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DETERMINATION OF THE MELTING POM I7M ELTING RANGE OF PFOS
WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: 454C-106
OECD Guideline for Testing o f Chemicals, 102 M elting Point/M elting Range
AUTHORS: Ronda L. Jacobs W illard B. Nixon, Ph.D.
STUDY INITIATION DATE: December 18,1998 STUDY COMPLETION DATE: February 24, 1999
Submitted to:
3M Corporation Environmental Laboratory
P.O .B ox 33331 S t Paul, Minnesota 55133
W ild life International ltd
8598 Commerce Drive Easton, Maryland 21601
(410) 822-8600
Page 1 o f 12
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PROJECT NO.: 454C-106
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT
SPONSOR: 3M Corporation
TITLE: Determination of the Melting Point/Melting Range of PFOS
WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER 454C-106
STUDY COMPLETION: February 24,1999
This study was conducted in compliance with Good Laboratory Practice Standards as published by the U.S. Environmental Protection Agency in 40 CFR Part 792,17 August 1989 and OECD Principles of Good Laboratory Practice, OCDE/GD (92) 32, Environment Monograph No. 45, Paris 1992.
STUDY DIRECTOR:
Senior Chemist W ildlife International Ltd.
DATE
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PROJECT NO.: 454C-106
QUALITY ASSURANCE STATEMENT
This study was examined for compliance with Good Laboratory Practice Standards as published by the U.S. Environmental Protection Agency in 40 CFR Part 792, 17 August 1989 and OECD Principles o f Good Laboratory Practice, OCDE/GD (92) 32, Environment Monograph No. 45, Paris 1992. The dates of all inspections and audits and the dates that any findings were reported to the Study Director and Laboratory Management were as follows:
ACTIVITY: Melting Point
Draft Report and Data
Final Report
DATE CONDUCTED: December 18,1998
DATE REPORTED TO:
STUDY DIRECTOR:
MANAGEMENT:
December 18,1998
December 18,1998
December 23,1998
December 23,1998
December 23,1998
February 1,1999
February 1,1999
February 1 ,1999
Linda R. Mitchell, B.S. Manager, Quality Assurance
DATE
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PROJECT NO.: 454C-106
REPORT APPROVAL
SPONSOR: 3M Corporation
TITLE: Determination o f the Melting Point/Melting Range o f PFOS
WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: 454C-106
STUDY DIRECTOR:
Ronda L. Jacobs Senior Chemist
MANAGEMENT:
r
W illard B. NSJixvonnn, PPlhi.DH .
7
Manager, Analytical Chemistry
DATE
DATE
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PROJECT NO.: 454C-106
TABLE OF CONTENTS
Title/Cover Page ................................................................................................................................................. 1
Good Laboratory Practice Compliance Statement ........................................................................................... 2
Quality Assurance Statement ............................................................................................................................ 3
Report Approval ...............................
4
Table o f Contents ............................................................................................................................................... 5
Summary ........................... ........\ ............................................ .......................................................................... 6
In tro d u c tio n .....................
7
Purpose ................
7
- Experimental D esig n ...........................
7
Materials and Methods .. ................................................................................................................................... 8
Test S ubstance........................................................................
8
Test P rocedure........................................................................
8
R e su lts............................... Melting Point and Melting Range ........................
9 9
C onclusions......................................................................................................................................................... 9
R eferences....................
10
TABLE
Table 1 - Determination o f M elting Point and Melting Range for Perfluorooctane Sulfonic Acid, Potassium Salt (P F O S ).......................................................... 11
APPENDIX Appendix I - Personnel Involved in the S tudy................................................................................................. 12
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SUMMARY
SPONSOR:
3M Corporation
sponsor's representative:
Ms. Susan A. Beach Environmental Laboratory P .0. Box 33331 St. Paul, Minnesota 55133
LOCATIONOF STUDY, RAWDATA AND A COPYOF THE FINAL REPORT:
Wildlife International Ltd. Easton, Maryland 21601
PROJECT NO.: 454C-106
WILDLIFE INTERNATIONAL LTD. PROJECT n u m b e r : TEST SUBSTANCE:
STUDY:
TEST DATES:
454C-106
Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) Determination o f the Melting Point/Melting Range o f PFOS
Experimental Start - December 18,1998 Experimental Termination - December 18,1998
Product Chem istry Test MELTING POINT:
R esu lts
M ethod
None, ;>400oC, discoloration observed /v0ECD 102
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INTRODUCTION
PROJECT NO.: 454C-106
Wildlife International Ltd. attempted to determine the melting point and melting range o f the test substance PFOS (perfluorooctane sulfonic acid, potassium salt). This study was conducted by Wildlife International Ltd. for 3M Corporation at the Wildlife International Ltd. analytical chemistry facility in Easton, Maryland. The study was performed following procedures in the OECD Guideline for Testing of Chemicals, 102, Melting Point/Melting Range (1). The experimental portion o f this study was conducted on December 18,1998. The original raw data generated by Wildlife International Ltd. and a copy o f the final report are filed under Project Number 454C-106 in archives located on the Wildlife International Ltd. site.
PURPOSE
The purpose of this study was to determine the melting point and melting range o f Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) .
