ASTM E698-11
(Test Method)Standard Test Method for Arrhenius Kinetic Constants for Thermally Unstable Materials Using Differential Scanning Calorimetry and the Flynn/Wall/Ozawa Method
Standard Test Method for Arrhenius Kinetic Constants for Thermally Unstable Materials Using Differential Scanning Calorimetry and the Flynn/Wall/Ozawa Method
SIGNIFICANCE AND USE
The Arrhenius parameters combined with the general rate law and the reaction enthalpy can be used for the determination of thermal explosion hazards (1)
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.
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Designation: E698 − 11
StandardTest Method for
Arrhenius Kinetic Constants for Thermally Unstable
Materials Using Differential Scanning Calorimetry and the
1
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.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
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 establish appropriate safety and health practices and deter-
mine the applicability of regulatory limitations prior to use.
1.1 This test method covers the determination of the overall
kinetic parameters for exothermic reactions using the Flynn/
2. Referenced Documents
Wall/Ozawa method and differential scanning calorimetry.
2
2.1 ASTM Standards:
1.2 Thistechniqueisapplicabletoreactionswhosebehavior
E473Terminology Relating to Thermal Analysis and Rhe-
canbedescribedbytheArrheniusequationandthegeneralrate
ology
law.
E691Practice for Conducting an Interlaboratory Study to
1.3 Limitations—Therearecaseswherethistechniqueisnot
Determine the Precision of a Test Method
applicable. Limitations may be indicated by curves departing
E968Practice for Heat Flow Calibration of Differential
from a straight line (see 11.2) or the isothermal aging test not
Scanning Calorimeters
closely agreeing with the results predicted by the calculated
E1142Terminology Relating to Thermophysical Properties
kinetic values. In particular, this test method is not applicable
E1445Terminology Relating to Hazard Potential of Chemi-
to reactions that are partially inhibited. The technique may not
cals
work with reactions that include simultaneous or consecutive
E1860Test Method for Elapsed Time Calibration of Ther-
reactionsteps.Thistestmethodmaynotapplytomaterialsthat
mal Analyzers
undergo phase transitions if the reaction rate is significant at
E1970PracticeforStatisticalTreatmentofThermoanalytical
the transition temperature.
Data
1.4 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
standard.
3.1 Technical terms used in this test method are defined in
1.5 This standard may involve hazardous materials, Terminologies E473, E1142, and E1445.
operations, and equipment. This standard does not purport to
address all of the safety concerns, if any, associated with its 4. Summary of Test Method
use. It is the responsibility of the user of this standard to
4.1 Asampleisplacedinasuitablecontainerandpositioned
in a differential scanning calorimeter (DSC).
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 March 1, 2011. Published March 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1979. Last previous edition approved in 2005 as E698–05. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E0698-11. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E698 − 11
4.2 The sample equipment temperature is increased at a 6.2.3 A data collection device, to provide a means of
linear rate and any exothermic reaction peaks recorded. acquiring, storing, and displaying measured or calculated
signals, or both. The minimum output signals required for
4.3 Steps 4.1 and 4.2 are repeated for several heating rates
–1 differential scanning calorimetry are heat flow, temperature,
in the range from 1 to 10Kmin .
and time.
4.4 Temperatures at which the reaction peak maxima occur
6.3 Containers (pans, crucibles, vials, etc), which are inert
are plotted as a function of their respective heating rates.
to the specimen and reference materials and which are suitable
4.5 Kinetic values calculated from the peak temperature-
structural shape and integrity to contain the specimen and
heating rate relationship are used to predict a reaction half-life
reference in accordance with the
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:E698–05 Designation:E698–11
Standard Test Method for
Arrhenius Kinetic Constants for Thermally Unstable
Materials Using Differential Scanning Calorimetry and the
1
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.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
one of several test methods being developed byASTM 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
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—Therearecaseswherethistechniqueisnotapplicable.Limitationsmaybeindicatedbycurvesdepartingfrom
astraightline(see11.2)ortheisothermalagingtestnotcloselyagreeingwiththeresultspredictedbythecalculatedkineticvalues.
In particular, this test method is not applicable to reactions that are partially inhibited.The technique may not work with reactions
thatincludesimultaneousorconsecutivereactionsteps.Thistestmethodmaynotapplytomaterialsthatundergophasetransitions
if the reaction rate is significant at the transition temperature.
1.4SI units are the standard.
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
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
3. Terminology
3.1 Technical terms used in this test method are defined in Terminologies E473, E1142, and E1445.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE27onHazardPotentialofChemicalsandisthedirectresponsibilityofSubcommitteeE27.02onThermal
Stability and Condensed Phases.
CurrenteditionapprovedMarch1,2005.2011.PublishedApril2005.March2011.Originallyapprovedin1979.Lastpreviouseditionapprovedin20042005asE698–015.
DOI: 10.1520/E0698-05.10.1520/E0698-11.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
E698–11
4. Summary of Test Method
4.1 A sample is placed in a suitable container and positioned in a differential scanning calorimeter (DSC).
4.2 The sample equipment temperature is increased at a linear rate and any exothermic reaction peaks recorded.
-1–1
4.3 Steps 4.1 and 4.2 are repeated for several heating rates in the range from 1 to 10Kmin .
4.4 Temperatures at which the reaction peak maxima occur are plotted as a function of their respective heating rates.
4.5 Kinetic values calculated from the peak temperature-heating rate relationship are used to predict a reaction half-life at a
selected temperature.
4.6 A sample is aged at the selected temperature for the predicted half-life time.
4.7 Theagedsampleistemperaturep
...
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