Document 44xwrGEadZLpzjLNDnYp7p6yG

M 236 - O 77#- ACUTE TOXICITY TO FISH (FATHEAD MINNOW) TEST SUBSTANCE___________________________________________ _ Identity: Mixture containing perfluorooctanesulfonate which may also be referred to as PFOS, FC-95, or as a component of FC-203FC. (1Octanesulfonic acid) (CAS # 2795-39-3). Remarks: The 3M production lot number was not noted. The test sample is FC-203FC, identified by the laboratory as R1335. Current information indicates it is a mixture of 0.85% PFOS, 17% diethylene glycol butyl ether, 74.46% water, 2.34% acrylic foamer, 1.7% alkyl ether sulfate, 2.55% sodium octyl sulfate, 0.12% sodium nitrite, 0.09% sodium molybdate, 0.85% triethanolamine, and 0.04% tolyltriazole. The following summary applies to a mixture with incompletely characterized concentrations of impurities. Data may not accurately reflect toxicity of the fluorochemical component of the test sample. MET HOD;_______________________________________________________ Method: OECD Guideline 203. Type: Acute static GLP: No Year completed: 1997 Species: Pimephales promelas Supplier: In-house cultures, maintained at AScl-DETD, Duluth, MN. Analytical monitoring: Temperature, pH, conductivity, and dissolved oxygen. Exposure period: 96-hours Statistical methods: The LC50 values were calculated by Trimmed Spearman-Karber method. The NOEC values were calculated by Fisher's Exact test using Toxstat statistical software, Version 3.5. Test fish age: Juveniles Length and weight: Average length = 16.6 mm Average weight = 0.036 g (wet) Loading: 0.12 g/L Pretreatment: None Test conditions: Dilution water: Dechlorinated City of Duluth, MN tap water, post- carbon filter. The water was aerated for 24 hours prior to the test. Dilution water chemistry: Hardness: 48 mg/L as C a C 0 3 Alkalinity: 44 mg/L as C a C 0 3 Conductivity: 119 pmhos/cm pH: 8.08 001383 Lighting: Cool-white fluorescent lights. A daily photoperiod of 16 hours light and 8 hours dark was maintained throughout the testing period. Stock and test solution preparation: The test material was added directly to the dilution water on a weight/volume basis. Concentrations dosing rate: Once. Stability of the test chemical solutions: Not noted. Exposure vessels: 4 L glass jars containing 3 L test solutions. Number of replicates: 2 Number of fish per replicate: 10. Number of concentrations: five plus a blank control Water chemistry during the study: pH range (0-96 hours): 7.68 - 8.08 (control exposure) 7.45 - 7.81 (1000 mg/L exposure) Temperature range (0-96 hours): 2 0 .5 -2 0 .7 C Conductivity range (0-96 hours): 119 - 141 pmhos/cm (control exposure) 1 1 9 - 1 4 3 pmhos/cm (1000 mg/L exposure) Dissolved oxygen range (0-96 hours): 6.9 - 8.7 mg/L (control exposure) 5.1 - 8.7 mg/L (1000 mg/L exposure) RESULTS__________________________________________________ :______ Nominal concentrations: Blank control, 130, 216, 360, 600, and 1000 mg/L Element values: 96-hour LC50 = >1000 mg/L 96-hour NOEC = 600 mg/L Element values based on nominal concentrations Remarks: Testing was conducted on the mixture as described in the Test Substance Remarks field. The values reported apply to that mixture and not the fluorochemical proportion alone. CONCLUSIONS___________________________________________________ The FC-203FC 96-hour LC50 for fathead minnow was determined to be >1000 mg/L. The 96-hour No Observed Effect Concentration (NOEC) was 600 mg/L. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St, Paul, Minnesota, 55133 DATA QUALITY______________________;_____________________________ Reliability: Klimisch ranking = 2. The study meets all the criteria for quality testing. However, sample purity was not properly characterized and the study 001384 lacks analytical confirmation of the amount of fluorochemical proportion in the solution. REFERENCES____________________________________________________ This test was conducted by AScI Corporation, Duluth Environmental Testing Division, Duluth, MN at the request of the 3M Company, Lab Request number R1335, 1997. OTHER____________________________________________________________ Last changed: 6/26/00 001385 AScI Corporation/AScI-Duluth Environmental Testing Division AScI Study ID# 5010-068 STUDY TITLE ACUTE TOXICITY OF R1335 TO FATHEAD MINNOW (Pimephales promelas) DATA STANDARD OECD GUIDELINE 203 STUDY COMPLETED June 26, 1997 TESTING FACILITY AScI Corporation/AScI-DuIuth Environmental Testing Division 4444 Airpark Boulevard Duluth, MN 55811 Tel. No. (218) 722-4040 Fax No. (218) 722-2592 STUDY IDENTIFICATION NUMBERS AScI Study ID# 5010-068 3M Company Lab Request# R1335 nr 0 nv- Sponsor. 3M Company Sponsor Study ID# R1335 1 4V 001386 AScl Corporation/AScI-Duluth Environmental Testing Division AScl Study ID# 5010-068 1.0 GENERAL INFORMATION ! Study Title Data Standard Sponsor Sponsor's Representative Sponsor's Lab Request# Testing Facility Principal Investigator Project Director Testing Facility Director Definitive Test Dates Data Validation and Report Review Acute Toxicity of R1335 to Fathead Minnow 1 (Pimephales promelas). | OECD Guideline 203. | 3M Environmental Technology and Safety Services, Building 2-3E-09, 935 Bush Avenue, St. Paul, MN 55133; Tel No. (612) 778-7452. Susan Beach, 3M Environmental Technology and Safety Services, Building 2-3E-09, 935 Bush Avenue, St. Paul, MN 55133; Tel No. (612) 778-7452. R1335. AScl Corporation/AScI-Duluth Environmental Testing Division, 4444 Airpark Boulevard, K Duluth, MN 55811; Tel. No. (218) 722-4040. | Joe Dierkes | Joe Amato | Donald Mount | June 17-21, 1997. | Alan Mozol Report Signature: ~ 1 1 Retention of Raw Data and Final Report Location of Raw Data and Final Report Two years from the date study is completed.^ AScl Corporation/AScI-Duluth Environmental Testing Division, 4444 Airpark Boulevard, Duluth, MN 55811; Tel. No. (218) 722-4040. Sponsor: 3M Company Sponsor Study ID# R1335 2 001387 2.0 OBJECTIVE(S) AScl Corporation/AScI-Duluth Environmental Testing Division AScl Study ID 50LW)68 .isf.n- To determine the 96-hour 10% and 50% effect concentrations (LC10 and LC50), and the 96-hour no observable effect concentration (NOEC) of the test substance, R1335, for fathead minnow (Pimephales promelas) under static test conditions. This study was conducted according to the AScl study plan retained by the Sponsor and OECD Guideline 203 (OECD 1993). 3.0 TEST METHODS I Test Substance Properties'. R1335, orange-yellow liquid, specific gravity = 1.1 (water y; = 1), stable and miscible with water. Test Organisms Test concentrations: 0 (dilution water control), 130, 216, 360, 600, and]: 1000 mg/L. Test solutions prepared by mass addition of test substance to, 6-L aliquots of dilution water followed by vigorous stirring. Source: Healthy, juvenile fathead minnows {Pimephales promelas) obtained from AScI-DETD in-house culture. Dilution Water Holding/acclimation: The fish used in the tests were obtained from AScI's fl in-house culture. The fish used in the study were hatched between May 17 1 and 23, 1997. For the 48 hours preceeding test initiation mortality was | 0%, and the fish were not fed for 24 hours before test initiation. The fish | mean length was 16.6 2.5 mm, and mean wet weight was 36 19 mg. Loading rate was calculated to be 120 mg of fish per L test solution. 'i Use in test: Used 10 organisms/replicate and 2 replicates/test concentration. i) Source: Dechlorinated City of Duluth, MN, tap water. The most recent chemical analysis is in Raw Data Package. 9. Characteristics: At test time, the water had a hardness of 48 mg/L (as CaC03) and a pH of 8.08. Aerated for 24 h prior to use in the test. .--L. n Sponsor. 3M Company Sponsor Study ID# R1335 3 00M 88 Exposure Chambers Incubation Observations Endpoint Calculations AScI Corporation/AScI-Duluth Environmental Testing Division AScI Study ID# 50-068 Type: 4-L glass jars. V ,. Use in test: 3.0 L of dilution water or test solution/chamber. During the test, kept covered, except when experimental observations were made. ' Solutions were not aerated during the exposures. 