Document 93D8X65g6rLqNEob16gOM9Q5

ACUTE TOXICITY TO FISH TEST SUBSTANCE Identity:Perfluorooctylsulfonadtied,ecyidimethylammoniumsalt;may alsobe referretdoas Fluoroalkyalmmonium derivative[.1Der-aminium,N-decyl-N,N-dimethyls-a,ltwith 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluoro-loctanesulfoniacid(1:1)C,AS # 251099-16-8) Remarks: The 3M productionlotnumber was Lot1. The testsample isL14394 referretdoby thetestlaboratorays P3025. The sample was labeledF-11615,Lot1. The testsample isa mixtureofthetestsubstance inwater (approximatel3y0-40% testsubstance,60-70% water,and 0-5% of residuaplerfluorochemicalsA)l.lvaluesreportedrelatetothismixture. The testsample appearstobe a 2-phasedispersion(clearliquiwdith opaque solidw)hich rapidlsyeparatesafteragitationN.o calculations were made toadjustfortheactualconcentratioonfthetestsubstance in the testsample. METHOD Method: OECD 203 Type: Staticacute GLP: No Year completed: 1996 Species: Pimephalespromelas Supplier:Not noted. Analyticalmonitoring:DO, pH, temperaturea,nd conductiviwteyre monitoreddaily. Exposure period: 96-hours Statisticamlethods: LL5ovaluescalculatedusingtheTrimmed Spearman-Kater method. The NOEL was calculateudsingFisher's Exact tests. Test fishage: Not given. Length and weight: Average length= 11.3mm, Average weight= 7.8 mg Loading: 0.26 g/L Pretreatment: None Test conditions: Dilutionwater: DechlorinatedCityof Duluth,MN tapwater. Water was aeratedfor24-hourspriortouse inthetest. Dilutiownaterchemistry: hardness: 48 mg/Las CaC03 pH: 8.08 Lighting: Cool-whitefluorescentbulbs. Photoperiod of16-hours light8,-hoursdark used. No transitiopneriodnoted. Stock and testsolutionpreparation:Water accommodated fractionsT.est solutionswere prepared individuallfyoreach test replicatceoncentrationby mass additionofvigorouslyshaken test substance in4 L ofdilutiownater. The solutionswere vigorously stirrefdor21-hours(vortex1/2to 1/3solutiondepth).The aqueous phase was siphoned from the vesselat mid-depth. Concentrations dosing rate:Once Stabilityof the testchemical solutions: Not noted. Exposure vessels: 4-L glassjarscontaining3-L oftestsolution. The jarswere sealed withTeflon-lineldidsfittewdithstoppersto accommodate oxygen flushingof headspace. Number of replicatest:wo Number of fishper replicatet:en Number of concentrations:threeplusa negativecontrol Water chemistry during the study: Dissolved oxygen range (0- 96 hours): 9.1- 14.6mg/L (controelxposure) 8.7- 18.2mg/L (700 mg/L exposure) pH range (0- 96 hours) 7.80- 8.08 (controelxposure) 7.78- 7.99 (700mg/L exposure) Test temperature range (0- 96 hours) . 20.8 - 20.90C Conductivity range (0- 96 hours): 128 - 142 pmhos/cm (controelxposure) 118 - 154 pmhos/cm (700 mg/L exposure) Remarks: Oxygen was added tothe headspace inthejars beforesealinginitialalnyd at each observationperiod.The dissolvedoxygen concentrationswere super-saturatedinthe testvessels,particularilnythe 700 mg/L exposure concentration. RESULTS Nominal loading concentrations: Bk control4,00,700, 1,000 mg/L. Element value: 24-hour LL50= 618 (568 -673) mg/L 48-hourLL50= 607 (554 - 664) mg/L 72-hourLL5o= 595 (551-643)mg/L 96-hourLL5o= 562 (523-604)mg/L 96-hourNOEL = <490 mg/L Allelementvaluesbased on nominalconcentrations. Biologicaolbservationsafter96-hours:No mortaliotryabnormal behaviorobservedinthenegativecontrodluringthetest.Mortalitwyas observedintheremainingexposureconcentrationSsu.rfacingwas observedinhalfofthefishatthe700 mg/L exposureconcentratioant24hours,and 2 fishwere quiescenatt96-hours.No abnormalbehaviorwas observedinthe400 mg/L exposureconcentration. Cumulative percentmortality: Nominal Loading Test Conc., mg/L 24-hours 48-hours 72-hours 96-hours Neg. Control 0 0 0 0 490 10 15 15 25 700 75 75 80 90 1,000 100 100 100 100 Lowest concentration causing 100% mortality: 1,000 mg/L Mortality of controls: None Remarks: Values reported are forthe test sample. No calculations were made to adjust for the concentration of the test substance in the test sample. CONCLUSIONS The test sample 96-hour LL5o for fathead minnow was determined to be 562 mg/L with a 95% confidence intervalof 523 -604 mg/L. The 96-hour no observed effects level(NOEL) was <490 mg/L. Submifter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY Reliability: Klimisch ranking 2. The study lacks analyticalmeasurement of test substance concentrations in the test solutions and sample purity is not sufficientclhyaracterized.Additionallyd,ata isfora mixtureand toxicitcyannot be positivelayttributetdodidecyldimethylammonium Perfluorooctylsulfonastaeltalone.Also, supersaturatioonfthe test solutionswithoxygen couldalso have contributetdothe toxicity. REFERENCES This study was conducted atAScl Corporation,EnvironmentalTesting DivisionD,uluth,MN, atthe requestofthe 3M Company. OTHER Last changed: 5/24/00 ASel Corporation/AScl-Duiuth EnvironmentTaelstinDgivision ASciStudy[D# 5010-068 STUDY TITLE ACUTE TOXICITY OF TO FATHEAD MINNOW DEVELOPMENTAL MATERIAL (PIMEPHALES PROMEL,4S) DATASTANDARD OECD GUIDELINE 203 STUDY COMPLETED January 2, 1997 TESTING FACILITY AScl Corporation/AScl-Duluth EnvironmentalTesting Division 4444 Airpark Boulevard Duluth,MN 55811 Tel.No. (218)722-4040 Fax No. (218)722-2592 STUDY IDENTIFICATION NUMBERS ASel Study ID# 5010-068 3M Company Lab Request# P3025 Sponsor:3M Company SponsorStudyID# P3025 ASet Ct)rporation/AScl-Duluth EnvironmentaTlestingDivision AScl Study[D# 5010-068 1.0GENERAL INFORMATION StudyTitle Data Standard Sponsor Sponsor's Representative Sponsor'sLab Request# TestingFacility PrincipalInvestigator ProjectDirector TestingFacilityDirector DefinitiveTest Dates Data Validationand Report Review Retentionof Raw Data and Final Report Locationof Raw Data and FinalReport Acute Toxicityof Developmental Materialto Fathead Minnow (Pimephales promelas). OECD Guideline203. 