Document 09K16r8QBvO2MyQY660g6X0b

A | U 2- 0 3 ^ ACUTE TOXICITY TO AQUATIC INVERTEBRATES (E.G.,DAPHNIA) TEST SUBSTANCE Identity: Perfluorodecanesulfonate, ammonium salt; may also be referred to as PFDS, FC-121-X, or 3M Sample E2112 and E2566-1. (1Decanesulfonic acid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heneicosafluoro-, ammonium salt, CAS # 67906-42-7) Remarks: Test sample is a mixture of the test substance in water and 2propanol, 1-(1,1-dimethylethoxy). This mixture contains approximately 2226% test substance, 33-37% propanol, 1-(1,1-dimethylethoxy), 0.5-1.5% perfluorononanesulfonate, ammonium salt and 38-42% water). All values reported relate to this mixture. No calculations were made to adjust for the actual concentration of the test substance in the test sample. Test sample was from 3M production lot 1. METHOD Method: EPA 660/3-75-009 and APHA (1980) Standard Methods for the Examination of Water and Wastewater Test type: Static acute GLP: Yes Year Completed: 1988 Species: Daphnia magna Analytical monitoring: pH, dissolved oxygen, temperature. Test substance concentration was not monitored. Statistical methods: EC50values calculated using Binomial method Test daphnid source: ABC Laboratories In-house cultures, Columbia, MO Test daphnid age at study initiation: < 24-hours Test conditions Dilution water. Well water Dilution water chemistry (from a representative sample): hardness. 246 mg/L alkalinity 178 mg/L pH: 8.0 Stock and test solutions preparation: Not given. A cloudy appearance and surface foam present at preparation in the 560 and 1000 mg/L concentrations was not noted at the 24- and 48-hour observation periods. Exposure vessels: 250 mL glass beakers containing 200 mL of test solution. 000.130 Number of replicates: 2 Number of daphnids per replicate: 10 Number of concentrations: five plus a negative control Water chemistry during the study: Dissolved oxygen range (0-48 hours): 8.7 - 9.2 mg/L (control exposure) 8.6 - 9.2 mg/L (1000 mg/L exposure) pH range (0-48 hours): 8.2 - 8.2 (control exposure) 8.2 - 8.4 (1000 mg/L exposure) Test temperature range (0 - 48 hours) 19 - 20 C Element basis: mortality and sublethal effects RESULTS Nominal concentrations: Bk control, 100, 180, 320, 560, 1000 mg/L Element value: 24-hour LC50 = 200 (100-320) mg/L 48-hour LC50 = 130 (100-180) mg/L 48-hour NOEC (sublethal effects) = < 100 mg/L Sublethal effects included quiescence and/or daphnids tending to the bottom of test vessels. Statistical Evaluation: The LC5ovalue and 95% confidence interval was calculated using the binomial method. All element values based on nominal concentrations. Mortality of controls: None Remarks: Values reported are for the test sample (mixture). No calculations were made to adjust for the concentration of the test substance in the test sample. Cumulative percent mortality: N om inal Test Cone., m g/L 24-hours 48-hours Neg. Control 100 180 320 560 1000 0 0 35 100 100 100 0 0 100 100 100 100 000191 CONCLUSIONS The test sample 48-hour ECsofor Daphnia magna was determined to be 130 mg/L with a 95% confidence interval of 100 - 180 mg/L. Testing was conducted on the "as-sold" mixture of the subject material in water (-22-26% subject matherial) The values reported apply to that mixture and not directly to the subject material. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY Reliability: Klimisch ranking 2. This study, while well conducted, lacks analytical data for: determination of the test substance concentration in the test solutions; and determination of the sample purity. Because a mixture was tested, care must be taken when interpreting the results. The solvent in the mixture could have enhanced or restricted biological uptake and/or toxicity of the fluorochemical component. REFERENCES This study was conducted by ABC Laboratories, Columbia, MO on behalf of the 3M Company. OTHER Last changed. 