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AR 226 -- 0837 ACUTE TOXICITY TO FISH (FATHEAD MINNOW) IESTSUBSTANCE ~~~ Identity: A mixture containing perfluorcoctanesulfonate, which may also be referred to as PFOS, FC-95, or as a component of FC-600. (1-Octanesulfonic acid, 1,1,2.2.3,3,4,4.5.5,6.6,7,7,8,8.8heptadecafluoro-, potassium salt, CAS# 2795-39-3) Remarks: The 3M production lot number was Belgium 2367. The test sample is FC-600, referred to by the laboratory as "3M-I". Current information indicates it is a mixture of 1.0% PFOS, 81.20% water, 12.00% diethylene glycol butyl ether, 1.00% sodium octyl sulfate, 2.00% propane Sultone foamer, 1.00% sodium decyl sulfate, 0.85% xanthan gum, 0.1% N-(3-chloroallyl) hexaminium chloride, 0.80% starch, and 0.05 % tolyltriazole. The following summary applies to a mixture with incompletely characterized concentration of impurities. Data may not accurately reflect the toxicity of the fluorochemical component of the test sample. M0 ETHO0 D: 00000000000 Method: EPA-660/3-75-009 and Std. Methods (APHA), 1980, 15" Ed. Test type: Acute flow-through GLP: No Year Completed: 1983 Species: :Pimephales promelas Supplier: In-house cultures maintained at ABC Laboratories, Inc. Columbia, MO. Analytical monitoring: Temperature, pH, DO, and ammonia Exposure period: 96-hours Statistical methods: LCso values and 95% confidence intervals calculated using binomial, the moving average, or the probit tests. - Test fish age: Juveniles. Average Length and weight: Length = 30 mm Loading: 0.35 g/L Weight = 0.52 g Pretreatment: None. Test conditions: Dilution water: Well water. _ Dilution water chemistry: pH: 7.8 Hardness (as CaCO): 255 mg/L Alkalinity (as CaCOy): ~~ 368 mg/L Conductivity: 50 pmhos/cm 002040 Lighting: A daily photoperiod of 16 hourslight and 8 hours dark was maintained. Stock and test solution preparation: A 381,000 mg/L stock solution was prepared by diluting 381 grams of test sample to 1-L with deionized water. Test solutions were prepared by a diluter delivering one nominal `concentration of the test sample and control water. Flow-through rate: At least 5 volume replacements in a 24 hourperiod. Stabilityofthe test chemical solution: Not noted. Exposure vessels: Aquaria with a maintained test solution volume of 15 liters. NNuummbbeerr ooff friesphlipcearterse:pltiwcoate: 10 Number of concentrations: Water chemistry during the 1 plus a study: blank control, in duplicate PH range (0-96 hours): - 8.08.1 (control exposure) 7.8-8.2 (1,000 mg/L exposure) Temperature range (0-96 hours): 21C (for all aquaria) Dissolved oxygen range (0-96 hours): 7.6 - 8.8 mg/L (control exposure) 2.7-9.2 mg/L (1,000 mg/L exposure) Remarks: The dissolved oxygen concentrations for the 1,000 mg/L `exposure aquaria fell to 5.7 and 2.7 mg/L after 96 hours. Since fathead minnows are generally more tolerant of low DO `concentrations, it