ASTM E1545-00

Standard Test Method for Assignment of the Glass Transition Temperature by Thermomechanical Analysis

SCOPE
1.1 This test method covers procedures for the assignment of the glass transition temperature of materials on heating using thermomechanical measurements under prescribed 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 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 test method to determine the necessary equivalency prior to use. In the case of dispute, only the manual procedures are to be considered valid.
1.5 The values stated in SI units are to be regarded as the 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 7.

General Information

• Status: Historical
• Publication Date: 09-Mar-2000
• ICS: 81.040.01 - Glass in general
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Relations

• Replaced By: ASTM E1545-05 - Standard Test Method for Assignment of the Glass Transition Temperature by Thermomechanical Analysis
• Effective Date: 01-Dec-2005
• Referred By: ASTM E1824-19 - Standard Test Method for Assignment of a Glass Transition Temperature Using Thermomechanical Analysis: Tension Method
• Effective Date: 10-Mar-2000
• Referred By: ASTM E1640-23 - Standard Test Method for Assignment of the Glass Transition Temperature By Dynamic Mechanical Analysis
• Effective Date: 10-Mar-2000
• Referred By: ASTM D3794-22 - Standard Guide for Testing Coil Coatings
• Effective Date: 10-Mar-2000
• Referred By: ASTM D1676-17 - Standard Test Methods for Film-Insulated Magnet Wire
• Effective Date: 10-Mar-2000
• Referred By: ASTM E2602-22 - Standard Test Methods for Assignment of the Glass Transition Temperature by Modulated Temperature Differential Scanning Calorimetry
• Effective Date: 10-Mar-2000

Standards Content (Sample)

