ASTM E698-18
(Test Method)Standard Test Method for Kinetic Parameters for Thermally Unstable Materials Using Differential Scanning Calorimetry and the Flynn/Wall/Ozawa Method
Standard Test Method for Kinetic Parameters for Thermally Unstable Materials Using Differential Scanning Calorimetry and the Flynn/Wall/Ozawa Method
SIGNIFICANCE AND USE
5.1 The kinetic parameters combined with the general rate law and the reaction enthalpy can be used for the determination of thermal hazard using Practice E1231 (1).3
SCOPE
1.1 This test method covers the determination of the overall kinetic parameters for exothermic reactions using the Flynn/Wall/Ozawa method and differential scanning calorimetry.
1.2 This technique is applicable to reactions whose behavior can be described by the Arrhenius equation and the general rate law.
1.3 Limitations—There are cases where this technique is not applicable. Limitations may be indicated by curves departing from a straight line (see 11.2) or the isothermal aging test not closely agreeing with the results predicted by the calculated kinetic values. In particular, this test method is not applicable to reactions that are partially inhibited. The technique may not work with reactions that include simultaneous or consecutive reaction steps. This test method may not apply to materials that undergo phase transitions if the reaction rate is significant at the transition temperature.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
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Designation: E698 − 18
Standard Test Method for
Kinetic Parameters for Thermally Unstable Materials Using
Differential Scanning Calorimetry and the Flynn/Wall/Ozawa
1
Method
This standard is issued under the fixed designation E698; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
The kinetics of exothermic reactions are important in assessing the potential of materials and
systems for thermal explosion. This test method provides a means for determining Arrhenius
activation energies and pre-exponential factors using differential thermal methods. This test method is
to be used in conjunction with other tests to characterize the hazard potential of chemicals.
1. Scope ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 This test method covers the determination of the overall
mendations issued by the World Trade Organization Technical
kinetic parameters for exothermic reactions using the Flynn/
Barriers to Trade (TBT) Committee.
Wall/Ozawa method and differential scanning calorimetry.
1.2 This technique is applicable to reactions whose behavior
2. Referenced Documents
can be described by the Arrhenius equation and the general rate
2
2.1 ASTM Standards:
law.
E473 Terminology Relating to Thermal Analysis and Rhe-
1.3 Limitations—There are cases where this technique is not
ology
applicable. Limitations may be indicated by curves departing
E691 Practice for Conducting an Interlaboratory Study to
from a straight line (see 11.2) or the isothermal aging test not
Determine the Precision of a Test Method
closely agreeing with the results predicted by the calculated
E967 Test Method for Temperature Calibration of Differen-
kinetic values. In particular, this test method is not applicable
tial Scanning Calorimeters and Differential Thermal Ana-
to reactions that are partially inhibited. The technique may not
lyzers
work with reactions that include simultaneous or consecutive
E968 Practice for Heat Flow Calibration of Differential
reaction steps. This test method may not apply to materials that
Scanning Calorimeters
undergo phase transitions if the reaction rate is significant at
E1142 Terminology Relating to Thermophysical Properties
the transition temperature.
E1231 Practice for Calculation of Hazard Potential Figures
1.4 The values stated in SI units are to be regarded as
of Merit for Thermally Unstable Materials
standard. No other units of measurement are included in this
E1445 Terminology Relating to Hazard Potential of Chemi-
standard.
cals
1.5 This standard does not purport to address all of the
E1860 Test Method for Elapsed Time Calibration of Ther-
safety concerns, if any, associated with its use. It is the
mal Analyzers
responsibility of the user of this standard to establish appro-
E1970 Practice for Statistical Treatment of Thermoanalytical
priate safety, health, and environmental practices and deter-
Data
mine the applicability of regulatory limitations prior to use.
E2890 Test Method for Kinetic Parameters for Thermally
1.6 This international standard was developed in accor-
Unstable Materials by Differential Scanning Calorimetry
dance with internationally recognized principles on standard-
Using the Kissinger Method
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
2
rimetry and Mass Loss. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2018. Published June 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1979. Last previous edition approved in 2016 as E698 – 16. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E0698-18. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E698 − 18
3. Terminology 6.2.1.4 A means of sustaining a test chamber environment,
of an inert purge gas at a rate of 10 mL ⁄min to 50 mL ⁄min.
3.1 Technical terms used in this test method are defined in
Terminologies E473, E1142, and E1445 including activation
NOTE 1—Typically, 99+ % pure nitrogen, argon, or helium are em-
energy, Arrhenius equation, Celsius, differential scanning ployed when oxidation in air is a concern. Unless effects of moisture are
to be studied, use of dry purge gas is recommended; especially for
calorimetry, enthalpy, general rate l
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E698 − 16 E698 − 18
Standard Test Method for
Kinetic Parameters for Thermally Unstable Materials Using
Differential Scanning Calorimetry and the Flynn/Wall/Ozawa
1
Method
This standard is issued under the fixed designation E698; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
The kinetics of exothermic reactions are important in assessing the potential of materials and
systems for thermal explosion. This test method provides a means for determining Arrhenius
activation energies and pre-exponential factors using differential thermal methods. This test method is
to be used in conjunction with other tests to characterize the hazard potential of chemicals.
1. Scope*Scope
1.1 This test method covers the determination of the overall kinetic parameters for exothermic reactions using the
Flynn/Wall/Ozawa method and differential scanning calorimetry.
1.2 This technique is applicable to reactions whose behavior can be described by the Arrhenius equation and the general rate
law.
1.3 Limitations—There are cases where this technique is not applicable. Limitations may be indicated by curves departing from
a straight line (see 11.2) or the isothermal aging test not closely agreeing with the results predicted by the calculated kinetic values.
In particular, this test method is not applicable to reactions that are partially inhibited. The technique may not work with reactions
that include simultaneous or consecutive reaction steps. This test method may not apply to materials that undergo phase transitions
if the reaction rate is significant at the transition temperature.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all
of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate
safety safety, health, and healthenvironmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E967 Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers
E968 Practice for Heat Flow Calibration of Differential Scanning Calorimeters
E1142 Terminology Relating to Thermophysical Properties
E1231 Practice for Calculation of Hazard Potential Figures of Merit for Thermally Unstable Materials
E1445 Terminology Relating to Hazard Potential of Chemicals
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Calorimetry
and Mass Loss.
Current edition approved April 15, 2016June 1, 2018. Published April 2016June 2018. Originally approved in 1979. Last previous edition approved in 20112016 as
E698 – 11.E698 – 16. DOI: 10.1520/E0698-16.10.1520/E0698-18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E698 − 18
E1860 Test Method for Elapsed Time Calibration of Thermal Analyzers
E1970 Practice for Statistical Treatment of Thermoanalytical Data
E2890 Test Method for Kinetic Parameters for Thermally Unstable Materials by Differential Scanning Calorimetry Using the
Kissinger Method
3. Terminology
3.1 Technical terms used in this test method are defined in T
...
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