Document YGwJGR8J9811z02n8oNvK8jGy

li Wildlife International, Ltd. -1- ProiectNumber454A.101 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 rotmding may be present: Attached is the revised summary page from the final report and the most recent certificate of analysis. " Wildlfe International, Ltd. -2" PrqjectNumber454A-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 WILDLIFEINTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY: MEAN MEASURED TEST CONCENTRATIONS: TEST DATES: LENGTH OF TEST: ,=, TEST ORGANISM: SOURCE OF TEST ORGANISMS: 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, 1.8, 2.9 and 5.2 mg a.i./L Experimental Start - March 8, 1999 Biological Termination - March 12, 1999 Experimental Terrnmation- March 12, 1999 96 Hours ,, , ,J,_J_l,, 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-EFFECTCONCENTRATION: 3.5 mg a.i./L 2.9 and 4.4 mg a.i./L 1.1 nag a.i./L 1.1 ra_ a.i./L " Wildlife International, Ltd. CERTI_CATE OF ANALYSIS ProjNeuctmgb5e4rA-101 INTERIM CERTIFICATE OF ANAL YSIS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-018A 3M Product: PFOS, Lot 217 Reference #: SD-018 Test Name Purity 1 Purity: 86.9% Specifications Result _iiii_iii.i!ii_i_!ii_!_i:_iii_!!i_!_!!i_ii!i_::ii_iii__i!i!i_:iiii.:!ii_i_!i.:_-i_!:q.i__ii.i_liii_iii:_:38ii?6_:.i!9{!%_i_ Appearance Identification NMR White Crystalline Powder i!!:!__;!,::!!_::!:!._!:!!_:i:i!:?_._ii__?-i?_t;!-!'!-:!:_!i!___-::(!'!:E}i:_!i::_i_!:_::!:!!_i.i:i_i:i_!_ii_i:_-_:i_::iii_:i!i!i_!:E!::_.!:!:-.i___."-_.!'_:_i::_iiY!i "i::_!-__!:_;,:!____ Conforms Positive Metals (ICP/MS) 1. Calcium 1. 0.005wt./wt.% 2. Magnesium 3. Sodium 2. 0.001 wt./wt.% 3. 1.439 wt./w.% 4. Potassium 2 5. Nickel 4. 6.849wt./wt.% 5. <0.001wt./wt.% 6. Iron 6. 0.005wt./wt.% 7. Manganese 7. <0.001wt./wt.% Total % Impurity (NMR) Total % Impurity (LC/M S) 1.93 wt./wt.% !_! :!"!-:.!i:_si:_.!::;i!:;!.!:i!::!.ui!.:i:,i:._i!f!si:!:;iiX_!i!-!:S:i!i.i!:i!_i;i_i!:-___i::i__:-_u:i_:ii;i_.__:__:d: -ia 8.41 wt./wt.% :_:_".u:._..:.-.-.:.:;.:;._..:.:__:::_:_:_:_r;:_:_:_:_..:.:._..::.:.:_._.:.:.:_:.:.s.._...:.:.:.:._..:.:.._..:.:............. Total % Impurity (GC/MS) None Detected Related Compounds - POAA Residual Solvents (TGA) 0.33 wt./wt.% None Detected Purity, by DSC Inorganic Anions (IC) Not Applicable 3 _._,uon_o_Y':rIi'C_i!,_U.i._.i!.i_-.?,._!i_:.=:.,i.:i_._!_.i.l._..i! i!_ _ _.<_o._o.x,__.._,_.%0._ 3. Bromide :::::::.::::::::.i i_i_._i;i=_:=_F_:;i_;iii.i:_iy_=d_i?d_d_=.=..=.._..:i.=i._.!./.i_=4::?:_/<i_==i3=.=i=<=0_.=04_0=_wi!._.=lw_t.._%;_=_i 4. Nitrate 5. Nitrite _.:_._._::_._.i!!!!_;!_.!i_![_!_._!!i_i?!X_.!_.?_qi_E_._._}i_!iU_._`_ 4. <0.009wt.A_t.% 5. <0.006wt./wt.% 6. Phosphate 7. Sulfate' ii}:::i::i:i::i:}::i:::i:i::!:::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::6::.::::<::0::.0::0::7::::w::t:.:/:w:::t:.:%:::::::::::::::::_} 7. 8.76 wt./wt.% 1. TFA 23. PHFFPBAA 4. NFPA Elemental Analysis_: 1. Carbon i:iiii!i'!i!ii!i!ii!i!iii!!lifiii!iliiii!iii: ii! 1. <0.1wt./wt.% 23. <0.01.01wt./wt.% 4. 0.28wt./wt.% 1. Theoretical Value = 17.8% 1. 12.48 wt./wt.% 2. Hydrogen 3. Nitrogen 4. Sulfur 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4. Theoretical Value = 5.95% 2. 0.244 v_x./wt.% 3. 1.74 wt./wt.% 4. 8.84 wt./w.% 5. Fluorine 5. Theoretical Value = 60% 5. 54.1 wt./wt.% COA023-018A Page 1of 3 INTERIM CER TIFICA TE OF ANAL YSIS Centre Analytical Laboratories COA Reference #: 023-018A Date of Last Analysis: 08/31/00 Expiration Date: 08/31/01 Storage Conditions: Frozen r-I-10C Re-assessment Date: 08/31/01 1Purity = 100% - (sum of 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 of 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. 5TFA HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid 6Theoretical value calculations based on the empirical formula, CffI7SO3"K+(MW=538) This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160). COA023-018A Page2 of3 INTERIM CERTIFICATE OF ANAL YSIS 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: Reviewed By: David S. Bell Date Scientist, Centre Analytical Laboratories John Flaherty Date Laboratory Manager, Centre Analytical Laboratories COA023-018A Page3 of 3 ldlife International, Ltd. COTOXICOLOGY & ANALYTICALTESTING SERVICES September 27, 2000 Ms. Susan A. Beach 3M Corporation EnvironmentaLlaboratory 935 Bush Avenue 3M Building2-3E-09 P.O.Box 33331 St. Paul, Minnesota 55133 Dear Susan: Enclosed please find Addendums for Wildlife International, Ltd. Project Numbers 454A-101, 454A- I02, 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/eyw8/3m Enclosures Km't R. Drottar Senior Biologist 8598 Commerce Drive Easton. Maryland 21601 Tel.410-822-8600 Fax 410-822-0632 - E-mail ecotox@wildlifeinternational.com EuropeanOffice:OverscheensewegI IA - [412AANaarden-The Netherlands-Tel.31(0)356949261 Fax31(0)336948229 E-maialleopold_worldonline.nl