ASTM E2602-22
(Test Method)Standard Test Methods for Assignment of the Glass Transition Temperature by Modulated Temperature Differential Scanning Calorimetry
Standard Test Methods for Assignment of the Glass Transition Temperature by Modulated Temperature Differential Scanning Calorimetry
SIGNIFICANCE AND USE
5.1 Materials undergo an increase in molecular mobility at the glass transition seen as a sigmoidal step increase in the heat capacity. This mobility increase may lead to kinetic events such as enthalpic recovery, chemical reaction or crystallization at temperatures near the glass transition. The heat flow associated with the kinetic events may interfere with the determination of the glass transition.
5.2 The glass transition is observed in differential scanning calorimetry as a sigmoidal or step change in specific heat capacity.
5.3 MTDSC provides a test method for the separation of the heat flow due to heat capacity and that associated with kinetic events making it possible to determine the glass transition in the presence of interfering kinetic event.
5.4 These test methods are useful in research and development, quality assurance and control and specification acceptance.
5.5 Other methods for assigning the glass transition temperature include differential scanning calorimetry (Test Method E1356), thermomechanical analysis (Test Method E1545) and dynamic mechanical analysis (Test Method E1640).
SCOPE
1.1 These test methods describe the assignment of the glass transition temperature of materials using modulated temperature differential scanning calorimetry (MTDSC) over the temperature range from –120 °C to +600 °C. The temperature range may be extended depending upon the instrumentation used.
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
- 31-Jan-2022
- Technical Committee
- E37 - Thermal Measurements
- Drafting Committee
- E37.01 - Calorimetry and Mass Loss
Relations
- Effective Date
- 01-Oct-2023
- Effective Date
- 01-Oct-2023
- Effective Date
- 15-Mar-2018
- Effective Date
- 01-May-2015
- Effective Date
- 15-Aug-2014
- Effective Date
- 15-Aug-2014
- Effective Date
- 01-Apr-2014
- Effective Date
- 15-Feb-2014
- Effective Date
- 01-Sep-2012
- Effective Date
- 01-Aug-2011
- Effective Date
- 15-Jun-2011
- Effective Date
- 15-Jun-2011
- Effective Date
- 01-Apr-2011
- Effective Date
- 01-Apr-2011
- Effective Date
- 01-Apr-2011
Overview
ASTM E2602-22: Standard Test Methods for Assignment of the Glass Transition Temperature by Modulated Temperature Differential Scanning Calorimetry (MTDSC) provides methodologies for determining the glass transition temperature (Tg) of materials using advanced differential scanning calorimetry techniques. The standard covers procedures for analyzing Tg over a temperature range from –120 °C to +600 °C using modulated temperature programs, which are especially beneficial when kinetic events occur near the glass transition region. This capability enables more accurate and reliable thermal analysis compared to conventional DSC methods, which may be affected by overlapping thermal phenomena.
Key Topics
- Glass Transition Temperature (Tg): The standard focuses on identifying the glass transition, characterized by a sigmoidal change in heat capacity, reflecting increased molecular mobility in the material.
- Modulated Temperature Differential Scanning Calorimetry (MTDSC): Utilizes a sinusoidal, step, or pulse temperature modulation superimposed on the typical DSC heating ramp, allowing the separation of reversing and nonreversing heat flow components.
- Separation of Thermal Events: MTDSC distinguishes between changes in heat capacity (reversing) and kinetic events such as curing, crystallization, or enthalpic recovery (nonreversing), enhancing the reliability of Tg determination even in complex material systems.
- Testing Methods: The standard describes multiple test methods including:
- Sinusoidal temperature modulation
- Step temperature procedure
- Temperature pulse method
- Calibration and Reporting: The document lays out procedures for instrument calibration, use of appropriate reference materials, and comprehensive reporting requirements to ensure traceability and reproducibility.
Applications
ASTM E2602-22 finds wide use across industries and research settings where accurate thermal characterization is critical:
- Material Research and Development: Reliable Tg measurements enable optimal material selection, formulation, and assessment of new polymers, composites, glasses, and other thermally sensitive materials.
- Quality Control and Assurance: Routine Tg determination aids in verifying material consistency and detecting batch-to-batch variations in production settings.
- Specification and Compliance Testing: The standard provides methodologies suitable for acceptance testing and specification compliance, ensuring materials meet performance criteria related to temperature stability and processability.
