Document By5ZJjJ7worKmmMxENG193KRL
.Wildlife International Ltd.
-1 -
Project Number 454A-1Q2
PFOS: A 96-HOUR STATIC ACUTE TOXICITY TEST WITH THE FATHEAD MINNOW (Pimephales promelas)
ADDENDUM
WILDLIFE INTERNATIONAL, LTD. PROJECT NUMBER: 454A-102 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. Easton, Maryland 21601
WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: TEST SUBSTANCE: STUDY:
MEAN MEASURED TEST CONCENTRATIONS: TEST DATES:
LENGTH OF TEST:
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
TEST ORGANISM: SOURCE OF TEST ORGANISMS:
Fathead Minnow (Pimephales promelas)
Wildlife International Ltd. cultures Easton, Maryland 21601
AGE OF TEST ORGANISMS:
MEASUREMENTS OF 10 NEGATIVE CONTROL FISH:
WEIGHT (g): TOTAL LENGTH (m m ):
Juveniles
Mean = 0.36; Mean = 35;
Range = 0.21 to 0.49 Range = 30 to 38
96-HOUR LC50: 95% CONFIDENCE LIMITS: NO MORTALITY CONCENTRATION:
NO-OBSERVED-EFFECTCONCENTRATION:
9.1 mga.i./L 7.7 and 11 mg a.i./L 3.2 mg a.i./L
3.2 mg a.i./L
____Wildlife International, Ltd.
-3-
CERTIFICATE OF ANALYSIS
Project Number 454A-1Q2
INTERIM CERTIFICATE OF ANALYSIS
Revision 1(9/7/00)
Centre Analytical Laboratories COA Reference #: 023-018A
3M Product: PFOS, Lot 217
Reference#: SD-018
_____________________Purity: 86.9%_______
Test Name
Specifications
Purity1
Result 86.9%
.
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
*
White Crystalline Powder
< / < 1. Theoretical Value =17.8% 2. Theoretical Value = 0% 3. Theoretical Value = 0% 4. Theoretical Value = 5.95% 5. Theoretical Value = 60%
Conforms
Positive
1. 0.005 wt./wt.% 2. 0.001 wt./wt.% 3. 1.439 wt./wt.% 4. 6.849 wt./wt.% 5. <0.001 wt./wt.% 6. 0.005 wt./wt.% 7. <0.001 wt./wt.%
1.93 wt./wt.% 8.41 wt./wt.%
None Detected
0.33 wt./wt.% None Detected Not Applicable3
1. <0.015 wt./wt.% 2. 0.59 wt./wt.% 3. <0.040 wt./wt.% 4. <0.009 wt./wt.% 5. <0.006 wt./wt.% 6. <0.007 wt./wt.% 7. 8.76 wt./wt.%
1. <0.1 wt./wt.% 2. <0.1 wt./wt.% 3. 0.10wt./wt.% 4. 0.28 wt./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 1 of 3
INTERIM CERTIFICA TE 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
'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 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.5
5TFA HFBA NFPA PFPA
Trifluoroacetic acid Heptafluorobutyric acid Nonofiuoropentanoic acid Pentafluoropropanoic acid
th e o re tic al value calculations based on the empirical formula, CgFi7S03'K+(MW=538)
This work was conducted under EPA Good Laboratory Practice Standards (40 CFR 160).
COA023-018A
Page 2 of 3
INTERIM CERTIFICATE OF ANALYSIS
Centre Analytical Laboratories COA Reference ft: 023-018A
LC/MS Purity Profile:
Im purity C4 C5 C6 Cl
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 B y : ______________________________ __________________
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.
E C O T O X IC O L O G Y & A N A L Y T IC A L T E S T IN G 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
If you have any questions, please let me know.
KRD/cyw8/3m Enclosures
Senior Biologist
8598 Commerce Drive Easton, Maryland 21601 -Tel.410-822-8600 Fax 4 10-822-0632 E-mail ecotox@wildlifeintemational.com
European Office: Overscheenseweg H A - 1412 A A Naarden The Netherlands Tel. 3 1(0)356949261 Fax 3 1(0)356948229 E-mail aleopold6worldonline.nl