ASTM E1867-22

Standard Test Methods for Temperature Calibration of Dynamic Mechanical Analyzers

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 dynamic mechanical analysis thermal curves must be accurately calibrated by adjusting the apparent temperature scale to match the actual specimen temperature over the temperature range of interest.  
5.2 This test method is useful for research, quality assurance, and specification acceptance.
SCOPE
1.1 These test methods describe the temperature calibration of dynamic mechanical analyzers (DMA) from –100 °C to 300 °C.  
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 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Sep-2022
• ICS: 17.200.20 - Temperature-measuring instruments
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1867 − 22
Standard Test Methods 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* Mechanical Analyzers Using Thermal Lag
1.1 These test methods describe the temperature calibration
3. Terminology
of dynamic mechanical analyzers (DMA) from –100 °C to
300 °C.
3.1 Definitions:
3.1.1 The technical terms used in these test methods are
1.2 The values stated in SI units are to be regarded as
defined in Terminologies E473, E1142, and E2161, including
standard. No other units of measurement are included in this
dynamic mechanical analysis, frequency, stress, strain, and
standard.
storage modulus.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Methods
responsibility of the user of this standard to establish appro-
4.1 In dynamic mechanical analysis, often large (for
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. example, 1 g to 10 g), low thermal conductivity test specimens
are characterized while being mechanically supported using
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard- high thermal conductivity materials, while a temperature sen-
sor is free-floating in the atmosphere near the test specimen.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- Under temperature programming conditions, where the atmo-
sphere surrounding the test specimen is heated or cooled at
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. rates up to 5 °C/min, the temperature of the test specimen may
lead or lag that of the nearby temperature sensor. It is the
2. Referenced Documents
purpose of this standard to calibrate the dynamic mechanical
2
analyzer temperature sensor so that the indicated temperature
2.1 ASTM Standards:
more closely approximates that of the test specimen. In
E473 Terminology Relating to Thermal Analysis and Rhe-
Methods A, B, and C, this is accomplished by separating the
ology
calibration specimen (with its first order transition) from its
E1142 Terminology Relating to Thermophysical Properties
mechanical supports and from the surrounding atmosphere
E1970 PracticeforStatisticalTreatmentofThermoanalytical
using a low thermal conductivity material. In Method D, the
Data
thermal lag between the temperature sensor and the test
E1640 Test Method for Assignment of the Glass Transition
specimenisdeterminedasafunctionofheatingrate.Thisvalue
Temperature By Dynamic Mechanical Analysis
is then used to adjust the indicated temperature following
E2161 Terminology Relating to Performance Validation in
calibration under isothermal ambient conditions.
Thermal Analysis and Rheology
E3142 Test Method for Thermal Lag of Thermal Analysis
4.2 An equation is developed for the linear correlation of
Apparatus
experimentally observed program or sensor temperature and
E3301 Test Method forTemperature Calibration of Dynamic
the actual melting temperature for known melting or glass
transition of the reference material. This is accomplished in
Method A by a melting point reference material loaded into a
1
These test methods are under the jurisdiction of ASTM Committee E37 on
polymer tube, or in Method B by wrapping the calibration
ThermalMeasurementsandarethedirectresponsibilityofSubcommitteeE37.10on
material with polymer tape or in Method C by placing the
Fundamental, Statistical and Mechanical Properties.
calibration material between glass or ceramic plates and
Current edition approved Oct. 1, 2022. Published October 2022. Originally
subjecting this test specimen to a mechanical oscillation at
approved in 1997. Last previous edition approved in 2018 as E1867 – 18. DOI:
10.1520/E1867-22.
either fixed or resonant frequency. The extrapolated onset of
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
melting is identified by a rapid decrease in the ordinate signal
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
(the apparent storage modulus, stress, inverse strain or probe
Standards volume information, refer to the standard’s Document Summary page on
the ASTM
...

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: E1867 − 18 E1867 − 22
Standard Test Methods 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*
1.1 These test methods describesdescribe the temperature calibration of dynamic mechanical analyzers (DMA) from –100 °C to
300 °C.–100 °C to 300 °C.
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 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E1142 Terminology Relating to Thermophysical Properties
E1970 Practice for Statistical Treatment of Thermoanalytical Data
E1640 Test Method for Assignment of the Glass Transition Temperature By Dynamic Mechanical Analysis
E2161 Terminology Relating to Performance Validation in Thermal Analysis and Rheology
E3142 Test Method for Thermal Lag of Thermal Analysis Apparatus
E3301 Test Method for Temperature Calibration of Dynamic Mechanical Analyzers Using Thermal Lag
3. Terminology
3.1 Definitions:
3.1.1 The technical terms used in these test methods are defined in Terminologies E473, E1142, and E2161, including dynamic
mechanical analysis, frequency, stress, strain, and storage modulus.
4. Summary of Test Methods
4.1 In dynamic mechanical analysis, often large (for example, 1 g to 10 g), low thermal conductivity test specimens are
1
These test methods are under the jurisdiction of ASTM Committee E37 on Thermal Measurements and are the direct responsibility of Subcommittee E37.10 on
Fundamental, Statistical and Mechanical Properties.
Current edition approved Aug. 1, 2018Oct. 1, 2022. Published August 2018October 2022. Originally approved in 1997. Last previous edition approved in 20162018 as
E1867 – 16.E1867 – 18. DOI: 10.1520/E1867-18.10.1520/E1867-22.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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E1867 − 22
characterized while being mechanically supported using high thermal conductivity materials, while a temperature sensor is
free-floating in the atmosphere near the test specimen. Under temperature programming conditions, where the atmosphere
surrounding the test specimen is heated or cooled at rates up to 5 °C/min, the temperature of the test specimen may lead or lag
that of the nearby temperature sensor. It is the purpose of this standard to calibrate the dynamic mechanical analyzer temperature
sensor so that the indicated temperature more closely approximates that of the test specimen. In Methods A, B, and C, this is
accomplished by separating the calibration specimen (with its first order transition) from its mechanical supports and from the
surrounding atmosphere using a low thermal conductivity material. In Method D, the thermal lag between the temperature sensor
and the test specimen is determined as a function of heating rate. This value is then used to adjust the indicated temperature
following calibration under isothermal ambient conditions.
4.2 An equation is developed for the linear correlation of experimentally observed program or sensor temperature and the actual
melting temperature for known melting or glass transition of the reference material. This is accomplish
...