- Analysis Under Complex Conditions: The advanced separation capabilities of MTDSC make this standard valuable for analyzing materials undergoing simultaneous thermal events, such as curing thermosets, crystallizing systems, or materials with overlapping thermal transitions.
Related Standards
In addition to ASTM E2602-22, several ASTM standards provide complementary guidance for thermal analysis and Tg assignment:
- ASTM E1356: Test Method for Assignment of the Glass Transition Temperatures by Differential Scanning Calorimetry
- ASTM E1545: Test Method for Assignment of the Glass Transition Temperature by Thermomechanical Analysis
- ASTM E1640: Test Method for Assignment of the Glass Transition Temperature by Dynamic Mechanical Analysis
- ASTM E473: Terminology Relating to Thermal Analysis and Rheology
- ASTM E967: Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers
- ASTM E968: Practice for Heat Flow Calibration of Differential Scanning Calorimeters
- ASTM E1142: Terminology Relating to Thermophysical Properties
Practical Value
Implementing ASTM E2602-22 helps organizations:
- Achieve higher confidence in thermal analysis results, particularly for materials with complex thermal behaviors
- Support product development by providing robust data for processing and performance optimization
- Ensure compliance with internationally recognized testing methodologies aligned with World Trade Organization (WTO) principles
- Facilitate clear communication in technical documentation and regulatory submissions
By using ASTM E2602-22, laboratories and manufacturers can advance their understanding of material properties, bolster quality protocols, and contribute to successful product development across the material sciences and engineering sectors.
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Frequently Asked Questions
ASTM E2602-22 is a standard published by ASTM International. Its full title is "Standard Test Methods for Assignment of the Glass Transition Temperature by Modulated Temperature Differential Scanning Calorimetry". This standard covers: SIGNIFICANCE AND USE 5.1 Materials undergo an increase in molecular mobility at the glass transition seen as a sigmoidal step increase in the heat capacity. This mobility increase may lead to kinetic events such as enthalpic recovery, chemical reaction or crystallization at temperatures near the glass transition. The heat flow associated with the kinetic events may interfere with the determination of the glass transition. 5.2 The glass transition is observed in differential scanning calorimetry as a sigmoidal or step change in specific heat capacity. 5.3 MTDSC provides a test method for the separation of the heat flow due to heat capacity and that associated with kinetic events making it possible to determine the glass transition in the presence of interfering kinetic event. 5.4 These test methods are useful in research and development, quality assurance and control and specification acceptance. 5.5 Other methods for assigning the glass transition temperature include differential scanning calorimetry (Test Method E1356), thermomechanical analysis (Test Method E1545) and dynamic mechanical analysis (Test Method E1640). SCOPE 1.1 These test methods describe the assignment of the glass transition temperature of materials using modulated temperature differential scanning calorimetry (MTDSC) over the temperature range from –120 °C to +600 °C. The temperature range may be extended depending upon the instrumentation used. 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.
SIGNIFICANCE AND USE 5.1 Materials undergo an increase in molecular mobility at the glass transition seen as a sigmoidal step increase in the heat capacity. This mobility increase may lead to kinetic events such as enthalpic recovery, chemical reaction or crystallization at temperatures near the glass transition. The heat flow associated with the kinetic events may interfere with the determination of the glass transition. 5.2 The glass transition is observed in differential scanning calorimetry as a sigmoidal or step change in specific heat capacity. 5.3 MTDSC provides a test method for the separation of the heat flow due to heat capacity and that associated with kinetic events making it possible to determine the glass transition in the presence of interfering kinetic event. 5.4 These test methods are useful in research and development, quality assurance and control and specification acceptance. 5.5 Other methods for assigning the glass transition temperature include differential scanning calorimetry (Test Method E1356), thermomechanical analysis (Test Method E1545) and dynamic mechanical analysis (Test Method E1640). SCOPE 1.1 These test methods describe the assignment of the glass transition temperature of materials using modulated temperature differential scanning calorimetry (MTDSC) over the temperature range from –120 °C to +600 °C. The temperature range may be extended depending upon the instrumentation used. 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.
