ASTM E1363-97e1

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: E 1363 – 97
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Temperature Calibration of Thermomechanical Analyzers
This standard is issued under the fixed designation E 1363; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Editorial changes were made throughout in March 1998.
cal analyzers at temperatures outside this range of temperature. However,
1. Scope
the accuracy of the calibration will be no better than that of the
1.1 This test method covers the temperature calibration of
temperature standards used.
thermomechanical analyzers from − 50 to 1100°C. (See Note
NOTE 3—It is possible to develop a more elaborate method of tempera-
2.)
ture calibration using multiple (more than two) fusion standards and
1.2 Computer or electronic based instruments, techniques, quadratic regression analysis. Since most modern instruments are capable
of heating rates which are essentially linear in the region of use, the
or data treatment equivalent to this test method may be used.
procedure given here is limited to a two-point calibration.
NOTE 1—Users of this test method are advised that all such instruments
or techniques may not be equivalent. It is the responsibility of the user of
5. Significance and Use
this test method to determine the necessary equivalency prior to use.
5.1 Thermomechanical analyzers are employed in their
1.3 The values stated in SI units are to be regarded as the
various modes of operation (penetration, expansion, flexure,
standard.
etc.) to characterize a wide range of materials. In most cases,
1.4 This standard does not purport to address all of the
the value to be assigned in thermomechanical measurements is
safety concerns, if any, associated with its use. It is the
the temperature of the transition (or event) under study.
responsibility of the user of this standard to establish appro-
Therefore, the temperature axis (abscissa) of all TMA thermal
priate safety and health practices and determine the applica-
curves must be accurately calibrated either by direct reading of
bility of regulatory limitations prior to use. Specific precau-
a thermocouple or by adjusting the programmer temperature to
tionary statements are given in Section 7 and Note 9.
match the actual temperature over the temperature range of
interest.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
E 473 Terminology Relating to Thermal Analysis
6.1 Thermomechanical Analyzer, consisting of:
6.1.1 Specimen Holder or Platform, in which the specimen
3. Terminology
can be placed. Changes in the position of a probe (which may
3.1 Definitions:
be either weighted or to which varying levels of force may be
3.1.1 The terminology relating to thermal analysis appear-
applied) must be sensed by the instrument. A variety of probe
ing in E 473 shall be considered applicable to this document.
types may be used for such instruments. For this test method,
the use of a penetration probe is recommended. A force of
4. Summary of Test Method
50-mN (5-g) load should be employed with the penetration.
4.1 An equation is developed for the linear correlation of the
(See Note 4.)
experimentally observed program temperature and the actual
6.1.2 Sensing Element—Means for sensing movement of
melting temperature for known melting standards. This is
the probe resulting from changes in the vertical position of the
accomplished through the use of a thermomechanical analyzer
probe due to penetration into the test specimen and for
with a penetration probe to obtain the onset temperatures for
converting this movement into an electronic signal suitable for
two melting point standards. An alternate, one-point method of
input to potentiometric recording devices. The sensing element
temperature calibration, is also given for use over very narrow
should be capable of producing an electrical output of at least
temperature ranges. (See Note 3.)
1 mV per micrometre of probe movement.
NOTE 2—This test method may be used for calibrating thermomechani-
NOTE 4—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 commer-
cially available thermomechanical analyzers. These probes have tip
This test method is under the jurisdiction of ASTM Committee E-37 on
diameters ranging from 0.89 to 2.0 mm and lead to pressures from 80 to
Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on
Test Methods and Recommended Practices.
16 kPa when using the recommended 5.0-g load. The use of probes which
Current edition approved February 10, 1997. Published March 1997. Originally
differ greatly from this range of tip diameters may require different
published as E 1363 – 90. Last previous edition E 1363 – 95.
loading (or force).
Annual Book of ASTM Standards, Vol 14.02.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 1363
A
TABLE 1 Recommended Melting Temperature Standards
6.1.3 Furnace:
6.1.3.1 A means for uniformly heating the specimen at a Melting Temperature
B
Calibration Material
predetermined rate over the temperature range of interest.
