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International, Ltd.----------------------------- _______Project Number 454A-102
PFOS: A 96-HOUR STATIC ACUTE TOXICITY TEST WITH THE FATHEAD MINNOW (,Pimephales promelas)
ADDENDUM
WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-I02 3M LAB REQUEST NO. U2723
U.S. Environmental Protection Agency Series 850 - Ecological Effects Test Guidelines
OPPTS Number 850.1075 and
OECD Guideline 203
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- -
Project Number 454A-102
REVISED STUDY SUMMARY BASED ON A PURITY OF 86.9%
SPONSOR: SPONSOR'S REPRESENTATIVE:
3M Corporation Ms. Susan A. Beach
LOCATION OF STUDY, RAW DATA AND A COPY OF THE FINAL REPORT:
Wildlife International Ltd. =E^to^JV[^^^_216013_
WILDLIFE INTERNATIONAL LTD. PROJECT NUM BER: TEST SUBSTANCE: STUDY:
M EAN M EASURED TEST C O N C E N T R A T IO N S: TEST DATES:
LENGTH OF TEST: TEST ORGANISM : SOURCE OF TEST ORGANISM S:
454A-102
PFOS (Perfluorooctane Sulfonic Acid Potassium Salt)
PFOS: A 96-Hour Static Acute Toxicity Test with the Fathead Minnow (Pimephales promelas)
Negative Control, 3.2, 5.4, 9.1, 16 and 27 mg a.i./L
Experimental Start - February 15, 1999 Biological Termination - February 19, 1999 Experimental Termination - February 19,1999
96 Hours
Fathead Minnow (Pimephalespromelas) Wildlife International Ltd. cultures Easton, Maryland 21601
AGE OF TEST ORGANISM S:
MEASUREMENTS OF 10 NEGATIVE CONTROL FISH:
W EIGHT (g ): TOTAL LENGTH (m m ):
Juveniles
Mean = 0.36; Mean = 35;
Range = 0.21 to 0.49 Range = 30 to 38
96-H O U R L C 50: 9 5 % CONFIDENCE LIM ITS: N O M ORTALITY CONCENTRATION: N O -O BSER V ED -EFFEC TCONCENTRAHON:
9.1mga.i./L 7.7 and 11 mg a.i./L 3.2mga.i./L
3.2m ga.i/L
Wildlife International. Ltd.
-3 CERTIFICATE OF ANALYSIS
Project Number 454A-102
INTERIM CERTIFICATE OF ANALYSIS
Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: Q23-018A
3M Product: PFOS, Lot 217 Reference #: SD-018 Purity: 86.9%
Test Name Purity1
Appearance Identification
NMR Metals (ICP/MS)
1. Calcium 2. Magnesium 3. Sodium 4. Potassium2 5. Nickel 6. Iron 7. Manganese
Total % Impurity (NMR)
Total % Impurity (LC/MS) Total % Impurity (GC/MS) 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. Sulfate4 Organic Acids5(IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA
Elemental Analysis6: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine
if ----- 7t ! i'l"'
1. 2. 3. 4. 5.
id 1 /% 1 ;
1^
li g 41 w t/vft0/
None Detected
None Detected
Theoretical Value = 17.8% Theoretical Value = 0% Theoretical Value = 0% Theoretical Value = 5.95% Theoretical Value = 60%
1. 12.48 wt./wt.% 2. 0.244 wt./wt.% 3. 1.74 wt./wt,% 4. 8.84wt./wt.% 5. 54.1 wt./wt.%
COAQ23-018A
Page 1 of 3
INTERIM CERTIFICATE OFANALYSIS
Centre Analytical Laboratories COA Reference #: 023-018A
Date o f Last Analysis: 08/31/00
Expiration Date: 08/31/01
Storage Conditions: Frozen []-10oC
Re-assessment Date: 08/31/01
'Purity = 100% - (sum o f 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 alltests= 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 o f 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.S
STFA HFBA NFPA PFPA
Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid
^Theoretical value calculations based on the empirical formula, CgFi7S03"K+(MW=538)
This work was conducted under EPA Good Laboratory Practice Standards (40 C F R 160).
COA023-018A
Page 2 of 3
INTERIM CERTIFICATE OF ANALYSIS
Centre Analytical Laboratories COA Reference #: 023-018A
LC/MS Purity Profile:
Im purity 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 B y :______________________ ;________
____
John Flaherty
Date
Laboratory Manager, Centre Analytical Laboratories
COA023-018A
Page 3 of 3
ildlife 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 find Addendums for Wildlife International, Ltd. Project Numbers 454A-101, 454A-102,454A-103A, 54A-104,454A-105,454A-106,454A-107,454A-108 and454A-109
Ifyou have any questions, please let me know.
K R D /cyw 8/3m Enclosures
Kurt R. Drottar Senior Biologist
8598 Commerce Drive Easton, Maryland 21601 -Tel.410-822-8600 F a x 4 10-822-0632 E-mail ecotox@wildlifeinternational.com
European Office: Overscheenseweg IIA 1412 A A Naarden -The Netherlands -Tel. 3 1(0)356949261 Fax 3 1(0)356948229 E-mail aleopoldeworldonline.nl