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TOXICITY TO AQUATIC PLANTS TEST SUB,9-TANCE Identity:Mixturecontainingperfluorooctanesulfonatwehich may also be referredtoas PFOS, FC-95, or as a component of FC-203FC. (1Octanesulfoniaccid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumber was notnoted. The testsample isFC-203FC, identifiebdy the laboratorays R1335. Currentinformation indicatesitisa mixtureof0.85% PFOS, 17% diethyleneglycolbutylether, 74.46% water,2.34% acrylifcoamer, 1.7% alkylethersulfate2,.55% sodium octylsulfate0,.12% sodium nitrit0e.,09% sodium molybdate,0.85% triethanolaminea,nd 0.04% tolyltriazole. The followingsummary applies to a mixture with incompletely characterizedconcentrations of impurities.Data may not accurately retlecttoxicityof the fluorochemical component of the testsample. MET-IOD: Method: OECD Guideline201 Type: Acute Static GLP: No Year study performed: 1997 Species: Selenastrumcapricomutum Source: Originalloybtainedfrom ATCC, MD, maintainedatASci-DETD, Duluth,MN. Element basis: Algalcellcounts (cells/mls)p,ecificgrowth rates. Exposure period: 96 hours StatisticaMlethods: Statisticanlalyseswere performed usingthe Trimmed Spearman-Karber method. Analyticalmonitoring: pH, conductivitya,nd temperature Test Conditions: Algal NutrientMedium: Nutrientmedium per OECD. This nutrientmedium providedallmineralnutrientesssentialforalgalgrowth and alsoserved as the diluentforallalgaloperations.The pH ofthissyntheticalgalmedium was 8.0. Stock and test solution preparation: A 2000 mg/L primarystock solution was preparedby dissolvin7g00 mg FC-203FC in350 mL algalmedium, followedby mechanical stirringE.ach testconcentrationwas made by volume additionofthestockto algalmedium. Exposure vessels: 250 mi Edenmeyer flaskscontaining100 mi test solutions,ealed withfoam stoppers. Agitation: 100 rpm. Number ofreplicates3:forexposureconcentratio6nfso,rblankcontrol. Initicaelllloading:1.0 X 104 cells/mL(1.3x 104 cells/mLactual). Number of concentrations:fiveplusa blankcontrol Lighting: Continuouslightinagt740 ft-candleussingcool-whitefluorescent lamps. Water Chemistry: pH range (0-96 hours): 8.00 - 9.90 (controelxposure) 5.20 - 7.83 (1000 mg/L exposure) Conductivityrange (0-96hours): 151 - 186 pmhos/cm (controelxposure) 194 - 205 pmhos/cm (1000 mg/L exposure) Test temperature range (0-96hours): 24.8 - 25.8 *C (incubator) RESULTS Nominal concentrations: Blank control,130,216, 360, 600, and 1000 mg/L Algal Growth Response EC50 Values Exposure (Contact) Hours 24 48 72 96 Cell-Count mg/L (95% C.I.) 298(207 -428) <130 (C.I.notcalculable) <130 (C.I.notcalculable) <130 (C.1.notcalculable) Average Specific Growth Rate mg/L (95% C.I.) 187 (16 - 209) 138 (Notreliable) 163 (145- 184) 271 (239- 308) Element values: 96-hourEC50 <130 mg/L (celclount) 96-hour ErC50 271 (239- 308)mg/L (growthrate) 96-hourNOEC = 17 rng/L(celclount) 96-hourNOEC = 57 mg/L (growthrate) Element valuesare based on nominal concentrations. Reversibilityof Growth InhibitionA:liquotsofthe 1000 mg/L testsolution were dilutedwithalgalmedium