ASTM E1356-98

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

SCOPE
1.1 This test method covers the determination of the glass transition temperature 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. 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. In the case of dispute, only the manual procedures described in this test method are to be considered valid.
1.5 This standard does not purport to address the safety problems 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: 09-May-1998
• ICS: 17.200.10 - Heat. Calorimetry
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.01 - Calorimetry and Mass Loss

Relations

• Replaced By: ASTM E1356-03 - Standard Test Method for Assignment of the Glass Transition Temperatures by Differential Scanning Calorimetry
• Effective Date: 10-Apr-2003
• Referred By: ASTM D7957/D7957M-22 - Standard Specification for Solid Round Glass Fiber Reinforced Polymer Bars for Concrete Reinforcement
• Effective Date: 10-May-1998
• Referred By: ASTM F3384-21 - Standard Specification for Polydioxanone Polymer Resins for Surgical Implants
• Effective Date: 10-May-1998
• Referred By: ASTM D8505/D8505M-23 - Standard Specification for Basalt and Glass Fiber Reinforced Polymer (FRP) Bars for Concrete Reinforcement
• Effective Date: 10-May-1998
• Referred By: ASTM D7338-14(2023) - Standard Guide for Assessment Of Fungal Growth in Buildings
• Effective Date: 10-May-1998
• Referred By: ASTM D3794-22 - Standard Guide for Testing Coil Coatings
• Effective Date: 10-May-1998
• Referred By: ASTM D6604-00(2022) - Standard Practice for Glass Transition Temperatures of Hydrocarbon Resins by Differential Scanning Calorimetry
• Effective Date: 10-May-1998
• Referred By: ASTM F2902-16e1 - Standard Guide for Assessment of Absorbable Polymeric Implants
• Effective Date: 10-May-1998
• Referred By: ASTM E3301-22 - Standard Test Method for Temperature Calibration of Dynamic Mechanical Analyzers Using Thermal Lag
• Effective Date: 10-May-1998
• Referred By: ASTM F2313-18 - Standard Specification for Poly(glycolide) and Poly(glycolide-co-lactide) Resins for Surgical Implants with Mole Fractions Greater Than or Equal to 70 % Glycolide
• Effective Date: 10-May-1998
• Referred By: ASTM D1676-17 - Standard Test Methods for Film-Insulated Magnet Wire
• Effective Date: 10-May-1998
• Referred By: ASTM F1925-22 - Standard Specification for Semi-Crystalline Poly(lactide) Polymer and Copolymer Resins for Surgical Implants
• Effective Date: 10-May-1998
• Referred By: ASTM F2150-19 - Standard Guide for Characterization and Testing of Biomaterial Scaffolds Used in Regenerative Medicine and Tissue-Engineered Medical Products
• Effective Date: 10-May-1998
• Referred By: ASTM E2602-22 - Standard Test Methods for Assignment of the Glass Transition Temperature by Modulated Temperature Differential Scanning Calorimetry
• Effective Date: 10-May-1998