was not considered to bea significant factor in the results of the test. R0 ESUL0 TS 00000000000 Nominal concentrations: Bk control and 1,000 mg/L. Percent mortality (based on 20 fish per concentration) |comioen im Far Nominal - [C Cow bo T 1 o0 10 1 15 0T |0 3 o]| Element value: 2484--hhoouurr LLCCssoo:: >>11,,000000 mmgg//LL. 72-hour LCso: >1,000 mg/L J. 96-hour LCso: >1,000 mg/L Element values based on nominal concentrations. 002041 SRuebmsatraknsc:eTReesmtianrgkwsafsieldc.onTduhcetveadluoen rtehpeormtiexdtuarpepalisesdetsoctrhiabtedmiixnttuhree Taensdt not the fluorochemical proportion alone. Behavior preceded observations by surfacing adunrdinlgostshoefteeqsutiilinbdriicuamt.ed that mortality was wAitrheifnerpeunbcleistheesdt wliatseractounreduvcaltueeds.using Antimycin A. Test results were conclusions 0000 The FC-600 86-hour >1,000 mglL. LCs for Pimephales promelas was determined to be Submitter: 3M Company, Paul, Minnesota, 55133 Environmental Laboratory, P.O. Box 33331, St. pataQuary 0000 tReelsitaibniglHitoyw:evKeiri,mtihsechsraamnpkliengpu2r.itTy hweasstnuodty pmreoepterslythcehacrriatcetriearifozredquaanlidtyit sloalcuktsioann.alyAtdidciatliocnoanllfyi,rmDatOiocnonocfetnhteraatmioounnstfeollfsfilgunoifrioccahnetmlyicbaellporwoportion in acceptable levels at the 1,000 mg/L exposure. R0 EFEREN0 CES 00000 tThheisresqtuuedsytwoafsthceon3dMucCtoemdpbaynyA,BC3MLaLboarbatRoerqiuees,stInnc.umofbeCrol8u8m7b5iaa,ndMO906at3, 1983. o0 THER 0000000 Last changed: 6/28/00 . 002042 --- = Bulgiun ht 23 FC-(60 wbtst--tzr AP.N0.ALYBoTxIC1A09L7 B+ICOoClHumEbMiIa,STMROY 8L5A2B0O5R+AT(O1R4I)E4S7,dIsN7C.s LR 8975 SMa LR F063 Flov-Through Acute Toxicity #30175 Report Subnitted To: At3HtnC:ompany M. T. Elnsbaravy 9E3n5viBruosnhmen-tBaulilLdaibnograt2o-r3y St. Paul, Minnesota 55146 to FatDhyenaadmicMinAncouwtse T(oPxiimceipthyaleosf p3rH-oImelas) Maxch 29, 1983 002043 Submitted By: A7n2a00lytEaiscta.lABBCioL-aCnheemistry Laboratories, Inc. PC.olu0.mbiBao,x M1i0s9s7ouri 65205 Prepared By: KAqa2unabt)iBc-PFBooiroltlioisgisst DBaiDvoilLdogiL.sKtKiinttuer 3/rDoa/tees 3/a3te/73 Approved By: [@ ATqauratiHc. STuhpoearpvsiosnor hoo Uelnsitey Asd0suErancKeul Supervisor LTaybleorgba.torJyohHnasnoanghe /gn1 has Bate - DZat0e[8 3-3D0at-e 05582044 TAOFBCOLNTEENTS Page to. LISTOP TABLES... ..................3.01.5.s SUMMARY LLL... somsa INTRODUCTION. oss METHODS ANDMATERIALS . . . . LL. ..........3...7.2 TooTestBish..................s ...s. II. Test System... .................. 30753 TIL Test Compound . . ...............3.0.15.3 IV. Test Procedure - Biological . . . . .. . ...... 30753 V. Test Procedure - Chemical and Physical. . . . . . . . 3017-3 VI. Statistical Analysis. . LL... ........30.5.3 RESULTS... ooo sous LITERATURE CITED. . . . .. ...............3.0.5.9 QUALITY ASSURANCE STATEMENT . . . . . ............. 