ASTM E1867-11
(Test Method)Standard Test Method for Temperature Calibration of Dynamic Mechanical Analyzers
Standard Test Method for Temperature Calibration of Dynamic Mechanical Analyzers
SIGNIFICANCE AND USE
Dynamic mechanical analyzers monitor changes in the viscoelastic properties of a material as a function of temperature and frequency, providing a means to quantify these changes. In most cases, the value to be assigned is the temperature of the transition (or event) under study. Therefore, the temperature axis (abscissa) of all DMA thermal curves must be accurately calibrated by adjusting the apparent temperature scale to match the actual temperature over the temperature range of interest.
SCOPE
1.1 This test method describes the temperature calibration of dynamic mechanical analyzers (DMA) from –150 °C to 500 °C.
1.2 The values stated in SI units are to be regarded as standard.
1.3 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 Note 7.
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Designation: E1867 − 11
StandardTest Method for
1
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
2
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
1
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 Aug. 1, 2011. Published September 2011. Originally
7.1 The function of the apparatus is to hold a specimen of
approved in 1997. Last previous edition approved in 2006 as E1867 – 06. DOI:
10.1520/E1867-11.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E1867 − 11
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
Tensi
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:E1867–06 Designation:E1867–11
Standard Test Method for
1
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
1.1This test method describes the temperature calibration of dynamic mechanical analyzers (DMA) from –150 to 500°C.
1.2The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.1 This test method describes the temperature calibration of dynamic mechanical analyzers (DMA) from –150 °C to 500 °C.
1.2 The values stated in SI units are to be regarded as standard.
1.3 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 Note 7.
2. Referenced Documents
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E1142 Terminology Relating to Thermophysical Properties Terminology Relating to Thermophysical Properties
E2161 Terminology Relating to Performance Validation in Thermal Analysis
3. Terminology
3.1 Definitions:
3.1.1 The technical terms used in this test method are defined in Terminologyies E473and Terminology , E1142. , and E2161,
including dynamic mechanical analysis, frequency, stress, strain and storage modulus.
4. Summary of Test Method
4.1 Anequationisdevelopedforthelinearcorrelationofexperimentallyobservedprogramorsensortemperatureandtheactual
meltingtemperatureforknownmeltingreferencematerials.Thisisaccomplishedbyloadingmeltingpointreferencematerialsinto
a polymer tube, or wrapping them with polymer tape and subjecting it to a mechanical oscillation at either fixed or resonant
frequency.The extrapolated onset of melting is identified by a rapid decrease in the ordinate signal (the apparent storage modulus,
stress, inverse strain or probe position). This onset is used for temperature calibration with two melting point reference materials.
5. Significance and Use
5.1 Dynamic mechanical analyzers monitor changes in the viscoelastic properties of a material as a function of temperature and
frequency, providing a means to quantify these changes. In most cases, the value to be assigned is the temperature of the transition
(or event) under study. Therefore, the temperature axis (abscissa) of all DMA thermal curves must be accurately calibrated by
adjusting the apparent temperature scale to match the actual temperature over the temperature range of interest.
6. Interferences
6.1 An increase or decrease in heating rates or change in purge gas type or rate from those specified may alter results.
6.2 Once the temperature calibration procedure has been executed, the measuring temperature sensor position shall not be
changed,norshallitbeincontactwiththespecimenorspecimenholderinawaythatwouldimpedemovement.Ifthetemperature
sensor position is changed or is replaced, then the entire calibration procedure shall be repeated.
6.3 Once the temperature calibration has been executed, the geometry deformation (bending study, versus tensile, and the like)
shall not be changed. If the specimen testing geometry differs significantly from that of the calibrants, then the calibration shall
1
This test method is under the jurisdiction ofASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,
Statistical and Mechanical Properties.
Current edition approved Sept.Aug. 1, 2006.2011. Published November 2006.September 2011. Originally approved in 1997. Last previous edition approved in 20012006
as E1867 – 016. DOI: 10.1520/E1867-06.10.1520/E1867-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
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E1867–11
be repeated in the geometry matching tha
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