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ASTM E2070-03

(Test Method)

Standard Test Method for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods

Standard Test Method for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods

SIGNIFICANCE AND USE
This test method is useful for research and development, quality assurance, regulatory compliance and specification acceptance purposes.
The determination of the order of a chemical reaction or transformation at specific temperatures or time conditions is beyond the scope of this test method.
The activation energy results obtained by this method may be compared with those obtained from Test Method E 698 for nth order and autocatalytic reactions. Activation energy, pre-exponential factor and reaction order results by this method may be compared to those for Test Method E 2041 for nth order reactions.
SCOPE
1.1 Test Method A determines kinetic parameters for activation energy, pre-exponential factor and reaction order using differential scanning calorimetry from a series of isothermal experiments over a small (~ 10 K) temperature range. This treatment is applicable to low nth order reactions and to autocatalyzed reactions such as thermoset curing or pyrotechnic reactions and crystallization transformations in the temperature range from 300 to 900 K (30 to 630 °C). This test method is applicable only to these types of exothermic reactions when the thermal curves do not exhibit shoulders, discontinuities or shifts in baseline.
1.2 Test Method B also determines the activation energy of a set of time-to-event and isothermal temperature data generated by this or other procedures.
1.3 Electronic instrumentation or automated data analysis systems or treatments equivalent to this test method may be used.Note 1
Since all electronic data systems are not equivalent, the user must verify the applicability of the treatment to this method.
1.4 SI units are the standard.
1.5 This test method is similar but not equivalent to ISO 11357, Part 5, and provides more information than the ISO 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. Specific precautionary statements are given in Section 8.

General Information

Status
Historical
Publication Date
30-Sep-2003
ICS
17.200.10 - Heat. Calorimetry
Technical Committee
E37 - Thermal Measurements
Drafting Committee
E37.01 - Calorimetry and Mass Loss
Current Stage
Ref Project

Relations

Replaces
ASTM E2070-00 - Standard Test Method for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods
Effective Date
01-Oct-2003
Replaced By
ASTM E2070-08 - Standard Test Method for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods
Effective Date
01-Feb-2008
Referred By
ASTM E2046-19 - Standard Test Method for Reaction Induction Time by Thermal Analysis
Effective Date
01-Oct-2003
Referred By
ASTM E3174-22 - Standard Practice for Determination of Kinetic Reaction Model Using Differential Scanning Calorimetry
Effective Date
01-Oct-2003
Referred By
ASTM E1231-19 - Standard Practice for Calculation of Hazard Potential Figures of Merit for Thermally Unstable Materials
Effective Date
01-Oct-2003
Referred By
ASTM E1860-23 - Standard Test Method for Elapsed Time Calibration of Thermal Analyzers
Effective Date
01-Oct-2003
Referred By
ASTM E2781-16 - Standard Practice for Evaluation of Methods for Determination of Kinetic Parameters by Calorimetry and Differential Scanning Calorimetry
Effective Date
01-Oct-2003

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ASTM E2070-03 - Standard Test Method for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal MethodsASTM E2070-03 - Standard Test Method for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods
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ASTM E2070-03 - Standard Test Method for Kinetic Parameters by Differential Scanning Calorimetry Using Isothermal Methods
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Standards Content (Sample)