30150 APPENDIX - RAWDATA LL. ............s.u.s. 602045 Table No. 1 2 3 " LIST OF TABLES Page No. The estimated dence limits LCso for tvhaelue9s6-whiotuhr their 95% fathead confiminnow toxicity study of M-T. . . . . . .........301755 ACqhueamtiiccalBicohaasrsaacyteLraisbtoircastoorf.ywe.ll. water ... at ABC's ...... 301756 Wtaotxeircitqyuasltiutdyy omfea3sHu-rIemteontsfatdhueraidngmintnhoews96. -h. ou. r. . 30175-7 fPievrecenctonmcoernttarlaittiyonosf fathead of 3M-I minnows during eaxp9os6e-dhoutro toxicity study. . . . . LLL... ....30175-8 30175-iv 002046 SuiARY acuteA todxyincaimtiyc o9f6-Mho-uIr ttooxifcaitthyeadstumdiynnowwass (cPoinmdeupchtaeldestoprdomeetlearsm)i.ne Tthhee Tmoextihcoidtsy emTpelsotysedwiwtehreAqtuhaotsiec ouOrtglainniesdmsb.y tWhaeteCromqiutatleiety onparMaemtehtoedrss foofr ttheeapetreastturaen,d vdeirsesowlivtehdinoxaycgceenp,tabplhe alnidmiatms.onia were measured throughout constaAntfltoews-tthrcooungchentprraotpioorntsi.onalNomdiinlaulteerxpossyusrteem cownascenutsreadtiotnos moafint3aM-iIn were duplicate 1,000 mg/l and duplicate controls. referAesncea cqoumaploiutnyd, chAeactki,myctihne Af.athTeahde moibnsneorwvsedwe9r6e-hcohuarlleLnCgseod.anwdith95a% dcnonftihdeencleitelriamtiutrse,(C.iIn.d)icwaetriengwitthhaitn tthhee 9f5i%shcownefriedenicne gloiomditsconrdeiptoirotne.d wouldThbee >o1b,s0e0r0vendg/m1o.rtality data for the study indicated that the LCso 30175-1 002047 INTRODUCTION Bio-Ch3eMmiCsotmrpyanyLacboonrtartaocrtieeds,theInAcq.u,atitco Toxicology conduct a Division of Analytical duplicate 1,000 mg/l concentration estimate the plus duplicate toxicity of 3H-I cotnotrfoalt,he9a6d-hmoiunrn,owsfl(oPwi-mtehprhoaulgehs bioassay to promelas). T3h-e1 pbryimaersytimoabtjiencgtivteheofmedtihaen stleutdhyalwacsontcoendterfaitnieontshe(LaCcsou'tse) tdouxriicnigtythoef c34ourCsoempaonfy,theinteast.protTohceolstduadtyedwasFebaruutahroyriz2e1d, by 1983 H. T. Elnabarawy, (Appendix) and was conducted from March 10 to March 14, 1983. causiTnhge 5t0e%rmmoLrCtasliatsy used in after a this report specified is that exposure cpoenrcieondt.ratTihoins ofre3pMo-rTt presents approach the used results to meet otfhethperojteocxticoibtjyecsttiuvdeys.and describes the technical METHODS AND MATERIALS test The are biological basically thmoestehoddsescursiebdedfoirn tShtean9d6a-rhdouMrethfoldosw-tfhorroutghhe toxicity Examina- Lion with FoifshW,atHeracraonidovWearstteebwraatteers (1) and Aanm d Mp eth(oh 2ds).oi f ATb chuetei stTuoxda iycitwyan r Tecs osntss ducted following (Appendix). the procedures outlined in ABC Protocol No. 8007 I. Test Fish ABC The fathead Laboratories miinn-nhoowusseusceudltuirne.the Thteestfiwsehreweroebtaiidneendtiffireodm to All species using test fish were thheeld tianxoncoumlitcureketyasnksdevoenloape1d6-hboyurEdddayyli(g3)h.t ptehsottionpge.riodFisahnd cuolbtsuerrevetdechfnoirqueast least 14 days were basically prior to those de- scribed by Brauhn