ASTM E1363-13
(Test Method)Standard Test Method for Temperature Calibration of Thermomechanical Analyzers
Standard Test Method for Temperature Calibration of Thermomechanical Analyzers
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.
SCOPE
1.1 This test method describes the temperature calibration of thermomechanical analyzers from − 50 to 1100°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 This standard is similar to ISO 11359–1 but addresses a larger temperature range and utilizes additional calibration materials.
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 7 and Note 10.
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Designation: E1363 − 13
Standard Test Method for
1
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Summary of Test Method
1.1 This test method describes the temperature calibration 4.1 Anequationisdevelopedforthelinearcorrelationofthe
of thermomechanical analyzers from−50 to 1100°C. (See experimentally observed program temperature and the actual
Note 1.)
melting temperature for known melting standards. This is
accomplished through the use of a thermomechanical analyzer
1.2 The values stated in SI units are to be regarded as
with a penetration probe to obtain the onset temperatures for
standard. No other units of measurement are included in this
twomeltingpointstandards.Analternate,one-pointmethodof
standard.
temperature calibration, is also given for use over very narrow
1.3 This standard is similar to ISO 11359–1 but addresses a
temperature ranges. (See Note 2.)
larger temperature range and utilizes additional calibration
NOTE1—Thistestmethodmaybeusedforcalibratingthermomechani-
materials.
cal analyzers at temperatures outside this range of temperature. However,
1.4 This standard does not purport to address all of the
the accuracy of the calibration will be no better than that of the
safety concerns, if any, associated with its use. It is the
temperature standards used.
NOTE 2—It is possible to develop a more elaborate method of
responsibility of the user of this standard to establish appro-
temperature calibration using multiple (more than two) fusion standards
priate safety and health practices and determine the applica-
and quadratic regression analysis. Since most modern instruments are
bility of regulatory limitations prior to use. Specific precau-
capable of heating rates which are essentially linear in the region of use,
tionary statements are given in Section 7 and Note 10.
the procedure given here is limited to a two-point calibration.
2. Referenced Documents
5. Significance and Use
2
2.1 ASTM Standards:
5.1 Thermomechanical analyzers are employed in their
E473Terminology Relating to Thermal Analysis and Rhe-
various modes of operation (penetration, expansion, flexure,
ology
etc.) to characterize a wide range of materials. In most cases,
3
the value to be assigned in thermomechanical measurements is
2.2 Other Standards:
the temperature of the transition (or event) under study.
ISO 11359–1 Thermomechanical Analysis (TMA)-Part 1:
Therefore, the temperature axis (abscissa) of all TMAthermal
General Principles
curvesmustbeaccuratelycalibratedeitherbydirectreadingof
a temperature sensor or by adjusting the programmer tempera-
3. Terminology
turetomatchtheactualtemperatureoverthetemperaturerange
3.1 Definitions:
of interest.
3.1.1 The terminology relating to thermal analysis appear-
ing inTerminology E473 shall be considered applicable to this
6. Apparatus
document.
6.1 Thermomechanical Analyzer (TMA), The essential in-
strumentation required to provide the minimum thermome-
chanical analytical or thermodilatometric capability for this
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
method includes:
Measurements and is the direct responsibility of Subcommittee E37.10 on
Fundamental, Statistical and Mechanical Properties. 6.1.1 A Rigid Specimen Holder or Platform, of inert, low
-1 -1
Current edition approved April 1, 2013. Published May 2013. Originally
expansivitymaterial(<1µmm K )tocenterthespecimenin
approved in 1990. Last previous edition approved in 2008 as E1363–08. DOI:
the furnace and to fix the specimen to mechanical ground.
10.1520/E1363-13.
2
6.1.2 A Rigid (expansion compression, flexure, tensile, etc.)
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
-1 -1
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Probe, of inert, low expansivity material (<1 µm m K ) that
Standards volume information, refer to the standard’s Document Summary page on
contacts with the specimen with an applied compressive or
the ASTM website.
3
tensileforce.Forthistestmethodtheuseofapenetrationprobe
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org. is recommended.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1363 − 13
TABLE 1 Recommended Melting Temperature Reference
6.1.3 A Sensing Element, linear over a minimum range of 2
A
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E1363 − 08 E1363 − 13
Standard Test Method for
1
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
1.1 This test method describes the temperature calibration of thermomechanical analyzers from − 50 to 1100 °C. 1100°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 This standard is similar to ISO 11359–1 but addresses a larger temperature range and utilizes additional calibration
materials.
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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific precautionary statements are given in Section 7 and Note 910.
2. Referenced Documents
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
3
2.2 Other Standards:
ISO 11359–1 Thermomechanical Analysis (TMA)-Part 1: General Principles
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 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
1
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 Sept. 1, 2008April 1, 2013. Published September 2008May 2013. Originally approved in 1990. Last previous edition approved in 20032008 as
E1363 – 03.E1363 – 08. DOI: 10.1520/E1363-08.10.1520/E1363-13.
2
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.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1363 − 13
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), The essential instrumentation required to provide the minimum thermomechanical
analytical or thermodilatometric capability for this method includes:
-1 -1
6.1.1 A Rigid Specimen Holder or Platform, of inert, low expansivity material (< 1 μm m K ) to center the specimen in the
f
...
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