ASTM E2041-13(2018)
(Test Method)Standard Test Method for Estimating Kinetic Parameters by Differential Scanning Calorimeter Using the Borchardt and Daniels Method
Standard Test Method for Estimating Kinetic Parameters by Differential Scanning Calorimeter Using the Borchardt and Daniels Method
SIGNIFICANCE AND USE
6.1 This test method is useful in research and development.
6.2 The determination of the appropriate model for a chemical reaction or transformation and the values associated with its kinetic parameters may be used in the estimation of reaction performance at temperatures or time conditions not easily tested. This use, however, is not described in this test method.
SCOPE
1.1 This test method describes the determination of the kinetic parameters of activation energy, Arrhenius pre-exponential factor, and reaction order using the Borchardt and Daniels2 treatment of data obtained by differential scanning calorimetry. This test method is applicable to the temperature range from 170 to 870 K (−100 to 600°C).
1.2 This treatment is applicable only to smooth exothermic reactions with no shoulders, discontinuous changes, or shifts in baseline. It is applicable only to reactions with reaction order n ≤ 2. It is not applicable to acceleratory reactions and, therefore, is not applicable to the determination of kinetic parameters for most thermoset curing reactions or to crystallization reactions.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This test method is similar, but not equivalent to, ISO 11357, Part 5, that contains provisions for additional information not supplied by this test method.
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: E2041 − 13 (Reapproved 2018)
Standard Test Method for
Estimating Kinetic Parameters by Differential Scanning
1
Calorimeter Using the Borchardt and Daniels Method
This standard is issued under the fixed designation E2041; 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 2. Referenced Documents
3
2.1 ASTM Standards:
1.1 This test method describes the determination of the
E473 Terminology Relating to Thermal Analysis and Rhe-
kinetic parameters of activation energy, Arrhenius pre-
ology
exponential factor, and reaction order using the Borchardt and
2
E537 Test Method for The Thermal Stability of Chemicals
Daniels treatment of data obtained by differential scanning
by Differential Scanning Calorimetry
calorimetry. This test method is applicable to the temperature
E698 Test Method for Kinetic Parameters for Thermally
range from 170 to 870 K (−100 to 600°C).
Unstable Materials Using Differential Scanning Calorim-
1.2 This treatment is applicable only to smooth exothermic
etry and the Flynn/Wall/Ozawa Method
reactions with no shoulders, discontinuous changes, or shifts in
E967 Test Method for Temperature Calibration of Differen-
baseline. It is applicable only to reactions with reaction order
tial Scanning Calorimeters and Differential Thermal Ana-
n ≤ 2. It is not applicable to acceleratory reactions and,
lyzers
therefore, is not applicable to the determination of kinetic
E968 Practice for Heat Flow Calibration of Differential
parameters for most thermoset curing reactions or to crystalli-
Scanning Calorimeters
zation reactions.
E1142 Terminology Relating to Thermophysical Properties
E1445 Terminology Relating to Hazard Potential of Chemi-
1.3 The values stated in SI units are to be regarded as
cals
standard. No other units of measurement are included in this
E1641 Test Method for Decomposition Kinetics by Thermo-
standard.
gravimetry Using the Ozawa/Flynn/Wall Method
1.4 This test method is similar, but not equivalent to, E1970 Practice for Statistical Treatment of Thermoanalytical
ISO 11357, Part 5, that contains provisions for additional Data
4
information not supplied by this test method. 2.2 ISO Standards:
ISO 11357 Part 5: Determination of Temperature and/or
1.5 This standard does not purport to address all of the
Time of Reaction and Reaction Kinetics
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety, health, and environmental practices and deter-
3.1 Definitions—Specific technical terms used in this test
mine the applicability of regulatory limitations prior to use.
method are defined in Terminologies E473, E1142, and E1445,
1.6 This international standard was developed in accor-
including calibration, calorimeter, differential scanning
dance with internationally recognized principles on standard-
calorimetry, enthalpy, peak, reaction, repeatability,
ization established in the Decision on Principles for the
reproducibility, and slope.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
4. Summary of Test Method
Barriers to Trade (TBT) Committee.
4.1 A test specimen is heated at a linear rate in a differential
scanning calorimeter or other suitable calorimeter through a
region of exothermic reaction behavior. The rate of heat
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal
Measurements and the direct responsibility of Subcommittee E37.01 on Calorimetry
3
and Mass Loss. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2018. Published May 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ε1
approved in 1999. Last previous edition approved in 2013 as E2041 – 13 . DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E2041-13R18. the ASTM website.
2 4
Borchardt, H.J., Daniels, F., Journal of the American Chemical Society, Vol 79, Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
1957, pp. 41–46. 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 ----------------------
E2041 − 13 (2018)
evolution, developed by a chemical reaction, is proportional to 5.6 The values for dα/dt, (1 − α) and T needed to solve Eq
the rate of reaction. Integration of the heat flow as a function of
...
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.
´1
Designation: E2041 − 13 E2041 − 13 (Reapproved 2018)
Standard Test Method for
Estimating Kinetic Parameters by Differential Scanning
1
Calorimeter Using the Borchardt and Daniels Method
This standard is issued under the fixed designation E2041; 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
ε NOTE—Warning statements were editorially corrected throughout in September 2013.
1. Scope
1.1 This test method describes the determination of the kinetic parameters of activation energy, Arrhenius pre-exponential
2
factor, and reaction order using the Borchardt and Daniels treatment of data obtained by differential scanning calorimetry. This
test method is applicable to the temperature range from 170 to 870 K (−100 to 600°C).
1.2 This treatment is applicable only to smooth exothermic reactions with no shoulders, discontinuous changes, or shifts in
baseline. It is applicable only to reactions with reaction order
n ≤ 2. It is not applicable to acceleratory reactions and, therefore, is not applicable to the determination of kinetic parameters for
most thermoset curing reactions or to crystallization reactions.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This test method is similar, but not equivalent to, ISO 11357, Part 5, that contains provisions for additional information not
supplied by this test method.
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 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
3
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E537 Test Method for The Thermal Stability of Chemicals by Differential Scanning Calorimetry
E698 Test Method for Kinetic Parameters for Thermally Unstable Materials Using Differential Scanning Calorimetry and the
Flynn/Wall/Ozawa 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
E1445 Terminology Relating to Hazard Potential of Chemicals
E1641 Test Method for Decomposition Kinetics by Thermogravimetry Using the Ozawa/Flynn/Wall Method
E1970 Practice for Statistical Treatment of Thermoanalytical Data
4
2.2 ISO Standards:
ISO 11357 Part 5: Determination of Temperature and/or Time of Reaction and Reaction Kinetics
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and the direct responsibility of Subcommittee E37.01 on Calorimetry and
Mass Loss.
Current edition approved Sept. 15, 2013April 1, 2018. Published September 2013May 2018. Originally approved in 1999. Last previous edition approved in 20082013
ε1
as E2041 – 08E2041 – 13 . DOI: 10.1520/E2041-13E01.10.1520/E2041-13R18.
2
Borchardt, H.J., Daniels, F., Journal of the American Chemical Society, Vol 79, 1957, pp. 41–46.
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 ----------------------
E2041 − 13 (2018)
3. Terminology
3.1 Definitions—Specific technical terms used in this test method are defined in Terminologies E473, E1142, and E1445,
including calibration, calorimeter, differential scanning calorimetry, enthalpy, peak, reaction, repeatability, rep
...
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