Document zo06evZomwYV8J58EEE1q3X27

Wildlife International, Ltd. -1- ,ro_o_ Number 454A-102 PFOS: A 96-HOUR STATIC ACUTE TOXICITY TEST WITH THE FATHEAD MINNOW (Pimephales promelas) ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-102 3M LAB REQUEST NO. U2723 U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines OPPTS Number 850.1075 and OECD Guideline 203 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. Wildlife International, Ltd. -2- P oi Number4 , REVISED STUDY SUMMARY BASED ONA PURITY OF 86.9% sPoNs6R: SPONSOR'S REPRESENTATIVE: 3M Corporation Ms. Susan A. Beach LOCATION OF STUDY, RAW DATA AND A COPY OF THE FINAL REPORT: WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY: MEANMEASUREDTEST CONCENTRATIONS: TESTDATES: LENGTH OF TEST: Wildlife International Ltd. Easton, Maryland 21601 454A- 102 PFOS (Perfluorooctane Sulfonic Acid Potassium Sal0 PFOS: A 96-Hour Static Acute Toxicity Test with the Fathead Minnow (Pimephales promelas) Negative Control, 3.2, 5.4, 9.1, 16 and 27 mg a.i./L Experimental Start - February 15, 1999 Biological Termination - February 19, 1999 Experimental Termination - February 19, 1999 96 Hours TESTORGANISM: SOURCEOF TESTORGANISMS: Fathead Minnow (Pimephales promelas) Wildlife International Ltd. cultures Easton, Maryland 21601 AGE OF TEST ORGANISMS: MEASUREMENTS OF 10 NEGATIVE CONTROL FISH: WEIGHT (g): TOTALLENGTH(ram): Juveniles Mean = 0.36; Mean = 35; Range = 0.21 to 0.49 Range = 30 to 38 96-HOURLC50: 95% CONFIDENCLEIM1TS": NO MORTALITY CONCENTRATION: NO-OBSERVED-EFFECT- CONCENTRATION: 9.1 mg a.i./L 7.7 and 11 mg a.i./L 3.2 mg a.i./L 3.2 mg a.i./L | Wildlife International, Ltd. -3- CERTIFICATE OF ANALYSIS _ro__ _-,o_ INTERIM CER TIFiCA TE OF ANAL YSIS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-018A 3M Product: PFOS, Lot 217 Reference #: SD-018 :Purity: 86.9% IIII I Test Name Specifications Result Purity _ Appearance Identification NMR 86.9% White Crystalline Powder Conforms ii_?_:._i_:_iii!;_i_i::::_i.i_%_i._-.:i:_i{ii__-:__ti_:.;;___i..z:_;_ii_:._ii-2_____.i_z%i_%?__..i'i:__;ii_ii_::.i:_.:i._:_{_i{_i_:, _;_;_`_._r_;_;`_:_::._:_;_*_`;_...:_._i.._.__;_t_m_-;._:.:_:_:::_._::_Positive 1. Calcium 3. Sodium 4. Potassium _ 5. Nickel 6. Iron _._._;_;_;;_[_;_*_;_*_ 1. 0.005wt./wt.% 3. 1.439 wt./wt.% 4. 6.849wtJwt.% 5. <0.001 wt./wt.% 6. 0.005wt./wt.% Total % Impurity (NMR) T(LotCal /%MISm)purity Total % Impurity _}___._;_j_[_{_ iliiii!}iiiiiiiliiliiilili ii!!!iili}ii}l!lii!!i!!i[!!ii[ii!iii}!ii!ii[i i!!!iiiii[f!ii!liililiii :::::::::::::::::::::::::::::::::::::::::: 1.93 wt./wt.% 8.41 Wt./Wt.% None Detected Related Compounds POAA '-i_esidual Solvents (TGA) 0.33 wt./wt.% None Detected 1. Chloride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate * iii_iiiii_iiiii:ii!iii_ii1.i<_0.0i15iw_t./w!t.%i_i!iiii :::::::::::::::::::.:::::_:::_:::_::_::-::_::_::-,::__:;:::_.:_:::,.:i,__:-_::_.:-__::__.,:_,_:,_:,_:;;:_;-_':;_,:_,:-,_:-::_-:__;:_2<.._-:_0;.:5_9:_w:-:t_./wt.% 3. <0.040wt./wt.% 4. <0.009 wt./wt.% _;_m_;_._._._;_r_._._:_:_:_.;.