11 Duration: 96 hours. Daily photoperiod: 16 h light and 8 h dark, maintained using cool white fluorescent lamps. Temperature: 21.0 1C. i-p Biological: Daily- Test organisms with abnormal behavior and signs o % stress, and dead test organisms. i Water chemistry: (1) At test initiation- total hardness and alkalinity, (2) ,, daily- temperature, DO, conductivity, and pH. All determinations were made according to APHA methods (1995). L C i q . Inhibition Concentration (ICp) Method. i LCS0's: Trimmed Spearman-Karber Method. NOEC: Fisher's Exact Test (TOXSTAT statistical software, Version 3.5, 1 West Inc., and University of Wyoming). | J\s Sponior 3M Company Sponsor Study ID# R1335 4 ' f* o o ijss 3.0 RESULTS AScI Coiporation/AScI-Duluth Environmental Testing Division AScI Study ID# 5010-068 Test Substance Toxicity (Pertinent data are in Table 1) | Ranges of Water Chemistry Parameters 24-h LCS0: > 1000 mg/L (Not Calculable). 48-h LCS0: > 1000 mg/L (Not Calculable). 72-h LC50: > 1000 mg/L (Not Calculable). 96-h LCi0: 116 mg/L (Not Reliable). 96-h LCS0: > 1000 mg/L (Not Calculable). 96-h NOEC: 600 mg/L. 't . Total hardness (as CaC03 mg/L): 46-48. 1 Alkalinity (as CaCO3 mg/L): 44-48. Temperature (C): 20.5-20.7. DO (mg/L): 5.1-8.8. pH: 7.45-8.08. Specific conductivity (umhos/cm): 119-143. `Iv Sponsor: 3M Company Sponsor Study ID# R1335 5 00190 4.0 TEST QA/QC AScI Corporation/AScI-Duluth Environmental Terng Division AScI Study ID# 5010-068 QA/QC Criteria Data Mortality in control exposure must not be more 0 % mortality. than 10%. The lowest DO concentration at test termination must be at least 60% of the air saturation value at test temperature. The lowest DO concentration measured was 57% of the air saturation value at 21.0C. 1 This value was measured at test termination 1 for the 1000_mg/L concentration. This sole I value was below 60% saturation. DO | depression did not appear to significantly affgct | the toxicity measurement for R1335. -> | Test duration must be 96 h. The test duration was 96 h. Reference Substance Toxicity Test (this test is Control chart for sodium chloride reference optional). toxicity testing is in Raw Data Package. 5.0 REFERENCES American Public Health Association (APHA). 1995. Standard Methods for the Examination of Water and Wastewater. APHA, Washington, D.C. Organization for Economic Cooperation and Development (OECD). 1981/1993. OECD Guidelines for Testing of Chemicals. OECD Publication Information Center, Washington, D.Cg* Hamilton, M.A., R.C. Russo, and R.V. Thurston. 1977. Trimmed Spearman-Karber Method fbr Estimating Median Lethal Concentrations in Toxicity Bioassays. Environ. Sci. Technol. 11(7).: 714-719; Correction 12 (4): 417 (1978). USEPA. 1993. A Linear Inteipolation Method for Sublethal Toxicity: The Inhibition Concentration (ICp) Approach. Version 2.0. West Inc., and University of Wyoming. Toxstat Software Package. Version 3.5. Cheyenne, Wyoming. ______ ________________________ Sponsor: 3M Company Sponsor Study ID# R1335 6 001391 AScl Corporation/AScI-Duluth Environmental Testing Division AScl Study ID# 5010-068 TABLE 1. ACUTE TOXICITY OF R1335 TO FATHEAD MINNOWS (P. promelas) 0 (control) 130 1 216 1 360 1 600 1 1000 * Percentages are in parenthesis. Cumulative Number o f Cfcad Organisms and Peroeptifortalityt 24 h 0(0) 48 b 0(0) 72 b 0(0) 96 b V | I0 (0 ) 0(0) 0(0) 0(0) 0(0) 0(0) 0(0) 0(0) 3 (15) I I0 ( 0 ) 2 <10> U 0(0) 2 (10) - I 0(0) 1(5) 1 (5) 2 do) : I 3(15) 5(25) 5(25) 5 (25) D.- I LETHAL AND NO-EFFECT CONCENTRATIONS WITH CORRESPONDING 95% CONFIDENCE INTERVALS 1 LC*a and N0C I 24-h LCJ0 B 48-h LCjo I 72-h LC50 1 96-H LC]0 H 96-h LC50 1 96-h NOEC Values based on nominal test concentrations. Data (mg/L)* >1000 >1000 >1000 116 >1000 600 95% Confidence Interval*-- Not calculable Not calculable _ Not calculable Not tebable Not calculable Not applicable T ty I | | || | | II | Sponsor: 3M Company Sponsor Study ID# R1335 7 o o ia