ASTM E3301-22

Standard Test Method for Temperature Calibration of Dynamic Mechanical Analyzers Using Thermal Lag

SIGNIFICANCE AND USE
5.1 Dynamic mechanical analysis monitors changes in the viscoelastic properties (that is, storage modulus, loss modulus, tangent angle delta) of a material as a function of temperature and frequency, providing a means to quantify these changes. In many cases, the value to be assigned is the temperature of the transition or event under study. Therefore, the temperature axis (abscissa) of the dynamic mechanical analysis thermal curve must be accurately calibrated by adjusting the measured temperature scale to match the assumed specimen temperature over the temperature range of interest.
SCOPE
1.1 This test method describes the temperature calibration of a dynamic mechanical analyzer using thermal lag over the temperature range of –100 °C to 300 °C.  
1.2 This standard may be compared to Test Methods E1867.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
1.5 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: 31-Dec-2021
• ICS: 17.200.01 - Thermodynamics in general
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Relations

• Refers: ASTM E473-23b - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 01-Oct-2023
• Refers: ASTM E1142-23b - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-Oct-2023
• Refers: ASTM E2877-12(2019) - Standard Guide for Digital Contact Thermometers
• Effective Date: 01-May-2019
• Refers: ASTM E1640-13(2018) - Standard Test Method for Assignment of the Glass Transition Temperature By Dynamic Mechanical Analysis
• Effective Date: 15-Mar-2018
• Refers: ASTM E3142-18 - Standard Test Method for Thermal Lag of Thermal Analysis Apparatus
• Effective Date: 15-Jan-2018
• Refers: ASTM E1867-16 - Standard Test Methods for Temperature Calibration of Dynamic Mechanical Analyzers
• Effective Date: 15-Feb-2016
• Refers: ASTM E2161-15 - Standard Terminology Relating to Performance Validation in Thermal Analysis and Rheology
• Effective Date: 01-Sep-2015
• Refers: ASTM E1142-15 - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-May-2015
• Refers: ASTM E473-14 - Standard Terminology Relating to Thermal Analysis and Rheology
• Effective Date: 15-Aug-2014
• Refers: ASTM E1142-14b - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 15-Aug-2014
• Refers: ASTM E1142-14a - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 01-Apr-2014
• Refers: ASTM E1142-14 - Standard Terminology Relating to Thermophysical Properties
• Effective Date: 15-Feb-2014
• Refers: ASTM E1867-13 - Standard Test Method for Temperature Calibration of Dynamic Mechanical Analyzers
• Effective Date: 01-Apr-2013
• Refers: ASTM E2161-13 - Standard Terminology Relating to Performance Validation in Thermal Analysis
• Effective Date: 01-Mar-2013
• Refers: ASTM E2877-12e1 - Standard Guide for Digital Contact Thermometers
• Effective Date: 01-Nov-2012

Overview

ASTM E3301-22 is an international standard developed by ASTM International that specifies a test method for temperature calibration of dynamic mechanical analyzers (DMA) using thermal lag. This standard is critical for ensuring accurate measurements of the viscoelastic properties of materials, especially in processes where temperature-dependent properties such as storage modulus, loss modulus, and tangent delta are studied. By calibrating the temperature axis of DMA instruments to account for thermal lag, laboratories can improve the reliability and comparability of their data across a temperature range of –100 °C to 300 °C.

Key Topics

• Dynamic Mechanical Analysis (DMA): Focuses on measuring viscoelastic properties of materials as functions of temperature and frequency.
• Temperature Calibration: Employs the concept of thermal lag to adjust the measured temperature, ensuring it reflects the actual specimen temperature.
• Thermal Lag: Accounts for differences between sensor and specimen temperatures due to heating/cooling rates, specimen geometry, and material properties.
• Calibration Procedure: Involves use of high-temperature polymer calibration materials with defined glass transition temperatures, precise mounting, and controlled temperature programming.
• Measurement Accuracy: Outlines the need for calibration validity per specimen geometry, and specifies repeatability and reproducibility guidelines.

Applications

The ASTM E3301-22 test method is widely used in materials characterization, research, and quality control where dynamic mechanical analyzers are employed. Key applications include:

• Polymers and Composites Testing: Accurate determination of glass transition temperature and other thermal transitions in plastics, rubbers, adhesives, and composites.
• Product Development: Ensures that engineers and scientists have reliable thermal-mechanical data when developing new materials or verifying product performance.
• Quality Assurance: Supports manufacturers and laboratories to validate instrument performance and maintain compliance with industrial or regulatory requirements.
• Comparative Studies: Facilitates comparison of DMA results across different instruments, labs, or methods by standardizing temperature calibration according to thermal lag.
• Research and Academic Work: Provides a robust framework for temperature measurement and calibration, suitable for academic investigations into the mechanical behavior of advanced materials.

