Document V3D6Zq64G1rkNxKbRyOkV7vDo

AR50&-O3H0. ACTIVATED SLUDGE RESPIRATION INHIBITION TEST TEST SUBSTANCE_________________________ Identity: N-Ethylperfluorooctanesulfonamide; may also be referred to as U1464, EtFOSA, EtPOSA, F-6309, or FX-12. (1Octanesulfonamide, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-N-ethyl-, CAS # 4151-50-2) Remarks: Material is a white solid. Sample purity and lot number were not recorded. METHOD Method: OECD 209 Test type: Static acute GLP: No Year Completed: 1998 Analytical monitoring: Dissolved oxygen concentrations. Test organism source: Activated sludge collected from the Western Lake Superior Sanitary district, Duluth, MN Test conditions: Dilution water: Carbon-treated dechlorinated City of Duluth, MN, tap water Synthetic Sewage: 1 liter Dl water 16.0 g Bacto. peptone 11.0 g Beef extract 3.0 g urea 0.7 g NaCI 0 .4 g C a C I2-2H2O 0.2 g MgS04'7H20 2.8 g K2HP04 Reference and test solution preparation: A 500 mg/L stock solution of the reference substance 3,5-dichlorophenol was prepared using Millipore water. Concentrations tested were 4,16, and 32 mg/L, prepared by diluting the stock solution with Millipore water. EtFOSA was added directly to test vessels rather than by volumetric addition of a stock solution. Test vessels: Mixtures were prepared (500 mL final volume) and aerated in 1000 mL borosilicate glass beakers and then transferred 006077 into 300 mL Biochemical Oxygen Demand (BOD) bottles to obtain oxygen uptake rates. Number of concentrations: One, in duplicate plus three reference substance concentrations and two Blank controls Temperature: 20.1-21.8C Total Suspended Solids of sludge on day of testing: 6.5 g/L (TSS in test solutions = 3.3 g/L). Sludge was used one day after collection. Element Basis: Respiration inhibition as determined by dissolved oxygen concentration. Test mixtures were prepared at 7-minute intervals and aerated. After 30-minutes and 3-hours of contact time, dissolved oxygen was measured every 0.5 minutes for up to 5.5 minutes. RESULTS_______________________________________________ Nominal concentrations: Two blank controls, three reference substance concentrations, 1000mg/L (in duplicate) test material solutions Statistical Analyses: EC50values were calculated for the reference material by the Trimmed Spearman-Karber Method. An EC50 value could not be calculated for the test substance. Analytical Methodology: Analysis of DO concentrations in all test solutions were performed at AScI Corporation using a YSI Model 54A dissolved oxygen meter. Dissolved oxygen readings were recorded every 30 seconds for 5.5 minutes. Respiration rates were normalized for 20C prior to calculating percent inhibition. Respiration Rates and Percent Inhibitions after 3-Hours Exposure Treatment Control 1 Control 2 Test substance Test substance 1000 mg/L 1000 mg/L (duplicate) Respiration Rate mg 0 2/L/min. (@ 20C) 0.2714 0.3134 0.3981 0.4081 Percent Inhibition NA NA -36 -40 Control response: satisfactory; difference between controls ranged from 6.8% at 30-minutes to 14.4% after 3-hours of exposure. 006078 Reference Substance: 3-hr EC50 = 18.4 mg/L indicating the sludge had normal sensitivity. CONCLUSIONS___________________________________________ The test substance exhibited a no inhibitory effect on respiration at a nominal test substance concentration of 1000 mg/L after 3-hours of exposure. The EC50 (respiration inhibition) is therefore greater than 1000 mg/L. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY_________________________________ Reliability: Klimisch ranking 2. This study, while well conducted using the methodology acceptable at the time, lacks analytical data for determination of the test substance concentration in the test solutions and determination of the sample purity. Testing was also done well above the solubility limit of the test substance REFERENCES_______________________________________________ This study was conducted at AScI Corporation of Duluth, Minnesota at the request of the 3M Company. OTHER___________________________________________ Last changed: 5/18/00 006079 AScI Corporation/AScl-Duluth Environmental Testing Division Submitted to 3M Co. - 5/98 AScI Study ID# 5010-068 STUDY TITLE INHIBITION OF U1464 FOR ACTIVATED SLUDGE RESPIRATION DATA STANDARD OECD GUIDELINE 209 STUDY COMPLETED MAY 15, 1998 TESTING FACILITY AScI Corporation/AScI-Duluth Environmental Testing Division 4444 Airpark Boulevard Duluth, MN 55811 Tel. No. (218) 722-4040 PROJECT IDENTIFICATION NUMBERS AScI Study ID# 5010-068 3M Company Lab Request# U1464 Sponsor: 3M Company Sponsor-Study ID# U1464 1 006080 AScI Corporation/AScI-Duluth Environmental Testing Division Submitted to 3M Co. - 5/98 AScI 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 Date Data Validation and Report Review Inhibition of U1464 For Activated Sludge Respiration. OECD Guideline 209.. 3M Environmental Technology and Safety Services, Building 2-3E-09, 935 Bush Avenue, St. Paul, MN 55133; Tel No. (612) 778-7452. Rochelle R. Robideau, 3M Environmental Technology and Safety Services, Building 2-3E-09, 935 Bush Avenue, St. Paul, MN 55133; Tel No. (612) 778-7065. U1464. AScI Corporation/AScI-Duluth Environmental Testing Division, 4444 Airpark Boulevard, Duluth, MN 55811; Tel. No. (218) 722-4040. Joe Dierkes Joe Amato Donald Mount . May 1, 1998 Alan Mozol Report Signature: ^ Retention of Raw Data and Final Five years from the date study is completed. Report Location of Raw Data and Final Report AScI Corporation/AScI-Duluth Environmental Testing Division, 4444 Airpark Boulevard, Duluth, MN 55811; Tel. No. (218) 722-4040. Sponsor: 3M Company Sponsor Study ID# U1464 2 006081 AScI Corporation/AScl-Dululh Environmental Testing Division Submitted to 3M Co. - 5/98 AScI Study ID# 5010-068 2.0 OBJECTIVE To determine, if possible, the 30-minute and 3-h (contact times) EC50's of the test substance U1464 for activated sludge respiration. This study was conducted according to the AScI study plan retained by the Sponsor and OECD Guideline 209 (OECD 1993). 3.0 TEST METHODS Test Substance Properties: U1464, white crystals, specific gravity = 1.7 (water = 1), stable, and negligible solubility in water. Reference Substance Test concentrations'. 0 and 1000 mg/L prepared by direct addition. Name: 3,5-dichlorophenol, purity 97%, Aldrich Chemicals, Lot# 09615KG. Test Organisms Test concentrations: 0, 4, 16, and 32 mg/L prepared by direct addition of 500 mg/L stock solution in Millipore water. The reference test was performed concurrently with the exposure for U1464. Results and control chart appended to report. Source: Activated sludge from the Western Lake Superior Sanitary District Duluth, Minnesota collected on April 30, 1998. Synthetic Sewage Feed Activated sludge characteristics: The sludge was determined to have a total suspended solids concentration of 6.5 g/L at test time. The total suspended solids concentration in the test solutions was 3.3 g/L. The mixture was fed synthetic sewage feed and aerated at 21 C until test initiation. The sludge was used one day after collection. Composition: Chemical g dissolved/L of deionized water Bacto. peptone Beef extract Urea NaCl CaCl2.2H20 M gS04.7H20 K2H P 04 16.0 11.0 3.0 0.7 0.4 0.2 2.8 Sponsor: 3M Company Sponsor Study ID# U1464 3 006082 AScI Corporation/AScI-Duluth Environmental Testing Division Submitted to 3M Co. - 5/98 AScI Study ID# 5010-068 Dilution Water Test Setup Determination of Respiration Calculation of Respiration Rate Endpoint Calculation Source: Carbon-treated dechlorinated City of Duluth, MN, tap water. The most recent chemical analysis of post carbon (PC) water is in the Raw Data Package. Exposure vessels: 4, 1-L borosilicate glass beakers; two inoculum controls and 1 test concentration exposure in duplicate. Order o fpreparation: At 7-minute time intervals: (1) first inoculum control, (2) test exposure concentration replicates, and (3) second inoculum control. The final volume in each