Designation: E1824 − 13

Standard Test Method for

Assignment of a Glass Transition Temperature Using
Thermomechanical Analysis: Tension Method1
This standard is issued under the fixed designation E1824; 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 Scanning Calorimetry

1.1 This test method covers a procedure for the assignment
3. Terminology
of a glass transition temperature (Tg) of materials on heating
using thermomechanical measurements in tension. 3.1 Definitions:
3.1.1 The following terms are applicable to this test method
1.2 This test method may be used as a complement to Test
and can be found in Terminology E473 and Terminology
Method E1545 and is applicable to amorphous or to partially
E1142: thermomechanical analysis (TMA),
crystalline materials in the form of films, fibers, wires, etc., that
thermodilatometry, glass transition, and glass transition tem-
are sufficiently rigid to inhibit extension during loading at
perature.
ambient temperature.
1.3 The generally applicable temperature range for this test 4. Summary of Test Method
method is −100 to 600°C. This temperature range may be 4.1 This test method uses thermomechanical analysis equip-
altered depending upon the instrumentation used. ment (thermomechanical analyzer, dilatometer, or similar de-
1.4 The values stated in SI units are to be regarded as vice) with the test specimen in tension to determine the change
standard. No other units of measurement are included in this in dimension of a thin specimen observed when the material is
standard. subjected to a constant heating rate through the glass transition
1.5 There is no ISO method equivalent to this standard. region. This change in dimension associated with the change
from vitreous solid to amorphous liquid is observed as move-
1.6 This standard does not purport to address all of the ment of a sensing probe in direct contact with the specimen and
safety concerns, if any, associated with its use. It is the is recorded as a function of temperature. The intersection of the
responsibility of the user of this standard to establish appro- extrapolation of the slope of the probe displacement curve
priate safety and health practices and determine the applica- before and after the transition is used to determine a tempera-
bility of regulatory limitations prior to use. ture that is assigned as the glass transition temperature.
2. Referenced Documents 5. Significance and Use
2.1 ASTM Standards:2 5.1 The glass transition is dependent on the thermal history,
E473 Terminology Relating to Thermal Analysis and Rhe- softening agents or additives of the material to be tested. For
ology amorphous and semicrystalline materials the assignment of a
E1142 Terminology Relating to Thermophysical Properties glass transition temperature may lead to important information
E1545 Test Method for Assignment of the Glass Transition about thermal history, processing conditions, stability, progress
Temperature by Thermomechanical Analysis of chemical reactions, and mechanical and electrical behavior.
E2602 Test Method for the Assignment of the Glass Transi-
tion Temperature by Modulated Temperature Differential 5.2 Thermomechanical analysis provides a rapid means of
detecting changes in hardness or linear dimensional change
associated with the glass transition. Dimensional changes
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal measured as a specimen is heated over the glass transition
Measurements and is the direct responsibility of Subcommittee E37.10 on region may include the interaction of several effects: an
Fundamental, Statistical and Mechanical Properties.
Current edition approved Aug. 1, 2013. Published August 2013. Originally increase in the coefficient of expansion, a decrease in the
approved in 1996. Last previous edition approved in 2009 as E1824 – 09ε1. DOI: modulus, which under a constant stress leads to increased
10.1520/E1824-13.
2
extension, stress relief leading to irreversible dimensional
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
change (shrinkage in one dimension, expansion in another
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 dimension), and physical aging effects which change the
the ASTM website. kinetics of the dimensional change.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 E1824 − 13
5.3 This test method is useful for research and development, ployed when oxidation in air is a concern. Unless effects of moisture are
quality control, and specification acceptance testing; particu- to be studied, use of dry purge gas is recommended; especially for
operation at subambient temperatures.
larly of films and fibers.
7.1.1.8 Data Collection Device, provide a means of
6. Interferences acquiring, storing, and displaying measured or calculated
6.1 This test method may be used for materials having a signals, or both. The minimum output signals required for