tions during the ehtoladli.ng (4p)e.riodA,daailloyngrewciotrhd aonfy fpirsohphoyblsaecrtviac- Aapnpdendtihxe.rapeDuutriicng dithseeasheoldtirnegatmpeenrtiso,d, is gthe ifnicslhuderdeceiinvedthea seqtuainvdaalredntcotmomer3cipaelrcefnitshoffootdhei(rRabnogdeny'swe)ighdta.ily Thien an amount test fish - were mot fed during fathead minnows used the for tahcicsliemxapteiroinmeanntd hatdesat periods. The mean veight of 0.52 g and a measurements mean were msatdaendaornd thleencgotnhtroofl30fimsmh. atWetiegsthtteanrdminlaetnigotnh and are fathead included in minnows were thcehalAlpepnegneddix.withAs aa rqeufaelrietnyce chceocmkp,ountdh,e AlnitmiitosyciwnereA. witThhien observed the 95% c9o6nfihdoeunrceLClsiomiatsnd 95% confidence reported in the ltiiotne.ratuRreesul(t5)s, oifnditchaitsingtestthataretheinfcilsuhdevderein in good condithe Appendix. 30175-2 002048 II. Test System uBsreudngsAfo(rp6r)o,tphoewrittiihonntaaelrmHiadtmitileluntttoenridnutsarylosdtsueycmrtiindogenescodrfiisbpe3eMdn-sIboyransMdyosudtnietlmuewanantsd dwaetleirveriendto aquarium, ttohe an ttheestglaaqsusariaaq.uarAiearaatted awelraltewatoefr 5(2Tambll/emi2)nutwea/s amount which was sufficient to replace the 15 tleistter aqtueasrtiavolweurmee iatmmelresaesdt 5 in by submerged heating elements. taimweasteirn a 24 bath hehloduratper2i2odC. The (41) III. Test Compouad v8i0s0cdouTcshoenadim3tbMie-orIn.lsitqauTnihddeardsanadmwpalwseasruepcsoetnoirveerddecaeotinptrFoeowbmarsutaeormbypsee2rr4av,teudr1e9t.8o3,bTehiean stock volume solution basis. Swatsandparredparweedighitns found in the Appendix. daenidonidzieldutiwoantervolounmeas weight/ can be IV. Test Procedure - Biological assignTmheentteosft aquaria after 10wasfathineiatdiamtiendnowosn March to each test solutions had been 10, of 1983, the 15 lbiyterratnedsotm flowing through the dn2uoqpmuliainrcaialatefcoocrnocn2et4nrothlrosau.triso.nTsheThofefisfh3iMs-whIe:rveerdoeubpselexirpcvoaestdeedfot1ro,0mt0oh0retamflgoi/ltllyowaiannndgd abnormal 96-hour tebsethavpieorriodi.nitiDaelaldy iannddiviodnucaelsevweerrye 24 hours removed for the at each observation. V. Test Procedure - Chemical and Physical Water oxygen, pH aqnudalaimtmyoniaparwaemreetemresasuroefd tthermopuegrhaotuutre,the dissolved test and were within acceptable limits (Table 3). tdiiovnidiTfnhagectnotorhm.einwaoTlrhkeciondngiclesuntttoircoaknticofonanccotefonrt1r,wa0at0si0odnmegt/belyrmwtiahnseeddciabllyuctudeliravtiedddiilnubgry - . tdheelivteorxyicsaynsttemmi.xinCgalbcouxlavtoilounmse arbey vinolutmhee Aipnpjeencdtiexd. by toxicant VI. Statistical Analysis (generSatlaltyistmiocratlaliatnya)lyswiass oofbtatihneedcobnyceenmtprlaotyiionng vs. a coefmfpeuctteridzaetda LcLiaCmlsictuslpartuoesgdirnagmthetdheeLvCebsliponpoesmdtiaatbliy,stStithceephamanondvineigttsaavl9e.5rapg(7ee)r,. ceanntTdhictshoenfppirrdooegbnricatem utseesdts.sincTehreneo donieffemreetnhtod