Document bBaGgXnaOYen3X50jo32KBvkO

Wildlife International, Ltd. - ]- Number 454A-103A PFOS: A 96-HOUR TOXICITY TEST WITH THE FRESHWATER ALGA (Selenastrum capricornumm) ADDENDUM WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A- 103A 3M LAB REQUEST NO. U2723 U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines OPPTS Number 850.5400 and OECD Guideline 201 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. Wildlife International, Ltd. -2- Proiect Number 454A-103A REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9% SPONSOR: ' SPONSOR'S REPRESENTATIVE: LOCATIONOF STUDY, RAW DATAAND A COPYOF THE FINALREPORT: WILDLIFEINTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY: MEAN MEASURED TEST CONCENTRATIONS: TEST DATES: LENGTHOF EXPOSURE: 3M Corporation Ms, Susan A. Beach Wildlife International Ltd. Easton, MD 21601 454A-103A PFOS (Perfluoroocatane Sulfonic Acid Potassium Salt) PFOS: A 96-Hour Toxicity Test with the Freshwater Alga (Selenastrum capricornutum) Negative Control, 5.3, 11, 20, 42, 83 and 172 mg a.i./L Experimental Start - April 1.2, 1999 Exposure Termination - April 16, 1999 Experimental Termination -April 21, 1999 96 Hours TEST ORGANISM: SOURCE OF TEST ORGANISMS: cELL DENS1TY 72-HOUR EC50: 95% CONFIDENCE LIMITS: 96-HOUR EC10: 95% CONFIDENCELIMITS: 96-HOUR EC50: 95% CONFIDENCE LIMITS: 96-HOUR EC90: 95% CONF/DENCE LIMYfS: 72-HOUR NOAEC: 96-HOUR NOAEC: Freshwater Alga (Selenastrum capricornutum) Wildlife International Ltd. Easton_ Maryland 2 ! 601 67 mg a.i./L 42 and 75 mg a.i./L 47 mg a.i./L 41 and 48 mg a.i./L 68 mg a.i./L 63 and 70 mg a.i./L 132 nag a.i./L 101 and 147 mg a.i./L 42 mg a.i./L 42 mg a.i./L g Wildlife Inte tational, Ltd. -3- REVISED SUMMARY (Continued) AREAUNDERTHEGROWTH CURVE 72-HOUREC50: 95% CONFIDENCELIMYrS: 11 naga.i./L 53 and 79 rag a.i./L 96-HOUREC 10: 95% CONFIDENCLEnvffrs: 96-HOUREC50: 95% CONFIDENCELIMITS: 96-HOUREC90: 95% CONFIDENCELIMrrs: 72-HOURNOAEC: 96-HOURNOAEC: 47 nag a.i./L 38 and 48 mg a.i./L 68 mg a.i./L 64 and 71 nag a.i./L 139 naga.i./L 120 and 149 nag a.i./L 42 mg a.i./L 42 mg a.i./L GROWTHRATE 72-HOUREC50: 95% CONFIDENCELIMITS: 96-HOUREC10: 95% CONFDENCELIMITS: 96-HOUREC50: 95% CONFIDENCELIMITS: 96-HOUREC90: 95% CONFIDENCELIMITS: 72-HOURNOAEC: 96-HOURNOAEC: 115 nag a.i./L 99 and 127 mg a.i./L 57 mg a.i./L 52 and 60 mg a.i./L 121 nag a.i./L 110 and 133 mg a.i./L >172 mg a.i./L Not Calculable 42 mg a.i./L 42 mg a.i./L PrqNjuemcbetr 454A-103A ! Wildlife International, Ltd. -4- CERTIFICATE OF ANALYSIS Project Number 454A-103A 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 Purity: 86.9% Test Name t Specifications [ Result Purity a Appearance Identification NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium: 86.9% White Crystalline Powder Conforms ili!i_i;.ii__:!i:ii:.ii!liiiil!iiiiiiii!i_:i_::iZ:i!i.Zi;!:ii:i!i.ii_iiiiiilii:_:i_ii:i_iiiiiii!iiiiiii!iiiiiiii:_:_i:: :::::::_:?::i:_::_::i:_::!:::::i:_::i:_:.:_::::::::.::.::._:..:..:.:..:.:._.:..:.:.:._.:..:.:..:_..:..._..:.i.:-._..:._..::.:..:..:..:._.-.:.:::?.<:i:_:::_.:::i._.:.:.._.:.::::::_::::i.._P: ositive ! :: : :!::ilz:iii_ii_:ii-!i.i!:.ii:i_i====:.==i ================== .:::_:::_.:::::___i:_..:._.................:._::::_::_._:.:_.:.._....._...:.:::: 1. 0.005 wt./wt.% . : :]:i::_::]iiii:i_!iii::_::_::_ , : ? : :71:i_:i:ii:.;ii:_:::i_:i!_i:!:!!:_:_:!?_.i:_i:i:il_:.! :: ....:.::-::".:....'............................... . 2. 0.001wt./v_.% 3. 1.439 ,vt./,_.% 4. 6.849wt./wt.