Document n9K9Vw6ZJmBogRDJDJ9d43kGa

4ZZ(;3772l ACUTE TOXICITY TO THE FRESHWATER AMPHIPOD (Hyalella azteca) TEST SUBSTANCE______________________________ Identity: Perfluorooctanesulfonate; may also be referred to as PFOS or FC-95. (1-Octanesulfonic acid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-, potassium salt, CAS # 2795-39-3) Remarks: The test substance is a white powder. Sample was taken from 3M lot number 217. Sample was stored under ambient conditions prior to testing. Purity determined to be 86.9% by LC/MS, 1H-HMR, 19F-NMR and elemental analyses techniques. The impurities were identified as: metals (1.45%); lower chain-length (C4-C7) perfluorinated sulfonates (8.41%); inorganic fluoride (0.59%); NMR impurities (1.905%); perfluorooctanoate anion (0.33%); and the total of tri-, penta-, hepta-, and nonapentafluoropropanoic acid (0.38%). METHOD_________________________ o--i Method: ASTM E729-96 ~ Type: Static renewal GLP: Yes ~ Date completed: Study completed 2007 ,, Species: Hyalella azteca " Supplier: Environmental Consulting and Testing (ECT), Superior, Wl Analytical monitoring: PFOS measured at initiation, prior to and after renewal at 48 hours and at test termination (96-hours) Exposure period: 96-hours Statistical methods: Bionomial probability method used to calculate the 24-hour LC50 values and probit analysis to calculate the 48, 72, and 96- hour LC50 values. The NOEC determined by visual interpretation of "T; mortality and observation data. .' Test organism age: 12-days old j Average wet weight at test initiation: Not measured Loading: 1 amphipod per chamber ^ Pretreatment: None ~~ Feeding: Fed YCT plus Tetramin flake food at Days 0 and 2 Acclimation: Prior to the test, the test organisms were acclimated to test conditions for 6 days by holding them in a container with gauze and water from the same source and at approximately the same temperature that would be used in the test. Temperatures ranged from 21.8 to 23.4 C. pH ranged from 8.1 to 8.5. Dissolved oxygen ranged from 6.4 to 8.0 mg/L. No signs of disease or stress were observed during the holding period. No information was provided on the characteristics of the "gauze" or its suitability for use in this application. Test conditions: CONTAINS NO CB <^6 P-2 Dilution water: Filtered, aerated, UV-sterilized well water Dilution water chemistry (during the 4-week period immediately preceding the test): Specific Conductance: 290 (285-295) |jmhos/cm Hardness: 136 (132-140) mg/L as CaC0 3 Alkalinity: 182 (180-184) mg/L as CaC03 pH: 8.1 (8.1-8.1) Stock and test solution preparation: A primary stock was prepared at a nominal concentration of 200 mg active ingredient per liter using a calculated amount of PFOS, and stirred overnight. For Day 0 solutions, the stock solution was sonicated for approximately 5 to 10 minutes the following day. The Day 2 stock solution was sonicated for only 5 minutes the following day. After mixing, primary stock solution was proportionally diluted with dilution water to prepare each test concentration. All test solutions were adjusted to 100% active ingredient during preparation, based on test substance purity. All test solutions appeared clear and colorless attest initiation and termination. Solvent: none Concentrations dosing rate: Static renewal after 48-hours Stability of the test chemical solutions: under test conditions: Stable as demonstrated by analytical monitoring. Exposure vessels: 30-mL Nalgene plastic beakers containing approximately 20 mL test solution. Water depth was 1.9 cm. A piece of Nitex screen was placed in each vessel as a substrate for the amphipods. Number of replicates: 10 (test substance), and 20 (negative controls) Number of amphipods per replicate: one Number of concentrations: Five plus a negative control Photo period: 16 hours light and 8 hours