ASTM E2070-08
(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 Test Method C determines the activation energy and initial heat flow from a series of isothermal experiments over a small temperature range. Because this approach only determines kinetic parameter of activation energy, no knowledge of the kinetic model is required. Therefore it is considered to be “model free”. This approach is broadly applicable to a variety of complicated reactions including those not well understood.
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.
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Designation: E2070 − 08
StandardTest 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
1.1 Test Method A determines kinetic parameters for acti- 2.1 ASTM Standards:
vation energy, pre-exponential factor and reaction order using D3550Practice for Thick Wall, Ring-Lined, Split Barrel,
differential scanning calorimetry from a series of isothermal Drive Sampling of Soils
experiments over a small (; 10 K) temperature range. This D3895Test Method for Oxidative-Induction Time of Poly-
treatment is applicable to low nth order reactions and to olefins by Differential Scanning Calorimetry
autocatalyzed reactions such as thermoset curing or pyrotech- D4565Test Methods for Physical and Environmental Per-
nic reactions and crystallization transformations in the tem- formance Properties of Insulations and Jackets for Tele-
perature range from 300 to 900 K (30 to 630 °C). This test communications Wire and Cable
method is applicable only to these types of exothermic reac- D5483Test Method for Oxidation Induction Time of Lubri-
tions when the thermal curves do not exhibit shoulders, catingGreasesbyPressureDifferentialScanningCalorim-
discontinuities or shifts in baseline. etry
D6186Test Method for Oxidation Induction Time of Lubri-
1.2 Test Method B also determines the activation energy of
cating Oils by Pressure Differential Scanning Calorimetry
a set of time-to-event and isothermal temperature data gener-
(PDSC)
ated by this or other procedures.
E473Terminology Relating to Thermal Analysis and Rhe-
1.3 Test Method C determines the activation energy and
ology
initial heat flow from a series of isothermal experiments over a
E537Test Method for The Thermal Stability of Chemicals
small temperature range. Because this approach only deter-
by Differential Scanning Calorimetry
mines kinetic parameter of activation energy, no knowledge of
E698Test Method for Arrhenius Kinetic Constants for
the kinetic model is required. Therefore it is considered to be
Thermally Unstable Materials Using Differential Scan-
“model free”. This approach is broadly applicable to a variety
ning Calorimetry and the Flynn/Wall/Ozawa Method
of complicated reactions including those not well understood.
E967Test Method for Temperature Calibration of Differen-
1.4 The values stated in SI units are to be regarded as tial Scanning Calorimeters and Differential ThermalAna-
lyzers
standard. No other units of measurement are included in this
standard. E968Practice for Heat Flow Calibration of Differential
Scanning Calorimeters
1.5 This test method is similar but not equivalent
E1142Terminology Relating to Thermophysical Properties
toISODIS11357, Part 5, and provides more information than
E1445Terminology Relating to Hazard Potential of Chemi-
the ISO standard.
cals
1.6 This standard does not purport to address all of the
E1860Test Method for Elapsed Time Calibration of Ther-
safety concerns, if any, associated with its use. It is the
mal Analyzers
responsibility of the user of this standard to establish appro-
E1958Guide for Sensory Claim Substantiation
priate safety and health practices and determine the applica-
E1970PracticeforStatisticalTreatmentofThermoanalytical
bility of regulatory limitations prior to use. Specific precau-
Data
tionary statements are given in Section 8.
E2041Test Method for Estimating Kinetic Parameters by
Differential Scanning Calorimeter Using the Borchardt
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
2
rimetry and Mass Loss. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2008. Published March 2008. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2000. Last previous edition approved in 2003 as E2070–03. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E2070-08. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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E2070 − 08
5,6
equation while Eq 3 is the autocatalytic (or Sestak-Berggren) equation .
and Daniels Method
Eq 2 is used for nth order reactions while Eq 3 is used for thermoset cure
E2046TestMethodforReactionInductionTimebyThermal
and crystallization transfor
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:E2070–03 Designation:E2070–08
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
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.
1.3Electronic instrumentation or automated data analysis systems or treatments equivalent to this test method may be used.
NOTE1—Since all electronic data systems are not equivalent, the user must verify the applicability of the treatment to this method.
1.3 Test Method C determines the activation energy and initial heat flow from a series of isothermal experiments over a small
temperature range. Because this approach only determines kinetic parameter of activation energy, no knowledge of the kinetic
model is required. Therefore it is considered to be “model free”. This approach is broadly applicable to a variety of complicated
reactions including those not well understood.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D3350Specification for Polyethylene Plastic Pipe 3550 Practice for Thick Wall, Ring-Lined, Split Barrel, Drive Sampling of
Soils
D3895 Test Method for Oxidative-Induction Time of Polyolefins by Differential Scanning Calorimetry
D4565 Test Methods for Physical and Environmental Performance Properties of Insulations and Jackets for Telecommunica-
tions Wire and Cable
D5483 Test Method for Oxidation Induction Time of Lubricating Greases by Pressure Differential Scanning Calorimetry
D6186 Test Method for Oxidation Induction Time of Lubricating Oils by Pressure Differential Scanning Calorimetry (PDSC)
E473 Terminology Relating to Thermal Analysis and Rheology
5
E537TestMethodforAssessingtheThermalStabilityofChemicalsbyMethodofDifferentialThermalAnalysis TestMethod
for The Thermal Stability Of Chemicals By Differential Scanning Calorimetry
5
E698Test Method for Arrhenius Kinetic Constants for Thermally Unstable Materials Test Method for Arrhenius Kinetic
Constants for Thermally Unstable Materials Using Differential Scanning Calorimetry and the Flynn/Wall/Ozawa Method
E967 Test Method for Temperature Calibration of Differential Thermal AnalyzersScanning Calorimeters and Differential
5
Scanning Calorimeters Thermal Analyzers
E968Test Method Practice for Heat Flow Calibration of Differential Scanning Calorimeters
E1142 Terminology Relating to Thermophysical Properties
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 Thermal
Analysis Test Methods and Practices.
Current edition approved Oct.Feb. 1, 2003.2008. Published October 2003.March 2008. Originally approved in 2000. Last previous edition approved in 20002003 as
E2070–003.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
, Vol 08.02.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Driv
...
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