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Wildlife International, Ltd.
P o e umbor4 4
PFOS: A 48-HOUR STATIC ACUTE TOXICITY TEST WITH THE CLADOCERAN (Daphnia magna)
ADDENDUM
WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-104 3M LAB REQUEST NO. U2723
U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines
OPPTS Number 850.1010 and
OECD Guideline 202
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.
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Proje Numb r4 4A-
REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9%
SPONSOR:
SPONSOR'S REPPRESENTATIVE:
LOCATIONOF STUDY, RAW DATAAND A COPY OF THE FINALREPORT:
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:
454A-104
PFOS (Perfluorooetane Sulfonic Acid Potassium Salt)
PFOS: A 48-Hour Static Acute Toxicity Test with the Cladoeeran (Daphnia magna)
Negative Control, 11, 19, 32, 54 and 87 mg a.i./L
Experimental Start - February 16, 1999 Biological Termination - February 18, 1999 Experimental Termination - February 18, 1999 48 Hours
TEST ORGANISM: SOURCEOF TEST ORGANISMS:
AGE OF TEST ORGANISMS:
Neonate cladocerans (Daphnia magna) Wildlife International Ltd. Cultures Easton, Maryland 21601 < 24 hours at test initiation
48-HOUR EC50:
95% CONFIDENCELIMITS:
NO MORTALITY/IMMOBE2TY CONCEI,_]LATION: NO-OBSERVED-EFFECTCONCENTRATION:
59 nag a.i./L 32 and 87 mg a.i./L 32 mg a.i./L 32 nag a.i./L .
Wildlife International, Ltd.
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CERTIFICATE OF ANALYSIS
proiNeumcbter454A-104
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: 86.9% Specifications
Purity 1 Appearance
i
White Crystalline Powder
Result 86.9% Conforms
NMR Metals (ICP/MS)
1. Calcium 2. Magnesium 3. Sodium 4. Potassium 2 5. Nickel 6. Iron 7. Manganese
Total % Impurity (NMR)
_,_s_,_
Total % Impurity
(GC/MS)
Related Compounds -
POAA Residual Solvents (TGA) Purity by DSC
,.
Positive
_ _i__:i__ r_ ::::::::::::::::::::::-::::::::::::::::::::::::::
, i iii
1. 0.005wt./wt.% 2. 0.001wt./wt.% 3. 1.439 wt./wt.% 4. 6.849wt./wt.%
5. <0.001wt./wt.%
6. 0.005wt./wt.%
7. <0.001wt./wt.%
i::ili_ji_ii::_iii_i:iziiiiiiii_i!ii_i!:i:iiiiiii_i!iii!_ii:i!!__::ii_!ii_!ii_iii_i_i_i_iii_ii!!:_i_1ii._9i3i_w!it!.i/_wiit_.%i_ii_i_i_i!ii!_!_._i!_:i_
ii!iiii!ii!iiiii!ii!!i!i!i:ili!lii!iiiliii!i:i!iiifiiliili!iii!_i_4!i1l_,_.
.........;.:..:.:.;.:._..:.:.;.:_.:!.::
None Detected
_:_:_;_:_:_:_:::_:_:_:_::;:_:_:_:_:_;_:::::_:_:_:_:_:_:_:::_:_:_:_0:._3;3:_w::t:._/w:;:t_.%:;:;_::_:_:_::_:._.:::.:.:_` _.;.z.:._._._._._:._._::_;;:._..;.:..:.:.._...._..:.._..:.:..._....:.:..:.._..:.:.:._..:._.:.;:..:_.:.:._:.:.:._:.:.::.::.::._.:.:.:_.:.:.N:_.:..:o_..n.:.e_. Detected
Not Applicable 3
1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate 4 Organic Acids _(IC)
1. <0.015wt./wt.%
2. 0.59 wt./wt.%
3. <0.040wt./wt.%
4. <0.009wt./wt.%
5. <0.006 wt./wt.%
_:_:_:-:_:i_:!i:i_:i:i:_:i_::__:_r.:-i:ii_:ii_i_:_,,:_,_:_,_.,..:_:i:
6. <0.007 wt./wt.%
7. 8.76 wt./wt.%
_:_:!:::_i!:_":_:'_.':.::_.::.:_.::_._::._.:.[:.;;.:.__.:_.:r.:_::.::_.::::._:.:[::.[::_:.:'::..[_:.:_:'.::.:.'::.:_.'::.:.:_.:._..:.'.:.:..:.::.:_.:.::._:...i.l._.:.::.::.::.::.:.::.::.::.::.:.::.::.::.::.:.::_.::.:':.::;.'::.: .:i.::.::.:.::...'..,.::.::.::.:.::.................................................................
2 PrPa
4. NFPA Elemental Analysis_:
1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine
_M_____
1. Theoretical Value = 17.8% 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4. Theoretical Value = 5.95% 5. Theoretical Value = 60%
2 <0._./_.%
4. 0.28wt./wt.%
1. 12.48 wt./wt.% 2. 0.244 wt./wt.% 3. 1.74wt./wt.% 4. 8.84 wt./wt.% 5. 54.1 wt./wt.%
COA023-018A
Page 1of 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 D-10C Re-assessment Date: 08/31/01
1Purity = 100% - (sum of metal impurities, 1.45% +LC/MS impurities, 8.41%+Inorganic Fluofide, 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, CgF17SO3"K +(1VIW=538)
This work was conducted under EPA Good Laboratory Practice Standards (40 CFP,,160).
COA023-018A
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11
INTERIM CER TIFICA TE OF ANAL YSIS
Centre Analytical Laboratories COA Reference #: 023-018A
LC/MS Purity Profile:
Impurity C4 C5 C6 C7
Total
wL/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
Page3 of 3
I w
tat "re t International Ltd. ECOTOXICOLOGY & 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 Addendurns 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/eyw8/3m Enclosures
8598CommerceDrive EastonM, aryland21601Tel.410-822-8"600Fax410-822-0632 E-maiel cotox@wildlifeinternational.com
EuropeanOffice: OverscheensewegII A i412AA NaardenThe Netherlands-Tel.31(0)356949261 Fax31(0)356948229 E-mailaleopoldeworldonline.nl