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ACUTE TOXICITY TO FISH (FATHEAD MINNOW) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatweh,ich may alsobe referredtoas PFOS, FC-95, or as a component of FC-787 or FC787X. (1-Octanesulfoniacid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumber was 101. The testsample isFC787. Currentinformationindicatesitisa mixtureof0.73% PFOS, 10% diethyleneglycolmonobutyl ether,79.74% water,5% ethyleneglycol,1.47% propane Sultonefoamer,0.73% sodium octylsulfate0,.73% sodium decyl sulfate0,.75% xanthan gum, 0.75% magnesium sulfate0,.10% N-(3chloroallyl)hexaminiucmhloridea,nd 0.05% benzotriazole. The followingsummary applies to a mixture with incompletely characterizedconcentrations of impurities.Data may not accurately reflectthe toxicityof the fluorochemical component of the testsample. METHOD: Method: OECD Method 203 and LJ.S.EPA Method -EG-9 Type: Acute Flow-through GLP: No Year completed: 1990 Species: Pimephalespromelas Supplier:Commercial supplier. Analyticalmonitoring: pH, temperature,conductivitayn,d dissolved oxygen. Exposure period: 96-hours Statisticamlethods: The LC.50valueswere calculatedusing a computer program by Stephan, 1983. Test fishage: Juveniles Length and weight: Average length 34 mm Average weight 0.32g (wet) Loading: 0.21g/L Pretreatment:None. Test conditions: Dilutionwater: Filterendaturawlellwater Dilutionwater chemistry: Hardness: 180 mg/L as CaC03 Conductivity: 1300 pmhos/cm pH: 8.3 Lighting: Cool-whitefluorescentlightsat 18 pE/seCIM2. A dailyphotopenod of 16 hours lighatnd 8 hours darkwas maintainedthroughoutthetesting period. Stockand testsolutiopnreparationA:primarsytocksolutiownas prepared by dissolvin6g00 g oftestsubstancewith 1000 mL dilutiownater. Exposure concentrationwsere preparedby serialdilutioonfthe stock solutionswithinthe proportionadliluter. Concentrations dosing rate:Continuous Flow-through rate:Average of6.7complete volume changes per 24 hours. Stabilityof the testchemical solutions: Not noted. Exposure vessels: 20 L glassaquaria(20x4Ox25 cm) containing15 L oftest solutionwitha water depth ofapprox.18 cm. Number of replicates:2 Number of fishper replicate:10 Number of concentrations: fiveplusa blankcontrol Water chemistry during the study: pH range (0-96hours): 8.0- 8.5 (controelxposure) 7.8- 8.3 (1000 mg/L exposure) Temperature range (0-96hours): 22.4- 22.7 OC (controelxposure) 22.3- 22.5 -C (1000 mg/L exposure) Conductivityrange: (0-96hours) 1300 - 1500 pmhos/cm (controelxposure) 1300 - 1500 pmhos/cm (1000 mg/L exposure) Dissolved oxygen range (0-96hours): 8.0- 8.7 mg/L (controelxposure) 3.0- 6.5 mg/L (1000 mg/L exposure) RESULTS Nominal concentrations: Bk control,140,240, 400, 610, and 1000 mg/L. Element values: 96-hour LC50 = >1000 mg/L Element valuesbased on nominal concentrations Remarks: Testingwas conducted on the mixtureas describedintheTest Substance Remarks field.The values reportedapplytothatmixtureand not the fluorochemicalproportionalone. CONCLUSIONS The testsample 96-hour LC50 forfatheadminnow was determined to be >1000 mg/L inboth replicatesN.o mortalitoyr sublethaleffectswere observed. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul, Minnesota,55133 DATA QUALITY ReliabilityK:limischranking2. The study meets the criterifaorquality testing.However, the sample puritywas notpropedy characterizedand the studylacksanalyticaclonfirmatioonfthe amount offluorochemicalproportion inthe solution. REFERENCES This studywas conducted by EnviroSystems DivisionR,esource Analysts, Inc.,of Hampton, NH atthe requestofthe 3M Company, St.Paul,MN, Lab Request number H1609,1990. OTHER Last changed: 6/28/00 Study Title Flow Through Acute Toxicity of FC-787 to the Fathead Minnow, Pimephales promelas Authors Timothy