilstts2uiAioccdrd, aauoulhecelahdesosoamannm milalypcyplawlelttehsooso,,cleotthhni1eettcfiesw W nwwhtohohruiuailtTlttddeFeiCobbbbneeaoa,ssfssddi0difo.lfl0ifwfiv0iinvci4csinuu ntglpgrltptemaiinnmtL.oo tt[~hshsrNeaeaoyy~m~pp~rtrtthee~hhsosaaCelet~nnp-cc~lttheeahenet. of higher fluorochemical concentration, downstream from Oftohlelrowipnogs:sible explanations for the higher TFC could be Other possible explanations for the higher TFC could be thethe the plant. following: SMMauacbdejeeAAcvtvataoiiPllaraobbtlleeecbbiyyiv33eMOMrfdfooerrrIInnIssnppePeccattiiioomnnevaarn.ndd3CCMo,oppyNyoii.nnggC2aa:ss0CC4o-on5nf3ifid0de8ennttiiaall IInnffoorrmmaattiioonn: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00000022 33MMAAD011440099556600 . : 2 "TTeennnn.. RRiivveerr FFiisshh//JJEEGG wim 5/22/79 I 5/22/79 TABLE 1 TABLE i FFLLUUOORRIOONCCHHTEEEMMNIINCCEAASTL.SEECCOONNRCCIEVENENTRTRRAAFTTIIISOIONN ((ppppmm)) IN TENNESSEE RIVER FISH SaSammppllee 1I4A -- WWhhoollee ffiisshh 11BB -- CCoorree ((33)) 24 2A - - core Core (5) (5) 33A -- GGiillllss 34 3A -- LLiivveerr 34 3A - - PPaarrttss ((77)) 33A4 -- MMuussccllee 33A4 -- FTaatt ((88)) 33A4 -- GGaallll bbllaaddddeerr WWaatteerr bbllaannkk BEtt`bhhlyyallnkaacceettaattee blank FFMN--33992233 00..4400 00..8822 00..0066 11..4488 22..177 11..3333 NN.DD.. 1313..8855 11..5577 NN.pD.. NN.DD.. FTFuM ---333049222552&1& ) FM-3422 (i) 0.73 0 73 33.0311 NN.DD.. ((68)) 0.80 0.80 0.38 0 38 0.43 0 43 N.D. N D. 6.12 6 12 00 .7744 Nb. N D. np. N D. i TToCottaialnl CFCioosmmhbbiinneedd | (oom) FC i~ (ppm) (2)Fish (2) 113 1.13 ! 00..4100 ((41)) o0..o0o044 ((44)) ! 22..7744 ((99)) ] ! ! Footnotes to Table 1: Footnotes to Table i: (1) (i) (2) uFBuFsaMM sees--dde33;;d9922o55tthnheeaarnrnfeeddrffoo oFzFreUrMeen--,3,31w42ea2a22igccohccomtaamnnbbniinononfoetectq~hbbeevevaarlrflueeuisesseoho.lliivsvseeddrreew ppwoioirttrhthteeddGG..CC ppaarraam meetteerrss (3)(2) (3) B SSoraaagm msapepndllsee,onccoournfreredo,, zpea53nr..6t61s1wecocim mfg,,hkt ii1dddoufoccyoo1,~nnhtetaariiefncinseleh udds.,sskkiainnn,d, bffaiillce ektbt,,onerreepprroodduuccttiivvee ((44)) (5) ASoA rresaersgsmppsuuparrm mlneeeessses,ees ncntottathrhnaaeatadt,ititvp veet3tahh.ree6oots1ff ccoototohnhmfneeccekiendirrndteetnrscsrtaeotaytnl~iit,ooooaffnniressntthcehtedoooubbmtffftaai,iisiilsnhhenae.ien.,ddd in the Gore backbone. in the core aarree vertebrae, skin, (5) (6) SaNa.nnaDdm d.pbblie=illeeNc,o.otre,det3e.6c1tedc.m id contained filet, vertebrae, skin, (6) (7)(7) (8)(8) N CCC C aoon.ooD dnnnnss. ssiifiissa=ssttttte.eeeNddddot oooffdf em mgtueausscscttcelrledoe,i., ntsskekisinnt,i, nabhlli.ocotodrd,a, ctbb,oonnere,,epraannoddduccctaairrtvtieillaasggyees.t.em, of gastrointestinal tract, reproductive system, (9) (9) B