ASTM E1867-12

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E1867 − 12
StandardTest 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 referencematerialsintoapolymertube,orwrappingthemwith
polymer tape and subjecting it to a mechanical oscillation at
1.1 This test method describes the temperature calibration
either fixed or resonant frequency. The extrapolated onset of
of dynamic mechanical analyzers (DMA) from –150 °C to
melting is identified by a rapid decrease in the ordinate signal
500 °C.
(the apparent storage modulus, stress, inverse strain or probe
1.2 The values stated in SI units are to be regarded as
position). This onset is used for temperature calibration with
standard.
two melting point reference materials.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5.1 Dynamic mechanical analyzers monitor changes in the
priate safety and health practices and determine the applica-
viscoelastic properties of a material as a function of tempera-
bility of regulatory limitations prior to use. Specific precau-
ture and frequency, providing a means to quantify these
tionary statements are given in Note 7.
changes. In most cases, the value to be assigned is the
temperature of the transition (or event) under study. Therefore,
2. Referenced Documents
the temperature axis (abscissa) of all DMA thermal curves
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must be accurately calibrated by adjusting the apparent tem-
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rhe- perature scale to match the actual temperature over the
temperature range of interest.
ology
E1142 Terminology Relating to Thermophysical Properties
6. Interferences
E2161 Terminology Relating to Performance Validation in
Thermal Analysis
6.1 An increase or decrease in heating rates or change in
purge gas type or rate from those specified may alter results.
3. Terminology
6.2 Once the temperature calibration procedure has been
3.1 Definitions:
executed, the measuring temperature sensor position shall not
3.1.1 The technical terms used in this test method are
be changed, nor shall it be in contact with the specimen or
defined in Terminologies E473, E1142, and E2161, including
specimen holder in a way that would impede movement. If the
dynamic mechanical analysis, frequency, stress, strain and
temperature sensor position is changed or is replaced, then the
storage modulus.
entire calibration procedure shall be repeated.
6.3 Once the temperature calibration has been executed, the
4. Summary of Test Method
geometry deformation (bending study, versus tensile, and the
4.1 An equation is developed for the linear correlation of
like) shall not be changed. If the specimen testing geometry
experimentally observed program or sensor temperature and
differs significantly from that of the calibrants, then the
the actual melting temperature for known melting reference
calibration shall be repeated in the geometry matching that of
materials. This is accomplished by loading melting point
specimen testing.
6.4 This method does not apply to calibration for shear or
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ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal compressive geometries of deformation.
Measurements and is the direct responsibility of Subcommittee E37.10 on
Fundamental, Statistical and Mechanical Properties.
7. Apparatus
Current edition approved Sept. 1, 2012. Published October 2012. Originally
7.1 The function of the apparatus is to hold a specimen of
approved in 1997. Last previous edition approved in 2011 as E1867 – 11. DOI:
10.1520/E1867-12.
uniform dimension so that the specimen acts as the elastic and
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
dissipative element in a mechanically oscillated system. Dy-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
namic mechanic analyzers typically operate in one of several
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. modes as outlined in Table 1.
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E1867 − 12
TABLE 1 Dynamic Mechanical Analyzer Modes of Operation
7.4 PTFE Tape, for wrapping metal point standards.
Mechanical Response
7.5 Calibration Materials—One or more suitable materials
Mode
Tensio
...