and culturedforan additionapleriod.Based on growth observed inthe recoveryphase,the effecton algalgrowth was found to be algistatic. Remarks: Testingwas conducted on the mixtureas describedinthe Test Substance Remarks field.The values reportedapplytothatmixtureand not the fluorochemicalproportionalone. CONCLUSIONS FC-203FC exhibitsa 96-hour EC50 cellcount valueof<130 mg/L and a 96hour EIC50 growth ratevalue of271 (239- 308) mg/L. The 96-hourNo Observed EffectConcentration(NOEC) is17 mg/L forcell count and 57 mg/L forgrowth rate.Thistestsubstance was determined to be algistatic. Submitter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota, 55133 DATA QUALITY ReliabilityK:limischranking= 2. This studymeets allthe criterifaorquality testing.However, sample puritywas notpropedy characterizedand the study lacksanalyticaclonfirmatioonfthe amount offluorochemicalproportioninthe solution. REFERENCES This testwas conducted by ASci Corporation,DuluthEnvironmentalTesting DivisionD,uluth,MN atthe requestofthe 3M Company, Lab Request number R1335,1997. OTHER Last changed: 6/26/00 ASci Corporation/ASci-Duluth EnvironmentaTlestingDivision ASci Study ID# 5010-069 STUDY TITLE GROWTH INHIBITION OF R1335 FOR GREEN ALGA (Selenastrumcapricornutum) DATASTANDARD OECD GUIDELINE 201 STUDY COMPLETED April7, 1997 TESTING FACILITY AScl Corporation/AScl-Duluth EnvironmentalTestingDivision 4444 AirparkBoulevard Duluth,MN 55811 Tel.No. (218)722-4040 Fax No. (218)722-2592 STUDY IDENTIFICATION NUMBERS AScl Study ID# 5010-068 3M Company Lab Request# R1335 Sponsor: 3M Company Sponsor Study [Dg R1335 AScl Corporation/ASci-Duluth EnvironmentaTlestingDivision AScl StudyID# 50io-o68 1.0 GENERAL INFORMATION StudyTitle DataStandard Sponsor Sponsor'sRepresentative Sponsor's Lab Request_# TestingFacility PrincipalInvestigator ProjectDirector TestingFacilityDirector DefinitivTeest Dates Data Validationand Report Review GrowthInhibitioofnR1335 forGreenAlga (Selenastrcuampricornutum). OECD Guideline201. 3M EnvironmentalTechnology and Safety Services,Building2-3E-09, 935 Bush Avenue, St.Paul,MN 55133; Tel No. (612)778-7452. Susan Beach, 3M EnvironmentalTechnology and SafetyServices,Building2-3E-09, 935 Bush Avenue, St.Paul,MN 55133; Tel No. (612)778-7452. R1335. ASel Corporation/AScI-DuluthEnvironmental TestingDivision,4444 Airpark Boulevard, Duluth,MN 55811; Tel.No. (218)722-4040. Todd McGuire Joe Amato Donald Mount March 25-29, 1997. Alan M0701 Report Signature- Retentionof Raw Data and FinalReport Locationof Raw Data and FinalReport Two yearsfrom the datestudy iscompleted. AScl CorporationA/S cI-DuluthEnvironmental TestingDivision,4444 AirparkBoulevard, Duluth,MN 55811; Tel.No. (218)722-4040. Sponsor: 3M Company Sponsor Study ID# R1335 2 AScl Corporation/ASel-Duluth EnvironmentaTlestingDivision AScl StudyID# 5010-068 2.0OBJECTIVE(S) To detennintehe4-dmedianeffecctoncentrat(iEoCnSO)andthe4-dno observabelfefect c,oncenfta(dNoOnEC)ofthetesstubstancRe1,335,forgreenalga(Selenxtrucmapricomutum) understatitcesctonditions. This studywas conductedaccordingtoOECD Guideline201 (OECD 1993). 