Document zR46DjzYqL6BR2ax7KnvJXvB

ACUTE TOXICITY TO FISH AR2T6-oS3q TEST SUBSTANCE Identity: Perfluorooctylsulfonate, didecyldimethylammonium salt; may also be referred to as Fluoroalkyl ammonium derivative. [1Decaminium, N-decyl-N,N-dimethyl-, salt with 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluoro-loctanesulfonic acid (1:1), CAS #251099-16-8] Remarks: The 3M production lot number was Lot 1. The test sample is L14394 referred to by the test laboratory as P3025. The sample was labeled F-11615, Lot 1. The test sample is a mixture of the test substance in water (approximately 30-40% test substance, 60-70% water, and 0-5% of residual perfluorochemicals). All values reported relate to this mixture. The test sample appears to be a 2-phase dispersion (clear liquid with opaque solid) which rapidly separates after agitation. No calculations were made to adjust for the actual concentration of the test substance in the test sample. METHOD Method: OECD 203 Type: Static acute GLP: No Year completed: 1996 Species: Pimephales promelas Supplier: Not noted. Analytical monitoring: DO, pH, temperature, and conductivity were monitored daily. Exposure period: 96-hours Statistical methods: LL50 values calculated using the Trimmed Spearman-Karber method. The NOEL was calculated using Fisher's Exact tests. Test fish age: Not given. Length and weight: Average length = 11.3 mm, Average weight = 7.8 mg Loading: 0.26 g/L Pretreatment: None Test conditions: Dilution water: Dechlorinated City of Duluth, MN tap water. Water was aerated for 24-hours prior to use in the test. G042C2 Dilution water chemistry: hardness: 48 mg/L as CaCC>3 pH: 8.08 Lighting: Cool-white fluorescent bulbs. Photoperiod of 16-hours light, 8-hours dark used. No transition period noted. Stock and test solution preparation: Water accommodated fractions. Test solutions were prepared individually for each test replicate concentration by mass addition of vigorously shaken test substance in 4 L of dilution water. The solutions were vigorously stirred for 21-hours (vortex 1/2 to 1/3 solution depth). The aqueous phase was siphoned from the vessel at mid-depth. Concentrations dosing rate: Once Stability of the test chemical solutions: Not noted. Exposure vessels: 4-L glass jars containing 3-L of test solution. The jars were sealed with Teflon-lined lids fitted with stoppers to accommodate oxygen flushing of headspace. Number of replicates: two Number offish per replicate: ten Number of concentrations: three plus a negative control Water chemistry during the study: Dissolved oxygen range (0 - 96 hours): 9.1 - 14.6 mg/L (control exposure) 8.7 - 18.2 mg/L (700 mg/L exposure) pH range (0 - 96 hours) 7.80 - 8.08 (control exposure) 7 .7 8 -7 .9 9 (700 mg/L exposure) Test temperature range (0 - 96 hours) 20.8 - 20.9C Conductivity range (0 - 96 hours): 1 2 8 -1 4 2 pmhos/cm (control exposure) 1 1 8 -1 5 4 pmhos/cm (700 mg/L exposure) Remarks: Oxygen was added to the headspace in the jars before sealing initially and at each observation period. The dissolved oxygen concentrations were super-saturated in the test vessels, particularly in the 700 mg/L exposure concentration. RESULTS Nominal loading concentrations: Bk control, 400, 700, 1,000 mg/L. Element value: 24-hour LL5o = 618 (568 - 673) mg/L 48-hour LLso = 607 (554 - 664) mg/L G042C3 72-hour LL5o = 595 (551 - 643) mg/L 96-hour LLso = 562 (523 - 604) mg/L 96-hour NOEL = <490 mg/L All element values based on nominal concentrations. Biological observations after 96-hours: No mortality or abnormal behavior observed in the negative control during the test. Mortality was observed in the remaining exposure concentrations. Surfacing was observed in half of the fish at the 700 mg/L exposure concentration at 24hours, and 2 fish were quiescent at 96-hours. No abnormal behavior was observed in the 400 mg/L exposure concentration. Cumulative percent mortality: Nom inal Loading T est C on e., m g/L 2 4 -h o u rs 4 8 -h o u rs 7 2 -h o u rs 9 6 -h o u rs Neg. Control 0 0 0 0 490 10 15 15 25 700 75 75 80 90 1 ,0 0 0 100 100 100 100 Lowest concentration causing 100% mortality: 1,000 mg/L Mortality of controls: None Remarks: Values reported are for the test sample. No calculations were made to adjust for the concentration of the test substance in the test sample. CONCLUSIONS The test sample 96-hour LL50 for fathead minnow was determined to be 562 mg/L with a 95% confidence interval of 523 -604 mg/L. The 96-hour no observed effects level (NOEL) was <490 mg/L. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY Reliability: Klimisch ranking 2. The study lacks analytical measurement of test substance concentrations in the test solutions and sample purity is 004234 not sufficiently characterized. Additionally, data is for a mixture and toxicity cannot be positively attributed to didecyldimethylammonium Perfluorooctylsulfonate salt alone. Also, supersaturation of the test solutions with oxygen could also have contributed to the toxicity. REFERENCES This study was conducted at AScI Corporation, Environmental Testing Division, Duluth, MN, at the request of the 3M Company. OTHER Last changed: 5/24/00 *(G7* AScl Corporation/AScl-Duluth Environmental Testing Division AScl Study (D# 5010-068 STUDY TITLE ACUTE TOXICITY OF DEVELOPMENTAL MATERIAL TO FATHEAD MINNOW {PIMEPHALES PROMELAS) DATA STANDARD OECD GUIDELINE 203 STUDY COMPLETED January 2, 1997 TESTING FACILITY AScl Corporation/AScI-Duluth Environmental Testing Division 4444 Airpark Boulevard Duluth, MN 55811 Tel. No. (218) 722-4040 Fax No. (218) 722-2592 STUDY IDENTIFICATION NUMBERS AScl Study ID# 5010-068 3M Company Lab Request# P3025 Sponsor: 3M Company Sponsor Study ID# P3025 1 004236 AScI Corporation/AScI-Duluth Environmental Testing Division 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 Dates Data Validation and Report Review Retention of Raw Data and Final Report Location of Raw Data and Final Report Acute Toxicity of P 3 Developmental Material to Fathead Minnow (Pimephales promelas). OECD Guideline 203. 3M Environmental Technology and Safety Services, Building 2-3E-09, 935 Bush Avenue, St. Paul, MN 55133. Susan A. Beach, 3M Environmental Technology and Safety Services, Building 23E-09, 935 Bush Avenue, St. Paul, MN 55133. Tel No. (612) 778-7452. P3025. AScI Corporation/AScI-Duluth Environmental Testing Division, 4444 Airpark Boulevard, Duluth, MN 55811; Tel. No. (218) 722-4040. Joe Dierkes. Joe Amato. Donald Mount. December 17-21, 1996. Alan Mozol. i u v fReport Signature: --------------------------------------- ----- ---- ---p-----------Two years from the date study is completed. AScI Corporation/AScI-Duluth Environmental Testing Division, 4444 Airpark Boulevard, Duluth, MN 55811; Tel. No. (218) 722-4040. Sponsor: 3M Company Sponsor Study ID# P3025 2 004237 AScl Corporation/AScI-Duluth Environmental Testing Division AScl Study ID# 5010-068 2.0 OBJECTIVE(S) To determine the 96-h LL50 (lethal loading) and 96-h NOEL (no observed effect loading) of the test substance, 1*10$ Developmental Material, for fathead minnow (Pimephales promelas). This study was conducted according to the AScl study plan retained by the Sponsor and OECD Guideline 203 (OECD 1993). The test solutions were water-accommodated fractions (WAF) prepared following Girling, Whale, & Adema 1994. Test Substance Test Organisms 3.0 TEST METHODS Properties: , two-phase liquid before agitated, light colored, nearly odorless slurry after agitation, specific gravity ca. 1.2 g/cc, and insoluble in water. Test loadings: 0 (dilution water control), 490 mg/L, 700 mg/L and 1000 mg/L. Test loading solutions were prepared individually for each test replicate. The 490 mg/L solutions were prepared by placing 1960 mg of vigorously shaken test substance in 4 L of dilution water. The 700 mg/L and 1000 mg/L solutions were prepared in the same manner using 2800 mg and 4000 mg of test substance, respectively. The solutions were vigorously stirred (vortex 1/3 to 1/2 solution depth) for 21 h. The aqueous phase was siphoned from the vessel at mid depth. Source: Healthy, juvenile fathead minnows (Pimephales promelas) obtained from a commercial supplier. Holding/acclimation: Held and acclimated for 12 days in the test dilution water. For the 48 hours preceding the test 0% mortality occurred. For the entire 12 days, mortality was 0%. At test termination, the fish were 1.1 cm in mean length and 7.8 mg in mean weight. Use in test: Used 10 organisms/replicate and 2 replicates/test concentration. Sponsor: 3M Company Sponsor Study ID# P3025 3 004238 ASc[ Corporation/AScl-Duluth Environmental Testing Division ASel Study ID# 5010-068 Dilution Water Exposure Chambers Incubation Observations Endpoint Calculations Source: Dechlorinated City of Duluth, MN, tap water. The most recent chemical analysis is in Raw Data Package. 