EXPERIMENTAL DESIGN
The melting point is defined as the temperature at which the phase transition from a solid to a liquid state at atmospheric pressure occurs. For some substances, the transition occurs over a range o f temperatures defined as the melting range. Subsamples o f the test substance were heated in a melting point tube in a temperaturecontrolled heating block. Measurements o f the melting point/melting range were limited to s400C (approximately 673 K), the maximum specification for the instrumentation used. The temperature at which fine droplets adhere uniformly to the wall o f the melting point tube would be accepted as the melting point. If a temperature range was noted between the formation of the fine droplets (beginning o f melting) and transition to a liquid (raid o f melting), a melting range would be reported. A BOchi Melting Point B-540 instrument was used.
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M ATERIALS AND METHODS
PROJECT NO.: 454C-106
Test Substance The test substance was received from 3M Corporation on October 29,1998 and was assigned Wildlife
International Ltd. identification number 4675 upon receipt. The test substance, a white powder, was identified as: FC-95, Lot Number: 217, Expiration Date: 2008. The test substance was stored under ambient conditions.
Test Procedure A Buchi Melting Point B-540 instrument with melting point tubes supplied by Buchi was used. The Buchi
M elting Point B-540 instrument was calibrated and inspected just prior to use using anthraquinone and 1,8naphthalimide.
The melting point and melting range determination attempts were performed as follows. Subsamples o f the test substance were transferred to four melting point capillary tubes to a depth o f approximately 3 mm. The tubes were tamped to pack the test substance. One subsample was subjected to a rapid temperature scan to determine an approximate melting point. An approximate melting point could not be determined. The test substance turned a light brown color and then blackened. Fine droplets were not observed. The instrument was then programmed to increment the temperature over a range of 300 to 400C at a rate o f 1C/minute. The melting point and range determinations for the remaining three subsamples w oe attempted. A t no time during the testing o f Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) were fine droplets observed to adhere uniformly or otherwise to the walls o f the melting point tubes. The three remaining subsamples reacted in a sim ilar manner as the rapid temperature scan subsample. The white powder turned to a light brown. As the temperature increased, Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) darkened until it eventually turned black. When approaching 400C, some of the test substance lost the blackened color and turned to a clear, crystal-like particulate. The remaining test substance stayed black. The barometric pressure was recorded at the time o f the melting point/melting range determinations.
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RESULTS
PROJECT NO.: 454C-106
M elting Point and Melting Ranee The results of the melting point and melting range determinations are presented in Table 1. Fine droplets
were not observed to adhere uniformly or otherwise to the walls o f the melting point tubes. Therefore, a melting point/melting range for Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) was not determined.
CONCLUSIONS
A product chemistry test was performed to determine the physical characteristics o f the test substance Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS). The melting point/melting range was not observed and therefore could not be determined.
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PROJECT NO.: 454C-106
REFERENCES
1. Organisation for Economic Cooperation and Development. 102. Guideline for Testing o f Chemicals, 102: Melting Point/Melting Range.
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PROJECT NO.: 454C-106
Table 1
Determination o f Melting Point and Melting Range for Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS)
Subsample ID
Subsample Amount (mm)
Instrument Gradient (C/min)
Rep 1
3
1
Barometric Pressure (m m H g)
770
Rep 2
3
1
770
Rep 3
3
1
770
Melting Point
(C and K) None observed
None observed
None observed
Melting Range (C and K) None observed
None observed
None observed
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APPENDEXI Personnel Involved in the Study
PROJECT NO.: 454C-106
The following key Wildlife International Ltd. personnel were involved in the conduct or management o f this study:
1. Willard B. Nixon, Ph.D., Manager, Analytical Chemistry 2. Ronda L. Jacobs, Senior Ghemist 3. Keri Leach, Technician
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MELTING POINT
TEST SUBSTANCE
Identity: Perfluorooctanesulfonate; may also be referred to as PFOS or FC-95. (1-Octanesulfonic acid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-, potassium salt, CAS # 2795-39-3)
Remarks: The test substance is a white powder. Sample was taken from 3M lot number 217. Sample was stored under ambient conditions prior to testing. Purity determined to be 90.49% by LC/MS, 1H-HMR, 19FNMR and elemental analyses techniques.
METHOD
Method: OECD 102 GLP: Yes Year completed: 1998
Remarks: Study utilized a Biichi Melting Point B-540 instrument, calibrated and inspected just prior to use using anthraquinone and 1,8naphthalimide.
RESULTS
Melting point value in C: >400C (No melting observed). Decomposition (yes-temperature C/ no /ambiguous): No Sublimation (yes/no/ambiguous): No
Remarks: Measurements of the melting point / melting range were limited to <400C, the maximum specification for the instrument used. Fine droplets were not observed to adhere uniformly or otherwise to the walls of the melting point tubes.
CONCLUSIONS
The melting point / melting range was not observed and therefore could not be determined.
Remarks: While no melting of the test substance was evident, discoloration of the test samples was observed. The white powder turned to a light brown and eventually black as temperatures rose.
Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133
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DATA QUALITY Reliability: Klimisch ranking 1. REFERENCES Study conducted at the request of 3M Company by Wildlife International, Ltd. of Easton, Maryland. OTHER Last changed: 5/3/00
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