3.0 TEST METHODS Test Substance Propenies: R1335, clearamber liquid,stable,and misciblewith water. Test Organisms Testconcentrations:0 (algalmedium control),130, 216, 360, 600, and 1000 mg/L. A stocksolutiownas preparedby mass additiontoalgal medium followedby mechanicalstirringE.ach testconcentratiownas made by volume additionof the stockto algalmedium. Source: ATCC 22662 AlgalMedium Inoculwn preparation:Algal stockwas subculturedin OECD recommended medium for4 days beforetestinitiation. Use intest:Stockculturewas dilutedand spikedintotestsolutiontso obtainan initiaclelldensityof 1.0 X 104 cellsper mi (1.3X 104 actual concentration). - Preparation:Deionizedwaterwas spikedwithnutriensttocks(including Na2EDTA) toOECD recommended concentrationsT.he most recent chemicalanalysisfordeionizedwaterisin Raw Data Package. Exposure Chambers CharacteristicsA:t testtime,themedium had a pH of 8.00. Sterilizevdia 0.22 um filtratiporniortouseinthetest. Type: Sterilizevdiaautoclave250-ml borosilicate-glaEsrslenmeyer flasks sealedwith foam stoppers. Use in test:100 ml of algalmedium or testsolution/chamber.Six control replicatesand threereplicatesper testsubstance concentrationwere employed. During thetest,keptstoppered,exceptwhen experimental 1observationswere made. Sponsor: 3M Company Sponsor Study ID# R1335 3 Incubation Observations Endpoint Calculations ASci Corpomtion/ASci-Duluth Environmental Testing Division ASC-IStudy ID# Soio-06s Duration:4 days. Dailyphotoperiod:Continuousat740 ft-candleusingcool-white fluorescenltamps. Testchambers heldon shakertablesetat 100 rpm. Temperature: 25.0 2*C. Biological:Daily cellcountsusingdirectmicroscopicenumerationvia Improved Neubauer hemacytometer. Water chemistry:(1)At testinitiatioannd termination-pH, conductivity, and temperature(,2)daily-temperature.Alldeterminationwsere made accordingto APHA methods(1995). 1-,2-,3-,and 4-d EC50's, and 4-d NOEC based on both cellcountsand averagespecifigcrowtb rates(IA).Statisticaanlalysesperformed using Trimmed Spearman-KarberMethod (ECSO's)and lCp (ICIO). 4.0 RESULTS TestSubstanceToxicity(Pertinendtataare in Tables 1 2, and 3) CellCount 1-dEC50: 298 mg/L (207-428).111-dEC50: 187 mg/L (168-209). CeU Count 2-dEC50: < 130 mg/L. 142-dEC50: 138 mg/L (NotReliable). CellCount 3-d ECSO: < 130 mg/L. IA 3-d EC50: 163 mg/L (145-184). CellCouni 4-d ECSO: < 130 mg/L. g 4-dEC50: 271 mg/L (239-308). CellCount4-d NOEC (ICIO):17 mg/L (17-18). A 4-dNOEC (ICIO):57 mg/L (53-62). Effectwas determinedto be algistatbiacsed on recoveryof cellspreviouslyexposedto the 1000 mg/L testsubstanceconcentration. Sponsor: 3M Company Sponsor Study ID# R1335 4 TestConditions ASci Corporation/AScl-Duluth EnvironmentaTlestingDivision AScl StudyID# 5oio-o6s Temperature(OC): 24.8-25.8. Lightintensilyft-cdl7s4:0. pH: 5.20-9.90. -_jkeeidc conductiyLq-(iimhoslcm)1:49-205. 5.0TEST QA/QC QA/QC Criteria Algalcountsincontrolmust increasbey at leasta factorof 16 duringthefirs3t-d of the exposure. Test durationmust be 4-d. Data During the firs3t-d of thetestcontrolalgal countsincreasedby a factorof approximately 157. The testdurationwas 4-d. 6.0 REFERENCES American PublicHealthAssociation(APHA). 