glass transition at or below ambient temperature providing care thermomechanical analysis are dimension change, temperature
is taken to avoid exposing the specimen to a tensile force prior and time.
to cooling the specimen below its glass transition. Applying a 7.1.2 Rigid Specimen Clamps, (clamps, grips, pins, or split
tensile load on a specimen that is above its glass transition will shot) of inert, low expansivity material (≤ 20 µm ⁄m-°C) that
result in elongation of the specimen which may introduce grip the specimen between the rigid specimen holder and the
orientation and residual stresses that will alter the specimen rigid tension probe without distortion (<1 %) or slippage
thermal history and may yield erroneous results during the (<1 %).
heating cycle. 7.2 Auxiliary equipment considered useful in conducting
6.2 Specimens of thickness less than 0.2 mm may be diffi- this test method includes:
cult to handle. 7.2.1 Coolant System, that can be coupled directly to the
6.3 Specimens of thickness greater than 5 mm may develop furnace/temperature controller to hasten recovery from el-
temperature nonuniformities of sufficient extent as to yield evated temperatures, to provide controlled cooling rates con-
erroneously high values for an assigned glass transition tem- stant to 61.0°C/min, and to sustain a subambient temperature
perature using this test method. to 60.5°C.
7.2.2 Calipers, or other measuring device to determine
7. Apparatus specimen dimensions to 60.01 mm.
7.1 The essential equipment required to provide the mini- 7.2.3 Balance, to determine the specimen mass to 60.1 mg.
mum instrument capability for this test method includes:
7.1.1 A Thermomechanical Analyzer (TMA) or 8. Sampling
Thermodilatometer, consisting of: 8.1 Analyze samples as received or after a prescribed
7.1.1.1 Rigid Specimen Holder, of inert, low expansivity pretreatment. If some treatment is applied to a specimen prior
material (≤20 µm ⁄m-°C), usually quartz, to center the speci- to analysis, note this treatment and any resulting changes in
men in the furnace and to fix the specimen to mechanical mass or appearance in the report. For samples with a glass
ground. transition below ambient, it may be desirable to form the glass
NOTE 1—Use of rigid specimen holders and tension probes constructed with a known thermal history by using a controlled constant
of lower thermal expansivity (≤20 µm ⁄ m-°C) materials or corrections for cooling rate to the starting temperature. Film samples may
hardware expansivity may be necessary if very small changes in specimen undergo stress relief related dimensional change that depends
dimensions are encountered with this test method. on whether the sample is prepared and measured parallel to the
7.1.1.2 Rigid Tension Probe, of inert, low expansivity ma- machine direction of manufacture or perpendicular to the
terial (≤ 5 µm ⁄m-°C), usually quartz, which contacts the machine direction.
specimen with an applied in-plane tensile force.
7.1.1.3 Sensing Element, with a dynamic range of at least 9. Calibration
5 mm, a linearity of 1 % or better, and sufficient sensitivity to
9.1 Perform temperature calibration in accordance with the
measure the displacement of the rigid tension probe within 61
apparatus manufacturer operator’s manual using the same
µm resulting from changes in length of the specimen.
heating rate, purge, and temperature sensor position to be used
7.1.1.4 Weight or Force Transducer, to generate a constant
with the test method.
force between 0 and 50 mN 6 2 % that is applied through the
rigid tension probe to the specimen.
10. Procedure
7.1.1.5 Furnace and Temperature Controller, capable of
executing a temperature program of uniform controlled heating 10.1 Attach a pair of rigid specimen clamps to a specimen
of a specimen at a constant rate of 5 6 0.2°C ⁄ min between with a minimum spacing of 5 mm between the contact points.
required temperature limits to 60.5°C. Weigh the specimen and clamps and record this value.
7.1.1.6 Temperature Sensor, that can be positioned repro-
NOTE 3—Use of between-clamp distances of less than 5 mm may
ducibly in close proximity to the specimen to measure its impart erroneous results because of end effects introduced by the clamp
temperature between −100 and 600°C with a resolution of pressure. Refer to the Precautions Section, if a thickness outside the range
60.1°C. of 0.2 to 5 mm is to be used.
7.1.1.7 Means of Providing a Specimen Environment, of an
10.2 Suspend the specimen with clamps between the contact
inert gas at a purge rate of 10 to 50 mL ⁄ min 6 5 %. The
points of the specimen holder and the tension probe. BE SURE
typical purge gas rate is usually given by the instrument
THE POSITION OF THE TEMPERATURE SENSOR IS
manufacturer.
UNCHANGED FROM THAT USED IN THE CALIBRA-
NOTE 2—Typically 99.99 % pure nitrogen, argon, or helium is em- TION PROCEDURE.

