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Vapor Pressure Determination:
DuPont report 12735
Test Guideline^)
Authors Mary A. Kaiser, Ph.D. (study director) Daryl P. Cobranchi, Ph.D. Chin Ping Kao Robert C Buck, Ph. D.
Study Completion Date 16 July 2002 Report Date 21 March 2003
Test Facility DuPont Corporate Center for Analytical Sciences Experimental Station 402/5321 Wilmington, DE 19880-0402 And DuPont Center for Engineering Research Experimental Station 320 Wilmington, DE 19880-0320
Sponsor Telomer Research Panel c/o Rand Corporation
ARLte- 370
Vapor Pressure
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Vapor Pressure Determinationi
2 Table of Contents
Title Page............................................................................................
1
Table o f C ontents............................................................................... ...................................................... 2
1.0 Summary.............................................................................................................................................3
2.0 General Study Information.............................................................................................................. 3
3.0 Materials and M ethods.....................................................................................................................4
3.1 Test G uidelines............................................................................................................................. 4
3.2 Chemical S ystem .......................................................................................................................... 5
3.3 Test V ehicle.....................
5
3.4 Parameters O bserved..................................................................................
.-6
3.5 Result A nalysis............................................................................................................................. 6
3.6 Validity Criteria o f the Study.......................................................................................................6
4.0 Results and D iscussion............................
7
5.0 Conclusions....................................................................................................................................... 7
6.0 Retention o f R ecords..............................................................................
7
7.0 Disposal o f Test Item....................................................................................................................... 7
8.0 R eference............................................................................................................................................7
Figures
Figure 1 Scott Method Apparatus..........................
8
Figure 2 Vapor P r e s s u r e ^ ^ p | | | | | B H | ^ ^ ........................................................................... 9
Table Table 1. Vapor Pressure V alu es............................................................................................................ 9
Appendix Appendix A Chemical Analysis Summay............................................................................................ 10
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Vapor Pressure
Authors Mary A. Kaiser, Ph.D. (study director) Daryl P. Cobranchi, Ph.D. Robert C Buck, Ph. D. Chin Ping Kao
1.0 Summary
Test System:
pressure as a function o f temperature.
was used to determine its vapor
Findings:
The vapor pressure at 23C is approximately 3 Pa (0.022 Torr).
Conclusions:
The vapor pressure o: lO lkPaat 201C.
anged from 3 Pa at 23 C to
2.0 General Study Information
Study Objectives The objective o f this study was to determine the vapor pressure o
lunder defined conditions between 25
Test System Justification The test system was determined by the sponsor.
Study Personnel
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Vapor Pressure Determinationi
Management: Study Director: Principle Investigator: Technical Personnel:
Marianne Marsi, Ph.D. Mary A. Kaiser, Ph.D. Daryl P. Cobranchi, Ph.D. Barry W. Wolstenholme
Study Execution Dates
Study Initiation Date: Experimental Start Date: Experimental Completion Date: Study Completion Date:
15-Jun-2001 15-Jun-2001 28-June 2002 12-July 2002
3.0 Materials and Methods
3.1 Test Guidelines
The vapor pressure of a substance is defined as the saturation pressure above a solid or liquid substance. At thermodynamic equilibrium, the vapor pressure is only a function of temperature. The SI unit of pressure which should be used is the Pascal (Pa, Newton/m2). Units which have been employed historically are 1 Torr (mm Hg) =1.33 x 102Pa; 1 atmosphere = 1.013 x 105Pa; 1 bar = 105Pa. A modified OECD Guideline 104 (modified) was used for this measurement.
