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Wildlife International, Ltdl
454C-107
DETERMINATION OF THE WATER SOLUBILITY OF PFOS BY THE SHAKE FLASK METHOD
ADDENDUM
WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454C-107 3M LAB REQUEST NO. U2723
OECD Guideline for the Testing of Chemicals, 105 Water Solubility
This study was originally reported using a test substance purity of 98.9%. 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 measured concentrations originally reported were simply corrected by the ratio of the two purifies, or a factor of 0.8787. No attempt was made to recalculate analytical standard concentrations. 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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Pro oot --bor, ,c-
REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9%
STUDY TITLE:
WILDLIFEINTERNATIONALLTD. PROJECT NUMBER: SPONSOR: TESTING FACILITY:
LOCATION OF STUDY, RAW DATA AND A COPY OF THE FINAL REPORT:
Determination of the Water Solubility of PFOS by the Shake Flask Method
454C- 107
3M Corporation Wildlife International Ltd. Easton, Maryland 21601 Wildlife International Ltd. Easton, Maryland 21601
TEST SUBSTANCE: TEST DATES:
PFOS
Experimental Start - February 11, 1999
Experimental Termination - February 20, 1999
,
' ,,,r
I TEST SYSTEM:
NANOpure Water
I
I SUMMARY:
T49h8e mogveraa.il.l/L m(SeaDn = s4o6lu.4b;ilitCyV c=on9c.3e2n%tra;tioNn = 6o)f. PFOS in NANOpure@ water was
Wildlife International, Ltd.
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, ojo.Number454C-107
CERTIFICATE OF ANALYSIS
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%
TestName Appearance
NM_
I[_........_........_. : _
.S__.c.,:a.t,,l.o:n.:.s:._..:. _.................... Cry_ Powder
"'_"'-'_ .......... _ "_'_"_ _ "_ ...........
*" "-_'__2"_
8R6e.9s%ult Conforms
I. Calcium 2. Magnesium
_:__7,_?_:___%_:_,_':_-_._[i_:_ _i_,:!_!_ ___'-_!_!_;_i_i
I. 0.005wtJwt.% _' 2. 0.001wtJwt.%
4. Pota_ium_ 5. Nickel
7. _ Total% Impurity(NMR) Total% Impurity
_.:_,_...,::::_,-._-,s::'_-_:_._:_,:::,_........._....:.:.:_:_--__:-'_,_,4,_. . 6,849wtJwt.%
.... : :_"' _ _'__-_4-
..... _#-_
5. <0.001wt./wt.%
_.:_.................". .'_._,,_:,_,_._= ......._:..-_......... _,_:::_:_:'__'_:_::_:_::_: :::':_"__ _-_ _
6. 0.005wtJwt.% 7. <0.001wL/wt.%
;:_"_Y_:_:_'_' _
_'_'_
_:_
".._._.-......:._._.:.':.:"._.-.*._..:.:.:.:.:_._.'._:._.:.'._._.,_..".._..:._._.':*._.'._..:._.._..":.:_.:_..".:.'":"
L93 wtdwt.% g.41wt.lw{:,%
Total% Impurity (GOMS)
....:.......!."..:._......._..:.".".._..._....:.:..'.:........................'......._..:.:. ........... _..............................................
POA,A
......._.......:..'-_::r_......... " _" " =-" ' ............_." 0.33wt./wt.%
R-esiduaSlo. lventOs"OA) _:_-_I'-,.;.._.:._...._:..).:.,.,._..,:._.,.,.:._..:._..:._..,,._..-;__-:'-:_-'-_..-...._........ ....N.on_Detected Not App.cablP
3. _==i_
_. N",,_
67. PShuolfsapth4eate
1. TFA
23.. PHFFPBAA
4. _vPA
ElementaAl ealym': I. Carbon 2. Hych'ogen 3. Nitrogen 4, Sulfur 5. Fluorine
.
_'_#__
__._
__
1. 2. 3. 4, 5.
