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.
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.
2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.
D3550 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 Telecommunications 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
E537 Test Method for The Thermal Stability of Chemicals by Differential Scanning Calorimetry
E698 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 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
E1860 Test Method for Elapsed Time Calibration of Thermal Analyzers
E1958 Guide for Sensory Claim Substantiation
E1970 Practice for Statistical Treatment of Thermoanalytical Data
E2041 Test Method for Estimating Kinetic Parameters by Differential Scanning Calorimeter Using the Borchardt and Daniels Method
E2046 Test Method for Reaction Induction Time by Thermal Analysis
ISO DIS 11357 Part 5: Determination of Temperature and/or Time of Reaction and Reaction Kinetics Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
activation energy; autocatalytic reactions; crystallization reactions; differential scanning calorimetry (DSC); frequency factor; kinetics; nth order reactions; pre-exponential factor; reactions; thermal analysis; thermoset cure; Activation reactions; Autocatalytic reactions; Crystallization transformation; Differential scanning calorimetry (DSC); Exothermic temperature analysis; Frequency factor; Isothermal conditions/testing; Kinetic behavior/characteristics/parameters; nth order reactions; Pre-exponential factor; Pyrotechnic reactions; Thermal analysis (TA); Thermoset cure;
ICS Number Code 17.200.10 (Heat. Calorimetry)
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Citing ASTM Standards
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