Document Yj1MD1OkKNrJm0QLwpMEGDq0O

ACUTE TOXICITY TO AQUATIC INVERTEBRATES (DAPHNIA MAGNA) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatweh,ich may alsobe referredtoas PFOS, FC-95, oras 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 followingsummaty applies to a mixture with incompletely characterizedconcentrations of impurities.Data may not accurately reflectthe toxicityof the fluorochemical component of the testsample. METHOD: Method: OECD Guideline202. Type: Acute static GLP: No Year completed: 1990 Species: Daphnia magna Supplier: In-houseculturemsaintainedatEnviroSystemsDivisionR,esource Analysts,Inc.,Hampton, NH. Analyticalmonitoring: pH, temperature,conductivitya,nd dissolved oxygen. Exposure period: 48-hours Test organism age: <24-hours old Statisticamlethod: The EC50 valueswere calculatedusinga computer program by Stephan, 1983. Test conditions: Dilutionwater: Filterednaturalwellwater Dilutionwater chemistry: Hardness: 180 mg/L as CaC03 Conductivity: 1300 pmhos/cm pH: 8.1 Lighting: Cool-white fluorescent lightsat 18 pE/sectm 2 . A dailyphotoperiod of 16 hours lighatnd 8 hours dark was maintainedthroughoutthe testing period. Stock and testsolution preparation: A 1000 mg/L stock solutionwas prepared by dissolving1 g oftestsubstance in1000 mL dilutiownater. Exposure concentrationwsere prepared by additionofstocksolutiontothe testvessels. Exposurevessels:250 mL glassbeakerscontaini2n0g0 mL oftestsolution and a water depth ofapproximately6 cm. Number of replicates:2 Number of daphnids per replicate:10. Number of concentrations: fiveplusa blankcontrol Water chemistry during the study: pH range (0-48hours): 8.0- 8.1(controelxposure) 8.0- 8.3(1000 mg/L exposure) Temperature range (0-48hours): 19.8- 20.9OC (controelxposure) 20.0- 20.9 -C (1000 mg/L exposure) Conductivityrange: (0-48hours) 1300 - 1300 pmhos/cm (controelxposure) 1200 - 1300 pmhos/cm (1000 mg/L exposure) Dissolved oxygen range (0-48hours): 8.5- 9.0mg/L (controelxposure) 8.0- 9.0mg/L (1000 mg/L exposure) RESULTS Nominal concentrations: Blank control,150,250, 400, 600, and 1000 mg/L. Elementvalues: 48-hourEC50=>1000mg/L Element valuesbased on nominal concentrations 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 >1000 mg/L. No mortalitoyr sublethaleffectswere observed. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota,55133 DATA QUALITY ReliabilityK:limischranking= 2.The study meets the criterifaorquality testing.However, the sample puritywas notproperlycharacterizedand the study lacksanalyticaclonfirmatioonfthe amount offluorochemicalproportion inthe solution. REFERENCES Thisstudywas conducted by EnviroSystemsDivisionR,esource Analysts, Inc.,Hampton, NH attherequestofthe3M Company, St.Paul,MN, Lab Request number H1609, 1990. OTHER Lastchanged: 6/28/00. Study Title Static Acute Toxicity of FC-787 to the Daphnid,Dapbniamagna Authors Timothy J. Ward Robert L. Boeri Study Completed September 4, 1990 Performina Laboratory EnviroSystems Division Resource Analysts, Incorporated P.O. Box 778 One Lafayette Road Hampton, New Hampshire 03842 EnviroSystems Page 1 of 16 Study Number 9070-3 ResourceAmNft Inc.S.ubWkiry ofMIWPM r. C-00t LABORliTORY PRACTrcs STATENEIFT 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 integrityof this study. The test substance was stored at room temperature,test specimens were added to test vessels indiscriminatelyand test vessels were ratdonized, and the test was conducted with 2 ratherthan 4 replicates. No deviations existed that significantlyaffectedthe validity of the study. Rc@bertL: Boeri Coauthor and Study Eirector l@@# qa4j--, TAiumtt by Ji W4frd or /AAg ati Tomxiigcaozlloislt ,o,.e-, Pdter L. Kowalski Aquatic Toxicologist o).:-5io EnviroSystems Study Number 9070-3 Page 2 of 16 ResourceAnalystsI.nc,SubsidiaroyfMILLIPORE 11. QUALITY ASSURANCE STATEKENT submitted by: Envir*Systess 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 section of the report entitled "Methods and Materials." The test was performed in accordance with EnviroSystems Protocol 9070-3, with the noted exceptions and the Product Registration Aquatic Toxicology Laboratory Standard Operating Procedures Manual. The toxicity test was performed by Jeanne Magazu, Peter Kowalski, Robert Doeri, and Timothy Ward. The original 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 chocked for accuracy, and all data were verified by Quality Assurance Auditors. Quality assurance audits were performed on Audit Date 5/ 5/90 7/25/90 8/14/90 10/25/90 Reported to Study Director S/ 7/90 7/25/90 8/14/90 10/25/90 Reported to Management -8/ 6/90 10/25/90 10/29/90 Doreen Newhouse Quality Assurance Officer EnviroSystems Study Number 9070-3 Page 3 of 16 ResourceAnalystsI,nc.S,ubsidiaroyfMIWPORE Ill. TABLE OF CONTENTS SECTION: I. Good Laboratory Practice Statement ii. Quality Assurance Statement Ill. Table of Contents IV. Index of Tables and Figures V. Sumnary VT. Introduction Vii.. Methods and gaterials viii Results IX. References Appendix k. Water Quality Data from Toxicity Test PAGE 2 3 4 5 6 7 7 10 13 14 EnviroSystems Study Number 9070-3 Page 4 of 16 ResourceAriol@-sltrst,cS.u,b0ioq ofWLUPORE IV. INDEX OF TABLES AND FIGURES Table 1. Chemical characterization of a representative sample of natural well water used as dilution water for toxicity test Table 2. Survival data from toxicity test Table 3. Median effective concentrations (EC509) from toxicity test Table A.l. Conductivity, pH, temperature, and dissolved oxygen concentration measured during toxicity test PAGE 8 11 12 is EnviroSystems Study Number 9070-3 Page 5 of 16 Remice ArolystIsn,c.S,ubsidiarOy(MUPORE V. SUMMARY The acute toxicity of FC-787 to the daphnid,Dapbnia magna, is described in this final report. The test was conductedfor 3M Company for 48 hours during July 23 to 25, 1990, at the EnviroSystemsDivision 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 9070-3. The test was performed under static conditions with five concentrationsof test substance and a dilution water control at a temperature of 20 10C. The dilution water was filtered natural well water collected from wells at Hampton, New Hampshire. Aeration was not employed to maintain dissolved oxygen concentrations above an acceptable level. Nominal concentrations of FC-787 were: 0 mg/L (control), 150 mg/L, 250 mg/L, 400 mg/L, 600 mg/L, and 1,000 mg/L. Nominal concentrations were used for all calculations. Daphnids used in the test were produced from an in-house culture and were less than 24 hours old at the start of the test. After 48 hours of exposure the control daphnids had an average wet weight (blotteddry) of 0.0002 g, resultingin a loadingrate of 0.01 g/L. All daphnids were in good condition at the beginning of the study. Exposure of daphnids to the test substance resulted in a 48 hour EC50 of > 1,000 mg/L FC-787. EnviroSystems Study Number 9070-3 Page 6 of 16 Resource AnaWL Inc.,Stibsidk3royf MIWPORE vi. INTRODUCTION This study was sponsored by 3M Company, St. Paul, Minnesota. The objective of the study was to determine the acute toxicityof FC-787 to the daphnid, a freshwater invertebrate. 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 collectedduring the test. VII. METHODS AND MATERIALS TEST SUBSTANCE: FC-787 (EnviroSystems Sample Number 2469E) was delivered to EnviroSystems on May 15, 1990. It was contained in a I gallon plastic bottle that was labelled with the following information: "Lot 101 surfactants/butylcarbtal, 5-10-90". FC-787 was supplied by 3M Company, St. Paul, Minnesota. Prior to use the test materialwas stored in the dark at room temperature. A reserve sample wilt be archived at EnviroSystems for a minimum of 10 years. DILUTION WATER: Water used for acclimationof