_.._ _
__
_!_
"::" ::*_,. "i_
"rheoreti_Value= 17.8%
TheoreticaVl alue= 0%
Theoreli_aVl alue= 0%
_
Velue= 5.95%
TheoreticaVl alue=60%
3. ,o.o4owt.,_% 5..,--o.oo6,,tJ,,_%
67. <80..7060w7wtJtwJwt.%t.%
1. <0.I wt./wt.% 23.. <0.01.0wIwtt..//wwtt..%%
4. o.2_w_.%
1. 12.48wt./v&% 2. 0.244wt./wt.% 3. [ 34 wt./wt.% 4. 8.84 wt./wt.% 5. 54.1wt./wt.%
COA023-018A
Pase 1 of 3
" Wildlife International, Ltd.
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ProjNecutmb4e5r4C-107
INTERIM CERTIFICATE OF ANAL YSI8
Centre Analytical Laboratories COA Reference #: 023-018A Date of Last Analysis: 08/31/00
Expiration Date: 08/31/01 Storage Coaditiom: Frozen _<-10C Re-assessment Date: 08/3 1/01
_Purity = 100% - (sum of metal impurities, 1.45% +LCdMS impurities, 8.41%+Inorganic Fluoride, 0.59%+NMK impurities, 1.93%+organic acid impurities, 0.3g%+POAA, 0.33%)
Total impurityfrom all tests = 13.09% Purity = 100%- 13.09% = 86.9%
2Potassium is expected in this salt form and is therefore not considered an impurity.
_Purityby DSC is generally not applicable to materials of low purity. No endotherm was observed for tiffs sample.
(Sulfur in the sample appears to be converted to 804 and hence detected using the inorganic anion method conditions. The anion result agrees well with the sulfur dgt_mination in the elemental analysis, lending confidence to this interpretation- Based on the results, the S04 is not comidered an impurity.
_'FA
I-IFBA
NFPA PFPA
Trifluomacetig acid
H_t_fluorobutytaic id
Nonofluoropentanoic acid Pentafluoropropanoic acid
t'rheoreticai value calcul_ons bash on the empirical formula,CtFtTS03_. +(MW=538)
work was czmdacted under EPA Good Laboratory Practice Standards (40 CFR lfi0).
/
COA023*018A
Page 2 of 3
Wildlife International, Ltd.
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INTERIM CERTIFICATE OF ANAL YSIS
Centre Analytical Laboratories COA Reference #: 023-018A
LC/MS Purity Profile: k
Impuri_
C4 C5
C6 C7
Total
wtJwt.%
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, respeaively. The C5 value was czkxdated using the average response factors from the C4 and C6 standard c_n,_. Likewise. the C7 value was cakxdated using the
average response factors from the C6 and C8 standard curves.
P,epar_ By:
David S. Bell
Date
1ohn l_aherty
Date
LaboratorMy msgerC, entreAmlyticaLl aboratories
COAD23-018A
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ldlife
International, Ltd.
ECOTOXICOLOGY & ANALYTICALTESTING SERVICES
November 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
f
Dear Susan:
Enclosed please fred Addendums for the following studies:
1. NoN-GLP STUDY: DETERMINATION OF THE SOLUBILITY OF PFOS IN WILDLIFE INTERNATIONAL, LTD. FRESHWATER, FRESHWATER ALGAL MEDIUM, AND SALTWATER WILDLIFE INTERNATIONAL, LTD. PROJECT NO.: 454C-101-1 3M LAB REQUEST NO. U2723
2. DETERMINATION OF THE WATER SOLUBILITY OF PFOS BY THE SHAKE FLASK METHOD WILDLIFE INTERNATIONAL, LTD. PROJECT NO.: 454C-107 3M LAB REQUEST NO. U2723
If you have any questions, please let me know.
RLV/eywS/3m Enclosures
Raymond L. Van Hoven, Ph.D. Scientist
8598 Commerce Drive ' Easton,Maryland 21601-Tel.410-822-8600 Fax 410-822-0632 - E-mail ecotox@wildlifeinternational.com EuropeaOn ffice:BergkarnpweI-g7231CL_Vamsvel.dTheNetherlandsT.el.31(0)575- 573848Fax3. 1(0)575- 574813E-maial;leopolcl_woddonline.nl