__.._::r__;.-_._:_-;__: _:_:_:_:_:_:_:_:_:_:_:5_.;_:<_0m.0_0r_6._w;_t./wt.% i_{_!:::.:_F_E_:._D_:._._!_>_:._${_?_T:_:?:;:_::>::_::y::_:.:.:_::.:i:!:.:::_::.r::::::i::i::i:S::;::i::_:::_: $i:i_:i:i(;'i_i_:/:_:_(.!:_;$1:i:'_!: _._._*_r_._:_:_:_;_:_:_:_:__::__::__*:_::;_:_:_.'_:_:_:_._._`;_.;_._;6_. <0.007 wt./wt.% 7. 8.76 wt./wt.% 3. HFBA 4. NFPA Elemental AnalysiNg: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine COA023-O18A !{i!!i!ii!ii!!iiii!iiii{!!!iil 2. <0.1 wt./wt.% :_i_!_i_!_}__:.:_:i:__::__::_,i_:i:__:_i:__,_i:_:__:::._-:._:_:_:_:_:_,_:::_:_:_:_:_:_:_:_:_ 3. 0.10 wt./wt.% ...................................... 4. 0.28wt./wt.% 1. Theoretical Value = 17.8% 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4. Theoretical Value = 5.95% 5. Theoretical Value = 60% 1. 12.48 wt./wt.% 2. 0.244 wt./wt.% 3. 1.74.wt./wt.% 4. 8.84 wt./wt.% 5. 54.1 wt./wt.% Page 1 of 3 INTERIM CERTIFICATE OF ANAL YSIS Centre Analytical Laboratories COA Reference #: 023-018A Date of Last Analysis: 08/31/00 Expiration Date: 08/31/01 Storage Conditions: Frozen t3-10C Re-assessment Date: 08/31/01 XPurity= 100% - (sum of metal impurities, 1.45% +LC/MS impurities, 8.4 l%+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. 3purity by DSC is generally not applicable to materials of low purity. No endotherm was observed for this sample. 4Sulfur in the sample appears to be converted to SO4 and hence detected using the inorganic anion method conditions. The anion result agrees well with the sulfur determination in the elemental analysis, lending confidence to this interpretation. Based on the results, the SO4 is not considered an impurity. 5TFA HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoie acid Pentafluoropropanoic acid 6Theoretical value calculations based on the empirical formula, CsF17SO3-K+(MW=538) This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). COA023-018A Page2 of3 INTERIM CERTIFICATE OF ANAL YSIS Centre Analytical Laboratories COA Reference #: 023-018A LC/MS Purity Profile: Impurity C4 C5 C6 C7 Total wt./wt. % 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. Bell Date Scientist, Centre Analytical Laboratories Reviewed By: John Flaherty Date Laboratory Manager, Centre Analytical Laboratories COA023-018A Page3 of3 I Idlife International, Ltd. COTOXICOLOGY & ANALYTICAL TESTING SERVICES September 27, 2000 Ms. Susan A. Beach 3M Corporation Environmental Laboratory 935 Bush Avenue 3M Building 2-3E-09 P.O. Box 33331 St. Paul, Minnesota 55133 Dear Susan: Enclosed please fred Addendums for Wildlife International, Ltd. Project Numbers 454A-101, 454A-102, 454A-103A, 54A-104,, 454A-105,454A-106, 454A-107, 454A-108 and 454A-109 If you have any questions, please let me know. KILD/cywgt'3m Enclosures Kurt R. lN'ottar Senior Biologist 8598 Commerce Drive Easton, Maryland 21601 -Tel.410-822-8600 - Fax 410-822-0632 - E-mail ecotox@wildlifeinternational.com EuropeanOffice: OverscheensewegI1A i412AA Naarden-The Netherlands"Tel.31(0)356949261 Fax31(0)356948229 E-mailaleopold@worldonline.nl