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ACUTE TOXICITY TO AQUATIC INVERTEBRATES (DAPHNIA MAGNA) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatweh,ich may alsobe referredtoas PFOS, FC-95, or as a component ofFC-603EF. (1Octanesulfoniaccid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumber isnotnoted. The testsample is FC-603EF. Currentinformationindicatesitisa mixtureof 1.30% PFOS, 10% diethyleneglycolbutylether,54.15% water,22.5% ethyleneglycol,2.6% propanesultonefoamer, 5% Alkylethersulfate0,.1% N-(3Chloroallyl)hexaminiucmhloride0,.9% Xanthan gum, 0.9% starch,1.0% triethanolaminea,nd 0.05% tolytldazole. The followingsummary appliesa mixture with incompletely characterizedconcentrations of impurities.Data may not accurately reflecttoxicityof the fluorochemical component of the testsample. METHOD: Method: OECD Guideline202 Type: Acute static GLP: No Year completed: 1996 Species: Daphnia magna Supplier:In-houseculturesm,aintainedatAScl-DETD, Duluth,MN. Analyticalmonitoring: Temperature,pH, conductivitayn,d dissolved oxygen. Exposure period: 48-hours Test organism age: <24 hours old Statisticamlethods: The EC50 valueswere calculatedby the Trimmed Spearman-Karber method. The NOEC was calculatedby Steel'sMany-One Rank test(Toxstatsoftware,Version3.1). Test conditions: Dilutionwater: DechlorinatedCityof Duluth,MN, tap water (post carbon filtetrh)atwas aeratedfor24 hours priorto use. Dilutionwater chemistry: Hardness: 45 mg/L as CaC03 Alkalinity: 43 mg/L as CaC03 pH: 7.92 Lighting:Cool-whitefluorescentlights.A dailyphotopedod of 16 hours light and 8 hoursdark was maintainedthroughoutthetestingperiod. Stock and testsolutionpreparation: A 2000 mg/L primarystocksolution was prepared by dilutin2g000 mg testsubstance in2 L ofdilutiownater. The remainingexposure concentrationswere prepared usinga 0.5serialdilution scheme. Stabilityof the testchemical solutions: Not noted. Exposure vessels: 250 mL borosilicatgelass beakers containing200 mL exposure solution. Number of replicates:4 Number of daphnids per replicate:5 Number of concentrations: fiveplusa blankcontrol Water chemistry during the study: pH range (0-48hours): 7.69 - 8.13 (controlexposure) 7.78- 7.94(1000 mg/L exposure) Temperature range (0-48hours): 20.1- 22.4 OC Conductivityrange (0-48hours): 152 pmhos/cm (controelxposure) 147 - 155 pmhos/cm (1000 mg/L exposure) Dissolved oxygen range (0-48hours): 8.3- 8.6mg/L (controelxposure) 7.4- 8.7 mg/L (1000 mg/L exposure) RESULTS Nominal concentrations:Blankcontrol6,2.5,125,250, 500, and 1000 mg/L. Element values: 48-hour EC50 = 479 (378 - 607) mg/L 48-hour NOEC = 250 mg/L Element values based on nominalconcentrations. Remarks: Testingwas conducted on the mixtureas describedinthe Test Substance Remarks field.The values reportedapplytothatmixtureand not the fluorochemicalproportionalone. CONCLUSIONS The testsubstance 48-hour EC50 was determined to be 479 mg/L witha 95% confidenceintervaolf378 to607 mg/L. The 48-hour No Observed Effect Concentration(NOEC) was determinedto be 250 mg/L. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota, 55133 DATA QUALITY ReliabilityK:limischranking= 2. Thisstudymeets thecriterifaorquality testing.However, sample puritywas notpropedy characterizedand the study lacksanalyticaclonfirmatioonfthe amount offluorochemicalproportionin solution. REFERENCES This studywas conducted by AScl Corporation,ASci-DuluthEnvironmental TestingDivisionD,uluth,MN attherequestofthe 3M Company, Lab Request number P2581, 1996. OTHER Last changed: 6/26/00 AS,:iStiti.IvD# 50 10 ()(,s ACu,rE,roxic,i,i*N,oi: i%TC 3,',,A'R;-.,\I-l@ll:'o i-IG[i'l' AScl Corporiitioii;'AS,:I-I)tiltitli Eii\,iroiiiiie'iIl'ieasltliIi)ii-,,.isioii 4444.Airl)@irk 13oLile%-.trd DL]Itltl%lI,N 55SI I 'rei.No. (218) 72'1-4040 Fax No. (218) 722-2592 S'FUD)' lDf--N'1'11--[Ct%TIONLINIBI--RS ASci SiLidvll)# 5010-068 3,%l Coiiipatiy 1.@ibIZeqLICSt#112581 Six)nsur3:.%tC,)njlv;ssiy Sjwawr StudyID# PI-581 AS,@l AS,,:D["Ikltll -Fc,iiiDi.i%4 3.\tC,l @ 1191) AScl Stud.IvDI,5010068 1.0GENERAI- INFOItNIAI'10.N StudyTitle Data Standard Sponsor Sponsor's Rel)reseiititti%,e Sponsor's 1-iibRequest# Testing Facility PrincipalInvestigator ProjectDirector Testing FacilityDirector DefinitiveTest Dates Data Validationand Report Review Actite'I'oxi,:iILt)1\I-'-C'-00I3-1i-l:-I@':\I'lititer(*rNi) A 'I'C3@,. AR-Al:f--I-I)tli@lillliilttlillil(l. 01-CD (;tiideiii'i-e'02. .;,\EIti\-irojiiiieiiLtl zi,,iSlelr,,,ices, 13iiii(i2i-i3iE--09. 9,i lillsAl\iciitc.St. ,%IN --iSI33. SLIs@iiAi. 3.\l1-ii%[roiiiiieiiiii 'recii,,L)Itii2i%idSer\@icesB.Liilditi'L-,-31---09. L@IISI:)\vCIILICS.t. llitil%.IN iil33. N,.). AS,:l ('orl)tlritti-L\)SiCiI-i@)LIIL1I'I1I1iI\rOllilletIlil Di, 4444 -\Irl)@ilr@kotilevard. DLIILIIIiI\.IN 11: 'I'clN.o. (218) 722-4040 Joe I)ierke@.. Joe Aiiiito. I)k)llii%iIiL)Llllt. October 29-31. 199o. Alaiii\lozol. Refxl,rSii-iiattire* Retention of Raw Data and Final Report Location of Raw Data and Final Report 1'%@oN-eirsfroiiithe dile sttid\i,scoiiiplete(l. ASci Corl-)oratioii/AScl-DLIII1l-t-i-l11\'irojiinental Di\isioii4.444 Airpark Boulevard, 1.)tiltiil\lIiN.55811; 'rei.No. (218) 722-4040. Spont,o3r.@kCf4,iripatiy SixonsSotrudyID# P2581 2 AS,:l Ci,nN)rjli,ptl:AS,:I-Dkiltitli .1%1C@, - 11 90 AS,:lSttj,fIsD$r5010 LX,S 2.0OIIJI:-'C'l'i%7E(S) To determineili4e8-liEC,,,and 48-11NOEC (no ot)ser%CcLtI't'cccLt)iicetitr@LOtfitOhlell)est substanceF,C-603EI7,forDLil)lltliti Thisstudy%%,aCsonductedaccordinot,o theASci siti(1l)\1.trieit@titite)d\tlleSI-K)iiasi(li(rO]ECI) Guideline202 (OECD 1993). 3.0 'I'ES'I''\IE'1'1101)S 're,,Sttibst@ince (@%ater SOILible 1:('6031-.1::. @@il)oIr)reNNLir:eit.ii.,@ @%@iter. ca. 1.06 'restOrcanisiiis Test concentrations:0 (diltitioii%iter 0'.5, 125,250. 500. iiii(i 1000 iiig/L.Higiitestcoticeiitritsi(l,iIititiIo)triei),LbrNecdiilijti-iOi(lK)1112 of'testsubstancein2 L of dillitio%i@i@LterI.-essecr(iilcentriti%o%nesre preparedusiiia-,0.5 seriadlilutionSCIICIIIC. .5otirceH:ealilivl.essill@i2i4i-11olliDiil)l?it'ti neonatesobtained t'roilAiSci stock CililLirei,i@iiiiii.iiiilile%tkt@LteOrf LIJILitiO%lkl-itteqrLjilit@'. DilutionWater Uve iiiievi: Grivid adults isoliiie,i.nl(liltitio%i%i-ater14 libefore the test initiationU.sed 5 orcjaiiisiiis/repliic-iitie4,.rleplicates,'iceosntcentration. Handled with a smooth bore pipet\%-it;liininsidediameter of 6 min. Did not feed durin0- the test. Sotirce:DecliloriiiatCeidty of DLiltitl%iI,N, tip A,iite'rI.'limeost recent chemical analysisis iiiRa%%@Data Piickii!e. Exposure Chambers At testtime. ilie%%aterlizi@diliir(.1iloefs4s5 incg-/L (as CACO,) and a pH of 7.92. Aerated for 24 lipriorto usingin the test. Ti*pe:250-iiiblorosilicitgtleitsbseakers. Use iiiitst: 200 1111of dilutioi%i%-zitoerr testSOILItioil/cliaiiiDbuerri.ng the test,kept covered, except %vlieieixperimentalobservationswere made. Sl%)nsor@ 3.