Document NeVgqn7V2Ze0rjjYy1rQw15np

AU 2 -2 ^ - W Wildlife International. Ltd. Project Number 454E-101 -1 - PFOS: AN ACTIVATED SLUDGE, RESPIRATION INHIBITION TEST ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER. 454E-101 3M LAB REQUEST NO. U2723 U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines OPPTS Number 850.1010 and OECD Guideline 202 This study was reported using a test substance purity of 90.49%. The test substance characterization was revised on 9/7/00 and the purity was determined to be 86.9%. The Sponsor requested that the results be revised based on the most recent purity analyses. The results previously presented were simply corrected by the ratio of the two purities or a factor of 0.9603. No attempt was made to recalculate analytical standard concentrations or measured concentrations from original raw data. As such, minor errors due to rounding may be present. Attached is the revised summary page from the final report and the most recent certificate of analysis. rc=o> 3E 33 o -T "O rn ~v CJ ro -- ! P I vjO ro Wildlife International. Ltd. 2- - Project Number 454E-101 REVISED STUDY ABSTRACT BASED ON A PURITY OF 86.9% The effect of the test substance on activated sludge microorganisms was assessed by the Activated Sludge Respiration Inhibition Test Method (OECD Guideline 209). The test contained a control, reference and treatment groups. The contiol group was used to determine the background respiration rate of the sludge and was not dosed with the test or reference substance. The reference group was dosed with 3,5-dichlorophenol, a known inhibitor of respiration, at concentrations of 3, 15 and 50 mg/L. The test substance was dosed at 0 87, 2.6, 8.7, 26, 87, 260 and 870 mg a.i./L.' After an exposure period o f 3 hours, the respiration rates of the test solutions were measured using a dissolved oxygen meter The respiration rates in the two controls were 39.8 and 41 1 mg OVL/hr. or a difference of 3 2%. The difference in control respiration rates was within the 15% difference limit established for the test. The validity of the test was further supported by the results from the 3,5-dichlorophenol reference group, which resulted in an EC50 of 9.0 mg/L. The EC50 was within the 5 to 30 mg/L range considered acceptable for the test. Differences in Oi respiration rates between the control group and test substance treatments were observed at all test substance concentrations. Following is a summary of the results. Treatment Respiration Rate Percent mg 02/L/hour Inhibition Control 1 Control 2 3,5-dichlorophenol 3 mg/L 3,5-dichlorophenol 15 mg/L 3,5-dichlorophenol 50 mg/L Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) 0.87 mg a.i./L Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) 2.6 mg a.i./L Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) 8.7mg a.i./L Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) 26 mg a.i./L Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) 87 mg a.i./L Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) 260 mg a.i./L Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) 870 mg a.i./L 39.6 41.1 31.3 14.6 5.1 38.9 35.1 33.5 37.9 32.7 28.1 24.7 NA NA 22.9 63.8 87.4 3.6 13.0 17.0 6.1 19.0 30.4 38.8 Wildlife International. Ltd.______ -3 - CERTIFICATE OF ANALYSIS Project Number 454E-101 INTERIM CERTIFICATE OF ANALYSIS R evision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-018A 3M Product: PFOS,Lot217 Reference#: SD-018 Puritv: 86.9% Identification NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium3 5. Nickel 6. Iron 7. Manganese Total % Imparity (NMR) Total % Impurity (LC/MS) Total % impurity (GC/MS> Related Compounds POAA Residual Solvents (TG) Purity by DSC Inorganic Anions (IC) 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5 Nitrite 6. Phosphate 7. Sulfate* Organic A d d s 5 (IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Elemental Analysis*; 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine ' "'*T "1. "" UM r % ik^'............ ......... ...........v,,............ '. 1 , " -J : SSPI^'is 5AS V~' 1 1 *' V JL. ^ f r r w TMf Sw.H*w *.:.=*$r5-si,. tab # vf* A/ .p**. Wb : *Ktt,mV,,m j $v>,, , adwwigggjwimnlwaahnwaa*^^ 1. Theoretical Value = 17,8% 2. Theoretical Value = 0% 3. Theoretical Value * 0% 4. Theoretical Value - 5.95% 5. Theoretical V alue 60% Positive 0.005 wt./wt,% 0.001 wt./wt.% 1.439 wt.Avt.% 6.849 wt/vrt.% <0.001 wt.Avt.% 0.005 wt/wt.% <0.001 wt.Avt.% 1.93 wt./wt.% 8.41 wt./wt.% None Detected 0.33 wt.Awt.% None Detected Not Applicable3 1. <0.015 wtAvt.% 2. 0.59 wt.Avt.% 3. <0.040 wtVwt.% 4. <0.009 wt./wt.% 5. <0.006 wt.Avt.% 6. <0.007 wt.Avt.% 7. 8.76 wt./wt.% 1. <0.1 wtAvt.% 2. <0.1 wtAvt.% 3. 0.10 wt.Avt.% 4. 0.28 wt.Avt.% 1. 12.48 wt.Avt.% 2. 0.244 wt.Avt.% 3. 1.74 wt./wt.% 4. 8.84 wt.Avt.% 5. 54.1 wt.Avt.% COA023-018A Page 1 of 3 Wildlife International, Ltd. -4 - Project Number 454E-101 INTERIM CERTIFICATE OF ANALYSIS Centre Analytical Laboratories COA Reference #: 023-018A Date o f Last Analysis: 08/31/00 Expiration Date: 08/31/01 Storage Conditions: Frozen <-10C Re-assessment Date: 08/31/01 `Purity 100% - (sum o f metal impurities, 1.45% +LC/MS impurities, 8.41%+Inorganic Fluoride, 0.59%+NMR impurities, 1,93%+organic acid impurities, 0.38%+POAA, 0.33%) Total impurity from all tests = 13.09% Purity = 100% - 13.09% 86.9% 2Potassium is expected in this salt form and is therefore not considered an impurity. 'Purity by DSC is generally not applicable to materials o f low purity. No endotherm was observed for tins sample. 4Suliur in the sample appears to be converted to SO* and hence detected using the inorganic anion method conditions. The anion result agrees well with the sul&r determination in the elemental analysis, lending confidence to this interpretation. Based on the results, the SO4 is not considered an impurity.5 5TFA HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoic add Pentafluoropropanoic add ^Theoretical value calculations based on the empirical formula, CsFnSOjTC* (MW=53 8) This work was conducted under EPA Good Laboratory Practice Standards (40 C F R 160). i COAO23-0I8A Page 2 of 3 Wildlife International. Ltd. -5 - Project Number 454E-101 INTERIM CERTIFICATE OF ANALYSIS Centre Analytical Laboratories COA Reference #: 023-018A LC/MS Purity Profile: Im purity C4 C5 C6 C7 Total Wt/wL % . 1:22 1.33 4.72 1.14 8,41 Note: The C4 and C6 values were calculated using the C4 and C6 standard calibration curves, respectively. The C5 value was calculated using the average response factors from the C4 and C6 standard curves. Likewise, the C7 value was calculated using the average response factors from the C6 and C8 standard curves. Prepared By: ______________________________ David S.BeU ____ _ Date Scientist, Centre Analytical Laboratories Reviewed By: _______________________ ________ ____ John Flaherty Date Laboratory Manager, Centre Analytical Laboratories COAO23-018A Page 3 o f3 ildlife International, Ltd. ECO TO XICOLOG Y & ANALYTICAL TESTING SERVICES December 1,2000 Ms. Susan A. Beach 3M Corporation Environmental Laboratory 935 Bush Avenue St. Paul, Minnesota 55144 Dear Susan: Enclosed please fmd the Addendum for the following study: 1 PFOS: An Activated Sludge, Respiration Inhibition Test Wildlife International, Ltd. Project No,: 454E-101 If you have any questions, please let me know. Sincerely, KRD/cyw8/beach Enclosures Edward C. Schaefer Manager, Biodegradation 8598 Com m erce Drive Easton, Maryland 21601 -Tel.410-822-8600 Fax 4 10-822-0632 E-mail ecotoxftwildlifeintemational.com European Office: Bergkampweg I 7231 CL Wamsveld The Netherlands Tel. 3 1(0) 575 - 573848 - Fax 3 1(0) 575 - 574813 E-mail: aleopold@worldonline.nl