Bafnaradsosezededfnaootn.nweitthghheet,aacctatuunadallww ewieegiighghthtt peoofrfcessanam tmpplolfee ueusasecedhd,, pa11r88t..8.8%% lleessss tthhaann frozen weight, and weight percent o~ each part. MSMauacbdejeeAAcvtvataoiPillaraobbtlleeecbbiyyiv33eMOMrdffooerrrIInnIssnppPeecactiiioomnnevaarnn.dd3CCMo,oppyNyoii.nnggC2aa:ss0CC4o-on5nf3ifid0de8enntitiaall IInnffoorrmmaattiioonn: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00000033 MAD1400561 3MA01409561 : TTeennnn.. RRiivveerr FFiisshh//JJEEGG re -4- 55//2222//7799 120. LLLooonnngggeeerrr rrliiovvceeartriorrneessiirddeeesnniccdeeenctteiimmeet,,imeoo.llddeerr ffiisshh.. 3. LD)DoiinffgfDfeeierrrfeefnnelttroecnassttppieeocclniieeeassdriensgideanndce ltiifmee.stylos bba))) ) wwDLCChhioaoiifnrnccfttghhaaeeiirrnnettssneeftnnlddulloaa~rrrtteoggooeeecdrrbbhiiienwwoomgeeaaiiicccaggaccnhhluudttmmpuullalppiaraeefttrrteeciceeetsnnitffttoyllnluueoooosfcfrroooecoocfrrhhfggeeaaimmnnciissiccaaellnssts o) Larger fluorochemical partition coefficients tftIIffhhleeunntothhreeoiittchccooeccrraameennicbbasseelaasmmpppploloteesosssttuuallaaaarrgtteereeeddarrteeettpprhhrraaeettsseeextncncehthtnaaaatnnttnniieevvtlleheanococfafatteffwwiiihhtssoohhhlleeerbbwiiffhooiiiaassthhcceccuuccmmoobuunnalclscaeseantnttteeorrraattiioonnss,, ccfrrlaauppoppriioeec..hemiRRceeaaalsssoonnssto ffooarrgtrthheiaistseraerreeextttehhenet ssaatmmheaen aasseitllhiiessrtteeddwhiaatbbeoovveeb..ass or TTfaalbbulloeerid22eggii(vvFeg)ss fluoride (Fv) ttchhoeencerrneetssruualltttissonoo,ff concentration, ttiinnhheeppppoommrr,,ggaanniiiinncc tthh((eeRRFF))ffiissaahhnnddssaaiimmnnppooilrrceggesaa..nniicc Sample Sample 1 IA 22A0 1B IB wWaatteerr TTAABBLLEE 22 ((55)) ORGANIC ORGANIC (RF) (RF) AANNDD IINNOORRGGAANNIICC ((5F0)) FFLLUUOORRIIDDEE CCOONNCCEENNTTRRAATTIIOONS (ppmm)) rr RF 0.7 9.7 1166..22 1I00..55 NI. N.L. #fo F@ 24.6 24.6 1133..33 66..22 0.01 0.01 sJpJseooerenneemmviBBoerreualalsittihlshsyeleleerrap pssnuoauolririypnn pzrttreissidss,iioonnuugg tft.o. rtthhaaH aNtitissditthofhoenfenlelyyrhheiigngeehthxxpplirilnaaennoqnoaurragtegtsiiaaotonnnoniircc,w waffaslwsluauo sotthrhriasiadthdteoewffnivvissaahhlLluuoeeffslshloaouvuerr psSitinotntraoeaottvcrregeagiosslaauncniutstihccllhyaaatlftfellauhhunoioilaggrorlhyihwidzdeeeiilndenov,vvoaerragllgfluousaaeennrssioiccfahhiod fifglgrliuhhgfuoefaoeernrrrriiidecdtthenehaatfnnvvlauraeloooluuq rrreieggusdsaaeenns.iw witccooouru,lfflddlluw uo ommarisraikikddeesehe.o.iiwtLnJdJdooitionnifrfiihaacelalsuu vsoroelet to calculate low levels of organic fluoride. C tChthhiooagammthpteparrass,raiaim smsoopvpnnlalelesuosofefsffrttrohhotmeehmanaooabrbrgogofavvoarneeniiccW WthhheeaaeneneddlsleaermijrnpnloDDoeararmgmgaafhnhnraiaoiccvvmeebffleljjuuluuoosostwrrtiidd@ateesshe