3M Environmental Technology and Safety Services,Building2-3E-09, 935 Bush Avenue, St.Paul,MN 55133. Susan A. Beach, 3M Environmental Technology and SafetyServices,Building23E-09, 935 Bush Avenue, St.Paul,MN 55133. Tel No. (612)778-7452. P3025. ASCI Corporation/AScI-DuluthEnvironmental TestingDivision,4444 Airpark Boulevard, Duluth,MN 55811; Tel.No. (218)722-4040. Joe Dierkes. Joe Amato. Donald Mount. December 17-21, 1996. Alan Mozol. Regort Signature- /@ZTwo yearsfrom the datestudy iscompleted. AScl Corporation/AScl-DuluthEnvironmental TestingDivision,4444 AirparkBoulevard, Duluth,MN 55811; Tel. No. (218)722-4040. Sponsor: 3M Company Sponsor Study ID# P3025 2 ASci Corporation/AScl-Dtiluth EnvironmentaTlestin,D,ivision AScl Study[D# 5010-068 2.0OBJECTIVE(S) To determintehe96-hLL50Gethalloadinga)nd96-hNOEL (noobserveedffecltoadinogf)the tesstubstanc?e@,3-c@) DevelopmentMaalteriaflo,rfatheamdinnow(Pimephalpersomelas). s studwasconducteadccordintgotheASCIstudyplanretainbeydtheSponsoarndOECD Guideline203 (OECD 1993).The testsolutionwsere water-accommodatedfraction(sWAF) preparedfouowing GirlingW,hale, & Adema 1994. TestSubstance Test Organisms 3.0 TEST METHODS PropertiesP:'@c,3@S,-two-phaseliquidbeforeagittaed,lightcolored,nearly odorlesslurryafteragitations,pecifigcravityca.1'.2g/cc,and insoluble in water. Testloadings:0 (dilutiownatercontrol)4,90 mg/L, 700 mg/L and 1000 mg/L. Testloadingsolutionwsere preparedindividuallfyoreach test replicateT.he 490 mg/L solutionwsere preparedby placing1960 mg of vigorouslyshakentestsubstancein4 L of dilutiownater. The 700 mg/L and 1000 mg/L solutionswere preparedin the same manner using2800 mg and 4000 mg of testsubstance,respectivelyT.he solutionwsere vigorously stirre(dvortex1/3to 1/2solutiondepth)for21 h. The aqueousphasewas siphonedfrom thevesselat mid depth. Source: Healthy,juvenilefatheadminnows (Pimephalespromelas)obtained from a commercial supplier. HoldinglacclimationH:eld and acclimatedfor 12 days inthe testdilution water. For the48 hoursprecedi0n-thetest0% mortalitoyccurred.For the entire12 days,mortalitywas 0%. At testterminationt,hefishwere 1.1 cm inmean len9 thand 7.8 m-0 in mean weight. Use in test: Used 10 oraanisms/replicate and 2 replicates/test concentration. Sponsor: 3M Company Sponsor Study ID# P3025 3 ASci Corporation/AScl-Dulutil EnvironmentTaelstinDgivision ASelStudyID# 5010-068 DilutioWnater Exposure Chambers Incubation Observations Endpoint Calculations Source: DechlorinatedCity of Duluth,MN, tapwater. The most recent chemical analysisisin Raw Data Packaa0e. Characteristics: At testtime, the water had a hardness of 48 mg/L (as CaC03) and a pH of 8.08. Aerated for24 h priorto usin0ciyn thetest. Type: 4-L glassjarssealedwith Teflon-linedlidsfittedwith stoppersto accommodate oxygen flushingof headspace. Use in test: 3 L of dilutionwater or testsolution/chamber.During the test,kept covered, except when experimentalobservationswere made or headspacewas flushedwith oxygen. Solutionswere not aeratedduring the exposures. Duration: 96 h. Daily photoperiod: 16 h lightand 8 h dark, maintainedusingcool-white fluorescentbulbs. Temperature: 21'C. Biological:Daily- Test organisms with abnormal behavior and signsof stress,and dead testorganisms. Water chemistry: (1)At testinitiationt-otalhardnessand alkalinity(,2) daily-temperature,DO, conductivitya,nd pH. All determinationwsere made accordingto APHA methods (1995). 