%lCtijiti,iii) SI,4insoSrtudy IDO V-591 3 \S.I AS, I 3NI C'. II Yt, IDW 5010 GOH Incubation Diti-tili(4i8liI:t. Diiil1- 16 li tltioresceiBiLiIIL)S. iiid8 Itkiiirk,iiiiiiii.iii,.cti :(@ol-%khite Obscr\,at;oiis Endpoint Calculations Bii)lo,,it.-Dt;itli:l\- ,eiitli\t-t!'It@LtIIICCC(\i1)0!.Lire ,tiiiLliciciotiliteci iiiiiilobiliizielddeid testor---.tiii(siiiiiiisiiiobilize(I %kcre tlio,,c tilatdid not s%%-iiii%,i,tiiii1i5 secoiids afterexl)t)stirk;::ti,Lii,,%Ik)ecrres -C,ill itL,it.itedI)).iLliit)rceiiit)\i,ieiivdipliiiill1s'rotii t]iC C\J-K)\L.,re cli,iiiii)ers 11 . iiiltiitioil- I)H.1)0, t!iLclotidLIC1I1t%\. ere .\IIHA iiivtlit1x1i9,9,51. Si)czirti-iKiiirit)eriiietliod. ,VOEC: Steel's\Iitii\-OiRi@eiii'kI'es(tI'OXS-i'A'Is'tttisti@:.Li Version 3.1, Utii@,erslotf\ Si)unt.or3..NfComliany Slit)nsoSrtudy ID# P-1581 4 AS@l 'AS, I AS,:l 3\1 C', . II IDZ 50100()8 3.0[tESUI-'I'S Test Stibstail'eFeoxicitV(ilertiiideiliti;atre in Table 1) Ranges of @\'zite(r'IietiiistPr@@i,raiiieters 24-liECsl,: > 1000 (Not CiLictilible). EC,,,:479 1111!,(1.-,7S-607). 48-11.\'01-'C2'@:O 7'4)tttl (ti.CNICO-, -45. .-Ilk,ilitfiiiji.@(\'(;CO.. -43-51. C): '-'U1.-'-'2.-C4. IZ.tiii-,e E\cee(Ltiik:leikel\ll.tli I)o 4.1)'I'ES'IQ'.\:QC QA/QC Criteria 1).Ita Test organism dead. immobilized or irtpped in 01@'d,ead. immobilized or tripped. controlexposure must not be more than 101,'c. The lowest DO concentrationitttest terminationmust be at least607c of tileair saturationvalue attestt'eiiiperiittire. Test durationmust be 48 li. The lo\%-esDtO concentration nicastired%%-.is 831;'o,f the ,tirsituratioi%i-altiaet 21.0'C. I'litcestdurationwas 48 11. Reference substancetoxicitytest (thistestis optional). CLirreiiciontrolcliartforD. iticil,,ticttiile testiiii_sRitlcltideidn the raw data package. Sp,nu)r:3.%Clotnil:iti) SlitinsoSrtudy IDM P'-581 5 ,%S,I AS,:lL)LiliJIll 1-i@i,f@.illilciit;il AS,:lSlti,IiD%.750:00" ';.0IZEI:I-'IZENCES American PublicHealilAissociatio(nAI)HA). 1995.StijitliNilredttiodl!',ortlle Water aridWaste%@-.iteArP.HA, \Vasliiii-2to1i)i.,(*. Hamilton, NI.A., IZ.('I.ZLI,,saon.(] 11)77.*I'riiiiiSiIi)eeL@liriiitii-K.i\rItc)tcli-octi-L)r Estiiiiati\tIievdiiiiIi-etliiCloiiceiiiritit')Ii)i',I,-L)\icil\- 17ii%lroiSic,i. 11(7):714-719:Cc)rrectioi1i2(-'.)-.(417 Organ.izatiofiolr EcoiioiilClcc)oi)er-.itiiioiid1i)"eltil)iii(cOiEiCtI)). 1993.01-('1)GLIldel;iite'.o,r, TestinC,gof Clieiiiical0s1.:Cl) PLiblic@ttiloiiill'oriii@Cietnite)ri,l z@ D.C. Uni@,ersitoyf \Vyoiiiiii21.989. -l'oxsti\i'tersili3i.i1. I:i@,li I L-ibor-,itoDre)[,),@irtiiike)tl'lZOtOlk)L,\ @illtl Sixinsur:3%1 Comp:kny Sli,)nsiSotrudy ID# 1"-Sgl 6 ASci CtirporAtit)n/ASDeull-uth Environmental TcsLing Divisi4)n Submitted to3NI Co. - 11196 A&-f Study ID# 5010-068 TABLE 1. ACUTE TOXICITY OF FC-603EF LIGIIT l@-ATER(TNt)ATC 3% AR-AFFF TO D. AtAGiVA Test Substance ConcentrAtion (mg/L) 0 62.5 125 250 500 1OL)O Cumulative Number and Percentof Dead and lmrmbilized OrganisrrL-;- 24 h 49 h 0(0) 0(0) 0(0) 0(0) 3(15) 5 (25) 1 0(0) o(o) o(o) 0(0) 12 460) 17 (Si) Percentagesare in parenthesis. EFFECT AND NO-EFFECT CONCENTRATIONS %%!ITti CORRESPONDING 95% CONFIDENCE INTERVALS EC, and NOEC 24-h EC, 48-h EC, 48-h NOEC Data(mg/L) > 1000 479 250 957c Confidencelnt@-.1@ Not Calculable 37"07 Not Applicable Sponsor: 3M Company Sponsor Study [D# P-1591 7