Document dYQo39ZNmexprb6dje6Dm1eMQ

Wildlife International, Ltd. - 1- Project Number 454C-101-1 NON-GLP STUDY: DETERM INATION OF THE SOLUBILITY OF PFOS IN W ILDLIFE INTERNATIONAL, LTD. FRESHWATER, FRESHW ATER ALGAL MEDIUM , AND SALTWATER ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUM BER. 454C -101-1 3M LAB REQUEST NO. U2723 This study was reported using a test substance purity o f 98.9% . The test substance characterization was revised on 9/7/00 and the purity w as determined to be 86.9% . The Sponsor requested that the results be revised based on the m ost recent purity analyses. The measured concentrations previously presented were sim ply corrected by the ratio o f the tw o purities or a factor o f 0.8787. N o attempt w as made to recalculate analytical standard concentrations. 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 o f analysis. Wildlife International, Ltd. 2- - Project Number 454C-10I-1 R E V ISED STU DY SUM M ARY 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 Rochelle Robideau W ildlife International, Ltd. Easton, Maryland . | | WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY: 454C -101-1 PFOS Non-GLP Study: Determination o f the Solubility o f PFOS in W ildlife International, Ltd. Freshwater, Freshwater Algal Medium, and Saltwater TEST DATES: Experimental Start - January 8 ,1 9 9 9 Experimental Termination - March 5 ,1 9 9 9 1 TEST SYSTEMS: Freshwater, Freshwater Algal Medium, and Saltwater SUMMARY: The mean solubility concentration o f PFOS in freshwater @ 20 C after a 24 hour shake period w as 326 mg/L 41.9 mg/L (CV = 12.9%; N = 3). The mean solubility concentration o f PFOS in freshwater algal medium @ 20 C after a 24 hour shake period w as 378 mg/L 22.9 mg/L (CV = 6.07% ; N = 3). The mean solubility concentration o f PFOS in saltwater @ 20 C after a 24 hour shake period was 21.8 mg/L 0.510 mg/L (CV = 2.34%; N = 3). Wildlife International, Ltd. -3 - Project Number 454C-101-1 CERTIFICATE OF ANALYSIS 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 ________ Purity; 86.9%______________ Specifications Result Purity* ' X , *' 86.9% Appearance Identification NMR White Crystalline Powder ' * > s ,,,, *x 4 ': Conforms Positive Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium* 5. Nickel 6. Iron 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. Manganese 7. <0.001 wt./vrt.% Total % Impurity (NMR) 1.93 wt/wt.% Total % Impurity (LC/MS) * -' -L - 8.41 wt/wt.% Total % Impurity (GC/MS) None Detected Related Compounds - POAA Residual Solvents (TGA) 033 wt/wt.% None Detected Purity by DSC Not Applicable3 Inorganic Anions (IC) 1. Chloride 2. Fluoride 3. Bromide 1. <0.015 wt/wt% 2. 0.59 wt/wt% 3. <0.040 wt/wt% 4. Nitrate 3. Nitrite 6. Phosphate 7. Sulfite* . 4. <0.009 wt/wt% 5. <0.006 wt/wt% 6. <0.007 wt/wt% 7. 8.76 wt/wt% Organic Acids3(IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Rlemmtn! Anslyin6- 1. <0.1 wt/wt% 2. <0.1 wt/wt.% 3. 0.10 wt/wt% 4. 038 wt/wt.% 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 1 5. Fluorine 1. Theoretical Value= 17.8% 2. Theoretical Value = 0% 3. Theoretical Value *0% 4. Theoretical Value - 5.95% 1 5. Theoretical Value * 60% 1. 12.48 wt/wt.% 2. 0.244 wttot% 3. 1.74 wt/wt.% 4. 8.84 wt/wt% 5. 54.1 wt/wt% COA023-O18A Page 1of3 Wildlife International. Ltd. -4 - Project Number 454C-101-1 INTER1M CERTIFICATE OF ANALYSIS C entre Analytical Laboratories COA Reference #: 023-018A Date of Last Analysis: 08/31/00 Expiration Date: 08/31/01 Storage Conditions: Frozen <-10C Re-assessment Date: 08/31/01 'Purity = 100% - (sum of metal impurities, 1.45% +LC/MS impurities, 8.41%+Inorganic Fluoride, 0.59%+NMR impurities, 1.93%+orgamc add impurities, 0.38%+POAA, 0.33%) . Total impurity from all tests = 13.09% Purity = 100% - 13.09% = 86.9% Potassium is expected in this salt form and is therefore not considered an impurity. P urity by DSC is generally not applicable to materials o f low purity. No endotherm was observed for this sample. ^Sulfur in the sample appears to be converted to SO* 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 tins interpretation. Based on the results, the SO* is not considered an impurity. *TFA HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric add Nonofiuoropentancic add Pentafluoropropanoic add ^Theoretical value calculations based on the empirical formula, CtFnSOjTC (MW=538) This work was conducted under EPA Good Laboratory Practice Standards (40 C FR 160). ( COA023-018A Page 2 of 3 Wildlife International. Ltd. -5 - Project Number 454C-101-1 INTERIM CERTIFICATE OF ANALYSIS C entre Analytical Laboratories COA Reference #: 023-018A LC/MS Purity Profile: Im purity C4 CS C6 C7 T o tal W t/W L % 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 CS 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: ____________________________ ____; DavidS. Bell Date Scientist, Centre Analytical Laboratories Reviewed B y ._____________________ _______ ____ JohnFlaherty Date Laboratory Manager, Centre Analytical Laboratories COA023-O18A Page 3 o f3 ildlife International, Ltd ECOTOXICOLOGY & ANALYTICAL TESTING SERVICES November 27,2000 Ms. Susan A. Beach 3M Corporation Environmental Laboratory 935 Bush Avenue 3M Building 2-3E-09 P .O .B ox 33331 St. Paul, Minnesota 55133 > Dear Susan: Enclosed please find Addendums for the following studies: . 1 Non-G LP St u d y : D e t e r m in a t io n o f t h e S o l u b il it y o f PFO S in W il d l ife I n ter n a tio n a l, L t d . F r e s h w a t e r , F r e sh w a t er A l g a l M ed iu m , and Sa l tw a t er W il d l if e In t er n a t io n a l , L t d . P r o je c t No .: 454C -101-1 3m Lab Request No . U2723 2. De t e r m in a t io n o f t h e W a t e r S o l u b il it y o f P FO S by t h e S h a k e F l a sk Method W il d l ife In t er n a t io n a l, L t d . P r o je c t No .: 454C -107 3m Lab Req uest No. U2723 If you have any questions, please let me know. RLV/cyw8/3m Enclosures Raymond L. Van Hoven, Ph.D. Scientist 8598 Commerce Drive Easton, Maryland 21601 -Tel.410-822-8600 Fax 4 10-822-0632 E-mail ecotox@wildlifeinternational.com European Office: Bergkampweg I 7231 CLWamsveld -The Netherlands -Tel. 3 1(0) 575 - 573848 Fax 3 1(0) 575 - 574813 E-mail: aleopold@woridonline.nl