J. Ward Robert L. Boeri Study Completed September 20, 1990 Performina Laboratory EnviroSystems Division Resource Analysts, Incorporated P.O. Box 778 One Lafayette Road Hampton, New Hampshire 03842 EnviroSystems Study Number 9069-3 Page 1 of 17 Remurce Amtyft Inc.S,ubsidlayofMWPORE 1. GOOD LABORATORY PRACTICE STATEKENT This study was conducted according to OECD Good Laboratory Practice Regulations. Neither the Study Director nor the sponsor are aware of any circumstances that would affect the integrity of tbi study. At the sponsors request, aeration was not employed to maintat: dissolved ozygen concentrations above 80% saturation. The average length of fish was outside the range specified in the protocol. The randomization of test specimens can not be verified by the raw data. No deviations existed that significantly affected the validity of the study. .ulhor and Study Director T'VILI z i66i'rtL.'Boiri Coauthor ,4AUU nne P. x gaz @ qau 'I'mToxi I i t PJj-r7,co@et4@ @e-t@r L. Kowalski Aquatic Toxicologist EnviroSystens Study Number 9069-3 Page 2 of 17 ResourceArolystsl,nc,S.ubsidiaroyfMILLPM II. QUALITY ASSURANCE STATEMENT Submitted by: EnviroSystess Division Resource Analysts, Incorporated P.O. Box 778 one Lafayette Road Hampton, New Hampshire 03842 Certification: Data presented in this report were derived by methods and with materials identified in the sectionof the report entitled "Methods and Materials." The test was performed in accordance with EnviroSy3tems Protocol 9069-3 and the Product Registration Aquatic Toxicology Laboratory Standard Operating Procedures Manual. The toxicity test was performed by Jeanne Magazu, Peter Kowalski, Robert Boeri, and Timothy Ward. The raw data and final report will be archived at Resource Analysts Inc. for at least 10 years. All data transcribed from the raw data to the report were checked for accuracy and all data were verified by Quality Assurance Auditors. Qua31ty assurance audits were performed on: Audit Date 5/ 5/90 S/ 7/90 8/13/90 12/08/90 Reported to Study Director 5/ 7/90 S/ 7/90 8/13/90 12/10/90 Reported to management -9/27/90 12/10/90 12/10/90 Doreen Newhouse Quality Assurance Officer EnviroSystems Study Number 9069-3 Page 3 of 17 ReswceAmWs, W@cS.u,bW;oroyfMIWPME III. TABLS OF CONTENTS SECTION: 1. Good Laboratory Practice Statement ii. Quality Assurance Statement Ill. Table of Contents IV. index of Tables V. Summary Vi. Introduction VII. Methods and Materials VIII. Results IX. References Appendix A. Water Quality Data from Toxicity Test PAGE 2 3 4 5 6 7 7 11 14 15 EnviroSysteas Study Number 9069-3 Page 4 of 17 Reswce Pnoysts,Inc.SubOkuy d MUJPOPE IV. INDEX OF TABLES Table 1. Cbetical characterizationof a representative sample of natural well water used as dilution water for toxicitytest Table 2. Survivaldata from toxicity test Table 3. Median lethal concentrations (LC50s) from toxicitytest Table A.I. Conductivity, pl, temperature, and dissolved oxygen concentration measured during toxicity test PAGE 8 12 13 16 EnviroSystems Study Number 9069-3 Page 5 of 17 Reswce AnoWs@ Inc.&,jbwlcrv ofMK.UPOQE V. SUM14ARY The acute toxicity of FC-787 to the fathead minnow, Pimepbales promelas, is described in this final report. The test was conducted under flow through conditions for 3M Company for 96 hours during August 3 to 7, 1990, at the EnviroSystems Division of Resource Analysts, Inc. in Hampton, New Hampshire. It was conducted by Jeanne Magazu, Peter Kowalski, Robert Boeri, and Timothy Ward according to the protocol developed for EnviroSystems Study Number 9069-3. The test was performed under flow through conditions with five concentrations of test substance and a dilution water control at a temperature of 23 20C. The dilution water was filtered natural well water collected