ASTM E1641-16
(Test Method)Standard Test Method for Decomposition Kinetics by Thermogravimetry Using the Ozawa/Flynn/Wall Method
Standard Test Method for Decomposition Kinetics by Thermogravimetry Using the Ozawa/Flynn/Wall Method
SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the temperature-decomposition profile of a material.
5.2 This test method can be used for estimating lifetimes of materials, using Test Method E1877 provided that a relationship has been established between the thermal endurance test results and actual lifetime tests.
SCOPE
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and pre-exponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kinetics using the Ozawa/Flynn/Wall isoconversional method (1, 2).2
1.2 This test method is generally applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change with a single maximum rate.
1.3 This test method is normally applicable to decomposition occurring in the range from 400 to 1300 K (nominally 100 to 1000°C). The temperature range may be extended depending on the instrumentation used.
1.4 This test method is similar to ISO 11358-2 but differs in its mathematical treatment.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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: E1641 − 16
Standard Test Method for
Decomposition Kinetics by Thermogravimetry Using the
1
Ozawa/Flynn/Wall Method
This standard is issued under the fixed designation E1641; 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.
1. Scope* 2. Referenced Documents
3
1.1 This test method describes the determination of the 2.1 ASTM Standards:
kinetic parameters, Arrhenius activation energy, and pre- E29Practice for Using Significant Digits in Test Data to
exponential factor by thermogravimetry, based on the assump- Determine Conformance with Specifications
tion that the decomposition obeys first-order kinetics using the E473Terminology Relating to Thermal Analysis and Rhe-
2
Ozawa/Flynn/Wall isoconversional method (1, 2). ology
E691Practice for Conducting an Interlaboratory Study to
1.2 This test method is generally applicable to materials
Determine the Precision of a Test Method
with well-defined decomposition profiles, namely, a smooth,
E1142Terminology Relating to Thermophysical Properties
continuous mass change with a single maximum rate.
E1582Test Method forTemperature Calibration ofThermo-
1.3 This test method is normally applicable to decomposi-
gravimetric Analyzers
tionoccurringintherangefrom400to1300K(nominally100
E1877Practice for Calculating Thermal Endurance of Ma-
to1000°C).Thetemperaturerangemaybeextendeddepending
terials from Thermogravimetric Decomposition Data
on the instrumentation used.
E1970PracticeforStatisticalTreatmentofThermoanalytical
1.4 This test method is similar to ISO11358-2 but differs in Data
E2040Test Method for Mass Scale Calibration of Thermo-
its mathematical treatment.
gravimetric Analyzers
1.5 The values stated in SI units are to be regarded as
4
2.2 Other Standard:
standard. No other units of measurement are included in this
ISO11358-2 Plastics Thermogravimetry (TG) of Polymers
standard.
Part 2: Determination of Kinetic Parameters
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions—Technical terms used in this test method
priate safety, health, and environmental practices and deter-
are defined in Terminologies E473 and E1142 and include
mine the applicability of regulatory limitations prior to use.
activation energy, Celsius, failure, failure criterion, and ther-
1.7 This international standard was developed in accor-
mogravimetric analyzer.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Summary of Test Method
Development of International Standards, Guides and Recom-
4.1 Thistestmethodisbaseduponthegeneralrateequation
mendations issued by the World Trade Organization Technical
that takes the form of:
Barriers to Trade (TBT) Committee.
dα⁄dT 5 A 1 2 α exp 2 E ⁄RT ⁄β (1)
~ ! @ #
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
3
rimetry and Mass Loss. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 15, 2016. Published February 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1994. Last previous edition approved in 2015 as E1641–15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1641-16. the ASTM website.
2 4
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
this standard. 4th Floor, New York, NY 10036, http://www.ansi.org.
*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 ----------------------
E1641 − 16
TABLE 1 Numerical Integration Constants
where:
E/RT a b
α = fraction reacted (dimensionless),
-1
8 5.3699 0.5398
A = pre-exponential factor (min ),
9 5.8980 0.5281
β = heating rate (K/min),
10 6.4167 0.5187
E = activation energy (J/mol),
11 6.928 0.511
R = gas constant (=8.316 J/(mol K)),
12 7.433 0.505
13 7.933 0.500
T = absolute temperature (K),
14 8.427 0.494
exp = Euler’s number exponential, and
15 8.918 0.491
dα/dT = rate of change of α with T.
16 9.406 0.488
17 9.890 0.484
4.2 Using the method of Ozawa, Flynn and Wall (1, 2), Eq
18 10.372 0.482
1 may be solved for activation energy:
19 10.851 0.479
20 11.3277 0.4770
E 5 R ⁄ b
...
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: E1641 − 15 E1641 − 16
Standard Test Method for
Decomposition Kinetics by Thermogravimetry Using the
1
Ozawa/Flynn/Wall Method
This standard is issued under the fixed designation E1641; 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.
1. Scope Scope*
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and preexponentialpre-
exponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kineticsusing kinetics
2
using the Ozawa/Flynn/Wall isoconversional method (1, 2).
1.2 This test method is generally applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous
mass change with a single maximum rate.
1.3 This test method is normally applicable to decomposition occurring in the range from 400 to 1300K 1300 K (nominally 100
to 1000°C). The temperature range may be extended depending on the instrumentation used.
1.4 This test method is similar to ISO 11358-2 but differs in its mathematical treatment.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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
3
2.1 ASTM Standards:
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E473 Terminology Relating to Thermal Analysis and Rheology
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1142 Terminology Relating to Thermophysical Properties
E1582 Practice for Calibration of Temperature Scale for Thermogravimetry
E1877 Practice for Calculating Thermal Endurance of Materials from Thermogravimetric Decomposition Data
E1970 Practice for Statistical Treatment of Thermoanalytical Data
E2040 Test Method for Mass Scale Calibration of Thermogravimetric Analyzers
4
2.2 Other Standard:
ISO 11358-2 Plastics Thermogravimetry (TG) of Polymers Part 2: Determination of Kinetic Parameters
3. Terminology
3.1 Definitions—Technical terms used in this test method are defined in Terminologies E473 and E1142 and include activation
energy, Celsius, failure, failure criterion, and thermogravimetric analyzer.
4. Summary of Test Method
4.1 This test method is based upon the general rate equation that takes the form of:
dα⁄dT 5 A 1 2 α exp@2 E ⁄ R T#⁄β (1)
~ !
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, 2015Feb. 15, 2016. Published March 2015February 2016. Originally approved in 1994. Last previous edition approved in 20132015
as E1641 – 13.E1641 – 15. DOI: 10.1520/E1641-15.10.1520/E1641-16.
2
The boldface numbers in parentheses refer to the list of references at the end of this standard.
3
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.
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
*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 ----------------------
E1641 − 16
where:
α = fraction reacted (dimensionless),
-1
A = pre-exponential factor (min ),
β = heating rate (K/min),
E = activation energy (J/mol),
R = gas constant (=8.316 J/(mol K)),
T = absolute temperature (K),
exp = Euler’s number exponential, and
dα/dT = rate of change of α with T.
4.2 Using the method of Ozawa, Flynn and Wall (1, 2),Eq 1 may be solved for activation energy:
E 5 ~R ⁄ b! Δlog@β#⁄Δ~1 ⁄ T! (2)
where:
E = the derivative of the Doyle approximation (3) with values tabulated in Table 1.
4.3 Using a point of constant conversion from a s
...
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