chhcioodigagnnmhht,t,e,enntLitffThsshehnnosooow tewt ss are hnancaoononiganalhccclyleyleesenrsiiat,isrsrr avtooccaifuuflutot nTT eseseeenxxnnuptpnheplelassaasnstnsneeraaeeteftoiiaoomR rRnniissvtvfhereerofrfomoww rsraatam thtttheehepriirlsseplsshaohofornbobow tswsm .eeeerddrvbvahAheattliitogigiw oohhtnnh.aoo.thirreggaaAtAnnindnimaim eccee,a.arffrlllLluitT uie oeohrwrrreiairdsedee are thought the samples may concentrations upstream thought the samples may have from have been mislabolod. With these the plant. At that time, it been mislabeled. With these results, was results, SMMauacbdejeeAAcvtvatoaiPillraaobbtlleeectbbiyyv33eMMOrffodorerrIInnIssnppPeecactilioomnneaarvnn.dd3CCMo,oppyNyoii.nnggC2aa-ss0CC4o-on6nf3ifid0de9enntitiaall IInnffoorrmmaattiioonn: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00000044 3MMADA101440099556622 I" TTeemnnn.. RRiivveerr FFiisshh//JJEEGG -obm- 55//2222//7799 miiattywwooauuclltddualssleeyeemmbettoo leiisnnsddiibcceaalttoeewttWhhaahtteelttehhree Dccaoomnn.cceennttTrrhaaisttiioomnnayooffbeffcllauuuoosrreoodcchheebmymiiccaallss msvvaoeoyltlatatltaiiicllntiiguzzaaalotltfiyioofnnbleuoooffrloescttshhheeombielfclluaouolworsroWochbcheehoefemlomiericrceaallDtahmeww.hheodnnamT.hggioosiinnmggayoovveberer ctthaheeusedddaammby((1I)),, settling of fluorochemicals before the dam. nCCooommpcaporraririsesoolnnatioooffn.oorrggaFanoniriccexffallumupoolrreiid,deethvveaalluuheeissgheffrsrotomm oTTragabablnleiescs lf1.lauanondrdid22esshhvoaowlwue, 1n1fo6l6.u.22coropporpcprmhmeelamffoioticrroanlsssaa.m mpeplFnleeaolry22z4Ae,ex,da.m hhaapddl4e,tthpheeothseslloiow bhwleiegesstht eexTTspFtClC,ao, nrag00t.a.0i0n0o0i4n4c ppm, for fluoride ppm, for the value, the is that there waafelrruereoerooornrcgoghtaaennim aiccniaclffalylluzsuoeodrraiinddfaeeolyssrzeppidrnree.dssieevnniAtdtupaiionlnslsyvvi.beerrleyy Thhehixigegphhlascpcnoeoacntniiccoeeensnnttwrirshaaittciitohhonnasshtadww thhhieticchrhehe w hhiileggurhheoeerssinttdoet ffacaattonnaccclyeooznnnttteeerdnnatttf,,ioornccshhi.naanndnnieevllidccuaaattlffliyiss.hh,, Thhaahdde ttshhpeeecllieooswweesw stthicoohrrggaahnnadiicc the fluoride concentrations. WoWfiitthheacllhiimmoiiftteedtdwossaaommpptllheeerppoospppeuuclliaaettsii)oo,nn ((22 it fifsiisshdhifooffficoounneletssppteeocciideerssawaannaddnyoonnee mtmofeehaaenneiiafnnclgghuffouuorllfoccthcoweoonmnciclclouuatsslhiiseoornnsssts..updeciieTTedhhsee)d,ooonnllaiyytppedidaseerffidintniioifttfeeibciuocclaootcnnccclultumuosusiildooarnntaew iissainnytthrhaaittver tffhiiesshh fuulnnuddoeerrrocnnhaaemttiuucrraaallls ccoosnntdduiidttiiieoodnnssd..o appear to bioaccumulate in river EEXXPPEERRTI MMEENNTTAALL 1I.. SSaammppllee mmaatteerriiaallss FEiisshh 11,.AA -- SSambmaoalvllel Wcchhheaaennnlneeelrl cDcaaatmtffiiissnhhTe((nIInccettsaaslleuuerruuseRivppeuurnncc.ttaattuuss)),, ccaauugghhtt above Wheeler Dam in Tennessee River. 