Document DMK32LJbxzNZa9bdR3gjmdOnd

ACUTE TOXICITY TO FISH TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfbnatweh,ich may alsobe referredtoas PFOS, FC-95, oras a component ofFC-203S. (1Octanesulfoniaccid)(CAS # 2795-39-3). Remarks: The 3M productlotnumber was 3086.The testsample isFC203S (F2132-1).Currentinformatioinndicatesitisa mixtureof 1.34% PFOS, 35% diethyleneglycolbutylether,37.85% water,2.66% Sultonefoamer, 3% sodium octylsulfate0,.10% sodium laurylsulfatea,nd 0.05% towazole.. The followingsummary appliesto a mixture wi@itihncompletely characterizedconcentrations of impurities.Data may not accurately reflectthe toxicityof the fluorochemical component of the testsample. METHOD: Method: U.S. EPA Type: Acute flow-through GLP: No Year completed: 1988 Species: Salmo gaifdnefi Supplier:hk.Lassen TroutFarm, Red BluffC,alifornia. Analyticalmonitoring:Temperature,pH, and DO Exposure period:96-hours Statisticamlethods: LC50valuescalculateudsingtheStephan etal. computer program,'1978. Test fishage: Juvenile's Length and weight: Loading: 0.57 g fish/L Average length 39 mm Average weight 0.86 g (wet) Pretreatment: Unknown Test conditions: Dilutionwater. Blended waterwhich isa mixtureofreverseosmosis and ABC wellwater. Dilutionwater chemistry: Hardness: Alkalinity: 40 -48 mg/L as CaC03 44 - 56 rng/Las CaC03 Lighting: A dailyphotopedod of 16 hours lightand 8 hours dark was maintainedthroughoutthe testingperiod. Stock and testsolubon preparation: The primarystocksolutionof 160,000 mg/L was prepared by dissolving160 g oftestmaterialin1 L ofdeionized water. Test solutionswere intermiftenbiyntroducedtothe testvesselsviaa proportionadlilutesrystem witha flowrateof 1 L oftestsolutionatan average rateof8 timesper hour. Flow-through rate:Appro)dmately6.4times per day. Stabilityof the testchemical solutions: Not noted Exposure vessels: Aquaria containing30 L oftestsolution Number of replicates:1 Number of fishper replicate:20 Number of concentrations: fiveplusa blankcontrol Water chemistry during the study: pH range (0-96hours): 7.4- 7.8 (controelxposure) 7.4- 7.8 (400 nig/Lexposure) Temperature range (0-96hours): 13 - 13 *C (controelxposure) 12 - 13 "C (400 MVIL exposure) Dissolved oxygen range (0-96hours): 7.7- 8.9mg/L (controelxposure) 7.2- 9.0 mg/L (400 rng/Lexposure) RESULTS Nominal concentrations: Bk control,25, 50, 100,200, and 400 nig/L Element values: 96-hour LC5o = >400 ffig/L 96-hour NOEC = 400 nig/L Element values based on nominal concentrations Remarks: Testingwas conducted on a mixtureas described intheTest Substance Remarks field.The values reportedapplytothatmixtureand not the fluorochemicalproportionalone. The testinglaboratorywas unableto conduct the studyatconcentrations greaterthan 400 mg/L due toinsufficiesnatmple size. CONCLUSIONS The testsample 96-hour LC50 forrainbow troutwas determined to be >400 mg/L. Submitter: 3M Company, Environmental Laboratory,P.O. Box 33331, St. Paul,Minnesota,55133 DATA QUALITY ReliabilityK:Jimischranking2. Testingmeets the criterifaorqualitytesting. However, sample puritywas not properlycharacterizedand the studylacks analyticaclonfimiatioonftheamount offluorocherricparloportioinnthe solution.The firsftivepages ofthefinalreportare missing. REFERENCES Test was conducted by ABC Labs,ofColumbia, MO atthe requestofthe 3M Company, 1988. OTHER Last changed: 6/28100 Internal Correspondence/3M cc: K. W. Livermore - 236-2A-01 M. T. Pike - 236-3A-01 D. P. Neuman - 236-2A-01 M. T. Elnabarawy - 21-2W-05 TO: FROM: SUBJECT: DATE: D. R. RICKER - 236-IB-10 E. A. REINER - ENVIRONMENTAL im DECEMBER 28, 1988 LAB/EE & PC 21-2W-05 In response to your request, a salmon fry bioassay was conducted on FC-203S Lot 3086. The results of this bioassay are attached. The highest concentration tested was 400 mg/l and there were no adverse effects at this concentration. According to ABC Labs, this was the highest concentration that could be tested with the amount of sample provided. Hopefully, these results are adequate to meet your needs. If you have any questions or concerns, please feel free to contact me on 778-5079. EAR/mb Attachment: Bioassay Results on FC-203S SUMMARY A 96-hour acute flow-through toxicity study of,4@.FC--'203,1-torainbow trout (Salmo gairdneri) was conducted for 3M