test organismsand for all toxicity testing was collected from wells at EnviroSysteas in Hampton, New Hampshire. Water was stored in 500-gallon polyethylene tanks where it was aerated. Results of chemical analysis of a representativesample of water are presented in Table 1. TEST ORGANISM: Juvenile daphnids employed as test organisms were from a single source and were identified using an appropriate taxonomic key. Daphnids used in the test were produced from an in-house culture and were less than 24 hours old at the start of the test. Control daphulds were weighed at the conclusionof the toxicity test. Prior to testing, daphnids were maintained in 100% dilution water under static c@nditions in 4 liter glass jars. During acclimation daphnids were not treated for disease and they were free of apparent sickness, injuries, and abnormalitiesat the beginning of the test. During the acclimation period 24 hours prior to the test initiationthe temperaturewas 20.0*C. Dapbnids were fed yeast, trout cbow, and/or the freshwater alga Selenastruscapricornutumonce or twice daily before the test. EnviroSysters Study Number 9070-3 Page 7 of 16 PesourceAmWs, Inc.S,ubsidioroyfMILLIPORE Tab@:: Chemical characterization of a representative sample of natural well water used as diluti*n water for toxicity test Parameter PH Conductivity Hardness Organochlorine pesticides Organophosphorus pesticides Polychlorinated biphenyls unit of Measurement Reporting Limit PR units umhos/cm mg/L as CaCO3 -- ug/L 0.5 ug/L 5.0 ug/L 0.5 Measured Value 8.1 1300 iso NDO NDs NDa anot detected above the reporting limit. EnviroSystems Study Number 9070-3 Page 8 of 16 PosoufceAnalystsI,nc.S,ubsidiaroyfMILLIPOPE TOXICITY TESTING: A screening test with the test substance was conducted during Nominal concentrations of test substance were July 20 to 22, 1990. 10 mg/L, 50 sg/L, 100 mi;/L,500 mg/L. and 1,000 mg/L. After 48 hours of exposure there was 50% survival at 1,,000mg/L, 90t survival at 500 mg/L, and 100% survival at &11 other tested concentrations. The 4efinitive toxicity test was performed during July 23 to 25, 1990, according to InviroSystess Test Protocol 9070-3 (Static, Acute Toxicity Test With FC-781 And The Daphnid, Dapha'a magna), which was signed by the Study Director on July 20, 1990. It is based on procedures of the OECD (1984). arget temperature of 20 IOC with The test was conducted at a t five concentrations of test substance and a d4lution water control. A 1,000 mg/L stock solution was prepared by c;mbining 1.0 9 of test substance with dilution water and adjusting the final concentration to 1,000 al without the use of a solvent. Nominal concentrations of the test material were: 0 mg/L (control), 150 mg/L, 250 mg/L, 400 mg/L, 600 mg/L, and 1,000 mg/L. Twenty dapbnids were randomly and equally distributed among two replicates of each treatment. The test was performed in 250 ml glass beakers that contained 200 al of test solution (water depth was Test vessels were randomly arranged in an approximately 6 es). incubator during the 48 hour test (a random numbers table-was used to select the location of each vessel). A 16 hour light and 8 hour dark pbotopiriod was automatically maintained with cool-white fluorescent lights that provided a light intensity of It uZs-la-2. Aeration was not required to maintain dissolved oxygen concentrations above acceptable levels. Bapbnids were not fed during the test. of surviving organisms and the occurrence of The number immobilization (inability to swim within 15 seconds after gentle gitation) or other sublethal effects (loss of equilibrium,erratic discoloration, or change in :wimming, loss of reflex, excitability behavior) were determined visually and reI corded initially and after 24 Dead test organisms were removed when first observed. and 46 hours. Dissolved oxygen (Y$l Model 57 