5/18/00 000V32 SPONSOR 3M Company Attn: Mr. Mohamed Elnabaravy EE & PC Environmental Labs Building 21-2W-05, 900 Bush Avenue St. Paul, Minnesota 35106 S U T Y TITLE Acute Toxicity of E2566-1 to Daphnia magna data requirement OECD Guideline 202 sJ l , , Biologist BEST COPY AVAILABLE STUDY COMPLETE!' UN January 9 , 1988 PERFORMING LABORATORY Analytical Bio-Chemistry Laboratories, Inc. Aquatic Toxicology Division 7200 East ABC*Lane P.O. Box 1097 Columbia, Missouri 6525 ABC LABORATORY PROJECT ID #36614 Page 1 of 45 000:193 Submitted By Analytical Bio-Chemistry Laboratories, 7200 East ABC Lane P. 0. Box 1097 Columbia, Missouri 65205 (314) 474-8579 Inc. Prepared ay: B ES TC O PU V M IM M 1* ' ' l'7- 1 V Scott Frazier Biologist II/Study Direct : Approved P> /, - / > , / / ^ Date ......-- >- A..................... -"------------t1._--_-_--_--_--_---_--_--_---_--_--_---_--_---_--_--_---_- ________ // '*( ' * f Alan D. Forbis Date Supervisor, Invertebrate/ Bioconrentration Investigations tfJ jiU f'i Kent Ediger / ......................................... Quality Assurance Officer / ii( M ! Date , Carl M. Thompson Aquatic Toxicology Manager Date :dab28 000194 ABC LABS #36614-2 of 45 iwiiii^wipi iiiiwi..wJiuwiiiBiPiw*MPMW, P ip w !i|w ^ w w f w i |wiw w iwwMM^iiijBMWiWlJWIWBWPWWilIPWWIWMfWIlPlip PROJECT PERSONNEL The Study Director of the project for Analytical Bio-Chemistry Laboratories, Inc. was Scott Frazier, Biologist II. Supervising the conduct of the study for 3M Company was Mr. Mchamed Elnabarawy. The following ABC personnel assisted with various phases of the study. Name Jeffrey Latham Michael Ruddy Scott Frazier Title Biological Technician I Biological Technician I! Biologist II Initials it. J lk O Q O X '? ABC LABS 036614-5 of 45 INVERTEBRATE ACUTE TOXICITY COMPENDIUM Subject: "Acute Toxicity of E2566-1 to Daphnia magra ABC Study Number 36614. Sponsor: 3M Company Testing Facility: Analytical Bio-Chemistry Laboratories, Inc. Aquatic Toxicology Division F.O. Box 1097 Columbia, Missouri 65205 (314-474-8579) Location of Original Raw Data arc Final Report: 3X Company EE a PC Environmental Labs Building 21-2V-05, 900 Bush Avenue St. Paul, Minnesota BEST COPY AVAILABLE Test Material: E25n6-1 Test Concentrations: Control, 100, 180, 320, 560 and 1CC0 mg/1. Dilution Water: 246 mg/1 (hardness), 178 mg/1 (alkalinity), k .0 (pH). Test Dates: Initiation - January 7, 1988 Termination - January 9, 1988 Length of Study: 48 hours Results: 24-hour LC,.q 200 mg/1 (952 C.l. - 100-320 mg/1) 24-hour NOEL <* 100 mg/1 48-hour LCj.q 130 mg/1 (952 C.l. - 100-180 mg/1) 48-hour NOEL - <100 mg/1 (estimated) Test Species: Daphnia magna Source of Organisms: ABC Laboratories in-house culture. Age of Organisms at Study Initiation: First-instar {<2A hours old) 0OOi ABC LABS i36614-6 of 45 SUMMARY The acute toxicity of E2566-1 to Daphnia magna as assessed using the methods outlined by the Committee on Methods for Toxicity Tests with Aquatic Organisms. Water quality parameters of temperature, dissolved oxygen and pH were measured at the termination of the test and were within acceptable limits. The results of the 48-hour static Daphnia magna toxicity study are summarised below. All reported values were based upon nominal concen trations. Compound F2566-1 24-Hour LC50 (952 C.I.) (100-320 mg/1) 48-Hcur LCjq (952 C.I.) 130 mg/1 ;100-180 mg/1) The no-efect level observed for E2566-I at 24 hours was 100 mg/i