Company from October 14, 1988 to October 18, 1988. Twenty fish per test concentration plus control were used in a nominal dosing regime of 25, 50, 100, 200, and 400 mg/l. Water chemistry measurements of dissolved oxygen, pH and temperature were consistent throughout the term of the experiment and were within the protocol specifications. From the data collected during this study, a 96-hour LC with 95% confidence limits was calculated to be >400 mg/l based on t'hoenominal concentrations of FC-203. Neither mortality nor sublethal/behavioral effects occurred at any exposure concentration or control. As determined by this study, a 96-hour no-effect concentration of FC-203 toxicity to rainbow trout was 400 mg/l based on a lack of mortality or abnormal responses. #37242-6 INTRODUCTION 3M Company contracted the Aquatic Toxicology Division of Analytical Bio-Chemistry Laboratories, Inc., to conduct a five concentrationplus control flow-throughtoxicity test to determine the toxicity of FC-203 to rainbow trout (Salmo gairdneri). The primary objectiveof this study was to estimate the acute toxicity of FC-203 to rainbow trout by de- termining the median lethal concentration (LC if possible, and examining sublethal/behavioralresponses during &oe course of the test. This was accomplished by exposing 20 rainbow trout per concentration and control and monitoring survival and sublethal/behavioral responses over a 96 hour exposure duration. The term LC , as used in this report, is that concentrationof FC-203 causing ;@i mortality after a specified exposure period. The study was conducted from October 14, 1988 to October 18, 1988 following ABC Protocol Number 8007 (APPENDIX) as approved by MohA-ed Elnabarawy. This report presents the results of the toxicity study and describes the technical approach used to meet the project objectives. METHODS AND MATERIALS The biological methods, as well as the recommended statistical analyses, used in this study were those described by the U. S. Environmental ProtectionAgency (1). I. Test Fish The 120 rainbow trout (Salmo gairdneri) (lot #3788) used in this study were obtained from Mt. Lassen Trout Farm in Red Bluff, California. The fish were reared and maintained at ABC Laboratories in ABC soft blended water and were fed newly hatched b.rineshrimp or a commercially available fish food daily. The laboratory environment was maintained on a 16-hour daylight photoperiod. Fish culture techniques were basically those describedby Brauhn et al. (2). A daily record of fish observations during the holding period, along with prophylac- tic and therapeutic disease treatments, is included in Appendix I. Seventy-twohours before the initiationof the test, fish were removed from the culture tank and placed in the temperature acclimation unit. During this time, the fish were held without food. At test initiation,rainbow trout were randomly placed in the testing unit. The rainbow trout used as the control group during this study had a mean weight of 0.86 (0.26)g and a mean standard length of 39 (4.2) mm when measured at the end of the test. The biomass loading rate was 0.57 g/l. These measurements are provided in Appendix I. II. Test System A proportional diluter system described by Mount and Brungs (3) and a Hamilton Model 420 syringe dispenser was used ABC LABS #37242-7 for the intermittent introduction of FC-203 test solutions and diluent water into each test chamber. Five concentrations of the test material and control comprised the test design. Each concentration and control held twenty fish. Chemical characteristics, typical of ABC soft blended water, are provided in Table 1. The diluter delivered one liter of test solution or control water to the test vessels at an average rate of 8.0 times per hour over the course of the study. This flow rate was sufficient to replace the 30 liter volume within the test chambers 6.4 times per day. The test aquaria were immersed in a circulating water bath that was thermostatically held at 12 10C. III. Test Material The FC-203 (F 2132-1) (Lot No. 3086) was received from 3M on September 8, 1988 in good condition. The sample was observed to be an amber liquid and was stored at room temperature. A diluter stock solution (160,000 mg/1) was prepared by dissolving 