(°C) (K)
Provisions should be made for precooling the furnace and
Mercury −38.8344 234.3156
specimen where near or sub-ambient temperature measure-
Water 0.01 273.16
Gallium 29.7646 302.9146
ments are to be made. The instrument should be capable of
Indium 156.5985 429.7485
providing heating rates up to 10°C per minute.
Tin 231.928 505.078
6.1.3.2 The temperature range of operation of commercial Zinc 419.527 692.677
Aluminum 660.323 933.473
thermomechanical analyzers vary from manufacturer to manu-
Silver 961.78 1234.93
facturer. The complete range of temperature of an instrument is
Gold 1064.18 1337.33
sometimes achieved by the use of two different furnaces. In Copper 1084.62 1357.77
A
this case, temperature calibration must be carried out for each
The values in Table 1 were determined using special, 99.9999 % pure
materials, and highly accurate steady state conditions that are not attainable or
furnace.
applicable to thermal analysis techniques. The actual precision of this test method
6.1.4 Thermocouple (or Other Temperature Measuring De-
is given in Section 12.
B
vice), that may be positioned in close proximity of the test
B. W. Mangnum and G. T. Furukawa, “Guidelines for Realizing the Interna-
tional Temperature Scale of 1990 (ITS-90),” National Institute of Standards and
specimen should be provided as a part of the TMA instrument.
Technology Technical Note 1265, page 8, 1990.
A chromel-alumel thermocouple is commonly used in com-
temperature calibration of the thermomechanical analyzer is
mercial instruments.
6.1.5 Pneumatic System, that provides for purging the speci- directly dependent upon it. The temperature standards given in
men with a dry inert gas. Nitrogen, argon, and helium are Table 1 will give a downward deflection on the thermal curve,
similar to that shown in Fig. 1, when placed under a weighted
commonly used for this purpose.
6.1.6 Data Handling Device, that provides a means of TMA penetration probe and heated to their respective melting
temperatures.
recording changes in the analyzer probe position as a function
of temperature. 9.2 The extrapolated onset temperature for such a penetra-
tion thermal curve is obtained by extending the pretransition
7. Hazards
portion of the thermal curve to the point of intersection with a
7.1 This test method may involve the use of hazardous
line drawn tangent to the steepest portion of the curve which
materials, operations, and equipment. It is the responsibility of
describes the probe displacement. The temperature correspond-
the user of this test method to establish appropriate safety
ing to this point of intersection is the penetration onset
practice and to determine the applicability of regulatory
temperature. This is shown graphically in Fig. 1. There are
limitations prior to use.
some materials (for example, aluminum metal) which show
pretransition probe displacement prior to the sharper down-
NOTE 5—Warning: Toxic or corrosive effluents, or both, may be
ward deflection observed on melting. In this case, the pretran-
released when heating some materials and could be harmful to personnel
and the apparatus. sition baseline is extended from the point which represents the
highest temperature the material reaches prior to exhibiting
7.2 Once this calibration procedure has been executed as
significant or measurable softening under the conditions of the
described in 10.1.2.1-10.1.2.8 of this test method, the measur-
experiment. Fig. 2 describes the assignment of the extrapolated
ing thermocouple position should not be changed, nor should it
onset temperature for a specimen which exhibits pretransition
be in contact with the sample or sample holder in a way that
penetration.
would impede movement. If for some reason the thermocouple
position is changed or the thermocouple is replaced, then the
10. Procedure
entire calibration procedure should be repeated.
10.1 Two-Point Calibration—For the purposes of this pro-
cedure, it is assumed that the relationship between observed
8. Calibration
8.1 For the temperature range covered by many applica-
tions, the melting transition of 99.99 % pure materials may be
used for calibration. (See Table 1.)
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 1968.
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.
9. Assignment of the Penetration Onset Temperature
9.1 The assignment of the TMA penetration onset tempera-
ture is an important procedure since,
...