based on the absence of all abnormal effects. The 48-hour no-effect level was estimated to be <100 mg/1 since abnormal effects were observed in all treated test concentrations. ABC LABS #36614-7 of 45 31gtnitrAVAd03iS 3& INTRODUCTION This definitive static bioassay was performed by the Aquatic Toxicology Division of Analytical Bio-Chemistry Laboratories, Inc., Columbia, Missouri, for 3M Company, from January 7, 1988 to January 9, 1988. The purpose of this test was to determine the 24- and 48-hour LC.q levels for E2566-1 to Daphnia magrta. The study was performed using ABC Protocol #7806 as approved by Mr. Mohamed Elnabarsvy, 3M Company, on January 7, 1988. METHODS AND MATERIALS The procedures for static bioassav, as described In Methods of Acute Toxicity Tests with Fish, Macroinvertebrates and Amphibians (1) and Standard Methods for Examination of Water and Wastewater (2), were used in this experiment. I . Test Organisms The Daphnia magna used in the test were cultured at the ABC facilities in well water (Table 1). The adult daphnids were fed algae (Selenastrur, capricornutum) at least every three days prior to testing and supplemented with a suspension of Tetramin, cereal leaves, vitamin solution and yeast. The daphnids were identified to species using the taxonomic key presented by Pennak (3). II. Test Procedure The static Daphnia bioassav was conducted in 250-ml glass beakers containing 200 ml of daphnid culture/test water. Test vessels were covered with loose-fitting petri dish covers to minimize evaporation and protect -.gainst contamination during the study. These vessels were kept at 20 (12.0) C iu a temperature controlled area. The lighting was maintained at 50-70 footcandles on a 16-hour daylight photoperiod with 30-minute simulated dawn and dusk periods. An Initial range-finding experiment was conducted using ten Daphnia each in exposure concentrations of 1.0, 10, and 100 mg/1. From these results, five treatment concentrations in duplicate with ten Daphnia (first instar less than 24 hours old) per beaker were selected for the definitive bioassay. These concentrations were a logarithmic series ranging from 100 to 1000 mg/1 and included a control. All concentrations were observed once every 24 hours for mortality ahd abnormal effects such as surfacing, clumping of the daphnids together and daphnids tending to the bottom of test chambers. Water chemistry parameters of temperature, dissolved oxygen and pH were measured In the control, low, middle and high concen trations at 0 and 48 hours. 000200 ABC LABS #36614-8 of 45 best copy available III. IV. Test Compound The E2566-1 sample was received on December 2 9 , 1987 as a light brown liquid and was stored at room temperature in darkness. Sample purity was unspecified. Test concentrations were prepared based on total product. All standard weights and dilutions can be found in the Appendix. Daphnid culture/test water was used in the preparation of all working stock solutions. Statistics RESULTS Statistical analysis of the concentration vs. eiiecr data generally mortality) was obtained by employing a computerized LC.