160 g of FC-203 in 1.0 liter of deionized water. The injector volume was adjusted to deliver 5.0 ml of stock to two liters of dilution water. The resulting nominal concentration regime of FC-203 was 25, 50, 100, 200, and 400 mg/l. IV. Test Procedure - Biological A preliminary static 96-hour range-finding test was conducted to determine a concentration range of FC-203 to use in the definitive test. This preliminary test was conducted from September 15, 1988 to September 19, 1988 using 1.0, 10, and 100 mg/l exposure concentrations. During this test, neither mortality nor abnormal effects were observed at any level. These results were discussed with the sponsor's representative and it was agreed that the definitive flowthrough test would be run at a nominal high concentration of 400 mg/l of FC-203. The definitive test was initiated after the test solutions had been flowing through the aquaria for approximately 48 hours. Twenty rainbow trout were impartially distributed to each test container. Observations for mortality and sublethal responses were made once every 24 hours during the 96 hour test period. V. Test Procedure - Chemical and Physical Temperature (*C), dissolved oxygen (mg/1), and pH were measured in the control, low, middle and highest concentration containing surviving fish at 0, 48 and 96 hours of testing. These results are provided in Appendix I of this report. ABC LABS #37242-8 Vi. RESULTS Statistical Analyses The results of the definitive study were statistically analyzed (4) for 24, 48, 72 and 96-hour LC values and their corresponding 95% confidence limits. 50 All calculations were performed on an IBM PC-XT computer using the nominal concen- trations of FC-203. Because no mortality occurred, neither an LC 50 or 95% confidence limits were determined. Water chemistry parameters measured at 0, 48 and 96 hours were within the specified limits for conducting aquatic toxicity tests (1). Dissolved oxygen ranged from 7.2 to 9.0 mg/l, and pH ranged from 7.3 to 7.8 (Table 2). Percent water saturation of dissolved oxygen given the above measurements ranged from 70% to 89% at temperatures of 12 and 13*C, respectively. From the data collected during this flow-through study, the 24-, 48-, 72- and 96-hour LC values were estimated to be >400 mg/l (Table .3). As shown in Table 0 no mortality or abnormal effects were seen at any exposure level or control. For this reason, the no effect concentration for the acute toxicity of FC-203 to rainbow trout was 400 mg/l, the maximum concentration tested. The study was conducted following the intent of the Good Laboratory Practice Regulations (5) and the preliminary report was reviewed by Analytical Bio-Chemistry Laboratories' Quality Assurance Unit. All original raw data will be provided to 3M Company with the final report, with a copy retained at Analytical Bio-Chemistry Laboratories. ABC LABS 137242-9 TABLE 1 Chemical Characteristics of Soft Blended Waler Used by ABC's Aquatic Toxicology Division Parameter Temperature Dissolved Oxygen b PH Hardness (CACO3) Alkalinity (CACO 3 Conductivity Suspended Solids Aluminum Arsenic Boron Cadmium Chromium Cobalt Copper Iron Lead Mercury Nickel Silver Zinc Concentration 18 - 230C 8.0 - 9.3 mg/l 7.1 - 7.9 40 - 48 mg/l 44 - 56 mg/l 100 - 160 umhos/cm 0 - 1.4 mg/l <0.2 mg/l <0.001 mg/l 0.181 mg/l <0.005 mg/l <0.010 mg/l 0.169 mg/l <0.025 mg/l 0.127 mg/l <0.003 mg/l <0.0004 mg/l 0.048 mg/l <0.001 mg/l <0.020 mg/l a Blended water is a mixture of reverse osmosis (R.O.) and ABC well water to achieve a final hardness of between 40 - 48 mg/l. b After aeration Note: The ranges of these selected parameters are from the time period April through June, 1988 or from the most recent quarterly screen for contaminants. All raw data supporting these ranges are on file at ABC Laboratories. ABC LABS #37242-10 TABLE 2 Water Quality Measurements During the Acute Flow-Through Toxicity Test of FC-203 to Rainbow Trout (Salmo gairdneri) Nominal Concentration (mg/1) Control 25 50 100 200 400 Temp. oc 13 13 0-hour Water Quality 48-hour 96@-hour a D.O. Temp. D.O. b Temp. D.O. mg/l pH: OC mg/l pIL OC mg/l pH 8.5 7.7 13 7.7 7.8 13 8.9 7.4 8.6 7.7 13 7.7 7.7 13 9.0 7.4 13 9.0 7.7 13 7.9 7.7 13 8.9 7.3 13 9.0 7.8 12 7.2 7.8 13 8.6 7.4 adissolved oxygen concentrations - Dissolved Oxygen Probe (YSI Model 54). b PH - pH Probe (Corning Model 476182) used with a Corning Model 125 pH and mV meter. NOTE: Altitude-adjusted dissolved oxygen saturation at the test temperatures of 12 and 13*C is 10.3 and 10.1 mg/l, respectively. ABC LABS #37242-11 TABLE 3 The Estimated LC52YValues with 95% Confidence Limits for the 96-Hour Toxicity Stu of FC-203 to Rainbow Trout (.Salmogairdneri) Period of Exposure, Hours 24. 