24-, 48-, 72-,and 96-h median lethalloading (LL50s),and 96-h no observableeffectloading (NOEL) LL50: Trimmed Spearman-Karber method. NOEL: TOXSTAT Wyoming. statisticsaolftware,Version 3.2,Universityof Sponsor: 3M Company Sponsor StudyID# P3025 4 AScl Corporatit)n/ASci-Duluth Environmental TestingDivision AScl Study ID# 5010-06& 3.0 RESULTS Test SubstanceToxicity(Peftinendtataare in Table 1) 24-h LL50: 618 mg/L (568-673 mg/L). 48-hLL50:607 ma,/L(554-664mg/L). 72-hLL50:595 mg/L (551-643mg/L). 96-hLL,50:562 mg/L (523-604mg/L). Ranges of Water Chemistry Parameters 96-hNOEL: <490 mg/L. Totalhardness(as CaCO3 mgll): 44-48. Alkalinit(yasCaC03 mgll): 44. Temperature('C): 20.8-20.9'C. DO (mg/L):9.6-20.0. pH: 7.71-9.08. 1Specificconductivi(tAymhoslcm):118-497. 4.0TEST QA/QC QA/QC Criteria Mortalityincontrolexposuremust notbe more than 10%. The lowestDO concentratioanttest terminationmust be atleast60% of theair saturatiovnalue at testtemperature. Data 0% dead. The lowestDO concentrationmeasured was 97% of theairsaturatiovnalueat21.0'C. Afterinitia0l-hour routinechemistriehsad been performed thechambers were sealedand each chamber's headspacewas flushedwith oxygen dailyto maintainadequateDO. Ensuing DO concentrationwsere 100% of saturatioonr greater. Sponsor: 3M Company Sponsor Study ID# P3025 5 ASel Corl)oratit)n/ASel-Duluth EnvironmentaTlcstingDivision ASci Study ID# 5010-06a Testduratiomnustbe 96 h. Referencesubstancetoxicitytest(thistestis optional). The testdurationwas 96 h. Controlchartforsodium chloridereference toxicittyestinaisinRaw Data Package. 5.0 REFERENCES American PublicHealth Association(APHA). 1995. StandardMethods forthe Examinationof Water.and Wastewater.APHA, Washington,D.C. Girling,A.E., G.F. Whale, and D.M.M. Adema. 1994. A GuidelineSupplementfor DeterminingtheAquaticToxicityof PoorlyWater-SolubleComplex MixturesusingWaterAccommodated Fractions.Chemosphere, Vol. 29, No. 12,pp. 2645-2649. Hamilton,M.A., R.C. Russo,and R.V. Thurston.1977.Trimmed Spearman-KarberMethod for EstimatingMedian LethalConcentrationsinToxicityBioassays.Environ.Sci.Technol. 11(7):714-719C;orrectio1n2(4):417(1978). OrganizationforEconomic Cooperationand Development (OECD). 1993.OECD Guidelinesfor Testingof Chemicals.OECD PublicatioInnformationCenter,Washington,D.C. Universityof Wyoming. 1996.'ToxstaVtersion3.2.Laramie,Wyomin-1. Sponsor: 3M Company Sponsor Study ID# P3025 6 ASci Corporation/ASel-Duluth Environmental Testin,,D,i,vision ASci Study ID# 5010-068 TABLE 1. ACUTE TOXICITY OF NDNNOWS (P.promelas) DEVELOPMENTAL I*VIATERIALTO FATHEAD TestSubstance Loading (mg/L) 0 (Control) 490 700 L 1000 Cumulative Number of Dead Organisms and Percent Mortalitya 1 24 h 48 h 72 b 96 h 0(0) 2(10) 15(75) 0(0) 3 (15) 15(75) 0(0) 3 (15) 16 (80) 0(0) 5(25) 18(90) 20 (100)___L_ 20(100) 20(100) 20(100) a Percentages are in parenthesis. EFFECT AND NO-EFFECT LOADINGS WITH CORRESPONDING 95% CONFUDENCE INTERVALS so:ai2d:.NOEL@::..: 24-h LL50 48-h LLSO 72-h LLSO 96-h LL50 96-h NOEL Data,(mgfl) 618 607 595 562 < 490 95 % Confidence Interval 568-673 554-664 551-643 523-604 Not applicable Sponsor: 3M Company Sponsor Study ID# P3025 7