Standard Test Method for Assignment of the Glass Transition Temperatures by Differential Scanning Calorimetry

SIGNIFICANCE AND USE
Differential scanning calorimetry provides a rapid test method for determining changes in specific heat capacity in a homogeneous material. The glass transition is manifested as a step change in specific heat capacity. For amorphous and semicrystalline materials the determination of the glass transition temperature may lead to important information about their thermal history, processing conditions, stability, progress of chemical reactions, and mechanical and electrical behavior.  
This test method is useful for research, quality control, and specification acceptance.
SCOPE
1.1 This test method covers the assignment of the glass transition temperatures of materials using differential scanning calorimetry or differential thermal analysis.
1.2 This test method is applicable to amorphous materials or to partially crystalline materials containing amorphous regions, that are stable and do not undergo decomposition or sublimation in the glass transition region.
1.3 The normal operating temperature range is from -120 to 500°C. The temperature range may be extended, depending upon the instrumentation used.
1.4 Computer or electronic-based instruments, techniques, or data treatment equivalent to this test method may also be used.
Note 1—Users of this test method are expressly advised that all such instruments or techniques may not be equivalent. It is the responsibility of the user of this standard to determine the necessary equivalency prior to use.
1.5 SI units are the standard.
1.6 ISO standards 11357-2 is equivalent to this standard.
1.7 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

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Historical
Publication Date
09-Apr-2003
Current Stage
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ASTM E1356-03 - Standard Test Method for Assignment of the Glass Transition Temperatures 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:E 1356–03
Standard Test Method for Assignment of the
Glass Transition Temperatures by Differential Scanning
1
Calorimetry
This standard is issued under the fixed designation E 1356; 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 Scanning Calorimeters and Differential Thermal Analyz-
2
ers
1.1 This test method covers the assignment of the glass
E1142 Terminology Relating to Thermophysical Proper-
transition temperatures of materials using differential scanning
2
ties
calorimetry or differential thermal analysis.
2.2 ISO Standard:
1.2 Thistestmethodisapplicabletoamorphousmaterialsor
11357–2 Differential Scanning Calorimetry (DSC)-Part 2
topartiallycrystallinematerialscontainingamorphousregions,
3
Determination of Glass Transition Temperature
that are stable and do not undergo decomposition or sublima-
tion in the glass transition region.
3. Terminology
1.3 Thenormaloperatingtemperaturerangeisfrom−120to
3.1 Definitions:
500°C. The temperature range may be extended, depending
3.1.1 The following terms are applicable to this test method
upon the instrumentation used.
and can be found in Terminology E473 and Terminology
1.4 Computer or electronic-based instruments, techniques,
E1142: differential scanning calorimetry (DSC); differential
or data treatment equivalent to this test method may also be
thermal analysis (DTA); glass transition; glass transition
used.
temperature (T ); and specific heat capacity.
g
NOTE 1—Users of this test method are expressly advised that all such
3.2 Definitions of Terms Specific to This Standard:
instrumentsortechniquesmaynotbeequivalent.Itistheresponsibilityof
3.2.1 There are commonly used transition points associated
the user of this standard to determine the necessary equivalency prior to
with the glass transition region.—(See Fig. 1.)
use.
3.2.1.1 extrapolated end temperature, (T ), °C—thepointof
e
1.5 SI units are the standard.
intersection of the tangent drawn at the point of greatest slope
1.6 ISO standards 11357–2 is equivalent to this standard.
onthetransitioncurvewiththeextrapolatedbaselinefollowing
1.7 This standard does not purport to address all of the
the transition.
safety concerns, if any, associated with its use. It is the
3.2.1.2 extrapolated onset temperature, (T), °C—the point
f
responsibility of the user of this standard to establish appro-
of intersection of the tangent drawn at the point of greatest
priate safety and health practices and determine the applica-
slope on the transition curve with the extrapolated baseline
bility of regulatory limitations prior to use.
prior to the transition.
3.2.1.3 inflection temperature, (T), °C—the point on the
i
2. Referenced Documents
thermal curve corresponding to the peak of the first derivative
2.1 ASTM Standards:
(with respect to time) of the parent thermal curve. This point
E177 Practice for Use of the Terms Precision and Bias in
corresponds to the inflection point of the parent thermal curve.
2
ASTM Test Methods
3.2.1.4 midpoint temperature, (T ), °C—the point on the
m
2
E473 Terminology Relating to Thermal Analysis
1
thermal curve corresponding to ⁄2 the heat flow difference
E691 Practice for Conducting an Interlaboratory Test Pro-
between the extrapolated onset and extrapolated end.
2
gram to Determine the Precision of Test Methods
3.2.1.5 Discussion—Midpoint temperature is most com-
E967 Practice for Temperature Calibration of Differential
monly used as the glass transition temperature (see Fig. 1):
3.2.2 Two additional transition points are sometimes iden-
tified and are defined:
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Test
Methods and Recommended Practices.
Current edition approved April 10, 2003. Published May 2003. Originallyap-
3
proved in 1991. Last previous edition approved in 1998 as E1356–98. Available from American National Standards Institute, 11 W. 42nd St., 13th
2
Annual Book of ASTM Standards, Vol 09.01. 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 ----------------------
E 1356–03
FIG. 1 Glass Transition Region Measured Temperatures
3.2.2.1 temperature of first deviation, (T ), °C—the point of solutions, or is miscible in the post-transition phase. If particle
o
firstdetectabledeviationfromtheextrapolatedbaselinepriorto
size has an effect upon the detected transition temperature, the
the transition.
specimens to be compared should be of the same particle s
...

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