Document XzdX8JBZ5D5b1ZRXaq3GD8r1J

^ZZC-3770 ACUTE TOXICITY TO FROG TADPOLES (Spring Peeper) TEST SUBSTANCE_______________________________ f!7 'i 1: l?i 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 Method: ASTM E729-96 Type: Static renewal GLP: Yes Date completed: Study completed 2007 Species: Pseudacris crucifer Supplier: Carolina Biological Supply Company, Burlington, North Carolina 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: Binomial probability method used to calculate all LC50 values. The NOEC determined by visual interpretation of mortality and observation data. Test organism age: Juveniles Average wet weight at test initiation: at Day 0 = 0.030 (0.010-0.044) g; 0.040 (0.023-0.063) g a tte st termination Loading: 0.12 g tadpole/L at Day 0, 0.16 g tadpole/L at test termination Pretreatment: None Acclimation: Prior to the test, tadpoles were held for 5 days in water from the same sources and at approximately the same temperature as used during the test. Temperatures ranged from 20.4 to 21.4C. pH ranged from 7.8 to 8.2. Dissolved Oxygen ranged from 7.0 to 9.0 mg/L. Tadpoles were fed a commercially-prepared food daily. Test conditions: Dilution water: Filtered, aerated, UV-sterilized well water CONTAINS NO CB P-2 Dilution water chemistry (during the 4-week period immediately preceding the test): Specific Conductance: 291 (290-295) pmhos/cm Hardness: 136 (132-140) mg/L as C aC 03 Alkalinity: 183 (182-184) mg/L as C aC 03 pH: 8.1 (8.1-8.1) Stock and test solution preparation: A primary stock solution was prepared at a nominal concentration of 50 mg active ingredient per liter using a calculated amount of PFOS, and stirred overnight using a top-down electric mixer. After mixing, the primary stock solution was proportionally diluted with dilution water to prepare each test concentration. Each test solution was stirred with a whisk. All test solutions were adjusted to 100% active ingredient during preparation, based on test substance purity. All test solutions appeared clear and colorless a tte s t initiation, renewal, 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: Approximately 3L plastic vessel containing 2.5 L of test solution; water depth approximately 9.3 cm. Number of replicates: two Number of tadpoles per replicate: ten Number of concentrations: Five plus a negative control Photoperiod: 16 hours light and 8 hours dark with a 30-minute transition in simulated natural sunlight from fluorescent bulbs. Feeding schedule: Tadpoles were fed a tte st initiation on day 0 and at test renewal on day 2 with 25 mg ground commercially supplied tadpole food. Water chemistry during the study: Dissolved oxygen range (0 - 96 hours): 7.6 - 8.6 mg/L (negative control exposure) 7.2 - 8.7 mg/L (all test substance exposures) pH range (0 - 96 hours) 8.3 - 8.5 (negative control exposure) 8.3 - 8.6 (all test substance exposures) Test temperature range (0 - 96 hours) 21.5 - 22.6C (negative control exposure) 21.2 - 22.7C (all test substance exposures) RESULTS Nominal concentrations: Bk control, 3.2, 6.3, 13, 25, and 50 mg/L 3 P-3 Measured concentrations: <LOQ, 3.6, 7.0, 14, 27, 51 mg/L Element value*: 24-hour LC50 = >51 mg/L (C.l. not calculable) 48-hour LC50 = >27 mg/L (C.l. not calculable) 72-hour LC50 = 47 mg/L (C.l. not calculable) 96-hour LC50= 38 mg/L (27 - 51 mg/L) 96-hour NOEC = 3.6 mg/L *AII element values based on mean measured concentrations Statistical Evaluation of Mortality: Binomial probability with nonlinear interpolation 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 spectrometric (LC/MS/MS) detection. The LOQ (limit of quantitation) was 1.00 mg/L in this study. The measured concentrations of matrix fortifications analyzed concurrently during sample analysis were 99.4-106% of nominal. Samples collected in exposure vessels at test initiation had measured values from 104 to 118% of nominal. New samples collected at 48 hours had measured concentrations from 105 to 131% of nominal. Old samples collected at 48 hours had measured concentrations ranging from 99.2 to 107% of nominal. Measured concentrations of PFOS in samples collected attest termination were 96.8 to 101% of nominal. Summary of analytical chemistry data: Nominal Test Concentration, mg/L Measured Values of New and Old Test Solutions Respectively, mg/L<1) Mean Measured Concentration, mg/L Percent of Nominal Negative Control 3.2 All < LOQ 3.77, 3.17,4.18, 3.24 <LOQ 36 113 6.3 7.15, 6.62, 8.28, 6.10 7.0 111 13 13.8, 13.4, 15.0. 12.9 14 108 25 28.1,26.8. 28.0. 25.2 27 108 50 51.9, 51 7, 52.3,49.2 51 102 (1) Samples are listed in this order: Day 0 (new), 48-hours (old), 48-hours (new), 96-hours (old) (2) LOQ = Limit of Quantitation = 1.00 mg/L as the active ingredient Biological observations after 96-hours: All tadpoles in the negative control and the 3.6 mg/L appeared healthy and normal throughout the exposure period with no mortalities or overt signs of toxicity observed. Tadpoles that survived to test termination in the 7.0 mg/L treatment appeared normal. A tte s t termination, mortality in the 7.0, 14, 27 and 51 mg/L treatment group was 15, 15, 15, and 80%, respectively. Signs of 4 toxicity observed in the affected tadpoles from the 14, 27 and 50 mg/L treatment groups included lethargy and curved tail and spine. Cumulative percent mortality: Mean Measured Test Cone., mg/L Negative Control 3.6 70 14 27 51 24-hours 0 0 0 5 0 10 48-hours 0 0 0 5 0 45 72-hours 0 0 0 10 0 60 96-hours 0 0 15 15 15 80 Lowest concentration causing 100% mortality: > 51 mg/L Mortality of controls: None CONCLUSIONS_____________________________________ The potassium perfluorooctanesulfonate 96-hour LCsofor spring peeper tadpole was determined to be 38 mg/L. The 96-hour no mortality concentration was 3.6 mg/L and no observed effects concentration was 3.6 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 CO,/v ;. 1 OB- Last changed: 06/26/07