1IBB -- WW DhahimitteeinbbaTasesssnne((sRRsooecceccuussRivccehhrrr.Hysoooppss)),, ccaauugghhtt bbeellooww W Whheeeelleerr Dam in Tennessee River. 22AA -- WW Dhahimitteein ccTrraeapnpnppeiieess((ePPeoo.m;Rooizmviecur.aannnnuulZaarriic~)),, ccaauugghhtt uabboovvee W Whheeeelleerr Dam in Tennessee River. 33A4 -- LaLabarorggveee Wcchhheaaennlnneeerll cDcaaatmtffiiissnhhFe((nIInecettsaalslueurreuussRivppeuurnn.ccttaattuuss)),, ccaauugghhtt above Wheeler Dam in q'ennessee River. SSttaannddaarrddss F-39023, FM-3923, FFMM--33992244,, aanndd FFMM--33442222.. bTTyeenn dppipplmmutsisttnaagnndd1aarrmddlssofooffaFF1iM0--033992p23p3,m, sFFMtM-a-3n39d92a25r5,d,, aanniddn eFFtMMh--y33l442222acewwteearrteee,pprreetppoaamrreaedrdk with ethyl by diluting with ethyl acetate 1 ml of acetate iinna separate I00 ppm separate 10 ml volumetric standard, in ethyl I0 ml volumetric flasks. acetate, flasks. to mark 2. Analysis Instruments/Materials Analysis Instrument~terials BBlleennddeerr:: W WWaaarrriiinnnggg PCCrooommdmm uecretcrisciaalDl ivbbilleseinnoddnee,rr,, HMM oouodtdeeell 44##,9911-N-22e66w33,H, araatvvfaaoiirlldaa,bblleeCT ffrroomm 06057. Waring Products Division, Route 44, New Hartford, CT 06057. SMMauacbdejeeAAcvtvatoaiPilrlaaobbtlleeectbbiyyv33eMMOrffdooerrrIInnIssnppePeccattiiioomnneavarnn.dd3CCMo,oppyNyoii.nnggC2aa:ss0CC4o-on6nf3ifid0de9enntitiaall IInnffoorrmmaattiioonn:: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00000055 33MMAA0011440099556633 Ls TTeennnn.. RRiivveerr FFiisshh//JJEEGG -o- 55//2222//7799 TTiissssuueemmiizzeerr:: MM 3o7od2de0el2], ##SSCDDiTTn,0cinaanvvaaatiiill,aabblOleeH ffr4ro5om2m22TT.eekkmmaarr CCoommppaannyy,, PP.. OO.. BBooxx 37202, Cincinnati, OH 45222. DDiinnkkeerr DDiiee:: b33.y.6611Jerccmmry 1idGdutA AhIIrSSiIIe--0022inhhiiCggehhntrccaaalrrbbooRnnesessattereceehll ccuuttttiinngg ddiiee m maaddee Labs, described biinyn 33JMMerrTTyeecchG hnnuiitcchaarllieN NoiontteebbCooeoonkktr##a55l115R566e88s-e-33a55r.c. h Labs, described MMixixere:r: ""V VIonordrtuteesxxtriGGeeesnn,iiee""IncM M.oo,ddeelBloh##eKKm--i55a55,00--GGN,Y, aavvaaiillaabbllee 11716. ffrroomm SScciieennttiiffiicc Industries, Inc., Bohemia, NY i1716. CCeennttrriiffuuggee:: DDaammoonn--IIEECC MMooddeell ##BB--22004A,, aavvaaiillaebbllee Corporation, Needham Heights, MA. ffrroomm DDaammoonn--TIEECC Corporation, Needham Heights, MA. B Boottttlleess": FFaooluuurrm--ioonuuunnmcceefowwiiilddeeammnooduuttahhleeuddmiccnllueemaarrfogiglllaa-sslssinebbdoottttcllapees.sseeaalleedd wwiitthh aluminum foil and aluminum foil-lined caps. 112255--mmli lliinneeaarr polyseal caps. ppoollyyeetthhyylleennee ((LLPPEE)) ppllaassttiicc bboottttllee wwiitthh polyseal caps. GGaass _CChhrroommaattooggrraapphh:: C CIhnhrtrooemgmaratatotogogrrraapp-hh He-- wHHleeewtwltel-etPtt~a-PcPkaaaccrkkdaarrddM MMooddeell odel 33 55771133 80A GGCC.. integrator Integrator - H pprreiiwnntlteeertrt..