ASTM E1867-06

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E1867–06
Standard Test Method for
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Temperature Calibration of Dynamic Mechanical Analyzers
This standard is issued under the fixed designation E1867; 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 melting is identified by a rapid decrease in the ordinate signal
(the apparent storage modulus, stress, inverse strain or probe
1.1 This test method describes the temperature calibration
position). This onset is used for temperature calibration with
of dynamic mechanical analyzers (DMA) from –150 to 500°C.
two melting point reference materials.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
5. Significance and Use
standard.
5.1 Dynamic mechanical analyzers monitor changes in the
1.3 This standard does not purport to address all of the
viscoelastic properties of a material as a function of tempera-
safety concerns, if any, associated with its use. It is the
ture and frequency, providing a means to quantify these
responsibility of the user of this standard to establish appro-
changes. In most cases, the value to be assigned is the
priate safety and health practices and determine the applica-
temperature of the transition (or event) under study. Therefore,
bility of regulatory limitations prior to use. Specific precau-
the temperature axis (abscissa) of all DMA thermal curves
tionary statements are given in Note 7.
must be accurately calibrated by adjusting the apparent tem-
2. Referenced Documents perature scale to match the actual temperature over the
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temperature range of interest.
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rhe-
6. Interferences
ology
6.1 An increase or decrease in heating rates or change in
E1142 Terminology Relating to Thermophysical Properties
purge gas type or rate from those specified may alter results.
3. Terminology 6.2 Once the temperature calibration procedure has been
executed, the measuring temperature sensor position shall not
3.1 Definitions:
be changed, nor shall it be in contact with the specimen or
3.1.1 The technical terms used in this test method are
specimen holder in a way that would impede movement. If the
defined in Terminology E473 and Terminology E1142.
temperature sensor position is changed or is replaced, then the
4. Summary of Test Method entire calibration procedure shall be repeated.
6.3 Once the temperature calibration has been executed, the
4.1 An equation is developed for the linear correlation of
geometry deformation (bending study, versus tensile, and the
experimentally observed program or sensor temperature and
like) shall not be changed. If the specimen testing geometry
the actual melting temperature for known melting reference
differs significantly from that of the calibrants, then the
materials. This is accomplished by loading melting point
calibration shall be repeated in the geometry matching that of
referencematerialsintoapolymertube,orwrappingthemwith
specimen testing.
polymer tape and subjecting it to a mechanical oscillation at
6.4 This method does not apply to calibration for shear or
either fixed or resonant frequency. The extrapolated onset of
compressive geometries of deformation.
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This test method is under the jurisdiction ofASTM Committee E37 onThermal 7. Apparatus
Measurements and is the direct responsibility of Subcommittee E37.10 on Funda-
7.1 The function of the apparatus is to hold a specimen of
mental, Statistical and Mechanical Properties.
uniform dimension so that the specimen acts as the elastic and
Current edition approved Sept. 1, 2006. Published November 2006. Originally
approved in 1997. Last previous edition approved in 2001 as E1867 – 01. DOI:
dissipative element in a mechanically oscillated system. Dy-
10.1520/E1867-06.
namic mechanic analyzers typically operate in one of several
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
modes as outlined in Table 1.
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 7.1.1 The apparatus shall consist of the following:
the ASTM website.
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E1867–06
TABLE 1 Dynamic Mechanical Analyzer Modes of Operation TABLE 2 Calibration Materials
A
Mechanical Response Transition Temperature
Mode Material Reference
Tension Flexural Torsion Compression °C K
A
Free/dec . . X . Cyclopentan
...