Document RpEb8wQwdv91X6ppQXpwZD74a

BIOCONCENTRATION - REVISED TEST SUBSTANCE____________________________________________ Identity: Perfluorooctanesulfonate; may also be referred to as PFOS or FC-95. (1-Octanesulfonicacid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-, potassium salt, CAS # 2795-39-3) Remarks: Sample from 3M production lot number 217. The test substance is a white powder. Purity determined to be 86.9% by LC/MS, 1H-HMR, 19F-NMR and elemental analyses techniques. METHOD: M ethod/guideline follow ed: US EPA OPPTS 850.1730 and OECD 305 Type: Flow-through exposure with flow-through depuration phase. GLP (Y/N): Yes Year: 2001, Report amended 2002 Species: Bluegill (Lepomis macrochirus) S upplier: Osage Catfisheries, Inc., Osage Beach, Missouri Length and w eight a t te st term ination: Mean length = 62 mm, range 56-66 mm Mean weight = 2.70 g, range 2.03 - 3.32 g Loading: 0.48 g fish/L/day (based on initial loading of 90 fish per tank, using mean fish weight at the end of the study and volume of water that passed through test chamber in 24-hours). Fish age: Approximately 7 months at test initiation A nalytical m onitoring: Concentration of PFOS in water and fish. Pretreatm ent: None Num ber o f concentrations: Two plus a negative control Test concentrations (mean m easured): Negative control, 0.086 and 0.87 mg/L Uptake period: 62-days (0.086 mg/L exposure) 35-days (0.87 mg/L exposure - this exposure ended after 35-days due to fish mortality) D epuration period: 56-days (0.086 mg/L exposure) None (0.087 mg/L exposure) Test conditions: D ilution w ater: Moderately-hard well water D ilution w ater chem istry: S pecific conductance: 313 (310 - 315 umhos/cm) Hardness: 130 (128 - 132 mg/L) A lka lin ity: 1 7 8 (1 7 6 -1 7 8 ) pH: 8.1 (8.0 - 8.2) Measured during the 4-week period immediately preceding the test. Test conditions (cont): Stock and test solution preparation: Two stock solutions were prepared at 10 and 100 mg a.i./L. Stock solutions stirred with an electric top-down mixer to aid in the solubilization of the test substance. After mixing, the stocks appeared clear and colorless. Stocks were prepared at approximately weekly intervals during the uptake phase. Stocks injected into the diluter mixing chambers at a rate of 3.5 mUminute where they were mixed with dilution water at a rate of 350 mUminute to achieve the desired test concentrations. All final test solutions appeared clear and colorless. Diluter flow rate: Approx. 6.3 volume additions per 24-hours Exposure vessels: 104 L stainless steel aquaria filled with approximately 80 L solution. Number of replicates: None - one vessel per concentration Number offish per vessel: 90 Diet: Flake food, Ziegler Brothers, Inc., Gardners, PA Water chemistry ranges during the study:___________________ Neg. Control 0.086 mg/L 0.87 mg/L Dissolved oxygen, mg/L: 6 .8 -8 .6 6 .8 -8 .6 6.4 - 8.2 Temperature, C: 21.8-22.0 21.7-22.0 21.7-21.9 _Efl:__________________ 7.9 - 8.2 7 .9 -8 .2 7.9 - 8.2 Photoperiod: 16 hours light and 8 hours dark with a 30 minute transition period. Light intensity: 278 lux at surface of the negative control vessel at test initiation Collection of tissue samples: Fish were collected from test chambers by random selection at 12 time points during the 62-day uptake phase. They were euthanized, blotted dry, weighed and measured. Fish then rinsed with dilution water, blotted dry again and dissected into edible and nonedible tissue fractions. The fractions were individually weighed. The head, fins and viscera were considered to be nonedible tissue. The remaining tissue, including skin was considered to be edible tissue. S tatistical m ethods: W hole fish concentrations were calculated based on the sum of the edible and nonedible parts. Steady-state bioconcentration BCF values were originally calculated from the tissue concentrations at apparent steady-state using the BIOFAC model. Upon further investigation, this model was deemed inappropriate for use with this data set. The tissue concentrations had reached a point where there were not statistically significant differences between the last three sample days. However, a plot of the data clearly shows a trend of increasing concentrations in the tissues. In addition, the BIOFAC program is not accepted as appropriate for surfactants. An amended report was issued with BCFK values calculated as outlined in the draft OPPTS 850.1730 Guidance Document. The kinetic bioconcentration factor (BCFK), uptake rate (ki) and depuration rate (k2) were calculated for the edible, nonedible and whole fish exposed to 0.086 mg/L. These rate constants were then used to calculate a BCFK (BCFK = K1/K2) and half-lives for clearance for each tissue type. The results from this data reanalysis are presented below. RESULTS____________________________________________ Nominal concentrations: Negative control, 0.1 and 1.0 mg/L Mean measured concentrations: < 0.05,0.086 and 0.87 mg/L Kinetic Bioconcentration factors (BCFK): 0.086 mg/L exposure BCFK: Edible 1124 Nonedible 4013 Time to reach 50% clearance: 86 days 116 days Whole Fish 2796 112 days 0.87 mg/L exposure Although BCF values were calculated using the BIOFAC software, the results are not reported here. All of the fish had died or been sampled prior to achieving steady-state. As a result, the BCF values were underestimated and are not relevant. PFOS Concentrations in Tissues of Bluegill Exposed to 0.086 mg/L Values are from 4 individual fish at each sample period. Uptake Day 0 (4-hours) 1 3 7 14 21 28 35 42 49 56 62 Edible Tissue, mg/kg 0.167, 0.155, 0.144, 0.182 0.734, 0.726, 0.631, 0.806 1.73,2.07, 2.03, 2.11 3.73,4.25,4.73, 6.25 11.4,9.07,13.7,12.6 11.7,12.0,12.9,10.6 18.3,13.7,23.9,23.1 22.6, 27.7,23.8, 20.6 27.6,25.3,21.2,27.6 33.3,36.2,39.0, 30.6 48.3,38.9,44.1,38.3 42.4,66.2,42.2, 39.2 Nonedible Tissue, mg/kg 0.415, 0.519,0.417,0.497 1.68,1.85,1.72, 2.07 4.59,5.50, 5.47, 5.97 10.2,10.6,11.9,15.2 27.3,23.2,35.3, 32.6 33.3,22.7,24.6, 24.4 49.4,40.7,65.3, 57.9 67.1,73.3,62.0,59.1 64.0,68.1,54.4, 79.6 85.0,95.1,93.1,77.7 122,94.2, 73.2,106 101,112,105, 96.4 Depuration Day 14 28 42 56 48.5, 31.8,31.6,42.0 26.0, 33.3, 38.7, 55.8 24.1,31.2, 30.0, 33.0 21.1,37.6,32.9, 31.2 124,79.4, 81.8,113 85.7,95.1, 85.7, 94.8 71.7,80.6, 78.3, 82.1 57.7, 80.3, 85.4, 84.4 Whole Fish Cone., mg/kg 0.293, 0.351,0.286, 0.363 1.26,1.34,1.29,1.53 3.21,4.04,4.18,4.38 7.33, 7.66, 8.73,11.4 20.2,16.9,26.0, 24.6 23.3,18.4,19.8,18.5 35.3,29.2,45.4,44.1 46.3,53.8,46.6,40.9 50.1,49.4,40.9,56.3 62.8,69.6, 70.8, 57.4 90.6, 71.6, 63.3, 74.8 77.0, 92.7, 79.6, 73.1 90.3,60.4, 61.6, 85.3 58.2,70.1,68.1,81.1 51.4,61.4,61.0,62.2 41.6,66.5,65.8,62.1 PFOS Concentrations in Tissues of Bluegill Exposed to 0.87 mg/L Values are from 4 individual fish at each sample period. Uptake Edible Tissue, Nonedible Tissue, Whole Fish Cone., Day 0 (4-hours) 1 mg/kg 1.46,1.48,1.19,1.39 4.68,6.59, 5.56, 5.64 mg/kg 3.52,4.37,4.22, 4.06 11.1,14.2,13.3, 12.1 mg/kg 2.71,3.08,2.84,2.89 8.00,10.9,10.2,9.47 3 17.3,15.8,19.0, 20.8 39.3,42.0,43.8, 51.8 30.5, 30.7,34.5, 39.1 7 42.0,44.0, 57.7,46.8 100,102,102,120 74.9, 77.0, 85.3, 89.8 14 87.1,81.6, 90.7,73.3 177, 207, 245, 214 141, 157, 180, 158 21 79.4,117, 104, 102 201, 278, 246, 229 146,210,185, 172 ---------- 2 8 ^ 102,131, 107, 133 289,372, 320,361 205,267, 232,263 (1) Sampling offish s topped after Uptake Day 28 due to mortality. Test organism mortality: Negative control: None during the uptake phase (62 days) or depuration phase (35 days) 0.086 mg/L exposure: One fish died after 49 days and one after 59 days of exposure in the uptake phase, none during the depuration phase (total of 2.2% mortality during the study). 0.87 mg/L exposure: Mortality first noted on Day 9 and continued through Day 35 of the uptake phase at which time all of the fish had either died or had been sampled A nalytical m ethodology: Analyses of test solutions and fish tissues were performed at W ildlife International, Ltd. Water samples were diluted and analyzed by HPLC with single quadrupole mass spectrometric detection. Tissue samples were homogenized, extracted, diluted and analyzed by HPLC with triple quadrupole mass spectrometric detection. When determining the concentration of the test substance in the samples, the same and most prominent peak response for perfluorooctanesulfonate was used. No attempt was made to quantify on the basis of individual isomeric components. The LOQ was 0.05 mg/L for water in this study. For tissue samples, the LOQ was calculated on an individual basis for each sample since each entire submitted sample, of differing weight, was extracted without an adjustment to constant weight. Recovery was excellent in both water and fish tissues, ranging from 84.9 to 122% of fortification levels. Analytical results were not corrected for procedural recovery. CONCLUSIONS PFOS bioconcentrated in the tissues of bluegill sunfish during this study. The BCFK values calculated for the edible, nonedible and whole fish tissues from the 0.086 mg/L exposure were calculated to be 1124,4013, and 2796, respectively. PFOS depurated slowly. The BIOFAC estimates for the time to reach 50% clearance for edible, nonedible and whole fish tissues from the 0.086 mg/L exposure were 86,116 and 112 days, respectively. DATA QUALITY_____________ R eliab ility: Klimisch ranking = 1 REFERENCES______________ This study was conducted at W ildlife International, Ltd., Easton, MD at the request of the 3M Company, Lab Request number U2723. The report was amended and reissued June 6,2002. OTHER_______________________________________________________ Last changed: 6/11/02