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ASTM E3174-19

(Practice)

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

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 1–3 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
Historical
Publication Date
14-Feb-2019
ICS
17.200.10 - Heat. Calorimetry
Technical Committee
E37 - Thermal Measurements
Drafting Committee
E37.01 - Calorimetry and Mass Loss
Current Stage
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ASTM E3174-19 - Standard Practice for Determination of Kinetic Reaction Model Using Differential Scanning CalorimetryASTM E3174-19 - Standard Practice for Determination of Kinetic Reaction Model Using Differential Scanning Calorimetry
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ASTM E3174-19 - Standard Practice for Determination of Kinetic Reaction Model Using Differential Scanning Calorimetry
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E3174 − 19
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 1–3 mg
Scanning Calorimetry Using Isothermal Methods
specimensizesoverthetemperaturerangefromambientto600
E2890 Test Method for Kinetic Parameters for Thermally
°C.
Unstable Materials by Differential Scanning Calorimetry
1.2 The values stated in SI units are to be regarded as
Using the Kissinger Method
standard. No other units of measurement are included in this
standard.
3. Terminology
1.3 This standard does not purport to address all of the
3.1 Definitions—Technical terms used in this standard are
safety concerns, if any, associated with its use. It is the
provided in Terminologies E473 and E1142 including:
responsibility of the user of this standard to establish appro-
calorimeter, Celsius, derivative, differential scanning
priate safety, health, and environmental practices and deter-
calorimeter, extrapolated onset, Kelvin, reaction, reaction
mine the applicability of regulatory limitations prior to use.
order, and temperature.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
3.2 Definitions of Terms Specific to This Standard:
ization established in the Decision on Principles for the
3.2.1 autocatalytic, n—a chemical reaction where one or
Development of International Standards, Guides and Recom-
more reaction products are a catalyst for the same reaction.
mendations issued by the World Trade Organization Technical
3.2.1.1 Discussion—An example of an autocatalytic model
Barriers to Trade (TBT) Committee.
is:
2. Referenced Documents
m n
dα⁄dt 5α ~1 2 α! (1)
2
2.1 ASTM Standards:
3.2.2 autocatalytic model, n—a kinetic model used to de-
E473 Terminology Relating to Thermal Analysis and Rhe-
scribe an autocatalytic reaction.
ology
3.2.3 exotherm, n—in thermal analysis, the thermal record
E537 Test Method for The Thermal Stability of Chemicals
of a transition where heat is evolved by the specimen.
by Differential Scanning Calorimetry
E698 Test Method for Kinetic Parameters for Thermally
3.2.4 model, kinetic, n—amathematicalconstructionusedto
Unstable Materials Using Differential Scanning Calorim-
describe the rates of a chemical reaction.
etry and the Flynn/Wall/Ozawa Method
3.2.5 nth order, n—a kinetic model in which the rate of
E967 Test Method for Temperature Calibration of Differen-
reaction (dα⁄dt) is proportional to the power of the current
tial Scanning Calorimeters and Differential Thermal Ana-
concentration of the reactant(s).
lyzers
3.2.5.1 Discussion—An example of an nth order model is:
1
This practice is under the jurisdiction of ASTM Committee E37 on Thermal n
dα⁄dt 5 k 1 2 α (2)
~ !
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
rimetry and Mass Loss.
where α is the fraction reacted, t is time, k is the rate
Current edition approved Feb. 15, 2019. Published March 2019. DOI: 10.1520/
constant, and n is the reaction order.
E3174-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.2.6 rate constant (k), n—a coefficient of proportionality
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
relating the rate of a chemical reaction at a given temperature
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. to a function of the reactant’s concentration.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E3174 − 19
4. Summary of Practice 6.3 A cooling system, to cool the chamber and the test
specimen to ambient temperature at an initial rate of 50 °C/min
4.1 A scouting experiment is conducted at a constant heat-
or greater.
ing rate to determine the overall exothermic profile of the
chemical reaction. From this thermal curve, the temperature of
7. Hazards
maximumrateandtheextrapolatedonset(test)temperatureare
determined.
7.1 This practice is applicable to thermally unstable
materials,
...

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