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:E2070–03
Standard Test Method for
Kinetic Parameters by Differential Scanning Calorimetry
1
Using Isothermal Methods
This standard is issued under the fixed designation E2070; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D4565 Test Method for Physical and Environmental Per-
formance Properties of Insulations and Jackets for Tele-
1.1 Test Method A determines kinetic parameters for acti-
3
communications Wire and Cable
vation energy, pre-exponential factor and reaction order using
D5483 Test Method for Oxidation Induction Time of Lu-
differential scanning calorimetry from a series of isothermal
bricating Greases by Pressure Differential Scanning Calo-
experiments over a small (; 10 K) temperature range. This
4
rimetry
treatment is applicable to low nth order reactions and to
D6186 Test Method for Oxidation Induction Time of Lu-
autocatalyzed reactions such as thermoset curing or pyrotech-
bricating Oils by Pressure Differential Scanning Calorim-
nic reactions and crystallization transformations in the tem-
4
etry
perature range from 300 to 900 K (30 to 630 °C). This test
5
E473 Terminology Relating to Thermal Analysis
method is applicable only to these types of exothermic reac-
E537 Test Method for Assessing the Thermal Stability of
tions when the thermal curves do not exhibit shoulders,
5
Chemicals by Method of Differential Thermal Analysis
discontinuities or shifts in baseline.
E698 Test Method for Arrhenius Kinetic Constants for
1.2 Test Method B also determines the activation energy of
5
Thermally Unstable Materials
a set of time-to-event and isothermal temperature data gener-
E967 Test Method for Temperature Calibration of Differ-
ated by this or other procedures.
ential Thermal Analyzers and Differential Scanning Calo-
1.3 Electronic instrumentation or automated data analysis
5
rimeters
systems or treatments equivalent to this test method may be
E968 Test Method for Heat Flow Calibration of Differen-
used.
5
tial Scanning Calorimeters
NOTE 1—Since all electronic data systems are not equivalent, the user
E1142 Terminology Relating to Thermophysical Proper-
must verify the applicability of the treatment to this method.
5
ties
1.4 SI units are the standard.
E1445 Terminology Relating to Hazardous Properties of
5
1.5 This test method is similar but not equivalent to ISO
Materials
11357, Part 5, and provides more information than the ISO
E1860 Test Method for Elapsed Time Calibration of Ther-
5
standard.
mal Analyzers
1.6 This standard does not purport to address all of the
E1958 Test Method for Oxidative Induction Time of Hy-
5
safety concerns, if any, associated with its use. It is the
drocarbons by Differential Scanning Calorimetry
responsibility of the user of this standard to establish appro-
E1970 Practice for Statistical Treatment of Thermoanalyti-
5
priate safety and health practices and determine the applica-
cal Data
bility of regulatory limitations prior to use. Specific precau-
E2041 Test Method for Kinetic Parameters by the Bor-
tionary statements are given in Section 8.
chardt and Daniels Method using Differential Scanning
5
Calorimetry
2. Referenced Documents
E2046 Test Method for Reaction Induction Time by Ther-
5
2.1 ASTM Standards:
mal Analysis
2
D3350 Specification for Polyethylene Plastic Pipe
2.2 ISO Standard:
D3895 Test Method for Oxidative Induction Time of Poly-
ISODIS11357 Part5DeterminationofTemperatureand/or
2
6
olefins by Differential Scanning Calorimetry
Time of Reaction and Reaction Kinetics
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
3
Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal Annual Book of ASTM Standards, Vol 10.02.
4
Analysis Test Methods. Annual Book of ASTM Standards, Vol 05.03.
5
Current edition approved Oct. 1, 2003. Published October 2003. Originally Annual Book of ASTM Standards, Vol 14.02.
6
approved in 2000. Last previous edition approved in 2000 as E2070–00. Available from American National Standards Institute, 11 W. 42nd St., 13th
2
Annual Book of ASTM Standards, Vol 08.02. Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E2070–03
3. Terminology Thisequationhastheformz=a+bx+cyandmaybesolved
using multiple linear regression analysis.
3.1 Specific technical terms used in this test method are
defined in Terminologies E473, E1142, and E1445.
NOTE 3—Subsequent discussions use the autocatalytic form of the rate
equation (Eq 3). It red
...

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5.1 The standard deviation, or one of its derivatives, such as relative standard deviation or pooled standard deviation, derived from this practice, provides an estimate of precision in a measured value. Such results are ordinarily expressed as the mean value ± the standard deviation, that is, X ± s.  
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5.1 Oxidation onset temperature is a relative measure of the degree of oxidative stability of the material evaluated at a given heating rate and oxidative environment (e.g., oxygen); the higher the OOT value the more stable the material. The OOT is described in Fig. 1. The OOT values can be used for comparative purposes and are not an absolute measurement, like the oxidation induction time (OIT) at a constant temperature (see Test Method E1858). The presence or effectiveness of antioxidants may be determined by these test methods.
FIG. 1 DSC Oxidation (Extrapolated) Onset Temperature (OOT)  
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1.1 These test methods describe the determination of the oxidative properties of hydrocarbons by differential scanning calorimetry or pressure differential scanning calorimetry under linear heating rate conditions and are applicable to hydrocarbons, which oxidize exothermically in their analyzed form.  
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5.1 Modulated temperature differential scanning calorimetric measurements provide a rapid, simple method for determining specific heat capacities of materials, even under quasi-isothermal conditions.  
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1.1 This test method describes the determination of specific heat capacity by modulated temperature differential scanning calorimetry. For the determination of specific heat capacity by a step-isothermal or multiple step-isothermal temperature program, the reader is referred to Test Method E1269.  
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