meotfhoadnsalyosfisaniaslyazpipnrgoptrhieatedatfaor wealrle 30175-3 002049 gcPaaovlsesciubltlaheteiosnneatrssreolowefecsttdeadtcaofnotfrhiadtuesnecmeayinlbiemtihtiossbtarfieonpreodr.tthewaTshLeCstomheatt(h7,owdh8i)co.hf RESULTS Table The1 Antiayein persetsimeanttesd A. The 9tL6hC-eshoouLrCfsoorLCs3voa-l1ufeorwsouAalnndtdimbye9c5i3%n1,cA0o0n0tfoimdgfe/anltcheeaafidtnetrmeirn9v6naolwhssourwfsao.sr 5.6X10 5 mg/1. BehaviMoorrtaolbisteyrvdaattiaonsis tphrreosuegnhtoeudt itnheTatbelset 4inadnidcawtaesd rpreecceendceydBbyySsuunrifaacciinngg 5a2nddJloossssooffeeqqruiilliibbrriinuag. 3t5h%atafmtoerrta9l6ithyourwsa.s ----t-- 2a4mmohnoiVuaartsewre(rTeqaubmaleelaist3uy).repdarTaihnmeettdehiresssocloovfnettdreomlopxeyargnaedtnur1e,c0,o0n0cdeimnsgts/rolaltivcooenndsceonixtnyrgatethnei,oncpoHnetvraeornlyd easxdtpeaoqysueuadrteebeatfqwoueraerntiea8s6twienargned (l21o)0v.0erptTehhraecnendttihsessaoctlouvnretadrtoioloxny(ga5e.tn72ca2onndCce2an.nt7draavtgai/so1n)csoanffsotiredrerteh9de6 hse" otfuufrde(9).syc..tT edThth ihpesHarvepe aspilelautreses.d twoerbeeAmonisccoonmspcioosunntcdeennttreerlwtaiittoehmd tbhuetdere wcoounlbtdroomlotrtEhhraovruegehaoduvtterrsteheeelty APnraalcyttiTichceealstRueBdgiyuol-waCatshieomncisosntdru(yc1t0e)Ldabfoaonrldaltoowrtiihneegs'thfeiQnuaialnltietnrytepooArfststuhrweaansGcoeodreULnvaiitbe.owreadtoALbrLyy AonrailgyitniaclalraBwiod-aCthaemiwsatsryprLoavbiodreadtotroies3.H Company, with a copy retained at 30175-4 002050 TABLE 1: Tlhienitesstfiomrattehde L9C6s-ohovuarlufeasthweiatdhmitnhneoiwr 9t5o%xicciotnyfidsetnucdey of Antimycin A. -_ Hours of Exposure 2 8 72 9% -_ LCso 6.5%1078 6.2%1078 5.6%1078 3-1 (mg/1) Confiden9c5e% Limits - 4.2X1075 - 1.4x107 4.2X1078 - 1.4x10"4 4.2X1075 - 7.5X1075 30175-5 002051 TABLE 2: ACBhCe'msicAalquacthiacraBcitoearsissatyicsLaboofrawteolrly.water at Parameter Dissolved Oxygen oH Hardness (Cac0y) Alkalinity (Cac05) Conductivity Total Nog Ammonia (NHs) Ortho-Phosphate Aluminum Arsenic Cadaiun Chroniun Cobalt Copper Iron Lead Mercury Nickel Silver Zinc Mpeeasstuirceiddesorganophosphorus MpeeasstuicrieddesorpglaunsocPhlCoBrsine Concentration 9.2 ppm 7.8 255 pom 368 pou 50 pmhos/cn <0.10 ppm 0.15 ppm 0.10 ppm <0.007 ppm <0.001 ppm <0.001 ppm <0.002 ppm <0.002 ppm <0.002 ppm <0.004 ppm <0.02 ppm <0.0001 ppm <0.004 ppm <0.002 ppm .<0.001 ppm 2 B : See appendix for individual analyses. 30175-6 002052 28a 3g8 TABLE 3: Mater quality seasurencats during the 96-hour toxicity study of 3-1 to fathead mianovs HEoxupross-- scoef TemopC. DsOiVlCntr oe Wald) Temp 1,000 ag/1* 00 . " i oi awlitd 0 aa sees 81,81 018,00 2,2 89,92 81,82 019,018 HAN BA 84 81,80 026,03 2,21 8685 61,80 0.41,03 4 a2 67.6 S181 035,030 2,2 51,43 80,79 0.26 0.20 am 83,83 81,80 02,050 2,2 56,39 80,78 018,02 SA, 2 Te, 8 81,81 005,026 2,21 5.627 79,78 051,03 | "Duplicate aquaria | Phissolved oxygen concentrations - YSI Hodel 54 Dissolved Oxygen meter and