ASTM E698-16

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 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 14-Apr-2016
• ICS: 19.040 - Environmental testing
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.01 - Calorimetry and Mass Loss

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E698 − 16
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.Anumber 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
activationenergiesandpre-exponentialfactorsusingdifferentialthermalmethods.Thistestmethodis
to be used in conjunction with other tests to characterize the hazard potential of chemicals.
1. Scope* 2. Referenced Documents
2
1.1 This test method covers the determination of the overall
2.1 ASTM Standards:
kinetic parameters for exothermic reactions using the Flynn/
E473Terminology Relating to Thermal Analysis and Rhe-
Wall/Ozawa method and differential scanning calorimetry.
ology
E691Practice for Conducting an Interlaboratory Study to
1.2 Thistechniqueisapplicabletoreactionswhosebehavior
Determine the Precision of a Test Method
canbedescribedbytheArrheniusequationandthegeneralrate
E968Practice for Heat Flow Calibration of Differential
law.
Scanning Calorimeters
1.3 Limitations—Therearecaseswherethistechniqueisnot
E1142Terminology Relating to Thermophysical Properties
applicable. Limitations may be indicated by curves departing
E1231Practice for Calculation of Hazard Potential Figures
from a straight line (see 11.2) or the isothermal aging test not
of Merit for Thermally Unstable Materials
closely agreeing with the results predicted by the calculated
E1445Terminology Relating to Hazard Potential of Chemi-
kinetic values. In particular, this test method is not applicable
cals
to reactions that are partially inhibited. The technique may not
E1860Test Method for Elapsed Time Calibration of Ther-
work with reactions that include simultaneous or consecutive
mal Analyzers
reactionsteps.Thistestmethodmaynotapplytomaterialsthat
E1970PracticeforStatisticalTreatmentofThermoanalytical
undergo phase transitions if the reaction rate is significant at
Data
the transition temperature.
E2890Test Method for Kinetic Parameters for Thermally
1.4 The values stated in SI units are to be regarded as Unstable Materials by Differential Scanning Calorimetry
standard. No other units of measurement are included in this Using the Kissinger Method
standard.
3. Terminology
1.5 This standard may involve hazardous materials,
operations, and equipment. This standard does not purport to
3.1 Technical terms used in this test method are defined in
address all of the safety concerns, if any, associated with its
Terminologies E473, E1142, and E1445 including activation
use. It is the responsibility of the user of this standard to
energy, Arrhenius equation, Celsius, differential scanning
establish appropriate safety and health practices and deter-
calorimetry, enthalpy, general rate law, Kelvin, kinetics, peak
mine the applicability of regulatory limitations prior to use.
value, pre-exponential factor, reaction, reaction order, and
temperature.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
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 April 15, 2016. Published April 2016. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1979. Last previous edition approved in 2011 as E698–11. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E0698-16. 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 − 16
4. Summary of Test Method between selected temperature limits at a rate of temperature
change between 0.5 and 10K⁄min constant to 60.1K⁄min or
4.1 A specimen is placed in a suitable container and
at an isothermal temperature constant to 60.1K.
positioned in a differential scanning calorimeter (DSC).
6.2.3 A data collection device, to provide a means of
4.2 The temperature surrounding the specimen is increased
acquiring, storing, and displaying measured or calculated
at a linear rate and any exothermic reaction peaks recorded.
signals, or both. The minimum output signals required for
4.3 Steps 4.1 and 4.2 are repeated for
...

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 − 11 E698 − 16
Standard Test Method for
Arrhenius Kinetic ConstantsParameters for Thermally
Unstable Materials Using Differential Scanning Calorimetry
1
and the Flynn/Wall/Ozawa 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
one of several test methods being developed by ASTM Committee E27 for chemical reactions. 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 and health practices and determine the applicability of regulatory limitations prior to use.
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
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
E1860 Test Method for Elapsed Time Calibration of Thermal Analyzers
E1970 Practice for Statistical Treatment of Thermoanalytical Data
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 March 1, 2011April 15, 2016. Published March 2011April 2016. Originally approved in 1979. Last previous edition approved in 20052011 as
E698 – 05.E698 – 11. DOI: 10.1520/E0698-11.10.1520/E0698-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 − 16
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 Terminologies E473, E1142, and E1445. including activation energy,
Arrhenius equation, Celsius, differential scanning calorimetry, enthalpy, general rate law, Kelvin, kinetics, peak value,
pre-exponential factor, reaction, reaction order, and temperature.
4. Summary of Test Method
4.1 A samplespecimen is placed in a suitable container an
...