~ program developed by Stephan et al. (4). This program calculated the LC. statistic and its 95 percent confidence limits using the binomial, the coving average and the probit tests. However, if no mortality occurred or if a ccse re sponse cculd not be demonstrated over a reasonable range (,<37 to "'63") an LC and/or its 95 percent confidence limits cculd not be calculated. Three different methods of analyzing the data were used since no one method of analysis is appropriate for all possible sets of data that may be obtained. The method of calculation selected for presentation in thin report was that which gave the narrowest confidence limits for the LC.q {4, 5) although all three models are valid. Table 2 presents the calculated i.t. values and 95-percent confi dence Intervals for E2506-1. The 24- arc 48-hour LC-.. values were 200 and 130 mg/1, respectively. All results were based on the nominal concentrations of 100, !C, 320, 560 and 1000 mg/1. The no-effect concentration based on the absence of mortality and abnormal effects was 100 mg/1 at 24 hours. At 48 hours the no-effec.t level was estimated to be <100 mg/1 since all treated concentrations exhibited abnormal effects. The abnormal effects observed during the study were mortality, quiescence and/or daphnids tending to the bottom of test vessels. A cloudy appearance and surface foam present at preparation in the 560 and 1000 mg/1 concentrations was not noted at the 24- and 48-hour observation periods. Table 3 presents the percent mortality and water quality parameters measured during the test. The dissolved oxygen concentrations ranged between 8.6 and 9.2 mg/1. These values represented 99 and 103-percent saturation at 20 and 19 C, respectively (corrected for local altitudinal pressure), and were considered adequate for testing (1). The pH values of the test solutions ranged from 8.2 to 8,4 and were consistent with the control. The study was conducted following the Intent of the Good Laboratory Practice Regulations (6) and the final report was reviewed by Analytical Bio-Chemistry Laboratories' Quality Assurance Unit. All original raw data were provided to 3M Company, with a copy retained at Analytical Bio-Chemistry Laboratories. 000201 ABC LABS #36614-9 of 45 BESTCOPY AVAILABLE TABLE 1 Chemical Characteristics of Veil Water Used by ABC's Aquatic Toxicology Division. Parameter Temperature Dissolved 0xygena pH Hardness (CaCO^) Alkalinity (CaCO^) Conductivity Total Organic Carbon Suspended Solids Aluminum Arsenic Boron Cadmium Chromium Cobalt Copper Iron Lead Mercury Nickel Silver Zinc Measured organophosphorus pesticides Measured organochlorine pesticides plus PCB's Concentration 17 - 22*Cb 7.4 - 9.1 ppmb 7.6 - 8.4b 206 - 275 ppmb 224 - 336 ppmb 500 - 650 ymhos/cmb 1.4 ppmC (0.9 - 2.8 ppm)d 0 - 1 . 3 ppmb <10 ppb <1 ppb 2.25 ppm <3 ppb <7 ppb <3 ppb <3 ppb 14 ppb <30 ppb 0.43 ppb <8 ppb <4 ppb 2 ppb <0.14 ppb <1.0 ppb t,aAfter aeration .1 ^Represents seasonal variation, difference from one month to the next, will not exceed 10Z cAverage of all well water values from January-September, 1987 dTotal monthly range of organic carbon Sample dates: Trace elements * June 3, 1987, organophosphate and organochlorine analyses " M a y 28, 1987. o0020Z ABC LABS #36614-10 of.45 TABLE 2 Acute Toxicity of E2566-I to Daphnia magna BEST COPY AVAILABLE Compound E2566-1 24 hours 200 (1) (100-320) ` LC50 (sg/i) 48 hours 130 (1) (100-180)1 aBicassay conducted at 20'C (i2.0). 95I confidence limits. The 24-hour no-effect concentration was 100 rrg/1, based on the absence of all abnormal effects. The 48-hcur no-effect concentration vas estimated to be <100 mg/1 since abnormal effects vere observed in all test concentrations. All values were rounded to two significant figures following the technique provided in ABC S.O.P. #8.7. LCjq calculated using: (1)Binomial Method `iA. ' , ` 000203 A v ABC LABS #36614-11 of 45 TABLE 3 BEST COPY AVAILABLE Percent Mortality and Water Quality Measurements During the Acute Toxicity Test of E2566-1 to Daphnia magna. Nominal Concentration (m/l) Control 100 180 320 560 1000 Percent Mortality 24 hr 0 48 hr r* 00 35 100 100 100 100 100 100 100 Water Quality 0 hours 48 hours Temp.a C D.0.b mg/l eh! Temp. D.O. ec mg/l P 19 9.2 8.2 20 8.7 8.2 19 9 . : 8.2 20 8.7 8.2 1 ^ 9.2 8.2 20 8.8 8.4 19 9.2 8.2 20 8.6 8.4 aTenperature - mercury thermometer. ^Dissolved oxygen concentrations - YSI 54 ARC dissolved oxygen meter. CpH - Corning 140 pH/mV meter with Beckman 34831 electrode. NOTE: Dissolved oxygen saturations at the test temperatures of 19 and 20C are 8.9 and 8.7 mg/l, respectively (corrected for altitudinal pressure at ABC Labs). 