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 using in the test. Type: 4-L glass jars sealed with Teflon-lined lids fitted with stoppers to accommodate oxygen flushing of headspace. Use in test: 3 L of dilution water or test solution/chamber. During the test, kept covered, except when experimental observations were made or headspace was flushed with oxygen. Solutions were not aerated during the exposures. Duration: 96 h. Daily photoperiod: 16 h light and 8 h dark, maintained using cool-white fluorescent bulbs. Temperature: 21 C. Biological: Daily- Test organisms with abnormal behavior and signs of stress, and dead test organisms. 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). 24-, 48-, 72-, and 96-h median lethal loading (LLS0's), and 96-h no observable effect loading (NOEL) LL50: Trimmed Spearman-Karber method. NOEL: TOXSTAT statistical software, Version 3.2, University of Wyoming. Sponsor: 3M Company Sponsor Study ID# P3025 4 C04239 ASe[ Corporation/AScl-Duluih Environmental Testing Division AScI Study ID0 5010-068 3.0 RESULTS Test Substance Toxicity (Pertinent data are in Table 1) Ranges of Water Chemistry Parameters 24-h LL50: 618 mg/L (568-673 mg/L). 48-h LLS0: 607 mg/L (554-664 mg/L). 72-h LL50: 595 mg/L (551-643 mg/L). 96-h LLS0: 562 mg/L (523-604 mg/L). 96-hNOEL: <490 mg/L. Total hardness (as CaC03 mg/L): 44-48. Alkalinity (as CaC03 mg/L): 44. Temperature (C): 20.8-20.9C. DO (mg/L): 8.6-20.0. pH: 7.71-8.08. Specific conductivity (umhos/cm): 118-487. 4.0 TEST QA/QC QA/QC Criteria Data Mortality in control exposure must not be more 0% dead. 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 97% of the air saturation value at 21.0C. After initial 0-hour routine chemistries had been performed the chambers were sealed and each chamber's headspace was flushed with oxygen daily to maintain adequate DO. Ensuing DO concentrations were 100% of saturation or greater. Sponsor: 3M Company Sponsor Study IDtt P3025 5 AScI Coqoration/ASoI-Duluth Environmental Testing Division AScl Study ID# 5010-068 Test duration must be 96 h. Reference substance toxicity test (this test is optional). The test duration was 96 h. Control chart for sodium chloride reference 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. Girling, A.E., G.F. Whale, and D.M .M . Adema. 1994. A Guideline Supplement for Determining the Aquatic Toxicity of Poorly Water-Soluble Complex Mixtures using WaterAccommodated Fractions. Chemosphere, Vol. 29, No. 12, pp. 2645-2649. Hamilton, M .A., R.C. Russo, and R.V. Thurston. 1977. Trimmed Spearman-Karber Method for Estimating Median Lethal Concentrations in Toxicity Bioassays. Environ. Sci. 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. University of Wyoming. 1996. Toxstat Version 3.2. Laramie, Wyoming. Sponsor: 3M Company Sponsor Study ID# P3025 6 004241 AScI Corporation/AScI-Duluth Environmental Testing Division AScI Study ID# 5010-068 TABLE 1. ACUTE TOXICITY OF P MINNOWS (P. promelas) DEVELOPMENTAL MATERIAL TO FATHEAD Test Substance Loading (mg/L) 0 (Control) 490 700 1000 Cumulative Number of Dead Organisms and Percent Mortality3 24 h 48 h 72 h 96 h 0(0) 2(10) 15 (75) 20 (100) 0(0) 3 (15) 15 (75) 20 (100) 0 (0) 3 (15) 16 (80) 20 (100) 0(0) 5(25) 18 (90) 20 (100) 1 Percentages are in parenthesis. EFFECT AND NO-EFFECT LOADINGS WITH CORRESPONDING 95% CONFIDENCE INTERVALS LL50 and NOEL 24-h LL50 48-h LLi0 72-h LL50 96-h LL50 96-h NOEL Data (mg/L) 618 607 595 562 <490 95% Confidence Interval 568-673 554-664 551-643 523-604 Not applicable Sponsor: 3M Company Sponsor Study ID# P3025 7 004242