-Packard Model 33SOA integrator- B 1B5oo0tthhPaoofgetthhMeeillaabbooRovvaeed,uavvPaaaiilllaoubblAleletoff,rroommCAlllicow 9w4ll3co0Ll4Ll.--PPaacckkuarrdd CCoo..,, 150 Page Mill Road, Pale Alto, CA 94304. Column Column - - Six-foot, Swiitxh-fo10o%t, 1/8 C1W2/80M inch OD, inocnh60O/D8, 0 sstCtaahiirnnollmeeasssssorbsstteeWe-elAl,W, . ppaacckkeedd with 10% CW20M on 60/80 Chromasorb W-AW. CCIoonlljuuemmcnntorTTeemm-ppeeOrrna-atctuourlreuemn-- Injector - On-column IIssootthheegrmmaall aatt 220000 CC.. 118800 CC.. DDeetteeccttoorr -Flow - "40 EElleeccttrroonn cc/minute CCaappttuurree aatt 330000 CC.. of Argon:Methane (95/5). Flow - %40 cciminute of Argon:Methane (95/5). E Etthhyyll A Acceettaattee:" "M"L LCi/iBC CMhharronosusofolalvvc""turccihhnrrogom maCahtteoomggirrasaptpshh,yy ss2oo9l0lvv9eennHtitghaalvvaaaniidllaabbAlvleeenufferro,omm Norwood, OH 45212, MC/B Manufacturing Norwood, OH 45212, as Catalog #6008638M. Chemists, 2909 Highland as Catalog #6008688M. Avenue, MMaacdee AAvvaaiillaabbllee bbyy 33MM ffoorr IInnssppeeccttiioonn aanndd CCooppyyiinngg aass CCoonnfifiddeenntitiaall IInnffoorrmmaattiioonn:: `SSuubbjejcetcttotoPrPortoetcetcitviveeOOrdredrer IInn PPaallmmeervrv.. 33MM,, NNoo.. 2C-20-044--66330099 11220088..00000066 33MMAAD011440099556644 : TTeennnn.. RRiivveerr FFiisshh//JJEEGG ---i%m- 55//2222//7799 VWaatteerr:: DDeeiioonniizzeedd wwaatteerr.. 33.. PPrroocceedduurree ((66)) wPPreroroceceeddouubrrteeassineuudsseeddfrbboeemllooewwa,,rlieeexxrcceepp3ttM were obtained from earlier 3M TTffeeoorrcchhnnmmiiiiccnnaaoollrr mmRRooeeddppiioofrfrtiitccaassttuuiimmoommnnaassrr,,iieess ((77)).. SaSnaadmmpppllleesasce1IA4d ttihhnrrooluuaggrhhge 33AAalaaunnmddinuI1BBm ww peaenrrsee, rreeimnmoov&veeddfumffreroommhootthdh,ee 2ffrnredeeezzeerr aaanllldloowpweeladdcettodo thaw. in large thaw. aluminum pans, in a fume hood, and A2Anwdwhhohololeemogccehhnaainnznneeeldl and homogenized cciinaanttffaaiissbbhhll,,eennddsseeaarrmmppwlwleeiitthh1IA,,2300w00waassmmll ccwuuwtatatteeiirrnn..ttoo 5 sseeccttiioonnss SSlaaamm tpeplrleael 1IBBlihhnaeaddbeaahiddniindnkketehrreddigieeillccooprrleeatsseaa.m mpplloeConttatakekenennts jjuoufsstt tohofefff tthhee 2r2la00e.p.t5e5r99ro11adul cggtrrlaiiam nvmee ssaobam rmegphpalilnneesd,wwetehrpreeaertssgkkiioilnnfl,, pfflaiillteeet.t,, kidney, sasCm mnoadnalltlrleencppttsaaurrmtot.f ooftfhebbaacckkbboonnee,, reproductive organs, part of kidney, and rectum. SSgaiamlmlppllepela22tAAe.hhaaddThaae vgeirltlebprlaaet,e. skiTnh,e