48, 72, 96 LC 50 >400 a (M 1) 95% Confidence Limits aNo mortality occurred at any exposure concentration; therefore, the LC 50 was considered greater than the maximum exposure concentration. No confidence limits could be determined. ABC LABS #37242-12 TABLE 4 Mortality and Behavioral Observations During the Acute Flow-Though Toxicity Test of FC-203 to Rainbow Trout (Salmo gairdneri) Nominal Test Concentration mg/l (ppm) No. Placed in test 24-Hours 48-Hours 72-Houre 96 Cumm. Cumm. Cumm. Mort. Observations Mort. ObservationsMort. Observations Mort. Control 20 0 20 N 0 20 N 0 20 N 0 25 20 0 20 N 0 20 N 0 20 N 0 50 20 0 20 N 0 20 N 0 20 N 0 100 20 0 20 N 0 20 N 0 20 N 0 200 20 0 20 N 0 20 N 0 20 N 0 400 20 0 20 N 0 20 N 0 20 N 0 0 Key to Observations: N Normal @j LITERATURE CITED (1) Committee on Methods for Toxicity Tests with Aquatic Organisms (C. E. Stephan, Chairman). 1975. Methods for Acute Toxicity Tests with Fish, Macroinvertebratea and Amphibians. Environmental Protection Agency, Ecological Research Series EPA-660/3-75-009, April 1975, 61 p. (2) Brauhn, J. L. and R. A. Schoettger. 1975. Acquisition and Culture of Research Fish: Rainbow Trout, Fathead Minnows, Channel Catfish and Bluegills. Environmental Protection Agency, Ecological Research Series EPA-660/3-75-011, May, 1975. 45 p. (3) Mount, D. I. and W. A. Brungs. 1967. A Simplified Dosing Apparatus for Fish Toxicological Studies. Water Res. 1:21-29. (4) Stephan, C. E., K. A. Busch, R. Smith, J. Burke and R. W. Andrew. 1978. A computer program for calculating an LC . U. S. Environ- mental Protection Agency, Duluth, 50 Minnesota, pre-publication manuscript, August, 1978. (5) Organization for Economic Cooperation and Development. 1981. OECD Guidelines for Testing of Chemicals, Principles of Good Laboratory Practice Annex 2, C(81) 30(Final):7-28. ABC LABS #37242-14 QUALITY ASSURANCE STATDMM Quality Assurance Statement for preliminary report #37242 entitled, "Acute Flow-Through Toxicity of FC-203 to Rainbow Trout (Salmo gairdneri)", for Mo Elnabarawy, 3M Company, St. Paul Minnesota. In accordance with ABC Laboratories' intent that all studies conducted at our facilities are designed and function in compliance with good laboratory practice regulations and the protocols for individual laboratory studies, an inspection of the report for FC-203 was conducted and found to be in an acceptable form by a member of our Quality Assurance Unit. An inspection of the daily mortality rate of the test organisms prior to the initiation of the study indicated they were in good health and should not bias the observed mortality in the study. A procedure audit was conducted on October 12, 1988 with results-reported to the study director on the sa- day. Audit findings were reported to ABC Laboratories' management on November 1, 1988. A final inspection of all data and records on November 14, 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 to the information provided in this statement or the function of our Quality Assurance Unit, please contact the Quality Assurance Unit at your convenience. Lowell G. Sensintaffae/ Quality Assurance Officer Date ABC LABS #37242-15 STUDY COMPLIANCE STATEMENT Study Compliance Statement for ABC report #37242 entitled, "Acute FlowThrough Toxicity of FC-203 to Rainbow Trout Salmo gairdneri)", for Mo Elnabarawy, 3M Company, St. Paul, Minnesota. In accordance with ABC Laboratories' intent that all aquatic toxicity tests conducted by our facility follow good laboratory practices, ABC's study director for the above test herein confirms that the study was conducted in compliance with Principles of Good Laboratory Practice Annex 2, C(81). All original raw data will be provided to 3M Company, with a copy retained at Analytical Bio-Chemistry Laboratories. Bowman dy Director Date ABC LABS 137242-16