ASTM E1363-23

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Designation: E1363 − 18 E1363 − 23
Standard Test Method for
Temperature Calibration of Thermomechanical Analyzers
This standard is issued under the fixed designation E1363; 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*Scope
1.1 This test method describes the temperature calibration of thermomechanical analyzers from −50 °C to 1500 °C. (See Note 1.)
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Warning—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious
medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use caution
when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional
information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national
law. Users must determine legality of sales in their location.
1.4 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. Specific precautionary statements are given in Section 7 and Note 1112.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E3142 Test Method for Thermal Lag of Thermal Analysis Apparatus
3. Terminology
3.1 Definitions:
3.1.1 The terminology relating to thermal analysis appearing in Terminology E473 shall be considered applicable to this
document.
4. Summary of Test Method
4.1 An equation is developed for the linear correlation of the experimentally observed program temperature and the actual melting
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 Dec. 1, 2018Aug. 1, 2023. Published January 2019August 2023. Originally approved in 1990. Last previous edition approved in 20162018 as
E1363 – 16.E1363 – 18. DOI: 10.1520/E1363-18.10.1520/E1363-23.
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.
*A Summary of Changes section appears at the end of this standard
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E1363 − 23
temperature for known melting standards. This is accomplished through the use of a thermomechanical analyzer with a penetration
probe to obtain the onset temperatures for two melting point standards. An alternate, one-point method of temperature calibration
is also given for use over very narrow temperature ranges. (See Note 2.)
NOTE 1—This test method may be used for calibrating thermomechanical analyzers at temperatures outside this range of temperature. However, the
accuracy of the calibration will be no better than that of the temperature standards used.
NOTE 2—It is possible to develop a more elaborate method of temperature calibration using multiple (more than two) fusion standards and quadratic
regression analysis. Since most modern instruments are capable of heating rates which are essentially linear in the region of use, the procedure given here
is limited to a two-point calibration.
5. Significance and Use
5.1 Thermomechanical analyzers are employed in their various modes of operation (penetration, expansion, flexure, etc.) to
characterize a wide range of materials. In most cases, the value to be assigned in thermomechanical measurements is the
temperature of the transition (or event) under study. Therefore, the temperature axis (abscissa) of all TMA thermal curves must
be accurately calibrated either by direct reading of a temperature sensor or by adjusting the programmer temperature to match the
actual temperature over the temperature range of interest.
6. Apparatus
6.1 Thermomechanical Analyzer (TMA)—(TMA)—The essential instrumentation required to provide the minimum thermome-
chanical analytical or thermodilatometric capability for this test method includes:
-1 -1
6.1.1 A Rigid Specimen Holder or Platform, of inert, low coefficient of expansion material (<1 μm m K ) to center the specimen
in the furnace and to fix the specimen to mechanical ground.
-1 -1
6.1.2 A Rigid (expansion compression, flexure, tensile, etc.) Probe, of inert, low coefficient of expansion material (<1 μm m K )
that contacts with the specimen with an applied compressive or tensile force. For this test method, the use of a penetration probe
is recommended.
6.1.3 A Sensing Element, linear over a minimum range of 2 mm to measure the displacement of the rigid probe to 650 nm 650 nm
resulting from changes in the length/height of the specimen.
6.1.4 A Weight or Force Transducer, to generate a constant force of 5050 mN 6 5 mN (5.0(5.0 g 6 0.5 g) that is applied through
the rigid probe to the specimen.
NOTE 3—The recommendation of a 5.0 g load (or a force of 50 mN) is based on the use of penetration probes commonly used in the commercially
available thermomechanical analyzers. These probes have tip diameters ranging from 0.89 mm to 2.0 mm and lead to pressures from 80 kPa 80 kPa to
16 kPa when using the recommended 5.0 g load. The use of probes which differ greatly from this range of tip diameters may require different loading
(or force).
-1 -1 -1
6.1.5 A Furnace, capable of providing uniform controlled heating (cooling) at a rate of 1 °C min to 10 10 °C min 6 1 °C min
of a specimen to a constant temperature within the applicable temperature range of this test method.