at Hampton, New Hampshire. Aeration was not employed to maintain dissolved oxygen concentrations above 80% saturation. Nominal concentrations of FC-787 were: 0 mg/L (control), 140 mg/l, 240 mg/L, 400 mg/L, 610 mg/L, and 1,000 mg/L. Nominal concentrations were used for all calculations. Fish used in the test were purchased from a commercial supplier and acclimated under test conditions for 14 days. After 96 hours of exposure the control fish had an average total length of 3.4 cm and an average wet weight (blotted dry) of 0.32 g, resulting in a loading rate of approximately 0.21 g/L. All fish were in good condition at the beginning of the study. The test substance was nontoxic to fathead minnows concentrations. Exposure of fathead minnows to the test resulted in a 96 hour LC50 of ) 1,000 mg/L FC-787. at tested substance EnviroSystems Study Number 9069-3 Page 6 of 17 Resource MaNst% Inc.,Subsidiaryof MIWPORE VI. INTRODUCTION This study was sponsored by 3H Company, St. Paul, Minnesota. The objective of the study was to determine the acute toxicity of FC-787 to the fathead minnow, a freshwater fish. The report contains sections that describe the methods and materials employed in the study, and the results of the investigation. The report also contains an appendix that presents the water quality data collected during the test. VII. METHODS AND MATERIALS TEST SUBSTANCE: FC-787 EnviroSysteas (EnviroSystems Sample Number 2469E) WA3 delivered to on May 15, 1990. It was contained in a I gallon plastic bottle that was labelled with the following information: "FC-787 Lot 101 surfactants/butyl carbtal, 5-10-90" and a 1 liter plastic bottle labelled as "FC 787, Lot 101, (1-12047)". FC-787 was supplied by 3M Company, St. Paul, Minnesota. Prior to use the test material was stored in the dark at room temperature. A reserve sample will be archived at EaviroSystems for a minimum of 10 years. DILUTION WATER: Water used for acclimation of test organisms and for all toxicity testing was collected from wells at EnviroSystems in Hampton, New Hampshire. Water was adjusted to a hardness of 180 mg/L as CaC03 and stored in 500-gallon polyethylene tanks, where it was aerated. Results of ctemical analysis of a representative sample of water are presented in Table 1. TEST ORGANISM: Juvenile fathead minnows employed as test organisms were from a single source and were identified using an appropriate taxonomic key. They were purchased from a commercial supplier and acclimated at the gavirosystess facility for 14 days. Control fish were weighed and measured at the conclusion of the toxicity test. Prior to testing, fish were maintained in 100% dilution water under flow through conditions in an all glass aquarium. During acclimation fish were not treated for disease and they were free of apparent sickness, injuries, and abnormalities at the beginning of the test. During the acclimation period prior to the test initiation the temperature ranged from 21.10 to 22.5*C, and the dissolved oxygen concentration was maintainel at or above 8.0 mg/G. Fish were fed a commercial fish food (EnviroSystems lot number TM01) once or twice daily except for the 48 hour period before the test. EaviroSystess Study Number 9069-3 Page 7 of 17 reswce Apolystsl,m.,SubsidiaroyfMILLIPORE Table 1. Chemical characterizationof a representative sample of natural well water used as dilutionwater for toxicitytest Parameter PH Conductivity Hardness: initial final Organochlorine pesticides Organophosphorus pesticides polychlorinated biphenyle Unit of Neasurement Reporting Limit pH units umhos/cm mg/L as C&CO* -- ug/L 0.5 ug/L 5.0 ug/L 0.5 Measured Value 8.3 1300 190 200 ND ND ND Notes: 1. ND 3*not detected above thmem@r@eporting limit. 