Related Standards

ASTM E3301-22 references and aligns with several related ASTM standards for calibration, terminology, and experimental practices:

• ASTM E1867: Test methods for temperature calibration of dynamic mechanical analyzers.
• ASTM E1640: Assignment of the glass transition temperature by dynamic mechanical analysis.
• ASTM E1356: Assignment of glass transition temperatures by differential scanning calorimetry.
• ASTM E3142: Thermal lag of thermal analysis apparatus.
• ASTM D4092, E473, E1142, E2161: Terminology standards for dynamic mechanical analysis and related fields.
• ASTM E2877: Guide for digital contact thermometers.
• ASTM E1970: Statistical treatment of thermoanalytical data.

Practical Value

Implementing ASTM E3301-22 ensures:

• Accurate DMA Temperature Measurement: Reduces systematic error, improving confidence in assignment of critical transitions in material testing.
• Consistency Across Tests: Supports repeatable and reproducible results by enforcing standardized calibration steps and reporting requirements.
• Regulatory Compliance: Meets requirements for international trade and laboratory accreditation by aligning with WTO Technical Barriers to Trade (TBT) principles.

Regular use of ASTM E3301-22 benefits industries working with thermoplastics, composites, coatings, adhesives, and elastomers, promoting high-quality data, smoother inter-laboratory collaboration, and more robust product validation processes.

Keywords: ASTM E3301-22, temperature calibration, dynamic mechanical analyzer, DMA, thermal lag, viscoelastic properties, polymers, glass transition, thermal analysis, material testing, standard test method.