NOTE 4—The temperature range of operation of commercial thermomechanical analyzers vary by manufacturer and mode. The complete range of
temperature of an instrument is sometimes achieved by the use of two different furnaces. In this case, temperature calibration must be carried out for each
furnace.
6.1.6 A Temperature Controller, capable of executing a specific temperature program by operating the furnace between selected
-1 -1
temperature limits at a rate of temperature change of 10 10 °C min 6 1 °C min .
6.1.7 A Temperature Sensor, that may be positioned in close proximity to the test specimen to provide an indication of the
-1
specimen/furnace temperature readable to within 60.1 °C min .
6.1.8 A means of sustaining an environment around the specimen with an inert purge gas (for example, nitrogen, helium, argon,
-1 -1
etc.) at a purge gas flow rate of 20 mL min to 50 mL min .
E1363 − 23
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 TMA are a change in linear dimension, temperature, and times.
7. Hazards
7.1 This test method may involve the use of hazardous materials, operations, and equipment. It is the responsibility of the user
of this test method to establish appropriate safety practice and to determine the applicability of regulatory limitations prior to use.
(Warning—Toxic or corrosive effluents, or both, may be released when heating some materials and could be harmful to personnel
and the apparatus.)
7.2 Once this calibration procedure has been executed as described in 10.1.2.1 – 10.1.2.7 of this test method, the measuring
temperature sensor position should not be changed, nor should it be in contact with the sample or sample holder in a way that would
impede movement. If for some reason the temperature sensor position is changed or the temperature sensor is replaced, then the
entire calibration procedure should be repeated.
8. Calibration
8.1 For the temperature range covered by many applications, the melting transition of 99.99 % pure materials may be used for
calibration. (See Table 1.)
NOTE 5—The values in Table 1 were determined using special 99.9999 % pure materials and highly accurate steady-state conditions that are not attainable
with this test method. The actual precision of this test method is given in Section 13.
NOTE 6—The melting temperatures of these materials have been selected as primary fixed points (see Table 1) for the International Practical Temperature
Scale of 1990.
NOTE 7—Some materials have different crystalline forms (for example, tin) or may react with the container. Such calibration materials should be discarded
after their initial melt.
NOTE 8—Committee E37 recommends calibration of all reported signals at least annually.
9. Assignment of the Penetration Onset Temperature
9.1 The assignment of the TMA penetration onset temperature is an important procedure since, when using this test method,
TABLE 1 Recommended Melting Temperature Reference
Materials
Melting Temperature
A
Calibration Material
(°C) (K)
Mercury −38.8344 234.3156
Water 0.01 273.16
Gallium 29.7646 302.9146
Indium 156.5985 429.7485
Tin 231.928 505.078
Bismuth 271.402 544.552
Cadmium 321.069 594.219
Lead 327.462 600.612
Zinc 419.527 692.677
Antimony 630.628 903.778
Aluminum 660.323 933.473
Silver 961.78 1234.93
Gold 1064.18 1337.33
Copper 1084.62 1357.77
Nickel 1455 1728
Cobalt 1495 1768
A
Della Gatta, G., Richardson, M. J., Sarge, S. M., and Stolen, S., “Standards,
Calibration, and Guidelines in Microcalorimetry, Part 2: Calibration Standards for
Differential Scanning Calorimetry,” Pure and Applied Chemistry, Vol 78, No. 7,
2006, pp. 1455–1476.
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E37-1011. Contact ASTM Customer
Service at service@astm.org.
E1363 − 23
FIG. 1 Assignment of the Extrapolated Onset Temperature (T ) from TMA Thermal Curve
o
temperature calibration of the thermomechanical analyzer is directly dependent upon it. The temperature standards given in Table
1 will give a downward deflection on the thermal curve, similar to that shown in Fig. 1, when placed under a weighted TMA
penetration probe and heated to their respective melting temperatures.
9.2 The extrapolated onset temperature for such a penetration thermal curve is obtained by extending the pre-transition portion
of the thermal curve to the point of intersection with a line drawn tangent to the steepest portion of the curve which describes the
probe displacement. The temperature corresponding to this point of intersection is
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