beaker was 500 ml. Preparation: (1) Added required amount of carbon-treated water, (2) added 16 ml of synthetic sewage feed to each beaker, and (3) in test exposures added the required amounts of the test substance, (4) and added 200 ml of the sludge, for a final test solution volume of 500 ml. Incubation and aeration: 20.1 to 21.8C and at an aeration rate of 0.5 to 1.0 liters per minute. Sequence: Same as exposures were prepared. Determination: At 30-min and 3-h contact times: (1) filled one 300ml BOD bottle with the exposure medium and continued to aerate the remaining medium, (2) using a YSI 54A oxygen meter with a self stirring probe, determined the DO concentration in the exposure medium every 0.5 minutes for up to 5.5 minutes (the first determination was made after 0.5 minutes), and (3) the sub-sample was placed back into the 1-L exposure chamber. DO meter calibration checks were made between the sets of measurements for each control or treatment. For each exposure, correlated DO depletion and time interval, and calculated the slope of the regression line as the respiration rate. ECS0: Trimmed Spearman-Karber Analysis (Hamilton, 1977). Sponsor: 3M Company Sponsor Study ID# U1464 4 006083 3.0 RESULTS Test Substance Toxicity 30-minute ECS0: > 1000 mg/L. (Pertinent data are in Table 1) 3-h ECTM: > 1000 mg/L. AScI Corporation/AScI-DuIuth Environmental Testing Division Submitted to 3M Co. - 5/98 AScl Study ID# 5010-068 4.0 TEST QA/QC QA/QC Criteria Respiration rates of two inoculum controls must not vary by more than 15%. 3-h EC50 of reference substance must be between 5-30 mg/L. Test duration must be 3 hi. Data Variations after 30-minute and 3-h contact times were 7% and 14%, respectively. 3-h EC50 was 18.4 mg/L, indicating the sludge had normal sensitivity. The test duration was 3 h. 5.0 REFERENCES Hamilton, M .A., R.C. Russo, and R.V. Thurston. 1977. Trimmed Spearman-Karber Method for Estimating Median Lethal Concentrations in Toxicity Bioassays. Environ. Sei. Technol. 11(7): 714-719; Correction 12(4):417. 1978. Organization for Economic Cooperation and Development (OECD). 1993. OECD Guidelines for Testing of Chemicals. OECD Publication Information Center, Washington, D.C. Sponsor: 3M Company Sponsor-Study ID# U1464 5 006084 TABL 1.0 OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 CALCULATION OF RESULTS Test Substance: U1464 ASoI Corporalion/ASol-Diiluth Environmental Testing Division Submitted to 3M Co. - 5/98 AScI Study ID# 5010-068 Analyst: DIERKES 30-Minute Exposure_____________________ Dissolved Oxygen Concentrations, mg/L mg/L 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 I iiii K w p BK1 8.5 8.2 7.9 7.7 7.5 7.2 6.8 6.6 6.3 5.9 5.7 1000A 8.1 7.8 7.5 7.2 6.9 6.6 6.3 6.0 5.7 5.3 5.0 1000B 8.4 8.1 7.9 7.6 7.3 7.1 6.8 6.5 6.2 5.9 5.6 ;||pTemp, C R (1) Ra (2) % 111111111 1 pp Inh. (3) 21.2 0.5648 0.5196 21.2 0.6194 0.5698 -6 21.2 0.5600 0.5152 4 BK2 8.5 8.2 7.9 7.6 7.3 7.0 6.6 6.3 6.0 5.7 5.4 % diff in controls{4): 6.8 EC50 (95% Cl): > 1 0 0 0 mo/L 21.8 0.6303 0.5562 RaCm (5): 0.5379 3-Hour Exposure mg/L 0.5 1.0 l i i i i i .... BK1 8.8 8.7 10O0 A 8.7 8.6 1000B 9.0 8.8 1.5 8.6 8.5 8.7 2.0 8.5 8.3 8.5 Dissolved Oxygen Concentrations, mg/L 2.5 3.0 3.5 4.0 4.5 5.0 5.5 liiiii 8.4 8.3 8.2 8.1 7.9 7.6 7.4 8.1 7.9 7.7 7.4 7.3 7.1 6.8 8.2 8.1 7.9 7.7 7.4 7.2 7.0 Temp, *C 20.2 20.2 20.1 R (1) 0.2752 0.4036 0.4109 Ra (2) % Inh. (3) 0.2714 0.3981 0.4081 -36 1 o BK2 8.7 8.6 8.4 8.3 8.1 7.9 7.6 7.5 7.4 7.3 diff in controls 4): 14.4 EC 50 (95% Cl): > 1 0 0 0 mail (1) R= Oxygen uptake rat# (mg 02/L-min) (2| Ra= R adjusted to 20 C= (R/e.ExI (3) % Inhibition ss [(RaCm)-RaS/(RaCm)|100 (4| % difference in control: (IRaBk1-RaBk2t/RaCml100 (Two control m u tt be within 15% of each other.) (51 Mean adjueted R. control = IRaBkl + RaBk2|/2 t 7 21.5 0.3479 0.3134 RaCm (5): 0.2924 ass 1.072 RaCm mean adjuated R, contrla Bk = blank control, S = ample Toba ts ample temp X Tob-2 0, C Sponsor. 3M Company Sponsor Study ID# U1464 GOGOLS