ASTM E1641-13
(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 preexponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kineticsusing 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 (nominally 100 to 1000°C). The temperature range may be extended depending on the instrumentation used.
1.4 This 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 − 13
StandardTest 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 Determine the Precision of a Test Method
E1142Terminology Relating to Thermophysical Properties
1.1 This test method describes the determination of the
E1582Practice for Calibration of Temperature Scale for
kinetic parameters, Arrhenius activation energy, and preexpo-
Thermogravimetry
nential factor by thermogravimetry, based on the assumption
E1877Practice for Calculating Thermal Endurance of Ma-
that the decomposition obeys first-order kineticsusing the
2 terials from Thermogravimetric Decomposition Data
Ozawa/Flynn/Wall isoconversional method (1).
E1970PracticeforStatisticalTreatmentofThermoanalytical
1.2 This test method is generally applicable to materials
Data
with well-defined decomposition profiles, namely, a smooth,
E2040Test Method for Mass Scale Calibration of Thermo-
continuous mass change with a single maximum rate.
gravimetric Analyzers
4
1.3 This test method is normally applicable to decomposi-
2.2 Other Standard:
tion occurring in the range from 400 to 1300K (nominally 100
ISO11358-2 Plastics Thermogravimetry (TG) of Polymers
to1000°C).Thetemperaturerangemaybeextendeddepending
Part 2: Determination of Kinetic Parameters
on the instrumentation used.
3. Terminology
1.4 This method is similar to ISO11358-2 but differs in its
mathematical treatment. 3.1 Definitions—Technical terms used in this test method
are defined in Terminologies E473 and E1142 and include
1.5 The values stated in SI units are to be regarded as
activation energy, Celsius, failure, failure criterion, and ther-
standard. No other units of measurement are included in this
mogravimetric analyzer.
standard.
1.6 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 This test method consists of heating a series of four or
responsibility of the user of this standard to establish appro-
more test specimens, taken from the original sample, each at a
priate safety and health practices and determine the applica-
different heating rate between 1 and 10 K/min, through their
bility of regulatory limitations prior to use.
decompositionregion.Thespecimenmassisrecordedcontinu-
ously as a function of temperature. The temperatures for
2. Referenced Documents
constant conversion are determined from the resultant mass
3
2.1 ASTM Standards:
losscurves.TheArrheniusactivationenergyisthendetermined
E473Terminology Relating to Thermal Analysis and Rhe-
from a plot of the logarithm of heating rate versus the
ology
reciprocal of the absolute temperature at constant conversion
E691Practice for Conducting an Interlaboratory Study to
level.
4.2 This activation energy may then be used to calculate
thermal endurance and an estimate of the lifetime of the
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
material at a certain temperature using Test Method E1877.
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
rimetry and Mass Loss.
Current edition approved Aug. 1, 2013. Published September 2013. Originally
5. Significance and Use
approved in 1994. Last previous edition approved in 2012 as E1641–07 (2012).
DOI: 10.1520/E1641-13. 5.1 Thermogravimetry provides a rapid method for deter-
2
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
mining the temperature-decomposition profile of a material.
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
4
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1641 − 13
5.2 This test method can be used for estimating lifetimes of 7.3 Toxic or corrosive effluents, or both, may be released
materials, using Test Method E1877 provided that a relation- duringtheheatingprocessandmaybeharmfultothepersonnel
ship has been established between the thermal endurance test or apparatus.
results and actual lifetime tests.
8. Sampling
6. Apparatus
8.1 Powdered or granular specimens that have a high
...
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 − 07 (Reapproved 2012) E1641 − 13
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
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and preexponential
factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kinetics. kineticsusing the
2
Ozawa/Flynn/Wall isoconversional method (1).
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 (100 to 1000 °C).
(nominally 100 to 1000°C). The temperature range may be extended depending on the instrumentation used.
1.4 Computer or electronic-based instruments, techniques, or data treatment equivalent to this test method may also be used.
This method is similar to ISO 11358-2 but differs in its mathematical treatment.
NOTE 1—Users of this test method are expressly advised that all such instruments or techniques may not be equivalent. It is the responsibility of the
user of this test method to determine the necessary equivalency prior to use.
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 method is similar to ISO 11358-2 but differs in its mathematical treatment.
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:
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:DefinitionsTechnical—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.
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 Sept. 1, 2012Aug. 1, 2013. Published September 2012September 2013. Originally approved in 1994. Last previous edition approved in 20072012
as E1641 – 07.E1641 – 07 (2012). DOI: 10.1520/E1641-07R12.10.1520/E1641-13.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1641 − 13
4. Summary of Test Method
4.1 This test method consists of heating a series of four or more test specimens, taken from the original sample, each at a
different heating rate between 1 and 10 K/min, through their decomposition region. The specimen mass is recorded continuously
as a function of temperature. The temperatures for constant conversion are determined from the resultant mass loss curves. The
...
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