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Wildlife International, Ltd. "1- Project Number 454A-105 PFOS: A 96-HOUR STATIC ACUTE TOXICITY TEST WITH THE FRESHWATER MUSSEL (Umo complamatus) ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-105 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 puriW 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- REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9% SPONSOR: SPONSOR'S REPRESENTATIVE: LOCATION OF STUDY, RAW DATA AND A COPY OF THE F/NAL REPORT: 3M Corporation Ms. Susan A. Beach Wildlife International Ltd. Easton, Maryland 21601 WILDLIFE_ATIONAL LTD. PROJECT NUMBER: 454A-105 TEST SUBSTANCE: STUDY: MEAN MEASURED TEST CONCENTRATIONS: TEST DATES: LENGTH OF TEST: PFOS (Perfluorooctane Sulfonic Acid Potassium Salt) PFOS: A 96-Hour Static Acute Toxicity Test with the Freshwater Mussel ( Unw complamatus) Negative Control, 5.1, 12, 19, 39 and 76 mg a.i./L Experimental Start - May 28, 1999 Biological Termination - June 1, 1999 Experimental Termination - June 3, 1999 96 Hours TEST ORGANISM: SOURCEOF TEST ORGANISMS: Freshwater Mussel (Unio complamatus) Carolina Biological Supply Company Burlington, North Carolina 27215 AGE OF TEST ORGANISMS: MEASUREMENTS OF 20 REPRESENTATIVEMUSSELS: WET WEIGHT (g): TOTAL LENGTH (ram): Unknown Mean = 76.5; Mean = 48.7; Range = 57.5 to 93.5 Range = 44.6 to 54.9 96-HOUR LC50: 95% CONFIDENCELIMITS: NO-MORTALrI'Y CONCENTRATION: 57 mg a.i./L 49 and 65 mg a.i./L 19 mg a.i./L J Wildlife International, Ltd. -3- CERTI_CATE OFANALYSIS Proiect Number 454A-105 INTERIM CER TIFICA TE OF ANAL YSIS Centre Revision 1(9/7/00) Analytical Laboratories COA Reference 3M Product: PFOS, Lot 217 Reference #: SD-018 #: 023-018A Test Name Purity I Ill Purity: 86.9% Specifications iiii::i:i::ii:i::i:ili::l::li;lii:i:ii:i::i::i::il.:;:ii::?:iiiii::i::i:::ii:::i::iiif:_i:ii:i:ii:i:iii::i:il::i_!!!i::i::,i:ii::i:i:i;iil_.!:::i.::!:i:ii:;::i:!:.i:i:_::iii::i_::i7!i!l_::.:i:.:iiiili:il_ii!il:i:::::iiiii:i!i_!_i:i!_:i:_i__i!._i.:...i.iii.: Result 86.9% Appearance White Crystalline Powder Conforms i_.tN_MR=t_ooi!li;;ii!ii!ii!ii!i_i!iilii!i!ilii!lii!ii!i!ii!i!_!if!iii!i!!i_iil;i_i;iPositive Metals (ICP/MS) 1. Calcium ......:.:.:.:..:.:.:.::,:_:::::_.:.:.:.:._.._:.:.:._.:.::.::.:.::.:i:_,:::!1::.:_ 0.005wt./wt.% 2. Magnesium 2. 0.001wt./wt.% 4. Potassium 2 5. Nickel 6. Iron 7. Manganese Total % Impurity (NMR) o__u._ Total %Impurity (GC/MS) Related Compounds - POAA Residual Solvents (TGA) Purity by DSC 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate 4 Organic Acids 5(IC) 2. PFPA 3. HFBA 4. NFPA Elemental Analysis*: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine : ) 3. 1.439 wt./wt.% 45.. 6<.08.40901wwtt..//wwtt..%% 6. 0.005wt./wt.% 7. <0.001 wt./wt.% 1.93 wt./wt.% iii!iliil!iiiiiiiiiiiii!i!i!i:ii!ii!liii!!ii!ii!ii!iiii:ii!i!i_i!4i_i,:,i_!i:ii!!!! None Detected 0.33 wt./wt.% None Detected iiiiiiii ?iiiiiii ................................................................................................N...o..t...A...p..p..l.icable3 1. <0.015wt./wt.% 2. 0.59 wt./wt.% 3. <0.040 wt./wt.% 4. <0.009 wt./wt.% 5. <0.006wt./wt.% 6. <0.007wt./wt.% 7. 8.76 wt./wt.% _7_J__:__3_:_W_ 2. <0.1 wt./wt.% 3. 0.10wt./wt.% 4. 0.28 wt./wt.% 1. Theoretical Value = 17.8% 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4. Theoretical Value = 5.95% 5. Theoretical Value = 60% I. 12.48 wt./wt.% 2. 0.244 wt./wt.% 3. 1.74 wt./wt.% 4. 8.84 wt./wt.% 5. 54.1 wt./wt.% COA023-018A 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 12-10C Re-assessment Date: 08/31/01 1Purity = 100% - (sum of 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/'0) 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. STFA HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoie acid Pentafluoropropanoic acid 6Theoretical value calculations based on the empirical formula, CsF17SO3"K + (NIW=538) This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). COA023-018A Page 2 of 3 INTERIM CERTIFICATE OF ANAL ISIS 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 Page 3 of 3 J t 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- I05,454A-106, 454A-107, 454A-108 and 454A-109 If you have any questions, please let me know. Sincerely, . _ Kurt R_Drottar Senior Biologist KRD/cywS/3m Enclosures 8598 Commerce Drive - Easton, Maryland 21601 Tel.410-822-8600 Fax 410-822-0632 E-mail ecotox@wildlifeinternational.com EuropeanOffice: OverscheensewegIIA i412AA Naarden-The Netherlands-Tel.31(0)356949261- Fax31(0)356948229 E-rn_laleopold@worldonline.nl