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: E3301 − 22
Standard Test Method for
Temperature Calibration of Dynamic Mechanical Analyzers
Using Thermal Lag
This standard is issued under the fixed designation E3301; 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 namic Mechanical Analyzers
E1970 PracticeforStatisticalTreatmentofThermoanalytical
1.1 This test method describes the temperature calibration
Data
of a dynamic mechanical analyzer using thermal lag over the
E2161 Terminology Relating to Performance Validation in
temperature range of –100 °C to 300 °C.
Thermal Analysis and Rheology
1.2 This standard may be compared toTest Methods E1867.
E2877 Guide for Digital Contact Thermometers
1.3 The values stated in SI units are to be regarded as E3142 Test Method for Thermal Lag of Thermal Analysis
Apparatus
standard. No other units of measurement are included in this
standard.
3. Terminology
1.4 This standard does not purport to address all of the
3.1 Definitions:
safety concerns, if any, associated with its use. It is the
3.1.1 The technical terms used in this test method are
responsibility of the user of this standard to establish appro-
defined in Terminologies D4092, E473, E1142, and E2161
priate safety, health, and environmental practices and deter-
including calibration, Celsius, damping, dissipative, elastic,
mine the applicability of regulatory limitations prior to use.
frequency, loss modulus, peak, storage modulus, strain, stress
1.5 This international standard was developed in accor-
tan δ, tan delta, tangent delta.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
3.2 Definitions of Terms Specific to This Standard:
Development of International Standards, Guides and Recom- 3.2.1 dew point, n—the temperature below which conden-
mendations issued by the World Trade Organization Technical sation of water vapor begins when the atmosphere is cooled.
Barriers to Trade (TBT) Committee.
3.2.2 relaxation, n—in a glass or viscous liquid, the change
in any material property (such as density, enthalpy, etc.) with
2. Referenced Documents
timefollowingaperturbation(suchasachangeintemperature,
2.1 ASTM Standards: stress. etc.).
D4092 Terminology for Plastics: Dynamic Mechanical
4. Summary of Test Method
Properties
E473 Terminology Relating to Thermal Analysis and Rhe- 4.1 In dynamic mechanical analysis, large (for example, 1 g
ology to 10 g), low thermal conductivity test specimens are charac-
E1142 Terminology Relating to Thermophysical Properties terized. These specimens are mechanically supported using
E1356 Test Method for Assignment of the Glass Transition high thermal conductivity materials of construction. A free-
Temperatures by Differential Scanning Calorimetry floatingtemperaturesensorisplacedascloseaspracticaltothe
E1640 Test Method for Assignment of the Glass Transition specimen. Under conditions of temperature change, where the
Temperature By Dynamic Mechanical Analysis
system atmosphere surrounding the specimen is heated or
E1867 Test Methods for Temperature Calibration of Dy- cooled at rates up to 5 °C/min, the temperature of the specimen
will lead or lag that of the temperature sensor. It is the purpose
of this standard to calibrate the dynamic mechanical analyzer
temperature signal so that the measured temperature more
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
Measurements and is the direct responsibility of Subcommittee E37.10 on
closely approximates that of the assumed test specimen.
Fundamental, Statistical and Mechanical Properties.
4.2 The thermal lag between the temperature sensor and the
Current edition approved Jan. 1, 2022. Published January 2022. DOI: 10.1520/
E3301-22.
testspecimenisdeterminedasafunctionoftemperaturerateof
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
change. This value is then used to adjust the indicated
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
temperature following calibration under isothermal ambient
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. temperature conditions.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E3301 − 22
5. Significance and Use 7. Apparatus
7.1 Dynamic Mechanical Analyzer—The essential instru-
5.1 Dynamic mechanical analysis monitors changes in the
mentation required to provide the minimum dynamic mechani-
viscoelastic properties (that is, storage modulus, loss modulus,
cal capability for this method includes:
tangent angle delta) of a material as a function of temperature
7.1.1 A drive motor, to apply force or displacement to the
and frequency, providing a means to quantify these changes. In
specimeninaperiodicmannercapableoffrequencyof1 60.1
many cases, the value to be assigned is the temperature of the
Hz.Thismotormayalsobecapableofprovidingstaticforceor
transition or event under study.Therefore, the temperature axis
displacement on the specimen.
(abscissa) of the dynamic mechanical analysis thermal curve
must be accurately calibrated by adjusting the measured
NOTE 2—Dynamic mechanical analyzers often have a frequency range
temperature scale to match the assumed specimen temperature of several decades. Other frequencies may be used but shall be reported.
Thermal lag of the glass transition is constant over a 30-fold range from
over the temperature range of interest.
1Hzto30Hz (2).
7.1.2 A coupling shaft, or other means to transmit the force
6. Interferences
or displacement from the motor to the specimen.
6.1 Once the temperature calibration procedure has been
7.1.3 A clamping system(s) to fix the specimen between the
executed, the temperature measuring sensor position shall not
coupling shaft and the stationary clamp(s).
be changed, nor shall it be in contact with the specimen or
7.1.4 A position sensor, to measure the changes in position
specimen holder in a way that would impede movement. If the
of the specimen during dynamic motion readable to1%of full
temperature sensor position is changed or it is replaced, then
scale, or
the entire calibration procedure shall be repeated.
7.1.5 A force sensor, to measure the force developed by the
specimen readable to1%of full scale.
6.2 The temperature calibration is valid only for the speci-
7.1.6 A temperature sensor, to provide an indication of the
men test geometry (bending, tension, and the like) used during
specimen temperature readable to 0.1 °C.
the calibration process. If multiple geometries are used, then
7.1.7 A furnace, to provide controlled heating or cooling of
calibration shall be performed for each geometry.
a specimen at a constant temperature or at a constant rate
6.3 Apparatus temperature calibration is known to be de- withintheapplicabletemperaturerangeof–100°Cto+300°C.
pendent upon the purge gas type (thermal conductivity) and 7.1.8 A temperature controller, capable of executing a
flow rate and upon specimen size. These experimental condi- specifictemperatureprogrambyoperatingthefurnacebetween
tions shall be the same for calibration as for the testing of selected temperature limits at a rate of temperature change of
up to 5 °C/min constant to within 0.1 °C/min or at an
unknown specimens.
isothermal temperature constant to 0.1 °C.
6.4 Thermal lag is reported to be a linear function of
7.1.9 A data collection device, to provide a means of
temperatureoverthetemperaturerangeofthisstandard (1). In
acquiring, storing, and displaying measured or calculated
principle, the dependence of thermal lag on temperature may
signals, or both. The minimum output signals required for
be determined using Test Method E3142 and a series of
dynamic mechanical analysis are storage modulus, loss
materials with differing glass transition temperatures.
modulus, tangent angle delta, frequency, temperature, and
time.
NOTE 1—In addition to polycarbonate used here, polystyrene and
polyimide have been found suitable by some users (see 8.1).
NOTE 3—Some instruments, suitable for this test, may display only
linearorlogarithmicstoragemoduluswhileothersmaydisplaybothlinear
6.5 The glass transition is a kinetic event and will increase
and logarithmic storage modulus. Care shall be taken to use the same
in temperature with increasing temperature-rate-of-change
modulus scale when comparing specimens and the comparison of results
(heating rate) and with oscillatory frequency. For low heating
from one instrument to another.
rates used in dynamic mechanical analysis, the increase in
7.1.10 Data analysis capability, to provide storage
temperature is assumed to be insignificantly small. In one case,
modulus, loss modulus, tangent angle delta, or other useful
the thermal lag effect was observed to be 0.25 min while the
parameters derived from the measu
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