Document o9nZ6DOOVK1EEwxdnRZ706kpX
Wildlife International, Ltd.
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PrqjNeumebter 454A-I09
PFOS: A SEMI-STATIC LIFE-CYCLE TOXICITY TEST
WITH THE CLADOCERAN (Daphnia magna)
ADDENDUM
WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-109 3M LAB REQUEST NO. U2723
U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines
OPPTS Number 850.1300 and
OECD Guideline 211
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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Project Number 454A-109
REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9%
SPONSOR: SPONSOR'S REPRESElffTATIVE:
LOCATIONOF STUDY, RAW DATA AND A COPY OF THE FINAL REPORT:
3M Corporation Susan A. Beach
Wildlife International Ltd. 'Eastort, Maryland 21601
WILDLI_EINTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY:
NOMINALTEST CONCENTRATIONS MEAN MEASURED TEST CONCENTRATIONS" TEST DATES:
LENGTH OF TEST:
TEST ORGANISM: SOURCE OF TEST ORGANISMS:
AGE OF TEST ORGANISMS:
NOEC: LOEC: MATC:
454A-109 PFOS (Perfluorooctane Sulfonic Acid Potassium Salt) PFOS: A Semi-Static Life-Cycle Toxicity Test with the Cladoeeran (Daphnia magna)
Negative Control, 1.3, 2.8, 5.5, l 1, 22 and 44 mg a.i./L
Negative Control, 1.4, 2.8, 5,4, 12, 23 and 46 mg a.i./L Experimental Start -'July 12, 1999 Biological Termination - August 2, 1999 Experimental Termination - August 4, 1999 21 Days
Neonate Cladocerans (Daphnia magna) Wildlife International Ltd. cultures Easton, Maryland 21601 Juveniles < 24 hours old
12 mg a.i./L 23 nag a.i./L 17 mg a.i./L
Wildlife International, Ltd.
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CERTIFICATE OF ANALYSIS
Project Number 454A-109
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
I
Purity: 8.6.9% Specifications
Result
Purity 1
86.9%
Appearance Identification
NMR
White Crystalline Powder :i :i::ii:_:-:.: _ :i:,: :.:i: ..- :!_:. .... i _._.:. _ _ ::::_:I"
!i!i
Conforms ' Positive
2. Magnesium 3. Sodium
4. Potassium 2
5. Nickel
6. Iron
,
7. Manganese
2. 0.001wt./wt.% 3. 1.439 wt./wt.% 4. 6.849wt./wt.% 5. <0.001 wt./wt.% 6. 0.005wt./wt.%
7. <0.001wt./wt.%
TToottaall%%ImIpmupruitryi(tyNMR) (LC/MS)
!}iiii!iii iiiiiii:ii!i:!!iiiiiiiiiiiiiiiii!i!iiiliilililiiiiiiil;iiiiiliili;i :i!i_ii i_ 81..4913Wwtt..//Wwt.% _:i:i@i_i:!_!i!!i_ii;i:i:i:,i:i_::iil!ii:ii_i:ii:!_:i!:!ii:i::i::_ii;!_:!i:i::_:i:)_::i!:!:ii:__ii::ii:;i_:il:!_t
(GC/MS)
.
None Detected
Related Compounds -
,
POAA
,
0.33 wt./wt.%
Residual Solvents (TGA)
None Detected
Purity' by DSC
Not Applicable 3
1. Chloride
_o_r__uco_no_onii_i_ii,i_!i!_,i_ii!iii!_'!ili_!!ii!_!ii!:!ii"_i_iii!i!i:_iii__;liiii !ii2i!i0!,i9__i,i_ 3. Bromide
::::::::::::::::::::::::::::::::::::
:::::::::::::::::::::::::::::::::::::::::::::::
.,::.: .:':. ::. ":: - :::.
1. <O.Ol5wt./wt.% 3. <0.040wt./wt.%
4. Nitrate
4. <0.009wt./wt.%
657. NSuitlrfaittee4
i?ii!ili!ii:iii:iiilii?ii:ii;7:ii<6iiii0i0!!0i!7i6i: ................................................:.:...............:..!.:.:..:.i.i.i.............!.i.i.i.i.:.:::L_? 5. <0.006 wt./wt.%
1. TFA
2. PFPA
-
3. I-IFBA
1. <0.1wt./wt.%
2. <0.1_./wt.% 3. 0.10wt./wt.%
4. NFPA Elemental Analysisr:
1. Carbon
2. Hydrogen
3. Nitrogen 4. Sulfur
5. Fluorine
!_i!!_i_._ii_ii_:i:i_i_!))_ii_ii_;_!_!i!::ii_::!:i_i_i!:i:i;i__ii_:;ii_i!:i!__i:ii:_il.;i_;!ii4!_;.ii!_::i0:_:.i2_i:8i_wii_t.}/wi_t!.%
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.A,_.% 3. 1.74 wt./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 &Last Analysis: 08/31/00 Expiration Date: 08/31/01 Storage Conditions: Frozen O-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 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
Tfifluoroacetic acid
Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid
6Theoretical value calculations based on the empirical formula, CsF17SO3K + (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:
David S. Bell
Date
Scientist, Centre Analytical Laboratories
Reviewed By:
John Flaherty
Date
Laboratory Manager, Centre Analytical Laboratories
COA023-018A
Page3 of3
I
lat Ce i 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 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, -. _
._
KurtR_Drottar SenioBriologist
KRD/eyw8/3m Enclosures
8598 Commerce Drive Easton, Maryland 21601 -Tel.410-822-8600 Fax 410-822-0632 E-mail ecotox@wildlifeintemational.com European Office: Overscheenseweg IIA - i4t2 AA Naarden The Netherlands. Te_.31(0)356949261 Fax31(0)356948229 E-mailaleolx_ldOworldonline.nl