meter; instrument number PRL-18), pE (Beckman model pRI 12 meter; instrument number PRL-4), conductivity (Labcoap SCT meter, instrument number PRL-9), and temperature (ASTM mercury thermometer; thermometer number 2211) were measured and recorded daily in each test chamber that contained live animals. STATISTICAL METHODS: Results of the toxicity test could not be interpreted by standard statistical techniques (Stephan, 1983) bqcause greater than 50% survival occurred at all tested concentrations. EnviroSystems Study Number 9070-3 Page 9 of 16 ResourceAndysts,Inc,S,ubs4laryolMILLIPORE VIII. RESULTS All test vessels containing FC-787 appeared clear initially and remained free of insoluble material 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 daphnids had an average wet weight (blotted dry) of 0.0002 g at the end of,the test. Loading rate during the toxicity test was approximately0.01 g/L. Exposure of daphnids to the reference toxicant sodium dodecyl sulfate resulted in a 48 hour LC50 and EC50 of 24.8 mg/L. The 24 and 48 hour EC50s for daphnids exposed to FC-787 are presented in Table 3. The test substance was nontoxic to daphnids at tested concentrations, resulting in a 48 hour EC50 of 1,000 mg/L FC-787. ZnviroSystems Study Number 9070-3 Page 10 of 16 ResourceArmlo& Inc.S.ubsidbyofMWPORE Table 2. Survival data from toxicity test Nominal Concentration (mg/L) rep. Number Alive 0 hr 24 hr 48 hr Number Affected Ohr 24hr 48hr 0 (control) 1 2 100 1 2 150 1 2 250 1 2 400 1 2 600 1 2 10 10 10 10 10 10 10 10 10 10 10 9 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 9 10 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 Note: No daphnids were immobilized (unable to swim within 15 seconds after gentle agitation) EnviroSystems Study Number 9070-3 Page 11 of 16 ResourceAnatyftInc.S,Lbsidkuyd MIWPORE Table 3. Median effective concentrations (EC50s) from toxicity test Exposure period 95 percent EC50 confidence limits Calculation method 24 hours ) 1,000 mv/L 48 hours ) 1,000 mg/L EnviroSystess Study Number 9070-3 Page 12 of 16 ResoLwceAnatvft Inc.S,ubWkW ofMUPORE 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. 1984. Guidelines for Testing of Chemicals. Section 2: Effects on Biotic Systems. Method 202, Dapbnid sp., Acute ImmobilizationTest and Reproduction Test. Adopted April 4, 1984. Stepban, C.E. 1983. Computer program for calculation of LC50 values. Personal communication. EnviroSystems Study Number 9070-3 Page 13 of 16 nesoliceAj)a@st5I,nc,Sub@@idiaorfyMILLIPOPE Appendix A. WATET OUALITY DATA FROM TOXICITY TEST EnviroSysteas Study Number 9070-3 Page 14 of 16 ResoufceApolystsI,nc,StibsidiaorfyMILLIPORE - ---m -- - m Table k.l. Conductivity, PH, temperature, and dissolved Oxygen concentrationmeasuredduring toxicitytest Nominal concentration (mg/L) Rep. 0 (control) 1 2 ISO 1 2 250 1 2 400 1 2 600 1 2 1,000 1 2 Conduciivity (umbo/es) 0 24 48 br br br 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1300 1200 1200 1200 1200 1200 1200 1200 1200 1200 1200 0 br 8.1 8.1 8.0 9.0 8.0 8.0 8.0 0.0 8.0 8.0 810 8.0 PH 24 br 8.0 8.0 8.1 8.1 8.1 8.1 8.1 8.1 8.1 8.1 8.2 9.2 48 hr 8.1 8.1 8.3 9.3 8.3 8.3 8.3 9.3 9.3 8.3 8.3 8.3 EnviroSystess Study Number 9070-3 page 15 of 16 Resovrce Analysts@rc, SubsidiaroyfMILLPORE Table A.l. Continued. Nominal concentration (mg/L) Rep. Temperature (OC) 0 24 48 hr hr hr 0 (control] 1 2 150 1 2 250 1 2 400 1 2 600 1 2 1,000 1 2 20.9 20.9 20.9 20.9 20.9 20.9 20.9 20.9 20.9 20.9 20.9 20.9 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 19.8 19.9 19.8 20.0 19.9 19.9 19.9 19.9 19.9 19.9 20.0 20.0 Dissolved Oxygen (mg/L) 0 24 48 br br br S.S 9.0 8.9 $.S 9.0 8.9 8.5 9.0 8.7 8.5 9.0 8.7 8.5 9.0 8.7 8.5 9.0 8.7 8.5 9.0 8.3 8.5 9.0 8.3 S.S 9.0 8.3 8.5 9.0 8.3 8.3 9.0 8.0 8.3 9.0 8.0 EnvirOSY3teSS Study Number 9070-3 Page 16 of 16 Reswce Arx3ly@tIsn,c.S,ubsidicwyofMILLIPORE