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:E1545–00
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.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 E473 Terminology Relating to Thermal Analysis
E691 Practice for Conducting an Interlaboratory Study to
1.1 This test method covers procedures for the assignment
Determine the Precision of a Test Method
oftheglasstransitiontemperatureofmaterialsonheatingusing
E831 Test Method for Linear Thermal Expansion of Solid
thermomechanical measurements under prescribed experimen-
Materials by Thermomechanical Analysis
tal conditions.
E1142 Terminology Relating to Thermophysical Proper-
1.2 This test method is applicable to amorphous or to
ties
partially crystalline materials that are sufficiently rigid below
E1356 Test Method for Glass Transition Temperatures by
the glass transition to inhibit indentation by the sensing probe.
Differential Scanning Calorimetry or Differential Thermal
1.3 The normal operating temperature range is from−100
Analysis
to 600°C. This temperature range may be extended depending
E 1363 Test Method for Calibration of Thermomechanical
upon the instrumentation used.
Analyzers
1.4 Computer- or electronic-based instruments, techniques,
2.2 IIPEC Standard:
or data treatment equivalent to this test method may also be
Test Method 2.4.24, Glass Transition Temperature TMA
used.
Method
NOTE 1—Usersofthistestmethodareadvisedthatallsuchinstruments
ISO11359-2 Plastics—ThermomechanicalAnalysis(TMA)
or techniques may not be equivalent. It is the responsibility of the user of
– Part 2: Determination of Coefficient of Linear Thermal
this test method to verify equivalency prior to use.
Expansion and Glass Transition Temperature
1.5 The values stated in SI units are to be regarded as the
standard. 3. Terminology
1.6 ThistestmethodisrelatedtoISO11359-2.ISO11359-2
3.1 Definitions—The following terms are applicable to this
additionally covers the determination of coefficient of linear
test method and can be found in Terminologies E473 and
thermal expansion not covered by this test method.
E1142: thermomechanical analysis(TMA), thermomechanical
1.7 This standard does not purport to address all of the
measurement, thermodilatometry, glass transition, glass tran-
safety concerns, if any, associated with its use. It is the
sition temperature, and linear thermal expansion.
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
4.1 Thistestmethodusesthermomechanicalanalysisequip-
tionary statements are given in Section 7.
ment (thermomechanical analyzer, dilatometer, or similar de-
vice)toassignthechangeindimensionofaspecimenobserved
2. Referenced Documents
when the material is subjected to a constant heating rate
2.1 ASTM Standards:
through its glass transition. This change in dimension associ-
D 832 Practice for Rubber Conditioning for Low-
atedwiththechangefromvitreoussolidtoamorphousliquidis
Temperature Testing
observed as movement of the sensing probe in direct contact
withthespecimenandisrecordedasafunctionoftemperature.
The intersection of the extrapolation of the slope of the probe
This test method is under the jurisdiction of ASTM Committee E-37 on
Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Annual Book of ASTM Standards, Vol 14.02.
Test Methods and Recommended Practices. Available from The Institute for Interconnecting and Packaging Electronic
Current edition approved March 10, 2000. Published June 2000. Originally Circuits, 7380 N. Lincoln Ave., Lincolnwood, IL 60646-1705.
published as E1545–93. Last previous edition E1545–95a. Available from American National Standards Institute, 11 W. 42nd St., 13th
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.
E1545
displacement curve before and after the transition is used to 7. Hazards
determine the glass transition temperature.
7.1 This test method may be used for amorphous and
semicrystalline materials having a glass transition that is at or
5. Significance and Use
below room temperature providing care is taken to avoid
contacting the specimen with a loaded probe prior to cooling
5.1 The glass transition is dependent on the thermal history
the specimen below its glass transition. Applying a loaded
ofthematerialtobetested.Foramorphousandsemicrystalline
probetoaspecimenthatisaboveitsglasstransitionmaycause
materials the assignment of the glass transition temperature
partial penetration by the probe which can lead to probe
may lead to important information about thermal history,
stickinguponcoolingbelowtheglasstransition.Thiscondition
processingconditions,stability,progressofchemicalreactions,
has been known to yield erroneous results during the heating
and mechanical and electrical behavior.
cycle.
5.2 Thermomechanical analysis provides a rapid means of
7.2 With some materials a transient may be observed
detecting changes in hardness or linear expansion associated
between the pre-transition slope and the final slope (Run 1 of
with the glass transition.
Fig. 1).This may occur due to settling, residual stresses within
5.3 Thistestmethodisusefulforresearchanddevelopment,
the specimen, or alteration of the specimen morphology. Refer
quality control, and specification acceptance.
to Note 6 for directions when this is encountered.
7.3 Specimens of thickness less than 0.2 mm may be very
6. Apparatus
difficult to handle. Thin films (50 to 200 µm) on a substrate
6.1 Thermomechanical Analyzer (TMA)—The essential in-
may be considered for this test method providing the substrate
strumentation required to provide the minimum thermome-
is mechanically stable in the temperature region of the film
chanical analytical capability for this test method includes the
glass transition.
following:
7.4 Forspecimensofthicknessgreaterthan5mm,tempera-
6.1.1 A rigid specimen holder, composed of inert low
turenonuniformitiesofsufficientextentcandevelopwithinthe
–1 –1
expansivity material#1µmm °C , to center the specimen
specimen as to yield erroneously high values of the glass
in the furnace and to fix the specimen to mechanical ground.
transition temperature using this test method.
6.1.2 A rigid circular expansion probe, 2 to 6 mm in
8. Sampling
diameter, composed of inert low expansivity material#1µm
–1 –1
m °C , that contacts the specimen with an applied compres-
8.1 Analyze samples as received or after pretreatment. If
sive force.
some treatment is applied to a specimen prior to analysis, note
6.1.3 Asensingelementlinearoveraminimum2-mmrange
this treatment and any resulting change in mass in the report.
to measure the displacement in length of the specimen.
9. Calibration
6.1.4 A weight or force transducer to generate a constant
9.1 Perform calibration in accordance with Test Method
force of 0 to 50 mN that is applied through the rigid
E1363.
compression probe to the specimen.
6.1.5 A furnace capable of providing uniform controlled
10. Procedure
heating (cooling) of a specimen to a constant temperature or at
10.1 Calibrate the thermomechanical analyzer in accor-
a constant rate over the temperature range of –100 to 600°C.
dance with Test Method E1363.
6.1.6 A temperature controller capable of executing a spe-
cific 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 6 0.1°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 2—Typically, 99.9+% pure nitrogen, argon or helium is used.
Unlesseffectsofmoisturearetobestudied,drypurgegasisrecommended
and is essential for operation at subambient temperatures.
6.1.9 Arecordingdevice,eitherdigitaloranalog,capableof
recording and displaying any fraction of the specimen dimen-
sion sign
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