probe. Cpl = pH Probe (Corning Model 476182) used vith Corning Model 125 pH and aV meter. "Ammonia concentrations - Asaoois Probe (Orion Hodel 95-10) used vith a Corning Model 125 pi and a meter. TABLE 4: 8Pe/r1ceonft 3mHo-rTtadluirtiyngofa f9a6t-hheoaudr mtionxaiocwistyesxtpuodsye.d to 1,000 J Concentration (ng/1) Control a Control b 1,00 a -_ 1,000 b Hours of Exposure 2 8 12 96 o o o 0 o 0 o o 10 0 a. 10 60 7 30175-8 002054 LITERATURE CITED (1) At1mh1ee36riEpxc.aamninPautbiloinc ofHeaWlatther AasnsdocWiaasttieowna.ter.19801.5th Setda.ndaWradshMientghtoodns, DfCo.r (2) Cv(ioC.tmhmiE.tFtieSsethe,pohanMna,cMreoCtihhaaovidersrmtaenfb)or.rateT1so9x7i5ac.nidtyMAemtTphehosidtbssiafnwosir.thAcEuAatqveuiarTtooimxcmiecniOttrayglaTneiPssrtoms.s t1e97c5t.ion6A1gpe.ncy, Ecological Research Series EPA-660/3-75-009, April, (3) ECdodmyp,anyS,amDuueblu.que1,96T9A.. T2h8e6 Fpr.eshwater Fishes. 2ad ed. W. C. Brown (4) oBrfauRheas,eaJr.chL.Fiasnhd: and Bluegills. R.RaAi.nbSocwhoTertotugte,r. Fat1h9e75a.d Enviromental Protection MiAacnqouwiss,itiCohannnaenld CCautlftiusrhe Agency, Ecological Re- search Series EPA-660/3-75-011, May, 1975. 43 p. (5) SBIentrtugederirie,osr,Bo.nInALvn.e,tsitmiRyg.caitEni.onAsLeamismnoFnaisafhnidsChoJn.ttorxoWil.caNHnoot.g.a2n6..U. 1S9.69.DepaLratbmoernattooryf 21 p. (6) fMooruntF,ishD.ToI.xicaonldogW.icaA.l BSrtuuadgise.s. 19W67a.terAReSsi.mpl1i:f21i.e2d0.Dosing Apparatus (1) SEHFta. ezpaLhr.adn,EMvaayCl.eurat1ai9no7dn7..J. AMSeLTt.HhoHdSaspmeecflioiarclkcTae(lcechdunsl.ia)ct.ailngPAuaqbnulaiLtcCiascot,iToonpx.i6c63o5.l-o8g6y.ASaTInH.dn Philadelphia. (8) mS1e9t7ne8tp.ahlan,AProCc.toemcEpt.ui,toenrK.ApgrAeo.ngcrByau,mscDhfu,olruRt.cha,lScmMuiiltnahnt,eisnoJg.taa,BnurpLkrCees-.paundbUl.iR.caS.tW.ioEnnAnvdimrraeonwnu.s script, August, 1978. (9) UNa.tSi.onaDlepaArctaadeenmty ooff SCcoimemnecrecse., PB1-97213.6 1V9a9.ter5Q9u2alp.ity Criteria, 1972. (10) FPoroadctiacned inDrNuoga-CAldimniinciasltrAantiimoanl. StuRdeigeusl.ati2o1nsCFfRorParGtoo5d8. Laboratory 30175-9 002055 | DRqoueuatleityTTormAisFesliuarsbayanccoeaFiySSstaTtae1actConotapFaafntoyhr,enfdaien.aMloFmeacmennp.oret(iPi3ma0co1ht7iaSalleenntpietalceed, se"nDynamTiice FfdoouorcdotreaILdtnaaobrtoayrcoactuoorrsrdtyaoFntocicpetirelaicvttioiitnachsetA`BeaCcapeulLmTaaetbniioioronanste.aottriaaenhstue.tiohnmeeteiesnnptieeoonrteohsea1stnhlssa,eloltn"fesa0nceauednvsiceeie?sduccnaooclnnk SQceuoaantltiuteoytregdAasnsiausarmdasncpfeoruiDnoadrtet.`tooAtnhbeeSbaisTnpaegcsituaicoisncocnoekpotfuomvehleetesStrtoyunymoBtrtosootnimneosmmeenrreenteo,kfhSaeuet KCEohEatSEontLdhe fhrneeeapploetrchtt.iboesnduboesfihtoeuan1ld)d Le IL bbooettap.obiusansbdetSmheeereHcnehematmrcmnteenHaeerfrriaiatBdYoicrahteaodhythdeyicvaetrEeyed lee in thiSsh.oualdtyooumhavoen atnhyn qSuoemsetritoonnsoFreoloartipngestoerthpeeiinaftoorrmmaatitoinonprporvoividdeedd ved A 0 faces s A. et Ault Snpezviere Date 05-10 00205