2. The values for pl, conductivity, &ad hardness were derived from a sample of dilutionwater collectedat the beginning of the toxicity test (hardnesswas also determined at the conclusion of the test) and all other valueswere derived from samples of dilution water that were analyzed as part of a routine, bi-annual water testing program. EnviroSystems Study Number 9069-3 Page 8 of 17 Re:,"Ce Amlysts.k@e.S,ub@diorVofMILLIPORE TOXIcrTY TESTING: A screening test with the test substancewas conductedunder static conditions during July 20 to 24, 1990. The nominal concentrations of test substancewere 10, 50, 100, 500, and 1,000 mg/l FC-7&7. After 96 hours there was loo% survival at all tested concentrations. The dafinitive toxicity test was performed during August 3 to 7, 1990, according to EviroSystems Text Protocol 9069-3 (Acute Flow Through Toxicity of FC-787 To The Fathead Minnow Pinephales projielas), which was signed by the Study Director on July 10, 1990. It is based on procedures of the OECD (1984). The test was conducted at a target temperatureof 23 1 2*C with five concentrations of test substance and a dilutionwater control. A stock solution was prepared by combining 600.0 9 of test substance and deionized water and adjusting the total volume to 1,000 mi. Nominal concentrations of the test materialwere: 0 mg/L (control), 140 mg/L, 240 mg/L, 400 mg/L, 610 mg/L, and 1,000. The test substance Was supplied to the test vessels under flow through conditionsby an intermittent flow proportionaldiluter. All parts of the diluterthat contacted the test substance were fabricated from glass or Teflon. During the test the diluter was activated806 times, resultingin an average of 6.7 media exchanges per 24 hours in each test vessel. Twenty fish were randomly and equally distributedamong two replicates of each treatment. The test was performed in 20 liter glass aquaria (approximately 20 ca in width, 40 cm in length, and 25 cm in height) that contained 15 liters of test solution (waterdepth Was approximately 18 em). Test vessels were randomly arranged in a water bath during the 96 hour test (a random numbers table was used to select the location of each vessel). A 16 hour light and 8 hour dark photoperiod was automatically maintained with cool-white fluorescent lights that provided a light intensity of 18 uSs-la-2. keration as not employed to maintain dissolved oxygen concentrationsabove :cceptablelevels. Fish were not fed during the test. The number of surviving organisms and the occurrence of sublethal effects (loss of equilibrium, erratic swimming, lose of reflex, excitability,discoloration,or change in behavior) were determined visually and recorded initially and after 24, 49, 72, and 96 hours. Dead test organisms were removed when first observed. Dissolved oxygen (YSI Model 57 meter; instrument number PRL-18), pH (Beckman model pRI 12 meter; instrument number PRL-4), conductivity (Labcomy SCT meter, instrument number PRL-9), and temperature (ASTM mercury thermometer; thermometer number 2160) were measured and recorded daily in each test chamber that contained live animals. EnviroSystems Study Number 9069-3 Page 9 of 17 ResourceAmlystsI,nc.&,jbsdoryofMUMRE STATISTICAL METHODS: Reau'@tsof the toxicity test could not be interpretedby standard statistical techniques (Stephan,1983) because 100% survival occurred at all tested concentrations. FnviroSystess Study Number 9069-3 Page 10 of 17 ReswceAr)a".IncS,u,bsidoifqMILLPM VIII. RESULTS Test vessels containing 0 mg/l to 400 mg/L FC-787 were initially clear and remained free of insoluble material throughout the test. Test vessels containing 610 mg/l and 1,000 mg/L FC-787 contained foam on the test media surface throughout the test. Biological and water quality data generated by the acute toxicity test are presented in