Standard Test Method for Heat of Reaction of Thermally Reactive Materials by Differential Scanning Calorimetry

SIGNIFICANCE AND USE
This method is useful in determining the extrapolated onset temperature, the peak heat flow temperature and the heat of reaction of a material. Any onset temperature determined by this method is not valid for use as the sole information used for determination of storage or processing conditions.
This test method is useful in determining the fraction of a reaction that has been completed in a sample prior to testing. This fraction of reaction that has been completed can be a measure of the degree of cure of a thermally reactive polymer or can be a measure of decomposition of a thermally reactive material upon aging.
The heat of reaction values may be used in Practice E 1231 to determine hazard potential figures-of-merit Explosion Potential and Shock Sensitivity.
This test method may be used in research, process control, quality assurance, and specification acceptance.
SCOPE
1.1 This test method determines the exothermic heat of reaction of thermally reactive chemicals or chemical mixtures, using milligram specimen sizes, by differential scanning calorimetry. Such reactive materials may include thermally unstable or thermoset materials.
1.2 This test method also determines the extrapolated onset temperature and peak heat flow temperature for the exothermic reaction.
1.3 This test method may be performed on solids, liquids or slurries.
1.4 The applicable temperature range of this method is 25 to 600°C.
1.5 SI units are to be regarded as the standard.
1.6 There is no ISO method equivalent to this standard.
1.7 This standard is related to Test Method E 537 and to NAS 1613, but provides additional information.
1.8 This standard may involve hazardous materials, operations, and equipment. 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.

General Information

Status
Historical
Publication Date
30-Apr-2004
Current Stage
Ref Project

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ASTM E2160-04 - Standard Test Method for Heat of Reaction of Thermally Reactive Materials by 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E2160 − 04
StandardTest Method for
Heat of Reaction of Thermally Reactive Materials by
1
Differential Scanning Calorimetry
This standard is issued under the fixed designation E2160; 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 E537 Test Method for The Thermal Stability of Chemicals
by Differential Scanning Calorimetry
1.1 This test method determines the exothermic heat of
E967 Test Method for Temperature Calibration of Differen-
reaction of thermally reactive chemicals or chemical mixtures,
tial Scanning Calorimeters and Differential Thermal Ana-
using milligram specimen sizes, by differential scanning calo-
lyzers
rimetry. Such reactive materials may include thermally un-
E968 Practice for Heat Flow Calibration of Differential
stable or thermoset materials.
Scanning Calorimeters
1.2 This test method also determines the extrapolated onset
E1142 Terminology Relating to Thermophysical Properties
temperature and peak heat flow temperature for the exothermic
E1231 Practice for Calculation of Hazard Potential Figures-
reaction.
of-Merit for Thermally Unstable Materials
1.3 This test method may be performed on solids, liquids or E1860 Test Method for Elapsed Time Calibration of Ther-
mal Analyzers
slurries.
2.2 Other Standard:
1.4 Theapplicabletemperaturerangeofthismethodis25to
NAS 1613 Seal Element, Packing, Preformed, Ethylene
600°C.
Propylene Rubber, National Aerospace Standard, Aero-
1.5 The values stated in SI units are to be regarded as
space Industries Association of America, 1725 DeSales
standard. No other units of measurement are included in this
St., NM, Washington, DC 20036
standard.
3. Terminology
1.6 There is no ISO method equivalent to this standard.
3.1 Specifictechnicaltermsusedinthisstandardaredefined
1.7 This standard is related to Test Method E537 and to
in Terminologies E473 and E1142.
NAS 1613, but provides additional information.
1.8 This standard may involve hazardous materials,
4. Summary of Test Method
operations, and equipment. This standard does not purport to
4.1 A small (milligram) quantity of the reactive material is
address all of the safety concerns, if any, associated with its
heated at 10°C/min through a temperature region where a
use. It is the responsibility of the user of this standard to
chemical reaction takes place. The exothermic heat flow
establish appropriate safety and health practices and deter-
produced by the reaction is recorded as a function of tempera-
mine the applicability of regulatory limitations prior to use.
ture and time by a differential scanning calorimeter. Integration
of the exothermic heat flow over time yields the heat of
2. Referenced Documents
reaction. If the heat flow is endothermic, then this test method
2
2.1 ASTM Standards:
is not to be used.
E473 Terminology Relating to Thermal Analysis and Rhe-
4.2 The test method can be used to determine the fraction of
ology
a reaction that has occurred in a partially reacted sample. The
heat of reaction is determined for a specimen that is known to
be 100 % unreacted and is compared to the heat of reaction
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
determined for the partially reacted sample. Appropriate cal-
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo-
rimetry and Mass Loss.
culation yields the fraction of the latter sample that was
Current edition approved May 1, 2004. Published June 2004. Originally
unreacted.
approved in 2001. Last previous edition approved in 2001 as E2160 – 01. DOI:
10.1520/E2160-04.
4.3 Subtracting the reaction fraction remaining from unity
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
(1) yields the fraction reacted. The fraction reacted may be
contact ASTM Customer service at service@astm.org. For Annual Book of ASTM
expressed as percent. If the sample tested is a thermoset resin,
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the percent reacted is often called the percent of cure.
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E2160 − 04
4.4 The extrapolated onset temperature and peak heat flow 7. Safety Precautions
temperature are determined for the exothermic heat flow
7.1 The use of this test method for materials of unknown
thermal curve from 4.1.
potential hazards requires that precautions be taken during the
sample preparation and testing.
5. Significance and Use
7.2 Where particle size redu
...

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