Document y8BJD8yLpng39rR3OBX7KvMd
Wildlife International, Ltd.
Numb
PFOS: A 96-HOUR SHELL DEPOSITION TEST WITH THE EASTERN OYSTER (Crassostrea virginica)
ADDENDUM
WILDLIFE INTERNATIONAL, LTD, PROJECT NUMBER: 454A-106 3M LAB REQUEST NO. U2723
U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines
OPPTS Number 850.1025
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.
WiMlife International, Ltd.
-m-
ProjectNumber454A-106
REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9%
SPONSOR: SPONSOR'S REPRESENTATIVE:
LOCATIONOF STUDY, RAW DATAANDA COPYOF THE FINALREPORT:
W_.DL_I_TE_WTiOnAL
LTD. PROJECT NUMBER:
3M Corporation Ms. Susan A. Beach
Wildlife International Ltd.
_n,
Maryland 21601
454A-106
TEST SUBSTANCE: STUDY:
MEAN MEASUREDTEST CONCENTRATIONS: "rESTDATES:
LENGTH OF TEST:
PFOS (Perfluorooctane Sulfonic Acid Potassium Salt)
PFOS: A 96-Hour Shell Deposition Test with the Eastern Oyster ( Crassostrea virginica)
Negative Control, 0.35, 0.38, 1.2, 1.8 and 2.9 mg a.i./L
Experimental Start - May 24, 1999 Biological Termination - May 28, 1999 Experimental Termination - June 14, 1999 96 Hours
TESTORGANISM: SOURCEOF TEST ORGANISMS:
OYSTER LENGTH (hi = 20): 96-HOUR EC50: 95% CONFIDENCELIMITS: NO-OBSERVED-EFFECTCONCENTRATION: LOWEST-OBSERVED-EFFECT CONCENTRATION:
Eastern Oyster (Crassostrea virginica) P. Cummins Oyster Company, Inc. 618 West 33 m Street Baltimore, Maryland 21211 Mean = 33.8 mm, Range = 27.8 to 41.5 mm >2.9 mg a.i./L Not Calculable
1.8 nag ai./L
2.9mg a.i./L
Wildlife International, Ltd.
-3-
CERTIFICATE OF ANALYSIS
ProjNeumcbter454A-106
6
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.,.ur ity1
Purity: 86.9% Specifications
i,|lm,,
Appearance Identification
...................i._.. .C_in e powder ................ iii:.tii!liiiii_i}}iii}i!gii:!i:iiii}iiti_iii}}}i_i}!iiliit}i:i}}iiitl:_:ii}:.t!i:ilii!:i:}itltili:l:.ii(il":.iiliii!ii:i
Result 86.9%
Conforms
Metals (ICP/MS) I. Calcium
::,... ::;?.fi:v:_:..'.'.':.*:'f_:'ff,_L.'..'ff,d'('.?.::?:'.. _;.:'.:" :??.';"..'?:.:?:E?.:..'::'.:'::::: :.. 5_ ..':... _'_7.':...
_::::.::r::_:::.::_::::::::::::_:::.::_:::::::_:::;::.::_:::::::::.::`::_::::.:_::::.::.:.::`:::::.::.::.:.::`::::::_.:-::.:::_:.:_:_-:::.:___:,:..:.`_-:_:,_:,::.+:`::._:.:..:._f`:..:.;_:,;.:::_.:::`::;:::_::::_-_::._::_::::*:;:::_::.:._'
_i!i_!_i_i_i_i_ii_i_i_i_i_ii_ii_ii_iiii_iiii_i_iii_:_:.:i::_:;ii_::!iil_i 1ii.i_i0_.i0_0!;5!!wiiit:._/wi_t!.I%!ii_iiiii_ii!_iiii_i]i_ii_ii_
3. Sodium 4. Potassium2 5. Nickel 6. Iron 7. Manganese
Total % Impurity
(L
ToCta!SlI_V"%_o )Impurity
(GC/MS) RelateCdompoundsPOAA Residual Solvents (TGA) Purity by DSC Inorganic Anions (IC)
1. Chloride 2. Fluoride 3. Bromide
45.. NNiittrraittee
6. Phosphate 7. Sulfate4
Organic Adds _ (IC) 1 TFA
3. HFBA
4. NFPA ElementalAnalysis6:
1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine
3. 1.439 wt./wt.% 4. 6.849wt./wt.% 5. <0.001 wt./wt.% 6. 0.005wt./wt.% ...................;.:.:.....:..;.......;..:.....:.._........._......................................._....:...:....:...,..,.7........<..O....O...0..1..w...t..l.w...t..%...............
