ASTM E3174-22

Standard Practice for Determination of Kinetic Reaction Model Using Differential Scanning Calorimetry

SIGNIFICANCE AND USE
5.1 Information concerning the reaction model aids in the selection of the appropriate method (and test method) for evaluation of kinetic parameters. nth order reaction may be treated by isoconversion methods such as Test Methods E698 and E2890. Autocatalytic reactions are treated by Test Methods E2070.  
5.2 This practice may be used in research, forensic analysis, trouble shooting, product evaluation, and hazard potential evaluation.
SCOPE
1.1 This practice describes a procedure for determining the “model” of an exothermic reaction using differential scanning calorimetry. The procedure is typically performed on 1 mg to 3 mg specimen sizes over the temperature range from ambient to 600 °C.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  
1.4 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

• Status: Published
• Publication Date: 31-May-2022
• ICS: 17.200.10 - Heat. Calorimetry
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.01 - Calorimetry and Mass Loss

Relations

• Refers: ASTM E537-20 - Standard Test Method for Thermal Stability of Chemicals by Differential Scanning Calorimetry
• Effective Date: 01-Feb-2020

Standards Content (Sample)

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.
Designation: E3174 − 22
Standard Practice for
Determination of Kinetic Reaction Model Using Differential
1
Scanning Calorimetry
This standard is issued under the fixed designation E3174; 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* E968 Practice for Heat Flow Calibration of Differential
Scanning Calorimeters
1.1 This practice describes a procedure for determining the
E1142 Terminology Relating to Thermophysical Properties
“model” of an exothermic reaction using differential scanning
E2070 Test Methods for Kinetic Parameters by Differential
calorimetry. The procedure is typically performed on 1 mg to
Scanning Calorimetry Using Isothermal Methods
3 mg specimen sizes over the temperature range from ambient
E2890 Test Method for Determination of Kinetic Parameters
to 600 °C.
and Reaction Order for Thermally Unstable Materials by
1.2 The values stated in SI units are to be regarded as
Differential Scanning Calorimetry Using the Kissinger
standard. No other units of measurement are included in this
and Farjas Methods
standard.
E3142 Test Method for Thermal Lag of Thermal Analysis
1.3 This standard does not purport to address all of the
Apparatus
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 standard are
priate safety, health, and environmental practices and deter-
provided in Terminologies E473 and E1142 including:
mine the applicability of regulatory limitations prior to use.
calorimeter, Celsius, derivative, differential scanning
1.4 This international standard was developed in accor-
calorimeter, extrapolated onset, Kelvin, reaction, reaction
dance with internationally recognized principles on standard-
order, and temperature.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
3.2 Definitions of Terms Specific to This Standard:
mendations issued by the World Trade Organization Technical
3.2.1 autocatalytic, n—a chemical reaction where one or
Barriers to Trade (TBT) Committee.
more reaction products are a catalyst for the same reaction.
3.2.1.1 Discussion—An example of an autocatalytic model
2. Referenced Documents
is:
2
2.1 ASTM Standards:
m n
dα⁄dt 5α k 1 2 α (1)
~ !
E473 Terminology Relating to Thermal Analysis and Rhe-
ology
where:
E537 Test Method for Thermal Stability of Chemicals by
α = the fraction reacted,
Differential Scanning Calorimetry
t = time,
E698 Test Method for Kinetic Parameters for Thermally
k = the rate constant, and
Unstable Materials Using Differential Scanning Calorim-
m and n = the reaction orders.
etry and the Flynn/Wall/Ozawa Method
3.2.2 autocatalytic model, n—a kinetic model used to de-
E967 Test Method for Temperature Calibration of Differen-
scribe an autocatalytic reaction.
tial Scanning Calorimeters and Differential Thermal Ana-
3.2.3 exotherm, n—in thermal analysis, the thermal record
lyzers
of a transition where heat is evolved by the specimen.
1
This practice is under the jurisdiction of ASTM Committee E37 on Thermal 3.2.4 model, kinetic, n—a mathematical construct used to
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
describe the rates of a chemical reaction.
rimetry and Mass Loss.
3.2.5 nth order, n—a kinetic model in which the rate of
CurrenteditionapprovedJune1,2022.PublishedJuly2022.Originallyapproved
in 2019. Last previous edition approved in 2021 as E3174 – 21. DOI: 10.1520/
reaction (dα⁄dt) is proportional to the power of the current
E3174-22.
concentration of the reactant(s).
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
3.2.5.1 Discussion—An example of an nth order model is:
Standards volume information, refer to the standard’s Document Summary page on
n
the ASTM website. dα⁄dt 5 k 1 2 α (2)
~ !
*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 ----------------------
E3174 − 22
where: signals, or both. The minimum output signals required for
differential scanning calorimetry are heat flow, temperature,
α = the fraction reacted,
and time.
t = time,
k = the rate constant, and 6.1.5 Containers (pans,
...

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: E3174 − 21 E3174 − 22
Standard Practice for
Determination of Kinetic Reaction Model Using Differential
1
Scanning Calorimetry
This standard is issued under the fixed designation E3174; 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 practice describes a procedure for determining the “model” of an exothermic reaction using differential scanning
calorimetry. The procedure is typically performed on 1 mg to 3 mg specimen sizes over the temperature range from ambient to
600 °C.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
1.4 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
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E537 Test Method for 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
E2070 Test Methods for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods
E2890 Test Method for Determination of Kinetic Parameters and Reaction Order for Thermally Unstable Materials by
Differential Scanning Calorimetry Using the Kissinger and Farjas Methods
E3142 Test Method for Thermal Lag of Thermal Analysis Apparatus
3. Terminology
3.1 Definitions—Technical terms used in this standard are provided in Terminologies E473 and E1142 including: calorimeter,
Celsius, derivative, differential scanning calorimeter, extrapolated onset, Kelvin, reaction, reaction order, and temperature.
1
This practice 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 May 1, 2021June 1, 2022. Published July 2021July 2022. Originally approved in 2019. Last previous edition approved in 20202021 as E3174
– 20.21. DOI: 10.1520/E3174-21.10.1520/E3174-22.
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 ----------------------
E3174 − 22
3.2 Definitions of Terms Specific to This Standard:
3.2.1 autocatalytic, n—a chemical reaction where one or more reaction products are a catalyst for the same reaction.
3.2.1.1 Discussion—
An example of an autocatalytic model is:
m n
α⁄dt 5 α k 1 2 α (1)
~ !
m n
dα⁄dt 5 α k~1 2 α! (1)
where:
α = the fraction reacted,
t = time,
k = the rate constant, and
m and n = the reaction orders.
3.2.2 autocatalytic model, n—a kinetic model used to describe an autocatalytic reaction.
3.2.3 exotherm, n—in thermal analysis, the thermal record of a transition where heat is evolved by the specimen.
3.2.4 model, kinetic, n—a mathematical construct used to describe the rates of a chemical reaction.
3.2.5 nth order, n—a kinetic model in which the rate of reaction (dα⁄dt) is proportional to the power of the current concentration
of the reactant(s).
3.2.5.1 Discussion—
An example of an nth order model is:
n
dα⁄dt 5 k 1 2 α (2)
~ !
where
n
dα⁄dt 5 k~1 2 α! (2)
...