000204 ABC LABS #36614-1? of AS LITERATURE CITED (1) Committee on Methods for Toxicity Tests with Aquatic Organisms. Methods of Acute Toxicity Tests with Fish, Macroinvertebrates and Amphibians. 1975. U.S. EPA, Ecol. Res. Ser. 660/3-75-009. (2) American Public Health Association. 1980. Standard Methods for the Examination of Water and Wastewater. 15th ed. Washington, DC. 1134 p. (3) Pennak, R. W. 1978. Freshwater Invertebrates of the United States. John Wiley & Sons, New York, 2nd ed. 803 p. (4) Stephan, C. E., K. A. Busch, R. Smith, J. Burke and R. K. Andrews. 1978. A Computer Program for Calculating an LC^q . U. S. Environ mental Protection Agency, Duluth, Minnesota, pre-publication manuscript, August, 1978. (5) Stephan, C. 1977. Methods for Calculating an L C ^ , p. 65-84. In F. L. Mayer and J. L. Hamelink (eds.). Aquatic' Toxicology and Hazard Evaluation. ASTM Special Technical Publication 634. ASTM. Philadelphia. (6) Organization for Economic Cooperation ar.d Eevelopaent. 1981. OECD Guidelines for Testing of Chemicals, Principles of Good Laboratory Practice Annex 2, C(81) 3CvFinal):7-28. QUALITY ASSURANCE STATEMENT Quality Assurance Statement for report 36614 entitled, "Acute Toxicity of E2566-1 to Daphnla magna>" for Hr. Mohansed Elnabaravy, 3M Company, St. Paul, Minnesota. In accordance with ABC Laboratories' intent that all studies con ducted at our facilities are designed and function in conformance with good laboratory practice regulations and the protocols for individual laboratory studies, an inspection of the final report for E2566-1 was conducted and found to be in an acceptable form by a member of our Quality Assurance Unit. A procedure audit was conducted on December 14, 1987. Results were reported to the study director on the same day and to management on December 30, 1987. A final inspection of all data and records on January 13, 1988, indicated that the report submitted to you is an accurate reflection of the study as it was conducted by ABC Laboratories. Should you have any questions relating :c the information provided in this statement or the function of our Quality Assurance Unit, please contact the Quality Assurance Unit at your convenience. Ik iiL illih Kenatt Ediger / Quality Assurance Officer YAVAILABLE ooo^os !Vi' " A ,r, ' ' A' T * . ,, 4 ^ -A- r? ABC LABS #36614-14 of 45 4- nw STUDY COMPLIANCE STATEMENT Study Compliance Statement for ABC report #36614 entitled, "Acute Toxicity of E2566-1 to Daphnla nagna," for Mr. Mohaued Elnabaravy, 3M Company, St. Paul, Minnesota. In accordance with ABC Laboratories' intent that all aquatic toxicity tests conducted by our facility follow good laboratory prac tices, ABC's study director for the above test herein confirms that the study was conducted in compliance with the OECD Guidelines for Testing of Chemicals, Principles of Good Laboratory Practice Annex 2, C(81) 30(Final):7-28. All original raw data were provided to 3M Company, and a copy retained at Analytical Bio-Chemistrv Laboratories. Scott Frazier ,} ABC Studv Director ^ i >; Date Vh ' v I ' ,' -- ,*-, - v, it * ' i1f ," , v y v- , * 1 / & 1;i ** AV -* y\ . V 1 1 ,? ' ' f"r VS vUiS vy. * 'ft'A ABC LABS #36614-15 of 45