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 E1824 − 13

FIG. 1 Determination of Tg

10.3 Move the furnace to enclose the specimen and clamps. 11. Calculation
Start the inert gas purge and equilibrate the specimen and 11.1 Derive a glass transition temperature as follows using
clamps at the desired starting temperature. graphics or software:
NOTE 4—Cool or heat the specimen, clamps and furnace to a tempera- 11.1.1 Construct a tangent to the lower temperature portion
ture equivalent to at least 3 min of heating below the first temperature of of the thermal curve,
interest to ensure stable heater control; for example, 15°C for a 5°C/min 11.1.2 Construct a tangent to the steepest portion of the
rate. The coolant used to lower the temperature should not come in contact
with the specimen or clamps.
slope beyond the transition, and
11.1.3 The temperature at which these tangents intersect is
10.4 Apply a constant tensile force to the specimen in the the derived glass transition temperature, Tg'.
range of either 5 to 10 mN (to observe shrinkage) or of 20 to
50 mN (to observe elongation). 11.2 Apply any temperature correction determined from the
instrument temperature calibration to Tg' to obtain the assigned
NOTE 5—The observed inflection temperature will be dependent upon glass transition temperature, Tg. (See Fig. 1.) Note, there are
the applied stress. Therefore, the applied force should be adjusted for three cases illustrated, namely, a sample that exhibits shrinkage
specimen cross-section area to ensure the same stress level is applied to all
specimens. (over the Tg region under the conditions utilized), a sample that
exhibits elongational reorientation, and a sample with no
10.5 Heat the specimen and clamps at a constant rate of apparent stress-relied induced dimensional change. Because Tg
5°C/min over the desired temperature range. is an assigned parameter its value may depend on experimental
NOTE 6—Other forces and heating rates may be used if applied both in conditions, namely on the applied stress on the sample, and in
the calibration and throughout the testing. The test conditions shall be the case of a film, the direction of the applied stress relative to
noted in the report. the vector of the stress relief.
10.6 Note the occurrence of an abrupt change in slope
12. Report
(positive for shrinkage and negative for elongation) of the
length versus temperature curve that indicates a transition of 12.1 Report the following information:
the material from one state to another. 12.1.1 A complete identification and description of the
material tested including specimen dimensions, clamp
10.7 Upon reaching the upper temperature limit of the
distance, and any pretreatment,
heating program, remove the applied tensile force and restore
12.1.2 Description of the instrument used for the test
the furnace, specimen, and clamps to ambient temperature.
including tensile force,
10.8 Reweigh the specimen and clamps reporting any 12.1.3 Test conditions including temperature program
change in mass. executed, purge gas composition and flow rate, and cooling
NOTE 7—Weighing of the specimen and clamps is required to determine medium if used,
whether changes such as loss of solvent or plasticizer which may alter the 12.1.4 Description of the temperature calibration procedure,
assigned glass transition temperature have occurred. 12.1.5 The thermomechanical analysis curves,

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 E1824 − 13
12.1.6 The assigned glass transition temperature, Tg, and obtained from different laboratories, operators or apparatus
12.1.7 Any change in mass associated with the test. should be considered suspect (at the 95 % confidence level) if
they differ by more than the reproducibility value.
13. Precision and Bias3 13.2.2.1 The between laboratory reproducibility standard
13.1 An interlaboratory test was conducted in 2007 on a deviation for polystyrene was 1.2°C with 28 degrees of experi-
polystyrene film. Ten laboratories participated in the test using mental freedom.
two instrument models from a single manufacturer. 13.3 Bias:
13.2 Precision: 13.3.1 Bias is the difference between the mean value ob-
13.2.1 Within laboratory variability may be describe using tained and an acceptable reference value for the same material.
the repeatability value (r) obtained by multiplying the repeat- 13.3.2 There is no accepted reference value for the glass
ability standard deviation by 2.8. The repeatability value esti- transition by thermomechanical analysis in tension of this
mates the 95 % confidence limits. That is, two results from the polystyrene material. No bias may be determined.
same laboratory should be considered suspect (at the 95 % 13.3.3 The overall mean value for the measurement of the
confidence level) if they differ by more than the repeatability glass transition on polystyrene was 106.9°C.
value. 13.3.4 The glass transition temperature for this same mate-
13.2.1.1 The within laboratory repeatability standard devia- rial was assigned using an alternative technique of modulated
tion for polystyrene is 0.53°C with 28 [( n – 1) (p – 1)] degrees temperature differential scanning calorimetry (Test Methods
of experimental freedom (with 5 replicates (n) and 8 laborato- E1545 and E2602) in a limited interlaboratory test of five
ries (p)). replicate determinations in two laboratories The mean value for
13.2.2 Between laboratory variability may be described the glass transition temperature was found be 103.2°C with a
using the reproducibility value (R) obtained my multiplying the gauge R&R standard deviation of 0.92°C for the half tempera-
reproducibility standard deviation by 2.8. The reproducibility ture midpoint method.
value estimates the 95 % confidence limit. That is, two results
14. Keywords
3
Supporting data have been filed at ASTM International Headquarters and may
14.1 glass transition; glass transition temperature; Tg; ten-
be obtained by requesting Research Report RR:E37-1037. Contact ASTM Customer sile mode; thermomechanical analysis (TMA); thermodilatom-
Service at service@astm.org. etry

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