Table 2 and Appendix A, respectively. One hundred percent survival occurred in the control exposure. Control fish had an average total length of 3.4 cm, and a wet weight (blotted dry) of 0.32 g, resulting in a loading rate of approximately 0.21 g/L. The 24, 48, 72, and 96 hour LC50s for fish exposed to FC-787 are presented in Table 3. Because toxicity did not occur at any tested concentration, the 96 hour LC50 value is )1,000 mg/L FC-787. EnviroSystems Study Number 9069-3 Page 11 of 17 ResourceAnoWt Inc.S,ubsidkuyof MWPORE Table 2. Survival data from toxicity test Nominal Concentration (mg/L) rep. Number Alive Ohr 24hr 48hr 72hr 96hr Number Affected Ohr 24hr 48hr 72hr 96hr 0 (control) 1 2 10 10 10 10 10 10 10 10 10 10 140 1 10 10 10 10 10 2 10 10 10 10 10 240 1 10 10 10 10 10 2 10 10 10 10 10 400 1 10 10 10 10 10 2 10 10 10 10 10 610 1 10 10 10 10 10 2 10 10 10 10 10 1,000 1 10 10 10 10 10 2 10 10 10 10 10 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Note: Sublethal effects that were not observed were loss of reflex, excitability,discoloration,lethargy, and change in behavior. EnviroSystems Study Number 9069-3 Page 12 of 17 Remurce ArmN-ftInc.S,ubsdioryofMIWPORE Table 3. Median lethal concentrations(LC50s) from toxicity test Exposure period 24 hours 48 hours 72 hours 96 hours 95 percent LC50 confidence limit > 1,000 mg/L > 1,000 mg/L > 1,000 mg/L )1,000 mg/L LC50 calculation method EaviroSysteas Study Number 9069-3 Page 13 of 17 ResotxceAnatyftft.,SubsldkuoyfMUJPORE ix. REFERENCES OECD. 1981. Decision of the Council Concerning the Mutual Acceptance of Data in the Assessment of Chemicals. Annex 2. OECD Principles of Good LaboratoryPractice. C (81) 30 (Final). OECD. Biotic 1984. 1984. Guidelines for Testing of Chemicals. Section 2: Effects on Systems. Method 203, fish Acute Toxicity Test. Adopted April 4, Stepban, C.E. 1983. Computer Program for the Calculation of LC50 Values. U.S. EPA. Duluth, MN. Personal Communication. EnviroSystems Study Number 9069-3 Page 14 of 17 Romice M-*ft Inc.S,ubskflofrMyIPM Appendix A. WATER OUALITY DATA FROM TOXICITY ?EST a EnviroSysteas Study Number 9069-3 Page 15 of 17 ResourceAnalystsl,x.,Subsidkwyd MLLIPORE Table A.l. Conductivity, pH, temperature, and dissolved oxygen concentration measured during toxicity test Nominal concentration (mg/L) Rep. Conductivity (umbo/cm) 0 24 48 72 96 br hr br hr hr 0 (control) 1 2 140 1 2 240 1 2 400 1 2 600 1 2 1,000 1 2 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 1300 ISOO 1500 1300 1300 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 1300 1500 1500 1300 1300 PH 0 24 49 72 96 hr hr hr br br 8.3 8.1 8.5 8 1 8.1 8.3 8.0 8.5 8.'1 8.2 8.2 8.0 8.5 8.0 8.1 8.2 8.0 8.5 9.0 8.1 8.2 8.0 9.4 8.0 8.0 8.2 8.0 8.4 9.0 8.0 8.1 7.9 8.4 7.9 8.0 8.1 7.9 8.4 7.9 7.9 8.1 7.9 9.4 7.9 7.9 8.1 7.9 9.4 7.9 7.9 8.1 7.9 8.3 7.8 7.9 6.1 7.9 8.3 7.8 7.9 EnviroSystems Study Number 9069-3 Page 16 of 17 RoMfce Am@ystsk.@c,SubwJoy QfMi LM?E Table A.I. Continued. Nominal concentration (mg/L) Rep. Temperature (*C) 0 24 48 72 96 hr hr hr br hr 0 (control) 1 2 22.4 22.4 22.5 22.7 22.4 22.5 22.5 22.5 22.1 22.5 140 1 22.4 22.5 22.4 22.5 22.5 2 22.5 22.4 22.5 22.5 22.5 240 12 2222..44 2222..54 2222..45 2222..55 2222..55 400 1 22.5 22.5 22.6 22.6 22.5 2 22.5 22.4 22.5 22.5 22.5 610 12 2222..55 2222..45 2222..56 2222..55 2222..S5 1,000 1 22.5 22.5 22.5 22.5 22.4 2 22.5 22.4 22.5 22.4 22.3 Dissolved Oxygen (mg/L) 0 24 49 72 96 hr hr hr hr hr 8.2 8.3 8.0 E.6 9.0 8.2 a.0 8.0 1,7 8.3 7.7 1.8 7.7 6.1 7.5 7.3 7.4 7.5 7.9 7.2 1.3 7.5 7.3 7.6 6.7 1.3 1.1 7.1 7.1 6.7 6.9 6.3 6.5 6.5 5.2 1.0 6.3 6.3 6.4 5.5 ?.o 5.8 5.8 6.2 4.5 6.8 5.8 5.6 6.2 4.1 6.4 4.7 5.0 4.8 3.0 6.5 5.0 5.0 5.1 3.0 EnviroSystems Study Number 9069-3 Page 17 of 17 Resm=eAnalystsI,nc.S.ubW!ofoyfWLLIPOK