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,I Wildlife International, Ltd. P o e umbor4 4 PFOS: A 48-HOUR STATIC ACUTE TOXICITY TEST WITH THE CLADOCERAN (Daphnia magna) ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-104 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. Wildlife International, Ltd. -2- Proje Numb r4 4A- REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9% SPONSOR: SPONSOR'S REPPRESENTATIVE: LOCATIONOF STUDY, RAW DATAAND A COPY OF THE FINALREPORT: 3M Corporation Ms. Susan A. Beach Wildlife International Ltd. Easton, Maryland 21601 WILDLIFEINTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY: MEAN MEASURED TEST CONCENTRATIONS: TEST DATES: LENGTH OF TEST: 454A-104 PFOS (Perfluorooetane Sulfonic Acid Potassium Salt) PFOS: A 48-Hour Static Acute Toxicity Test with the Cladoeeran (Daphnia magna) Negative Control, 11, 19, 32, 54 and 87 mg a.i./L Experimental Start - February 16, 1999 Biological Termination - February 18, 1999 Experimental Termination - February 18, 1999 48 Hours TEST ORGANISM: SOURCEOF TEST ORGANISMS: AGE OF TEST ORGANISMS: Neonate cladocerans (Daphnia magna) Wildlife International Ltd. Cultures Easton, Maryland 21601 < 24 hours at test initiation 48-HOUR EC50: 95% CONFIDENCELIMITS: NO MORTALITY/IMMOBE2TY CONCEI,_]LATION: NO-OBSERVED-EFFECTCONCENTRATION: 59 nag a.i./L 32 and 87 mg a.i./L 32 mg a.i./L 32 nag a.i./L . Wildlife International, Ltd. -3- CERTIFICATE OF ANALYSIS proiNeumcbter454A-104 INTERIM CERTIFICATE OF ANAL YSIS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-018A 3M Product: PFOS, Lot 217 Reference #: SD-018 Test Name Purity: 86.9% Specifications Purity 1 Appearance i White Crystalline Powder Result 86.9% Conforms NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium 2 5. Nickel 6. Iron 7. Manganese Total % Impurity (NMR) _,_s_,_ Total % Impurity (GC/MS) Related Compounds - POAA Residual Solvents (TGA) Purity by DSC ,. Positive _ _i__:i__ r_ ::::::::::::::::::::::-:::::::::::::::::::::::::: , i iii 1. 0.005wt./wt.% 2. 0.001wt./wt.% 3. 1.439 wt./wt.% 4. 6.849wt./wt.% 5. <0.001wt./wt.% 6. 0.005wt./wt.% 7. <0.001wt./wt.% i::ili_ji_ii::_iii_i:iziiiiiiii_i!ii_i!:i:iiiiiii_i!iii!_ii:i!!__::ii_!ii_!ii_iii_i_i_i_iii_ii!!:_i_1ii._9i3i_w!it!.i/_wiit_.%i_ii_i_i_i!ii!_!_._i!_:i_ ii!iiii!ii!iiiii!ii!!i!i!i:ili!lii!iiiliii!i:i!iiifiiliili!iii!_i_4!i1l_,_. .........;.:..:.:.;.:._..:.:.;.:_.:!.:: None Detected _:_:_;_:_:_:_:::_:_:_:_::;:_:_:_:_:_;_:::::_:_:_:_:_:_:_:::_:_:_:_0:._3;3:_w::t:._/w:;:t_.%:;:;_::_:_:_::_:._.:::.:.:_` _.;.z.:._._._._._:._._::_;;:._..;.:..:.:.._...._..:.._..:.:..._....:.:..:.._..:.:.:._..:._.:.;:..:_.:.:._:.:.:._:.:.::.::.::._.:.:.:_.:.:.N:_.:..:o_..n.:.e_. Detected Not Applicable 3 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate 4 Organic Acids _(IC) 1. <0.015wt./wt.% 2. 0.59 wt./wt.% 3. <0.040wt./wt.% 4. <0.009wt./wt.% 5. <0.006 wt./wt.% _:_:_:-:_:i_:!i:i_:i:i:_:i_::__:_r.:-i:ii_:ii_i_:_,,:_,_:_,_.,..:_:i: 6. <0.007 wt./wt.% 7. 8.76 wt./wt.% _:_:!:::_i!:_":_:'_.':.::_.::.:_.::_._::._.:.[:.;;.:.__.:_.:r.:_::.::_.::::._:.:[::.[::_:.:'::..[_:.:_:'.::.:.'::.:_.'::.:.:_.:._..:.'.:.:..:.::.:_.:.::._:...i.l._.:.::.::.::.::.:.::.::.::.::.:.::.::.::.::.:.::_.::.:':.::;.'::.: .:i.::.::.:.::...'..,.::.::.::.:.::................................................................. 2 PrPa 4. NFPA Elemental Analysis_: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine _M_____ 1. Theoretical Value = 17.8% 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4. Theoretical Value = 5.95% 5. Theoretical Value = 60% 2 <0._./_.% 4. 0.28wt./wt.% 1. 12.48 wt./wt.% 2. 0.244 wt./wt.% 3. 1.74wt./wt.% 4. 8.84 wt./wt.% 5. 54.1 wt./wt.% COA023-018A Page 1of 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 D-10C Re-assessment Date: 08/31/01 1Purity = 100% - (sum of metal impurities, 1.45% +LC/MS impurities, 8.41%+Inorganic Fluofide, 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 Nonofluoropentanoic acid Pentafluoropropanoic acid 6Theoretical value calculations based on the empirical formula, CgF17SO3"K +(1VIW=538) This work was conducted under EPA Good Laboratory Practice Standards (40 CFP,,160). COA023-018A Page2 of 3 11 INTERIM CER TIFICA TE OF ANAL YSIS Centre Analytical Laboratories COA Reference #: 023-018A LC/MS Purity Profile: Impurity C4 C5 C6 C7 Total wL/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 of 3 I w tat "re t International Ltd. ECOTOXICOLOGY & 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 Addendurns 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. Sincerely, -. /_ Kurt R. Drottar Senior Biologist KRD/eyw8/3m Enclosures 8598CommerceDrive EastonM, aryland21601Tel.410-822-8"600Fax410-822-0632 E-maiel cotox@wildlifeinternational.com EuropeanOffice: OverscheensewegII A i412AA NaardenThe Netherlands-Tel.31(0)356949261 Fax31(0)356948229 E-mailaleopoldeworldonline.nl