3.2.1
Chemical System
3.2.1.1 Test Substance
The test substance was obtained from Clarij chromatography, j is tentatively identified asl
Name: Synonym: Active substance(s) CAS Name:
CAS Number(s):
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H Number Lot Number: EMSE Sample Number: Concentration, nominal: Concentration, analyzed: Certifcate of Analysis Date: Date Received: Solubility at 25C.: Vapor pressure: Stability: Appearance/Color: Storage Conditions:
H-24691
03-Apr. 2001 15-June -2001 -140 ng L'1 TBD via this report Stable at ambient room temperature White solid Room temperature; keep tightly closed
3.2.1.2 Test Vehicle The test substance was th
3.3 Test Conduct
Two techniques were used to obtain the vapor pressure. The first method was based on a dynamic measurement procedure by Scott1w her^he equilibrium temperature is measured at a controlled pressure. Approximately 30 grams otV H B H vas placed in a boiler. The pressure was held constant to 0.01% (O.OlkPa) and m easuH ^M n accuracy of 0.01%. The apparatus consisted of a Mensor (San Marcos, TX) PCS400 pressure controller, a Paroscientific (Redmond, WA) 740 pressure transducer, and a Hart Scientific (American Fort UT) stack base unit for
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Vapor Pressure Determination:
. / `" " 'N temperature measurement. The temperature varied from 80 to 200C. A diagram of the apparatus is given in Figure 2. Table 1 shows the individual data points. The second procedure was based on the EPA OPPTS gas saturation method2. This second procedure is intended to confirm the lineagty of the curve obtained at the higher temperatures from the Scott method. T h e H M Iw a s placed directly in a glass thermostated tube. Gas-chromatographic grade h e l i u m j P |H || flowed over the powder. The flow was controlled by a flow controller on a Hewlett Packard (now AgfientJLittle Falls, DE) model 5890 gas chromatograph. Due to the adsorptive properties of th ^ H H flith e vapor pressure was calculated from weight loss rather than from the weight of trappecunaterial downstream. The vapor pressure at 21C was 0.02 Torr. Figure 3 gives the vapor pressure curve obtained from both sets of measurements.
3.3 Parameters Observed
With the Scott apparatus, pressure and temperature are observed.
With the GC/MS apparatus, peak height and peak area are observed.
3.4 Result Analysis
With the GC/MS apparatus the peak height or area is compared to the same parameter of a standard carefuly prepared in methanol.
3.5 Validity Criteria o f the Study
For GC/MS the peak areas of standards run before and after the test substance are compared. The results must agree within 5%.
4.0 Results and Discussion
The vapor pressure of t h e J H J |H H H H |H w a r i e d continuously from 3 Pa at 21C to 101 kPa at 201C. The results from the single point taken at 21C were aligned with the results from the 11 points taken at elevated temperatures taken by the Scott method.
5.0 Conclusions
The vapor pressure of thej 201C.
3 Pa at 21C and 101 kPa at
6.0 Retention of Records
Study documents and materials will be stored in the archives of the DuPont Experimental Station including but not limited to:
study protocol; any protocol and/or report amendments or addenda or deviations; all raw data; one original signed copy of the final report;
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Vapor Pressure Determination
laboratory-specific or site-specific raw data such as personnel files, instrument, equipment, refrigerator, and/or freezer raw data.
7.0 Disposal of Test Item
After issuance of the final report, the remaining test substance will be stored at the DuPont Glasgow site until its expiration date and then destroyed by burning, unless other arrangements are made between the sponsor and the Test Facility.
8.0 References
1. L. Scott, "Determination of Activity Coefficients by Accurate Measurement of Boiling Point Diagram", Fluid Phase Equilibrium, 26,(1986), 149-163.
2. United States Environmental Protection Agency, Prevention, Pesticides and Toxic Substances (7101), OPPTS 830.7950, Vapor Pressure, August 1995, page 4, Gas Saturation Method.
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Vapor Pressure Determination
Figure 1. Scott Method Apparatus Boiler
Platinum e tist n c c
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Vapor Pressure Determination:
Figure 2. Vapor Pressure
T em perature (C)
Table 1. Vapor Pressure Values
Tem perature (C) Vapor Pressure (Torr) Vapor Pressure (Pa)
Method
21 0 .0 2 2
3 Gas Saturation M ethod
84 5
708 Scott Method
96 11
1465
Scott Method
107 21
2774
Scott Method
119 37
4910
Scott M ethod
130 62
8284
Scott M ethod
142 103 155 171 166 258 179 388 190 543
13798 22752 34449 51667 72339
Scott Method Scott M ethod Scott Method Scott Method Scott Method
201
755
100607
Scott Method
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Vapor Pressure Determination
Appendix A
Analysis Summary
The subject material was analyzed by gas-chromatography using a
standard method toassess its composition. This analysis showecHhaUhe
m aterialeom prisedB B M ttfiS ii^to
The b a fa n e e J jB jJ v a s not
_ ______ ______
l a ta lim itofquantitation of
'/o. rurther analysis by GC/MS suggests ffiat
a single impurity,
whose chemical structure is|*
"*
Finally, the subject material was evaluated by High Performance Liquid
^ h ro ijijjjj^
for the presence of
Based upon these analyses, we conclude that methods are in hand to determine and confirm the composition of H-24691 to be as follows:
Material
Wt. % f+0.3)
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