ASTM E1545-11(2016)

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Designation: E1545 − 11 E1545 − 11 (Reapproved 2016)
Standard Test Method for
Assignment of the Glass Transition Temperature by
Thermomechanical Analysis
This standard is issued under the fixed designation E1545; 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
1.1 This test method describes procedures for the assignment of the glass transition temperature of materials on heating using
thermomechanical measurements under compression experimental conditions.
1.2 This test method is applicable to amorphous or to partially crystalline materials that are sufficiently rigid below the glass
transition to inhibit indentation by the sensing probe.
1.3 The normal operating temperature range is from − 100 to 600°C. This temperature range may be extended depending upon
the instrumentation used.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This test method is related to ISO 11359-2. ISO 11359-2 additionally covers the determination of coefficient of linear
thermal expansion not covered by this test method. This test method is related to IEC 61006 but uses a slower heating rate.
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 7.
2. Referenced Documents
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1142 Terminology Relating to Thermophysical Properties
E1363 Test Method for Temperature Calibration of Thermomechanical Analyzers
2.2 Other Standard:Standards:
ISO 11359-2 Plastics—Thermomechanical Analysis (TMA) – Part 2: Determination of Coefficient of Linear Thermal Expansion
and Glass Transition Temperature
IEC 61006 Methods of Test for the Determination of the Glass Transition Temperature of Electrical Insulating Materials
3. Terminology
3.1 Definitions—The following terms are applicable to this test method and can be found in Terminologies E473 and E1142:
thermomechanical analysis (TMA), thermomechanical measurement,thermodilatometry,glass transition,glass transition
temperature, and linear thermal expansion.
4. Summary of Test Method
4.1 This test method uses thermomechanical analysis equipment (thermomechanical analyzer, dilatometer, or similar device) to
assign the change in dimension of a specimen observed when the material is subjected to a constant heating rate through its glass
transition. This change in dimension associated with the change from vitreous solid to amorphous liquid is observed as movement
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,
Statistical and Mechanical Properties.
Current edition approved April 1, 2011Sept. 1, 2016. Published May 2011September 2016. Originally approved in 1993. Last previous edition approved in 20052011 as
E1545 – 05.E1545 – 11. DOI: 10.1520/E1545-11.10.1520/E1545-11R16.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1545 − 11 (2016)
of the sensing probe in direct contact with the specimen and is recorded as a function of temperature. The intersection of the
extrapolation of the slope of the probe displacement curve before and after the transition is used to determine the glass transition
temperature.
5. Significance and Use
5.1 The glass transition is dependent on the thermal history of the material to be tested. For amorphous and semicrystalline
materials the assignment of the glass transition temperature may lead to important information about thermal history, processing
conditions, stability, progress of chemical reactions, and mechanical and electrical behavior.
5.2 Thermomechanical analysis provides a rapid means of detecting changes in hardness or linear expansion associated with the
glass transition.
5.3 This test method is useful for research and development, quality control, and specification acceptance.
6. Apparatus
6.1 Thermomechanical Analyzer (TMA)—The essential instrumentation required to provide the minimum thermomechanical
analytical capability for this test method includes the following:
–1 –1
6.1.1 A rigid specimen holder, composed of inert low expansivity material ≤1 μm m °C , to center the specimen in the
furnace and to fix the specimen to mechanical ground.
–1 –1
6.1.2 A rigid circular expansion probe, 2 to 6 mm in diameter, composed of inert low expansivity material ≤1 μm m ° C°C ,
that contacts the specimen with an applied compressive force.
6.1.3 A linear sensing element with a nominal range of 2-mm capable of measuring the displacement in length of the specimen
readable to within 650 nm.
6.1.4 A weight or force transducer to generate a constant force of 0 to 50 mN that is applied through the rigid compression probe
to the specimen.
6.1.5 A furnace capable of providing uniform controlled heating (cooling) of a specimen to a constant temperature or at a
constant rate over the temperature range of –100 to 600°C.
6.1.6 A temperature controller capable of executing a specific temperature program by operating the furnace between selected
temperature limits at a rate of temperature change of 5 6 0.5°C/minute.
6.1.7 A temperature sensor that can be attached to, in contact with, or reproducibly placed in close proximity to the specimen
to provide an indication of the specimen/furnace temperature to 60.1°C.
6.1.8 A means of sustaining an environment around the specimen of a dry inert purge gas of 45 to 55 mL/minute.
NOTE 1—Typically, 99.9+ % pure nitrogen, argon or helium is used. Unless effects of moisture are to be studied, dry purge gas is recommended and
is essential for operation at subambient temperatures.
6.1.9 A data collection device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.
The minimum output signals required for thermomechanical analysis are change in linear dimension, temperature and time.
6.2 Micrometer or other measuring device to determine specimen dimensions of up to 8 mm to within 6 of 10 μm.
7. Hazards
7.1 This test method may be used for amorphous and semicrystalline materials having a glass transition that is at or below room
temperature providing care is taken to avoid contacting the specimen with a loaded probe prior to cooling the specimen below its
glass transition. Applying a loaded probe to a specimen that is above its glass transition may cause partial penetration by the probe
which can lead to probe sticking upon cooling below the glass transition. This condition has been known to yield erroneous results
during the heating cycle.
7.2 With some materials a transient may be observed between the pre-transition slope and the final slope (Run 1 of Fig. 1). This
may occur due to settling, residual stresses within the specimen, or alteration of the specimen morphology. Refer to Note 5 for
directions when this is encountered.
7.3 Specimens of thickness less than 0.2 mm may be very difficult to handle. Thin films (50 to 200 μm) on a substrate may be
considered for this test method providing the substrate is mechanically stable in the temperature region of the film glass transition.
7.4 For specimens of thickness greater than 5 mm, temperature nonuniformities of sufficient extent can develop within the
specimen as to yield erroneously high values of the glass transition temperature using this test method.
8. Sampling
8.1 Analyze samples as received or after pretreatment. If some treatment is applied to a specimen prior to analysis, note this
treatment and any resulting change in mass in the report.
9. Calibration
9.1 Perform calibration in
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