Document 7ZMEbRYBx14V3Ndr3DE3Y0K8

-AflUlo- Wildlife International, Ltd. -1 - Project Number 454C-107 DETERMINATION OF THE W ATER SOLUBILITY OF PFOS BY THE SHAKE FLASK METHOD ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUM BER: 454C -107 3M LAB REQUEST NO. U2723 OECD Guideline for the Testing o f Chem icals, 105 W ater Solubility This study w as originally reported using a test substance purity o f 98.9% . T he test substance characterization w as 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 most recent purity analyses. The measured concentrations originally reported were sim ply corrected by the ratio o f the tw o purities, or a factor o f 0.8787. N o attempt was made to recalculate analytical standard concentrations. A s 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-107 R E V ISED STU D Y SU M M A R Y B A SED O N A PU R IT Y O F 86.9% STUDY TITLE: | WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: SPONSOR: TESTING FACILITY: LOCATION OF STUDY, RAW DATA AND A COPY OF THE FINAL REPORT: Determination o f the W ater Solubility o f PFOS by the Shake Flask Method 454C -107 3M Corporation W ildlife International Ltd. Easton, Maryland 21601 W ildlife International Ltd. Easton, Maryland 21601 TEST SUBSTANCE: TEST DATES: PFOS Experimental Start - February 11, 1999 Experimental Termination - February 20, 1999 TEST SYSTEM: NANO pure W ater Z3 The overall mean solubility concentration o f PFOS in NANOpure water was | 498 mg a.i./L (SD = 46.4; CV = 9.32% ; N = 6). ISS B H B B B B a SS SS-- Wildlife International. Ltd. -3 - Project Number 454C-107 CERTIFICATE OF ANALYSIS INTERIM CERTIFICATE OF ANALYSIS Revision 1(9/7/00) C entre A nalytical L aboratories COA Reference #: 023-018A 3M Product: PFO S,L ot217 Reference#: SD-018 ________ ________Purity: 86.9%____________ Test Name Specifications Purity1 ; - 4'S IU" ^ > Result 86.9% Appearance Identification White Crystalline Powder Conforms NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium3 5; Nicket 6. In 7. Manganese ^ "* 5 *. * r , *: 1 i '* t * ' i p gf ,* t" * "l* ` - , 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.% Total % Impurity (NMR) ' ` ' .V W ) < " 4 1.93 wt/wt.% Total % Impurity (LC/MS) Total % Impurity (GC/MS) Related Compounds POAA Residual Solvents (TGA) Purityby DSC Inorganic Anions (IC) 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate" u,/. , . t . v .1 IJ",1 3 . ............ ................ ^ f-a,- 8.41 wt/wt.% None Detected 0.33 wt/wt.% None Detected Not Applicable* 1. <0.015 wt/wt% 2. 0.59 wt/wt% 3. <0.040wt/wt% 4. <0.009 wt/wt% 5. <0.006 wt/wt% 6. <0.007 wt/wt% 7. 8.76 wt/wt% Organic Addss (IQ 1. TFA 2. PFPA 3. HFBA 4. NFPA fM a*'T' Tt '`*'^ * *- - . ,*8.8*1 ' ^ ' 1. <0.1 wt/wt% 2. <0.1 wt/wt.% 3. 0.10wt/wt% 4. 0.28 wt/wt.% Elemental Analysis*: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine 1. Theoretical Value= 17.8% 2. Theoretical Value= 0% 3. Theoretical Value = 0% 4. Theoretical Value - 5.95% 5. Theoretical Value = 60% 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-O18A Page I of 3 Wildlife International. Ltd. -4 - Project Number 454C-107 INTERIM CERTIFICATE OF ANALYSIS C entre A nalytical L aboratories CO A R eference #: 023-018A D ate o f Last Analysis: 08/31/00 Expiration Date: 08/31/01 Storage Conditions: Frozen <-10C Re-assessment Date: 08/31/01 lPurity = 100% - (sum o f metal impurities, 1.45% +LC/MS impurities, 8.41% +Inorganic Fluoride, 0.59% +NM R impurities, 1.93% +organic acid 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. 5Purity by DSC is generally not applicable to materials o f low purity. No endotherm was observed for tins sample. ''Sulfur in the sample appears to be converted to SO4 and hence detected using the inorganic anion method conditions. The anion result agrees well w ith the sulfur determ ination in the elemental analysis, lending confidence to tins interpretation. Based on the results, the SO* is not considered an impurity. JTFA HFBA NFPA PFPA Trifluoroacetic add H eptafluorobutyric ad d N onofluoropentanoic ad d Pentafluoropropanoic ad d `Theoretical value calculations based on the empirical formula, C*FnS03X +(MW =538) This w ork was conducted under SPA Good Laboratory Practice Standards (40 C F R 160). ( COA023-OI8A Page 2 of 3 Wildlife International, Ltd. -5 - Project Number 454C-107 INTER1M CERTIFICATE OF ANALYSIS C en tre A nalytical L aboratories COA R eference #: G23-018A LC/MS Purity Profile: v:v Im purity , C4 CS C6 .itbr . W t/W t.% A S f ' 1.33 4.72 1.14 8.41 N ote: The C 4and 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; _ _ _ _ _ _ _ _ _________________ ____ ! David S. Bell D ate Scientist, Centre Analytical Laboratories Reviewed By. ______________________ [______ ____ John Flaherty D ate Laboratory Manager, Centre Analytical Laboratories COA23-018A Page 3 of 3 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, M innesota 55133 Dear Susan: Enclosed please find Addendums for the following studies: 1. Non-GLP Study: Determination of the Solubility of PFOS in Wildlife International, Ltd. Freshwater, Freshwater Algal Medium, and Sa l t w a t e r Wildlife International, Ltd. Project No.: 454C-101-1 3m Lab Request No. U2723 2. Determination of the Water Solubility of PFOS by the Shake Flask Method Wildlife International, Ltd. Project No.: 454C-107 3m Lab Request No. U2723 If you have any questions, please let m e know. RLV/cyw8/3m Enclosures Raymond L. Van Hoven, Ph.D. Scientist 8598 Com m erce Drive Easton, Maryland 21601 -Tel.410-822-8600 Fax 4 10-822-0632 E-mail ecotOx0wildlifeintemational.com European Office:Bergkampweg 1-7231 CLWamsveld The Netherlands -Tel. 3 1(0)575 - 573848 - Fax 3 1(0)575 - 574813 E-mail: aleopold@worldonline.nl