ddi1inn6kk.e6er8r4ddigieeramccoorsreeampssalam empplcleeontttaaakikenennedbbeefhhiliinentdd, 1an6d.68b4ileg.rsmSasamm plpelse 1c3onatandine2dA wfeilreet, tthhee homogenized with vertebrae, skin, homogenized with 10 ml of and bile. I0 ml of water in Samples water in aa "tissuemizer." IB and 2A were "tissuemizer." SwSeaarmmepplleehom33A4ogwweanasiszeddidissssweeicctttheeddw,,ataaennrdd. tthheeInvdvaiarvriiiooduuusasl iinpnaddriivtvsiidduuwaealilghppiaanrrtgtss w mm toheororreseeehtthoohafamnnolg22ee5s5n.s.i00ezredggwrraw eamimigssthhtw ww eewrraeeetreehhroo. mhmooogmIgneoengdnieiivnzzieeidzddeudiainnl inpua abbarltlsee"nntdw dieseersri,,tgehw mwinihhgziiellree." wTTthaaaotbbelsleree ao33dfdlleiilsedststsssfeortrthhew ehoemssiaoagm mghpetplnlew ie,z,eirenssagam mhpeopalmlceeohgwweeseniaiigmzghpehtldt,e,.inaanndda amount of "tissuemizer." amount of water added for homogenizing each sample. dA Ailllvlidooeffdtthhieentoaabboofvvieevessaaam mlpiplqleuesos,t, s uafaftnteedrrplhhaoocmmeodoggeeinnniiazpiarlteioocnnl,e, anwweeedrreebottles, Td((hdidvriiceicdheherrdooam mlaiin atqtcuteo/o/atacsfciiivddw,ee, rew waalaiptq tleeuarrcoerrtsidinnssiaoenn,d, LPpddErlrayy,cb,eodvtLioollileunusec,nnpcer,e,wchldd ierlrayeyn)).e.tdhebottles, T oointthhhreeeaerr rteatwfwlioorqiuw gweeoerrtraseetow pprlleaarcceaeteddpi4l.ain5nc%eogdglCla.aIsnsssunLtbb PEiootlttDtlnloeee~sesU .d.eleds.SS, aamw mphpllieeless were the were ssttoorreedd in a refrigerator at 4.5 C. until needed. SSppfaroaremrm epppplwaaleerreesiesdgdhaatnanaaccalocclyyfoozzrreeddsddiiannmggpffoloerttrooFaFNnttMh-dh-e3e39m92iff23ol3o,ll,llilolFFowiMwMt-iin-3en39grg92s25pp5,ro,roofccaaenneodddtduhuryFFreleM H.-.-3a34c42SS2e22eteeeaww teeTTeraraebeublsleeed44 fifooorrr extractions. weight of sample extractions. and milliliters of ethyl acetate used wAAaspprrweeevviiiogohuuessdllyy (hhnooom mologagerengneiirzzeeddthassnaam mp4pl.le0e,0, sgs)ttoorraeenddd iainnddeaadggltlaaossssa b b3o0ot-ttmtlllee,, pw parcraeeescctw llaeeteaaeinngeewhddaedsggla(lnaadosdsssedlaccreaegtnnettrtrriihffetuhugagrneeate4ttuu.0bob0fee.. 1g.) 0AA anvmvldoolluueamtdmhedeyedlooff taoeectethht&ayytl3le0-m pelr maggirrcaxaememtdaootefff ow hrhooam1m so.og5agedenmdnaieatndteue.ta. ets TTthhiheene Tmhiexedsamfoplres1.5wermeinruetmesoveind aeeratthhmteyiylxleorafaccac1ett.t0aatatem e/s/lfpfiieessethhhdyhshl oeotm matocoigegnetegnanataetotefepww 3e.ererree aandmicxeenrtraitfuagesdpeeatd s15e0tt0inrgpmoaft 3. The samples were removed and centrifuged at 1500 rpm at SMMauacbdejeeAAcvtvatoaiPilrlaaobbtlleeectbbiyyv33eMMOrffdooerrrIInnIssnppPeeccattiiioomnnevaarnn.dd3CCMo,oppyNyoii.nnggC2aa:ss0CC4o-on6nf3ifid0de9enntitiaall IInnffoorrmmaattiioonn:: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00000077 