1995.StandardMethods forthe Examinationof Water and Wastewater.APHA, Washington,D.C. OrganizationforEconomic Cooperationand Development (OECD). 1993.OECD Guidelinesfor Testingof Chemicals.OECD PublicatioInnformationCenter,Washington,D.C. Hamilton,M.A., R.C. Russo, and R.V. Thurston,1977.Trimmed Spearman-KarberMethod for EstimatingMedian LethalConcentrationisnToxicityBioassays.Environ.Sci.Technol. 11(7): 714-719;Correction12 (4):417 (1978). US EPA. 1993.A LinearInterpolatiMoenthod forSublethalToxicity:The Inhibition Concentratio(nlCp)Approach (Version2.0).EnvironmentalResearchLaboratory,Duluth, Minnesota. Sponxor: 3M Company Sponsor Study M# R1335 5 ASci Corpomtion/ASci-Duluth Environmental TestingDivision ASci Study ID# 5010-068 TABLE 1- ECso'S,95% CoaridenceIntervalsa,nd 4-dNOECIS from AlgalGrowth Inhibition Test withR1335 CellCount Endpoint Average Specific Growth Rate (a) Time 1-d EC50 2-d EC50 3-d ECSO 4-d EC50 4-d NOEC (1clo) Time Data* 1-d EC50 2-d EC50 3-d ECSO 4-d EC50 4-d NOEC (,CIO) Values Based on NorninalTest Concentrations (mg/L) 298 < 130 < 130 < 130 17 (mg/L) 187 138 163 271 57 95 % Confidence Interva(lmgtl) 207-428 Not Calculable Not Calculable Not Calculable 17-18 95% Confidence Interva(lmg/L)'; 168-209 Not Reliable 145-184 239-308 53-62 Sponsor: 3M Company Sponsor Study ID# R1335 6 ASe-qCorporation/ASci-Duluth Environmental TestingDivision ASci Study ID# 5010-069 TABLE 2. Cellsper ml and PercentageDifferencefrom Mean ControlValue for Seknastrum capticomutum Exposed to R1335 Control 130 216 360 600 1000 licaft A B c D E F Mean A B c Mean A B c Mean A B c Mean A B c Mean A B c Mean Id 4 2 3 5 3 5 3.7 3 3 3 3.0(-19) 1 I 2 1.3 (-64) 3 3 I 2.3 (-37) I I 2 1.3(-64) 2 1 2 1.7(-55) Cells/ml(104) 2d 3d 35 200 35 215 35 200 40 195 31 205 30 210 34.3 204 8 8 9 8.3 (-76) 2 1 1 1.3 (-96) 1 1 1 1.0(-100) <1 <1 <1 <I (-100) 33 33 30 32.0(-84) 6 10 6 7.3 (-96) <1 2 1 1(-Ioo) <1 <1 <1 <1 (-100) <1 2 <1 0.7(-98) <1 <1 <1 <I (-100) 41d 726 666600 627 6166 770044 639638 662 140165 180 162(-76) 58 51 65 58.0(-91) 16 20 15 17.0(-97) <1 <1 <1 <I (-100) <1 I 0.3(-100) ParentheticValues % Differencefrom Control Mean Value 0-d Mean Algal Count 1.3 X 104 Sponsor: 3M Company Sponsor Study ID# R1335 7 AScl Corpomtion/AScl-Duluth Environmental TestingDivision ASel Study ID# 5010-068 TABLE 3. Average SPecilriGcrowth Rates (&L)and PercentageDifferencefrom Mean Control Value forSelenastrumcapticornutumExposed to R1335 Control Id 1.046 Average SpecificGrowth Rate (jL)& 2d 3d 1.636 1.686 4d 1.558 130 0.836(-20) 0.927(-43) 1.068(-37) 1.206(-23) 216 0(-100) 0(-100) 0.575 (-66) 0.950(-39) 360 0.571 (-45) 0(-100) 0(-100) 0.643 (-59) 600 1000 0(-100) 0.268 (-74) 0(-100) 0(-100) 0(-100) 0(-100) 0 100) 0(-100) IA InCoUs permi t,- In Cells/mtlo tu- to b ParentheticValues = S Diffemnce from ControlMean Value 0-d Mean AlgalCount 1.3 X 104 Sponsor: 3M Company Sponsor Study [D# R1335