Document YrYexVmBkD4xYZGdgZKkvpkbn

P-1 ACUTE TOXICITY TO THE MIDGE (CHIRONOMUS TENTANS) TEST SUBSTANCE Identity: Perfluorooctanolc acid, ammonium salt; may also be referred to as PFOA, PFOA ammonium salt, Ammonium perfluorooctanoate, FC-116, FC-126, FC-169, or FC-143. (Octanoic acid, pentadecafluoro-, ammonium salt, CAS # 3825 26-1) Remarks: The test substance is a solid. Sample was taken from 3M lot number 332. Sample was stored under frozen conditions prior to testing. Purity determined to be 95.0% by LC/MS, 19F-NMR, and elemental analyses techniques. The impurities were identified as: metals (0.002%); lower chain-length (C6 and C7) perfluorinated sulfonates (4.68%); NMR impurities (0.36). METHOD Method: ASTM E729-96 Type: Static renewal GLP: Yes Date completed: Study completed 2007 - Species: Chironomus tentans Supplier: Environmental Consulting and Testing (ECT), Superior, Wl Analytical monitoring: PFOA measured at initiation, prior to and after renewal at 48 hours and at test termination (96-hours) Exposure period: 96-hours Statistical methods: The NOEC determined by visual interpretation of mortality, immobility and observation data. Test organism age: 2ndto 3rd instar larvae (approximately 10 days old) Average wet weight at test initiation: Not provided Loading: 1 midge per test chamber Pretreatment: None Acclimation: Prior to the test, midges were held for 3 days with sand and water from the same sources and at approximately the same temperature as used during the test. Temperatures ranged from 22.0 to 22.8C. pH ranged from 8.1 to 8.4. Dissolved Oxygen ranged from 7.2 to 8.6 mg/L. Midges were fed a 56 g/L suspension of Tetramin flake food daily during holding. Test conditions: Dilution water: Filtered, aerated well water CONTAINS NO CBI P-2 Dilution water chemistry (during the 4-week period immediately preceding the test): Specific Conductance: 293 (285-300) |jmhos/cm Hardness: 136 (132-140) mg/L as C aC 03 Alkalinity: 183 (182-184) mg/L as C aC 03 pH: 8.0 (7.9-8.1) Stock and test solution preparation: A primary stock solution was prepared at a nominal concentration of 1000 mg active ingredient per liter using a calculated amount of PFOS, and sonicated for 5 minutes and mixed by inversion. After mixing, the primary stock solution was proportionally diluted with dilution water to prepare each test concentration. Each test solution was mixed by inversion. All test solutions were adjusted to 100% active ingredient during preparation, based on test substance purity. All test solutions appeared clear and colorless in the test chambers at test 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 filled with approximately 20 mL of water. Beakers had approximately oneeighth teaspoon of sand on the bottom as substrate. Vessels were covered with plastic wrap. Number of replicates: ten Number of tadpoles per replicate: one 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: Midges were fed a tte st initiation on day 0 and a tte st renewal on day 2 with 4 g/L Tetramin flake food Water chemistry during the study: Dissolved oxygen range (0 - 96 hours): 7.9 - 8.7 mg/L (negative control exposure) 7.6 - 8.7 mg/L (all test substance exposures) pH range (0 - 96 hours) 8.2 - 8.5 (negative control exposure) 7.9 - 8.5 (all test substance exposures) Test temperature range (0 - 96 hours) 22.0 - 22.6C (negative control exposure) 21.7 - 23.0C (all test substance exposures) RESULTS P-3 Nominal concentrations: Bk control, 63, 125, 250, 500, and 1000 mg/L Measured concentrations: <LOQ, 74, 153, 277, 579, 1090mg/L Element value*: 24-hour LC5o = > 1090 mg/L (C.l. not calculable) 48-hour LC50 = > 1090 mg/L (C.l. not calculable) 72-hour LC50 = > 1090 mg/L (C.l. not calculable) 96-hour LC50 = > 1090 mg/L (C.l. not calculable) 96-hour NOEC = 277 mg/L *AII element values based on mean measured concentrations Statistical Evaluation of Mortality: Visual interpretation of observations and subsequent recorded data was utilized for assignment of NOEC. 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 10 mg/L in this study. The measured concentrations of matrix fortifications analyzed concurrently during sample analysis were 97.0-107% of nominal. Samples collected in exposure vessels at test initiation had measured values from 102 to 106% of nominal. New samples collected at 48 hours had measured concentrations from 1052to 104% of nominal. Old samples collected at 48 hours had measured concentrations ranging from 120 to 141% of nominal. Measured concentrations of PFOS in samples collected at test term nation were 107 to 160% of nominal. Summary of analytical chemistry data: Nominal Test Concentration, mg/L Measured Values of New and Old Test Solutions Respectively, mg/Lt1) Mean Measured Concentration, mq/L Percent of Nominal Negative Control 63 All < LOQ(2) 65 4, 75.5, 65.1,91.2 <LOQ 74 117 125 130, 154, 129, 200 153 122 250 259, 302, 259, 289 277 111 500 532, 707, 511,566 579 116 1000 1020, 1260, 1020, 1070 1090 109 (1) Samples are listed in this order: Day 0 (new), 48-hours (old), 48-hours (new), 96-hours (old) (2) LOQ = Limit of Quantitation = 10 mg/L active ingredient Biological observations after 96-hours: A 10% mortality rate was observed in the negative control and the 74 mg/L treatment groups. No mortalities or signs of toxicity were observed among midges in the 153 and 277 treatment groups during the test. Midges that suivived to test termination in the in all treatments appeared normal. At test term nation, P-4 mortality in the 579 and 1090 mg/L treatment group was 30 and 40%, respectively. The only sign of adverse effects observed in the affected midges from the 1090 mg/L treatment group was pale appearance. Cumulative percent mortality: Mean Measured Test Cone., mg/L Negative Control 74 153 277 579 1090 25-hours 0 0 0 0 20 20 48-hours 0 0 0 0 20 20 72-hours 0 0 0 0 20 30 96-hours 10 10 0 0 30 40 Lowest concentration causing 100% mortality: > 1090 mg/L Mortality of controls: 10% CONCLUSIONS_____________ The perfluorooctanoic acid, ammonium salt 96-hour LCsofor Chironomus tentans was determined to be > 1090 mg/L. The 96-hour no mortality concentration was 3277mg/L and no observed effects concentration was 277 g/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: 07/10/07 /Vt