33MMAA0011440099556655 7 tenn. Raver Pisn/gEG = Tenn. River Fish/JEO 5/22/70 5/22/79 p22aal11ccaeectteaCaC.dtt.ee fifonollararyyaeei10r0vriawmwmliaa.inssnuutssteeeFespips.av.areraatA t1Aee1ffddtt,o,oefrrbbyyScceaenmuuntpsstreelrieiffoouuf(fggoiiatannaggRnp,id,ipuperttehrdht,)eo, waeeaontnthsdhdyyll Injected placed in injected fora for gas vial. gas chromatographic aulyeis. Five ~i of sample (standard) chromatographic analysis. was SBSiinnaoamsmpcILplPaPlESerescshbbo1IoAatLt,ia,tllbeeo22s4Asr,,,a, tww osaernneyrddreeIf1BoBsserennnh~tooomrmogttoogaegenneiJJanocotannetaesB Bns,de,ellpipiilsnsluulolessergeoo&anffiwwcattahthteeeerrrlCC uebbcenlelnaatintsrdrkakea,l,l aRneasleyasricsh. Laboratory for organic and inorganic fluoride analysis. REFRRENCES REFERENCES (1) (i) 33tRtoMoMepT RTRoe..ercLcthLh..n.niicBBcaoaohlhloonR Rn,e,eppo""orFFrtatatteeSSuumm oomffmaraFFrylyl,ua, oorAA roouugccguhhuseestmm tiic33ca00a,l,lss 11P p997r7r8o8o,j,jeecAcAtrtrtthh--uurPPrrrooMMgegernrnededseseslsl Report." (2) (2) 1CC9ee7nn8t,trraalJ!onRReeBsseeelaairrscclhhe.LLaabboorraattoorryy RReeppoorrtt NNuummbbeerr 66990022,, A Apprriill 2200,, (3) (3) 1978, Jon Belisle. "Bioconcentration of "Bioaoncentration of NCahyann1o7,l 1C0a7t7t.isn," . Channel Catfish," M. TFFM U--3E34l42n222abaiinrnewB Bylluuo1eg6giilAll:l T. Elnabarawy to A. NSSXu.unnfWfieisishthoraa,nndd N. Welter, iinn (4) (4) May 17, 1977. 33"MBvaTTMlRSuS,k, tiA Aouungguuossftt t116h6,e, B119i97o75e8,o, neAA.i.ntNN.r.atWWieolentlteePrrotIt:eoontDDi..alLI.. oflB~aacFaovon-n,3, 422." (5) (5) bCyentdronalBeRleisselaer,chMeLyabo7,rat1o9r7y5. Report on hequost "Evaluation of the Bioconc~ntration Potential Central Research Laboratory Report on Request of FM-3422." ##A A7722119999 by Jon Belisle, May 7, 197@. (6) (6) ETEoohxffxeppettehr`hredemim iesEEnesnntnevvcatiatilrrliooonnwwnmom soerrenkkantntadddaloolnhneoeL LmaaobiibngonoerrniccaitootzooooerprpytyeeirroaC(aEntEtsEHiio.onn& w bwiCitt:hh PC), wAA.h. op.No. rW Wefleotlrtmeeerrd who perormed the dissections and homogenizations. ((77)) 33MoM TDT.eeccLhh.nniicBcaaacllonR R,eeppo"orArtntalSSyuutmmimmcaararyly,, MN eNtoohvvoeedmmobbleeorrgy1155,o, n119P977u77-,,31AA2..3.HMoennddoell to D. L. Bacon, "Analytical Methodology on ~M-3422." ier &rSguppn t con ~cen SWMauacbdejeeAAcv1vtaaiPilarabobltleeecbbiyyve33OMMrdffooerrrrInsnsppePeccattlioomnneaarvnn.dd3CC4o,oppyNyoii,nnggC2aa.ss0CC4o-on5nf3ifid0de9enntitiaall IInnffoorrmmaattiioonn: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00000088 3aMmoAt01s4o0s9s5e6s6 : Tenn. Tenn. River River FFiisshh//JJEEGG -o- -9- 55//2222//7799 TTAABBLLEE 33 FISU ISH WEIGHTS WEIGHTS AND AND WWAATTEERR VVOOLLUUMMEESS UUSSEEDD FFOORR IHIOOMMOOGGEENNIIZZAATTIIOONN DescSSaarm nipppltleeion .D,e_scription 1IAa 22Aa 1IBB 33A4 -- M msuescllee 33A4 -- G Gaallll bbllaaddddeerr 33A4 -- L Liivveerr 33A4 -- lr~aaut 33A4 -- PPaarrttss 33A4 -- G Giillllss IFInrnioitztieiaanll WW Wehihgoohlltee Frozen Weight 114466..00 gg 226666..55 g 221100..00 gg 775522..00 gg 775522..00 gg 775522..00 gg 775522..00 gg 775522..00 gg 775522..00 g AWAcectitguuhaatll SSUasamemdppllee Weight Used mmll sWW eadatteerr Used WWhhoollee fiisshh ((11))((22)) 220000 1166.668844 gg ((33)) I100 2200.559911 gg ((33)) I100 220099.9933 gg 220000 11.3377S8 gg I100 55.994499 g I100 5522.223300 gg i10000 332211.5577 gg 330000 1199.3388 g I10000 FFoooottnnootteess:" (1) (I) AiA s:fhFiisshhandhhooowokak,s, w wrieitmthhovennodo baaepplppoaarrrcceantht ormru uosgstetnioozrratlliiinonene,, wwaass f~oouunndd ii.nn gish and was removed beore homogenization. (2) (2) TtThohee coffinissshhtanaatppppeaeaiarrreeddflttoowo bboeveerssll% isgughrhtftlalyyce ddoeefhhyydfdrirasahtte)eddso((pptoohssessiibbalclyytuaddluuee weight of fish used may have been to constant air flow over surface weight of fish used may h&ve been loss than of fish) less than frozen so the frozen weight. actual weight. ((33)) SSaammppllee ccoorree 33..6611 eamm iidd.. MSMauacbdejeeAAcvtvatoaiPilrlaaobbtlleeectbbiyyv33eMMOrffdooerrrIInnIssnppePeccattiiioomnnevaarnn.dd3CCMo,oppyNyoii.nnggC2aa:ss0CC4o-on6nf3ifid0de9enntitiaall IInnffoorrmmaattiioonn:: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00000099 33MMAA0011440099556677 A "+ Tenn. Tenn. RRiivveerr FFiisshh//aJmEeG --I100-- 5/22/79 5/22/79 TTAABBLLEE 44 FISH FISH WWEEIIGGHHUTTSSSEDAAFNNODDRBETETUXITY~RLLACAATCCIEEOTTNAASTTEE VOLUMES VOLUMES , USED FOR EXTRACTIONS DesSScaarmmipppllteeion Description 34 3A - - GGaallll B Bllaaddddeerr 34 3A - - L Liivveerr 34 3A - - MMuussccllee 33A4 -- FFaatt 33A4 -- PPaarrttss 34 - oils 3A - Gills Water Water B Bllaannkk 1IA ft} IB 2a 2A WWeHeioiggmhhottgenooaffteFPiisshh Ho( mggorgarmeasn a)mt es) 1.20 1.20 2.20 2.2o 22..4400 22..1400 33.. 0O00 3.00 3.00 2.40 2.40 22..4400 2.10 2.40 22.,4400 %iWWnaatteerr Homoign enate Homogen at e 8877..99 62.7 62.7 488..88 6655..77 48.3 48 3 83.8 83 8 100.0 i00 0 5577 .88 52.7 32 7 37.5 37 5 A AFcictstuhuaalNlt. _EE Fxixst(thrmrgaa)cW ctttee.dd (rag) 145.2 145.2 820.6 820.6 1228.8 1228.8 882233..22 1551.0 1551.0 486.0 486.0 - 1012.8 1012.8 1615.2 1615.2 1500.0 1500.0 Etm moll ae EtOAc 11.22 2.2 2.2 2.4 2.4 2.4 2.4 3.0 3.0 33..00 2.4 2.4 2.4 2.4 22..44 2.4 2.4 MSMauacbdejeeAAcvtvatoaiPillraaobbtlleeectbbiyyv33eMMOrffodorerrIInnIssnppePeccattliioomnneaarvnn.dd3CCMo,oppyNyoii.nnggC2aa-ss0CC4o-on6nf3ifid0de9enntitiaall IInnffoorrmmaattiioonn: Subject to Protective Order In Palmer v. 3M, No. C2-04-6309 11220088..00001100 3MMAA104104909550688