% 5. Nickel 67.. IMroannganese Total % Impurity (b/MR) (LC/MS) Total% Impurity 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. Sulfate" Organic Acids s (IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Elemental Analysisr: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur " 5. Fluorine . i : :.:i.}i i.iii::: : :if i!ii.iliii ii i:_i 5. <0.001wt.A_.% _:_,7:i_ i::: i_._.i_l.i7i:._i:7i:i:_i:5i:_i:i/:i:i:_:_:i:_!:7!::_:i;:i_::i:_i:.i_isi7:ii_:_i:2_-__ii_:;_i!i_ii:i_!i,.,i_ii._!:.:_!"i:..i:.:i_.i:i_:i:;_!!_i67.i_i..:_i ).O<_0:._O:0:00_51v,w.t/.w/wt.t%.% .....!.!;:.ii 1.93 wt./wt.% ii:!: iiii:iii:iii: i!ii:iii:iii ii'"i 8.41 wt./wt.% . : : i_ii_ii:i NoneDetected :::::. :::::: ::-.-:.;::::::::::.::::: :7::.::: :-:::'"'" :.: ::.:::::::::::::::.:::::: .:::: ::. : ::'--:::- ....... . ........... 0.33 wt./wt.% None Detected ::!-!!).!i):i:!-_.i.!!Ni!o!!tiA::ipplicable 3 1. <0.015wt./wt.% :::: :,:.::.:.;,-:.;::. :::::::::::::::::::::::::::::::::: :::- : .. -,.:,. ::.::: :::.:..: 2. 0.59 wt./wt.% ::.:::-::-:i::.:i::!:::_:::-:i::#::: iii!:_:::::::::::::::;::::::::::!;iiii;:.;..:.?..::ii::!:.,..i:::_:_.!:_:_.:..::i-:_::-:!i:--:.:_....i-.i..:ii!!:!::.:::::.!:._:: :::__:.: ::_:_-_3.:._ <0 040 wt./wt.% -ii!_::!i:ii:_ii::)i;i;iiiii!i!::i_!i;:i.;::i'i:::i.:;iii:?:;.:!:;_i;.;;ii_:.:i:i::.i:i:::.i:;i:.i;; 4. <0.009 wt./wt.% 2:!!:!22!:3:Xii22!ii_kli_::i2?:_.!:!!!!!:![_.i:'::!::5!!!,:!i: .:!:: !"}:::::!:?::-_"::.:!:.. ;iii;_i!_i.i_.!_.i_;}i`ii_!_;_;.;i_;i;._i;;_)_)i_i_i!_!_.!:_;_!_!?;5_.!_ii<!0;!.!0_0!6?)w{ti._/w:_t.%_: 6. <0.007v, l./wt.% 7. 8.76 wt./wt.% :_:,::!i!:!__ii':i.:':::':i::.i._..._.i.:::i::::.::;:::':.?.:_i_:-:i_:z:i:z_i:_:._:i?ii:_!!:_i!iiil_i;ii_:.:;_.:_:._, i;iiiiii_.i_i_iiii;.iiii:_i;i_ii;ii_:;ii:_iii_;iii_ii_iiiii.;!!!_;i;i_ii;._1i_. i.:_<i0_.i1.iw_ti.:/iw_iti.i%;_.i:i!._i;:_;ii_ ,!ii:i_ii:i!i!i:iiiiiiiiiii;:iil;_i:+i_.i.i._..i.i.l.;:.:-i:i.i:_::i:.i.-i.__..i.i..i.i.i.:...i.-.:..::....... 2. <0.1wt./wt.% i::::ii_;i;i::.::?]]i:i:::ii::ii:::::::i::i:ii:;:_]:i;_.ii_.;i_ii1_7: _i:_:_}_::::iii.:i:i_::;_:::i_U: :i::il)ii:i:i:::::iil::ili_i_) ::::::::.:::::::;.:;..:::::..-,..:.,..."..-.........-. ....................... 3. 0.10 wt./wt.% ,:.:.:.:.............:..:..:..:..:.:.:.:..:.:.:.:.:.i:.i:._.:.:!.:i.::..:i..:.;.:.:.:._.:..:.:i.:.::_:::-:::_::i:::_::i_:.i_..:._...:_.:,.:_.'..::.:-_._..:.'._..:._..:.:_...:..:..:..:.:._......_. ._:::4. 0.28 wt./wt.% 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 m./wt.% 3. 1.74 wt.A_.% 4. 8.84 wt./wt.% 5. 54.1 wt./wt.% COA023-018A Page I of 3 INTERIM CERTIFICATE 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 []-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%+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 SOs 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 Trifluoroacefic acid Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid 6Theoretical value calculations based on the empirical formula, CsF17SO3"K + (MW=538) This work was conducted under EPA Good Laboratory Practice Standards (4.0CFR 160). COA023-018A Page2 of 3 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: David S. Bell Date Scientist, Centre Analytical Laboratories Reviewed By: John Flaherty Date Laboratory Manager, Centre Analytical Laboratories COA023-018A Page 3 of 3 ! t ldlife International, Ltd. COTOXICOLOGY & 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 fred 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. Sincerely, -. _ ._ Kurt R. Drottar Senior Biologist KRD/eywS/3m Enclosures 8598CommerceDrive - EastonM, aryland21601-Tel.410-822-8600Fax410-822-0632 E-maiel cotox@wildlifeinternational.corn EuropeanOf_ce: OverscheensewegIIA /412AA Naarden-The Netherlands-Tel.31(0)356949261 Fax31(0)356948229 E-mailaleopoldOworldonline_l