dark with a 30-minute transition in simulated natural sunlight from fluorescent bulbs. Water chemistry during the study: Dissolved oxygen range (0 - 96 hours): 8.2 - 8.5 mg/L (negative control exposure) 8.1 - 8.5 mg/L (all test substance exposures) pH range (0 - 96 hours) 8.2 - 8.6 (negative control exposure) 8.1 - 8.6 (all test substance exposures) Test temperature range (0 - 96 hours) 22.4 - 23.7C (negative control exposure) 22.2 - 23.8C (all test substance exposures) RESULTS Nominal concentrations: Bk control, 13, 25, 50, 100, and 200 mg/L 47 P-3 Measured concentrations: <LOQ, 13, 25, 51,102, and 199 mg/L Element value: 24-hour LC50 = >161 mg/L (C.l.> 102 mg/L) 48-hour LC50 = 93 (70 - 125) mg/L 72-hour LC50 =29 (20 - 40) mg/L 96-hour LC50 = 15 (4.5 - 24) mg/L 96-hour NOEC = < 13 mg/L All element values based on mean measured concentrations Statistical Evaluation of Mortality: Binomial probability with nonlinear interpolation or probit analysis Analytical Methodology: Analyses of test solutions were performed at Wildlife International Ltd. The method consisted of dilution of the samples 1:1, v/v with acetonitrile, followed by secondary dilution using acetonitrile: HPLC-grade bottled water (50:50, v/v) and analysis by direct injection high performance liquid chromatography with mass spectromtrie (LC/MS/MS) detection. The LOQ (limit of quantitation) was 2.00 mg/L in this study. The measured concentrations of matrix fortifications analyzed concurrently during sample analysis were 98.4-114% of nominal. Samples collected in exposure vessels at test initiation had measured values from 100 to 105% of nominal. New samples collected at 48 hours had measured concentrations from 95 to 100% of nominal. Old samples collected at 48 hours had measured concentrations ranging from 96.4 to 103% of nominal. Measured concentrations of PFOS in samples collected at test termination were 100 to 102% of nominal. Summary of analytical chemistry data: Nominal Test Concentration, mg/L Measured Values of New and Old Test Solutions, mg/L(1) Mean Measured Concentration, mg/L Percent of Nominal Negative Control 13 All < LOQ(2) 13.4, 13.5, 12.3, 13.0 <LOQ 13 100 25 25.1,24.9, 24.3, 25.4 25 100 50 52.6, 50.2, 49.4, 50.8 51 102 100 102, 103, 100, 101 102 102 200 204, na|J', 193, na'J) 199 99.5 (1) Samples are listed in this order: Day 0 (new), 48-hours (old), 48-hours (new), 96-hours (old) (2) LOQ = Limit of Quantitation = 2.00 mg/L (3) Not analyzed due to 100% mortality. Value not used In statistical calculations Biological observations after 96-hours: All but two amphipods in the negative control appeared healthy and normal throughout the exposure period with no mortalities or overt signs of toxicity observed. Two control amphipods exhibited lethargy that resulted in mortality. At test termination, mortality in the 13, 25, and 51 mg/L treatment groups was 40, 80, and 80%, respectively. Signs of toxicity observed in the affected 4% P-4 amphipods from all treatment groups included lethargy. All surviving amphipods at test termination appeared normal. Cumulative percent mortality: Mean Measured Test Cone., mg/L 24-hours Negative Control 0 13 0 25 0 51 0 102 0 199 10 48-hours 0 0 0 10 50 80 72-hours 5 10 40 80 100 100 96-hours 10 40 80 80 100 100 Lowest concentration causing 100% mortality: 102 mg/L Mortality of controls: 10% CONCLUSIONS________________________ The potassium perfluorooctanesulfonate 96-hour LC50for Hyalella azteca was determined to be 15 mg/L. The 96-hour no mortality concentration was <13 mg/L and no observed effects concentration was <13 mg/L. Submitter: 3M Environmental Laboratory, Maplewood, Minnesota, 55144 DATA QUALITY Reliability: Klimisch ranking = 1 REFERENCES This study was conducted at Wildlife International Ltd., Easton, MD at the request of 3M. OTHER Last changed: 07/10/0/