Document DR452o7RN2jXJJ89B6rR4N4d

-422r 1*7 Wildlife International, Ltd. Project Number 454A-109 -1 - PFOS: A SEMI-STATIC LIFE-CYCLE TOXICITY TEST WITH THE CLADOCERAN {Daphnia magna) ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-109 3M LAB REQUEST NO. U2723 U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines OPPTS Number 850.1300 and OECD Guideline 211 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 basal 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 die final report and the most recent certificate o f analysis. Wildlife International. Ltd.____________________________Project Number 454A-1Q9 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 FINAL REPORT: 3M Corporation Susan A. Beach 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: TEST ORGANISM: SOURCE OF TEST ORGANISMS: AGE OF TEST ORGANISMS: I NOEC: LOEC: 1 MATC: 454A-109 PFOS (Perfluorooctane Sulfonic Acid Potassium Salt) PFOS: A Semi-Static Life-Cycle Toxicity Test with the Cladoceran (Daphnia magna) Negative Control, 1.3, 2.8, 5.5,11, 22 and 44 mg a.i./L Negative Control, 1.4, 2.8, 5.4, 12, 23 and 46 mg a.i./L Experimental S tart-Ju ly 12, 1999 Biological Termination - August 2, 1999 Experimental Termination - August 4, 1999 21 Days Neonate Cladocerans (Daphnia magna) Wildlife International Ltd. cultures Easton, Maryland 21601 Juveniles < 24 hours old 12 mg a.i./L 23 mg a.i./L 17 mg a.i./L Wildlife International, Ltd. -3 - CERTIFICATE OF ANALYSIS Project Number 454A-1Q9 INTERIM CERTIFICATE OF ANALYSIS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-018A 3M Product: PFO S,Lot217 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 A cids5 (IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Elemental Analysis6: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine White Crystalline Powder ' N illllif ' % J*> >*' - **S *w\ v '' V: *<.>,x t ^ f || iif iijj:i; ' ' : ' " ...... *"<' ........ ........4........................... lllllllllll $xVx:: !::ii::WM:'i:#\V:v: i::': :::::::. '' > 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.Avt.% 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 vvt./wt.% 6. <0.007 wt./wt.% 7. 8.76wt./wt.% 1. <0.1 wt./wt.% 2. <0.1wt./wt.% 3. 0.10wt./wt.% 4. 0.28 wt./wt.% 1. 12.48 wt./wt.% 2. 0.244 wt./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 o f Last Analysis: 08/31/00 Expiration Date: 08/31/0.1 Storage Conditions: Frozen D-10C Re-assessment Date: 08/31/01 Purity = 100% - (sum o f metal impurities, 1.45% +LC/MS impurities, 8.41%+Inorganic Fluoride, 0.5 9%+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. 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.56 5TFA HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid 6Theoretical value calculations based on the empirical formula, CgFi7S03'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: 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 ildlife International, Ltd. ECO TO X ICO LO G Y & 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 Drive Easton, Maryland 21601 Tel. 410-822-8600 Fax 4 10-822-0632 - E-mail ecotox@wildlifeinternational.com European Office: Overscheenseweg II A 1412 A A Naarden -The Netherlands -Tel. 31(0)356949261 Fax 31(0)356948229 - E-mail aleopold@worldonline.nl