Document dQYY7yVmVVQDbMook0zv1DzaB

p. 1 / 70 ACUTE TOXICITY TO FROG TADPOLES (Spring Peeper ) TEST SUBSTANCE n 7 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, 'H-HMR, 19F-NM R 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%) ; perfluorooctanbate 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 : Juvenile s Average wet weight at test initiation : at Day 0= 0 .030 (0 .010-0 .044) g; 0.040 (0 .023-0.063) g at test terminatio n Loading : 0 .12 g tadpole/L at Day 0, 0 .16 g tadpole/L at test termination Pretreatment: Non e 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 wate r CONTAINS NO CBI -2 p. 2 Dilution water chemistry ( during the 4-week perio d immediately preceding the test) : Specific Conductance : 291 (290-295) pmhos/cm Hardness : 136 (132-140) mg/L as CaCO3 Alkalinity: 183 (182-184) mg/L as CaCO3 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 at test initiation, renewal, and termination . Solvent : non e 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 attest 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 (aII 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) RESULT S 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 .I . not calculable) 48-hour LC50 =>27 mg/L ( C .I . not calculable) 72-hour LC50 = 47 mg/L ( C .I . not calculable) 96-hour LC50 = 38 mg/L (27 - 51 mg/L) 96-hour NOEC = 3 .6 mg/L *All element values based on mean measured concentrations Statistical Evaluation of Mortality : Binomial probability with nonlinear interpolatio n Analytical Methodology : Analyses of test solutions were performed at Wildlife International Ltd . The method consisted of dilution of the samples 1 :1, vlv 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 fo rtifications 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 measure d 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 Measured Values of New and Old Mea n Concentration, Test Solutions Respectively, mg/L(l) Measured Percent of mg/L Concentration, Nominal mg/ L Negative Control 3 .2 All < LOQ ") <LOQ - 3 .77, 3 .17, 4 .18, 3 .24 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 10 2 (1) Samples are listed in this order : Day 0(new), 48-hours (old), 48-hours (new), 96-hours (old) (2) L00 = Limit of Quantitation = 1 .00 mg/L as the active ingredien t 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 mo rt alities or ove rt signs of toxicity observed . Tadpoles that survived to test termination in the 7 .0 mg/L treatment appeared normal . Attest termination, mo rtality in the 7 .0, 14, 27 and 51 mg/L treatment group was 15, 15, 15, and 80%, respectively . Signs of 4 p. 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 mo rtality: Mean Measured 24-hours 48-hours 72-hours 96-hours Test Conc . , mg/L Negative 0 0 0 0 Control 3 .6 0 0 0 0 70 0 0 0 15 14 5 5 10 15 27 0 0 0 15 51 10 45 60 8 0 Lowest concentration causing 100% mortality: > 51 mg/L Mortality of controls : None CONCLUSIONS The potassium perfluorooctanesulfonate 96-hour LC50for 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 QUALIT Y Reliability : Klimisch ranking = 1 REFERENCE S This study was conducted at Wildlife International Ltd ., Easton, MD at the request of 3M . 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