Document jB27g12YE7EgYyRKYb29qYDq9

A&ZZb-f 7S W ild li fe International, Ltd.______________ __ _________Project Number 454A-108 - 1- PFOS: AN EARLY LIFE-STAGE TOXICITY TEST WITH THE FATHEAD MINNOW (.Pimephales promelas) ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-108 3M LAB REQUEST NO. U2723 U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines OPPTS Number 850.1400 and OECD Guideline 210 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. W ildlife International. Ltd.__________________________ Project Number 454A-108 - 2- REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9% SPONSOR: SPONSOR'S REPRESENTATIVE: 3M Corporation Susan A. Beach LOCATION OF STUDY, RAW DATA AND A COPY OF THE FINAL REPORT: Wildlife International Ltd. Easton, Maryland 21601 WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY: NOMINAL TEST CONCENTRATIONS: MEAN MEASURED TEST CONCENTRATIONS: TEST DATES: LENGTH OF TEST: 454A-108 PFOS (Perfluorooctane Sulfonic Acid Potassium Salt) PFOS: An Early Life-Stage Toxicity Test with the Fathead Minnow (Pimephales promelas) Negative Control, 0.13, 0.28, 0.55, 1.1, 2.2 and 4.4 mga.i./L Negative Control, 0.14, 0.29, 0.58, 1.2, 2.3 and 4.4 mg a.i./L Experimental Start - August 5, 1999 Biological Termination - September 21, 1999 Experimental Termination - September 22, 1999 47 Days TEST ORGANISM: SOURCE OF TEST ORGANISMS: AGE OF TEST ORGANISMS: Fathead Minnow {Pimephales promelas) Wildlife International Ltd. Cultures Easton, Maryland 21601 Eggs <24 hours old at test initiation NO-OBSERVED-EFFECTCONCENTRATION: LOWEST-OBSERVED-EFFECTCONCENTRATTON: MAXIMUM ACCEPTABLE TOXICANT CONCENTRATION: 0.29 mg a.i./L 0.58 mg a.i./L 0.41 mga.i./L Wildlife International. Ltd. -3 - CERTIFICATE OF ANALYSIS Project Number 454A-108 INTERIM CERTIFICATE OFANALYSIS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-018A 3M Product: PFOS, Lot 217 Reference #: SD-018 __________ ______ Purity: 86.9%_____ _________ _ Test Name Specifications Purity1 Result 86.9% 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 White Crystalline Powder ' .............................. '.............. , , '....s,............ ' > \ s: v . ,<-', ` ', , k -- " 7' '> i ' S*, : W i 3 B i l i i i l f 'JY '- ' ' .............x . ..................................................... Si ;:ii! i l i i S ifllillliilitelif!?!i lyil.i-ri-iW:::}'1'' - ----- `' ^... .........' ..?.........................------ X.......................... ' 1. Theoretical Value = 17.8% 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4. Theoretical Value = 5.95% 5. Theoretical Value = 60% Conforms Positive 1. 0.005 wt./wt.% 2. 0.001 wt./wt.% 3. 1.439 wt/wt.% 4. 6.849 wt./wt.% 5. <0.001 wt./wt.% 6. 0.005 wt./wt.% 7. <0.001 wt,/wt.% 1.93 wt./wt.% 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. <0.1 wt/wt.% 3. 0.10 wt/wt.% 4. 0,28 wt/wt.% 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.% COA023-018A Page 1 of 3 INTERIM CERTIFICA TE OF ANAL YSIS 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. 3Purity by DSC is generally not applicable to materials o f low purity. N o endotherm was observed for this sample. 4Sulfixr 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 sulfhr determination in the elemental analysis, lending confidence to this interpretation. Based on the results, the SO4 is not considered an impurity.56 5TFA HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid 6Theoretical value calculations based on the empirical formula, CsFnSOa'K4 (MW=538) This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). COA023-018A Page 2 o f 3 INTERIM CERTIFICATE OFANALYSIS C entre Analytical Laboratories COA Reference #: 023-018A LC/MS Purity Profile: m ' / / C51 . ' 7; 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, th e 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 C o m m e rce D rive Easton, Maryland 21601 Tel. 410-822-8600 Fax 410-822-0632 E-mail ecotox0wildlifeinternational.com European Office: Overscheenseweg IIA 1412AA Naarden -The Netherlands -Tel. 31(0)356949261 Fax 31(0)356948229 E-mail aleopold@worldonline.nl