!_i![_ii?_i_i_i_i_i_i!i_!_i_;i_`_!_i_:_!!?_:_:i:!.;_i_i_.i!:!:_:!:_:i:!!ii!_._i:_i:i::!:!_:!_!iiii_i_::3`:!:i:i_?.ii_!i!F:i;i_:_1ii,_9:3:i:_ Wt.[wt.%
8.41 wt./wt.%
:::::__: :::::::::;___!::!:::_::_:__:--:___!h/__]?!_::;:;-!_
?:;:!i_: _!!_:;_;
None Detected
-_--::;--_::!-::::,--:i-"__!!-'-:__'-!_!:-__-::'_!_.':_!;__-_-___"--,::_:-:--:::_':--:_._-;,:-__--:":-:'--:.
0.33 wt./wt.%
None Detected
_:_:_:_:_:._:_::_;_];_]_:_::_::_J_:_:_:_:_
Not Applicable_
_-_:_;__"_::._::.:_.__".:_._:...``._.._.::...__._.:._........_._...:__:_`:_:_;`_;_._._ :::::::::::::::::::::::::_::::_::_::::::.::::::::::::::::::::::::::::::::_:::::::_.-::??i_:::::.:-_::_: _:"::._::_:::_:_: :':::__::_::_?-::.":::f::::::':_:.::L:::_:.:_::::::::
:::::::::::":":::::::::::::::::::.::.:.::._:.:.::.::.:.::.::.":.:.:..:_.::: ::::::::::::_:::::::::_::::::::::::::::_::::::_1:-:.:i:l::<::0::.0::1::5:::w::t:.:/:w::t:.:%::::::::_:_ !ii:_!_!_i_i_:.i,_..:_i!i_i:'_.`!:i._.:....!i!i_!_!_ii_!_i:_%i_!_ii_!_i!i!i!2i_.ii_i%0.i5_9ii_w!ft._/wii:t..%_._i!i%!!!i_i_!_!ii!i!_!i_
3. <0.040wt./wt.%
::_:-:_:_;:;;:_:._:_:_:;::_;r:_.:`_:_:._._;_:z:_._:_`._:_:_..`._:_:_:_:45`.._:_<<:_00:,._00;00:_96;w_wt:J:t_Jw:w_t.t:%._%:_:_:_:._:_:_:_:_:_._:_.
_iii_iii_iii!_i_!iii_i_i_i!ii!ii!_i_!i!!i!ii_iii!iiiii!_iii!i_i_ii_i6i!.i_!<!_0!.0i_0i7iiwi_ti.i/iwiiti.i%i!ii_i_ii_ii_i_i !::_i_i_:__i_:i._::i._i!__._._ii_`_i:_.i_i_._._i.-.i_`_i_i_ii_._:_!_ 7. 8.76 wt.twt.%
i!!_ii_iii_!]ii_i_::ii_..!_i!_i_ii!i__.!ii!_ii:i:ii_ii_ii:i,i_iiii_iii__i!!_i_i!iii_!iiiiiii_!_!i_i_!_!i!_!i_!i_i!i?_i_iiii_!!!!_!ii_!_ .:"_:::::::!:-::!:_::_:f!:!_::_!:_::.::_::!::-:::_:'.:_-:.!::__::_:__:[;::"!__:i:_.:i.:_.::.::._:.i::.i_.:i.::::!_'">:_:'_::.:!._:.:._.:!.:_.:!.'!::.!i:._:_.-!.!_._i.!_.-!.'._.:._.!._._.:;.!_!.:.:!.;_.i_....':,::_!:-!:!__i!:]:_! I. <0.1 wt./wt.%
!:[:_:?:::::"-":::::_:__::F::_::_::_:_:_:_::_'_".-:_',.:_::::_::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::?::::::::::!:_:H::! :
......._..-.:.:.:..:.:.:.:.:.:.":.:._:..:'_.:*.:<..:.":.':._:.'_*.::.':.::.:.::.'-._.':.:..:.::._::._:..:._..:..:..:...:.".:..._:..:....................._....:..:...:..:..:....:..:..:............................3.......0.10 wt./wt.%
:::::;:::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::::: :,::.:::._:::::::.::::: :::::::::
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%
I. 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-O8l A
Page 1of 3
INTEPM 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
1Purity = 100% - (sum of metal impurities, 1.45% +LC/MS impurities, 8.41%+Inorganic Fluoride, O.59%+NMR impurities, 1.93%+orgaaic 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 S04 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
I-IFBA NFPA PFPA
Trifluoroacetic acid
Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid
6Theoretical value calculations based on the empirical formula, CgFITSO3"K+(MW=538)
This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160)
COA023-01gA
Page 2 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
ldlife
International, Ltd.
ECOTOXICOLOG&YANALYTICALTESTINSGERVICES
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 find 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
K1LD/cyw8/3m Enelosurcs
8598CommerceDrive EastonM, aryland21601Tel.410-822-8600 Fax410-822-0632 E-maiel cotox@wildlifeintemational.com EuropeaOnfficeO: verscheenseIwIAe-gi412AANaarde"nTheNetherlandTsel3: 1(0)35694926F1ax31(0)3569482-2E9-maailleopoldOworldonline.nl