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: E 1356 – 98
Standard Test Method for Assignment of the
Glass Transition Temperatures by Differential Scanning
Calorimetry or Differential Thermal Analysis
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This test method covers the assignment of the glass 3.1 Definitions:
transition temperatures of materials using differential scanning 3.1.1 The following terms are applicable to this test method
calorimetry or differential thermal analysis. and can be found in Terminology E 473 and Terminology
1.2 This test method is applicable to amorphous materials or E 1142: differential scanning calorimetry (DSC); differential
to partially crystalline materials containing amorphous regions, thermal analysis (DTA); glass transition; glass transition
that are stable and do not undergo decomposition or sublima- temperature (T ); and specific heat capacity.
g
tion in the glass transition region. 3.2 Definitions of Terms Specific to This Standard:
1.3 The normal operating temperature range is from −120 to 3.2.1 There are commonly used transition points associated
500°C. The temperature range may be extended, depending with the glass transition region.—(See Fig. 1.)
upon the instrumentation used. 3.2.1.1 extrapolated end temperature, (T ), °C—the point of
e
1.4 Computer or electronic-based instruments, techniques, intersection of the tangent drawn at the point of greatest slope
or data treatment equivalent to this test method may also be on the transition curve with the extrapolated baseline following
used. the transition.
1.5 Users of this test method are expressly advised that all 3.2.1.2 extrapolated onset temperature, (T ), °C—the point
f
such instruments or techniques may not be equivalent. It is the of intersection of the tangent drawn at the point of greatest
responsibility of the user of this standard to determine the slope on the transition curve with the extrapolated baseline
necessary equivalency prior to use. prior to the transition.
1.6 The values stated in SI units are to be regarded as the 3.2.1.3 inflection temperature, (T ), °C—the point on the
i
standard. thermal curve corresponding to the peak of the first derivative
1.7 This standard does not purport to address all of the (with respect to time) of the parent thermal curve. This point
safety concerns, if any, associated with its use. It is the corresponds to the inflection point of the parent thermal curve.
responsibility of the user of this standard to establish appro- 3.2.1.4 midpoint temperature, (T ), °C—the point on the
m
priate safety and health practices and determine the applica- thermal curve corresponding to ⁄2 the heat flow difference
bility of regulatory limitations prior to use. between the extrapolated onset and extrapolated end.
3.2.1.5 Discussion—Midpoint temperature is most com-
2. Referenced Documents
monly used as the glass transition temperature (see Fig. 1):
2.1 ASTM Standards: 3.2.2 Two additional transition points are sometimes iden-
E 177 Practice for Use of the Terms Precision and Bias in
tified and are defined:
ASTM Test Methods 3.2.2.1 temperature of first deviation, (T ), °C—the point of
o
E 473 Terminology Relating to Thermal Analysis
first detectable deviation from the extrapolated baseline prior to
E 691 Practice for Conducting an Interlaboratory Test Pro- the transition.
gram to Determine the Precision of Test Methods
3.2.2.2 temperature of return to baseline, (T ), °C—the
r
E 967 Practice for Temperature Calibration of Differential point of last deviation from the extrapolated baseline beyond
Scanning Calorimeters and Differential Thermal Analyz-
the transition.
ers
4. Summary of Test Method
E 1142 Terminology Relating to Thermophysical Proper-
ties 4.1 This test method involves continuously monitoring the
difference in heat flow into, or temperature between, a refer-
1 ence material and a test material when they are heated or
This test method is under the jurisdiction of ASTM Committee E-37 on
cooled at a controlled rate through the glass transition region of
Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on
Test Methods and Recommended Practices.
the test material and analyzing the resultant thermal curve to
Current edition approved May 10, 1998. Published December 1998. Originally
provide the glass transition temperature.
published as E 1356 – 91. Last previous edition E 1356 – 91 (1995).
Annual Book of ASTM Standards, Vol 09.01.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 1356
FIG. 1 Glass Transition Region Measured Temperatures
5. Significance and Use 7. Apparatus
5.1 Differential scanning calorimetry or differential thermal 7.1 Apparatus shall be either type listed as follows:
analysis provides a rapid test method for determining changes 7.1.1 Differential Scanning Calorimeter, capable of heating
in specific heat capacity in a homogeneous material. The glass (or cooling) at rates up to at least 20°C/min and of automati-
transition is manifested as a step change in specific heat cally recording the differential heat flow input between a
capacity. For amorphous and semicrystalline materials the specimen and a reference material, both to the required
determination of the glass transition temperature may lead to sensitivity and precision, as given in Practice E 967.
important information about their thermal history, processing 7.1.2 Differential Thermal Analyzer, capable of heating (or
conditions, stability, progress of chemical reactions, and me- cooling) at rates up to at least 20°C/min and of automatically
chanical and electrical behavior. recording the differential temperature between a specimen and
5.2 This test method is useful for research, quality control, a reference material, both to the required sensitivity and
and specification acceptance. precision. Typically, the differential temperature sensitivity
should be sufficient to provide specimen temperature readabil-
6. Interferences
ity to at least 61°C.
6.1 A change in heating rates and cooling rates can affect the 7.2 Specimen Capsules, composed of aluminum or an inert
results. The presence of impurities will affect the transition,
material of high thermal conductivity, are used for DSC. For
particularly if an impurity tends to plasticize or form solid DTA, sample cups or tubes composed of borosilicate glass,
solutions, or is miscible in the post-transition phase. If particle
alumina, or quartz may be used. The specimen capsules, pans,
size has an effect upon the detected transition temperature, the or tubes must not react with the specimen.
specimens to be compared should be of the same particle size.
7.3 For ease of interpretation, an inert reference material
6.2 In some cases the specimen may react with air during
with an heat capacity approximately equivalent to that of the
the temperature program causing an incorrect transition to be specimen may be used. The inert reference material may often
measured. Whenever this effect may be present, the test shall
be an empty specimen capsule or tube.
be run under either vacuum or an inert gas atmosphere. Since 7.4 Nitrogen, or other inert purge gas supply, of purity equal
some materials degrade near the glass transition region, care
to or greater than 99.9 %.
must be taken to distinguish between degradation and glass 7.5 Analytical Balance, with a capacity greater than 100 mg,
transition.
capable of weighing to the nearest 0.01 mg.
6.3 Since milligram quantities of sample are used, it is
8. Specimen Preparation
essential to ensure that specimens are homogeneous and
representative, so that appropriate sampling techniques are 8.1 Powders or Granules—Avoid gri
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