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Wildlife International. Ltd. -1- Project Number 454A-1Q1 PFOS: A 96-HOUR STATIC ACUTE TOXICITY TEST WITH THE SALTWATER MYSID (.Mysidopsis bahia) ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-101 3M LAB REQUEST NO. U2723 U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines OPPTS Number 850.1035 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- - Project Number 454A -101 REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9% SPONSOR: SPONSOR'S REPRESENTATIVE: LOCATION OF STUDY, RAW DATA AND A COPY OF THE FINAL REPORT: 3M Corporation Ms. Susan A. Beach Wildlife International Ltd. Easton, Maryland 21601 WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY: MEAN MEASURED TEST CONCENTRATIONS: TEST DATES: LENGTH OF TEST: 454A-101 PFOS (Perfluorooctane Sulfonic Acid Potassium Salt) PFOS: A 96-Hour Static Acute Toxicity Test with the Saltwater Mysid (Mysidopsis bahia) Negative Control; 0.55, 1.1, 1.8, 2.9 and 5.2 mg a.i./L Experimental Start - March 8,1999 Biological Termination - March 12,1999 Experimental Termination - March 12, 1999 96 Hours TEST ORGANISM: SOURCE OF TEST ORGANISMS: Saltwater Mysid (Mysidopsis bahia) Wildlife International Ltd. cultures Easton, Maryland 21601 AGE OF TEST ORGANISMS: Juveniles 96-HOUR LC50: 95% CONFIDENCE LIMITS: NO MORTALITY CONCENTRATION: NO-OBSERVED-EFFECTCONCENTRAHON: 3.5 mg a.i./L 2.9 and 4.4 mg a.i./L 1.1 mg a.i./L 1.1 mg a.i./L Wildlife International, Ltd. -3 - CERTIFICATE OF ANALYSIS Project Number 454A-101 INTERIM CERTIFICATE OF ANALYSIS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-018A 3M Product: PFOS, Lot 217 Reference #: SD-018 Test Name Purity1 Appearance Identification NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium2 5. Nickel 6. Iron 7. Manganese Total % Impurity (NMR) Total % Impurity (LC/MS) Total % Impurity (GC/MS) Related Compounds POAA Residual Solvents (TGA) Purity by DSC Inorganic Anions (IC) 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate4 Organic Acids 5(IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Elemental Analysis6: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine Specifications White Crystalline Powder 1. Theoretical Value = 17.8% 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4. Theoretical Value = 5.95% 5. Theoretical Value = 60% Result 86.9% Conforms Positive 1. 0.005 wt./wt.% 2. 0.001 wt./wt.% 3. 1.439 wt./wt.% 4. 6.849 wt.Avt.% 5. <0.001 wt./wt.% 6. 0.005 wt./wt.% 7. <0.001 wt./wt.% 1.93 wt./vvt.% 8.41 wt./wt.% None Detected 0.33 wt./wt.% None Detected Not Applicable3 1. <0.015 wt./wt.% 2. 0.59 wt./wt.% 3. <0.040 wt./wt.% 4. <0.009 wt./wt.% 5. <0.006 wt./wt.% 6. <0.007 wt./wt.% 7. 8.76 wt./wt.% 1. <0.1 wt./wt.% 2. <0.1wt./wt.% 3. 0.10wt./wt.% 4. 0.28 vvt./wt.% 1. 12.48 wt./wt.% 2. 0.244 vvt./wt.% 3. 1.74wt./wt.% 4. 8.84 wt./wt.% 5. 54.1wt./wt.% COA023-018A Page 1 of 3 INTERIM CERTIFICATE OF ANALYSIS Centre Analytical Laboratories COA Reference #: 023-018A Date of Last Analysis: 08/31/00 Expiration Date: 08/31/01 Storage Conditions: Frozen D-10oC 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. 3Purity by DSC is generally not applicable to materials o f 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.5 5TFA HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid th eo retical value calculations based on the empirical formula, C8FnS03"K+(MW=538) This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). COA023-018A Page 2 of 3 INTERIM CERTIFICATE OF ANALYSIS Centre Analytical Laboratories COA Reference #: 023-018A LC/MS Purity Profile: Im purity C4 C5 C6 C7 Total wt./Svt. % 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 ildlife 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 find 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. KRD/cyw8/3m Enclosures Senior Biologist 8598 Com m erce D rive Easton, M aryland 21601 -Tel.410-822-8600 Fax 410-822-0632 E-mail ecotox@wildlifeinternational.com European O ffice: O verscheensew eg 11A - 1412 A A N aard en -The N eth erland s -Tel. 3 1(0)356949261 Fax 3 1(0)356948229 - E-mail aleopoldQ w orldonline.nl