ASTM E2602-22 is classified under the following ICS (International Classification for Standards) categories: 17.200.10 - Heat. Calorimetry. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM E2602-22 has the following relationships with other standards: It is inter standard links to ASTM E473-23b, ASTM E1142-23b, ASTM E1640-13(2018), ASTM E1142-15, ASTM E473-14, ASTM E1142-14b, ASTM E1142-14a, ASTM E1142-14, ASTM E1142-12, ASTM E1142-11b, ASTM E473-11a, ASTM E1142-11a, ASTM E1142-11, ASTM E473-11, ASTM E1545-11. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM E2602-22 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
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: E2602 − 22
Standard Test Methods for
Assignment of the Glass Transition Temperature by
Modulated Temperature Differential Scanning Calorimetry
This standard is issued under the fixed designation E2602; 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 E1356 Test Method for Assignment of the Glass Transition
Temperatures by Differential Scanning Calorimetry
1.1 These test methods describe the assignment of the glass
E1545 Test Method for Assignment of the Glass Transition
transition temperature of materials using modulated tempera-
Temperature by Thermomechanical Analysis
ture differential scanning calorimetry (MTDSC) over the
E1640 Test Method for Assignment of the Glass Transition
temperature range from –120 °C to +600 °C. The temperature
Temperature By Dynamic Mechanical Analysis
range may be extended depending upon the instrumentation
used.
3. Terminology
1.2 The values stated in SI units are to be regarded as
3.1 Definitions—Specific technical terms found in these test
standard. No other units of measurement are included in this
methods are defined in Terminologies E473 and E1142 includ-
standard.
ing differential scanning calorimetry, extrapolated onset, glass
1.3 This standard does not purport to address all of the
transition, glass transition temperature, non-reversing,
safety concerns, if any, associated with its use. It is the
reversing, specific heat capacity, and thermal curve.
responsibility of the user of this standard to establish appro-
3.2 Definitions of Terms Specific to This Standard:
priate safety, health, and environmental practices and deter-
3.2.1 extrapolated end temperature (Te), n—the point of
mine the applicability of regulatory limitations prior to use.
intersection of the tangent drawn at the point of greatest slope
1.4 This international standard was developed in accor-
(that is, the inflection point) in the transition region with the
dance with internationally recognized principles on standard-
extrapolated baseline following the transition.
ization established in the Decision on Principles for the
3.2.2 extrapolated onset temperature (Tf), n—the point of
Development of International Standards, Guides and Recom-
intersection of the tangent drawn at the point of greatest slope
mendations issued by the World Trade Organization Technical
(that is, the inflection point) in the transition region with the
Barriers to Trade (TBT) Committee.
extrapolated baseline prior to the transition.
2. Referenced Documents
3.2.3 midpoint temperature (Tm), n—the point on the ther-
mal curve corresponding to the average of the extrapolated
2.1 ASTM Standards:
onset and extrapolated end temperatures.
E473 Terminology Relating to Thermal Analysis and Rhe-
ology 3.2.4 modulated, n—a prefix indicating that a parameter
E967 Test Method for Temperature Calibration of Differen-
changes in a periodic manner during the experiment.
tial Scanning Calorimeters and Differential Thermal Ana-
3.2.5 modulated heat flow, n—the heat flow resulting from
lyzers
an applied modulated temperature program.
E968 Practice for Heat Flow Calibration of Differential
3.2.6 modulated temperature differential scanning calorim-
Scanning Calorimeters
etry (MTDSC),n—a method of differential scanning calorim-
E1142 Terminology Relating to Thermophysical Properties
etry (DSC) that varies the temperature sinusoidally or with a
periodic step-and-hold or pulse program to the test specimen
1 over a traditional isothermal or temperature ramp program.
These test methods are under the jurisdiction of ASTM Committee E37 on
Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Results from the experiment include reversing and nonrevers-
Calorimetry and Mass Loss.
ing heat flow and specimen temperature.
Current edition approved Feb. 1, 2022. Published May 2022. Originally
3.2.7 total heat flow, n—the value of the modulated heat
approved in 2009. Last previous edition approved in 2015 as E2602 – 09 (2015).
DOI: 10.1520/E2602-22.
flow averaged over one modulation period or impulse.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.2.7.1 Discussion—The total heat flow is equivalent to the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
heat flow signal of conventional differential scanning calorim-
Standards volume information, refer to the standard’s Document Summary page on
theASTM website. etry.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2602 − 22
3.2.7.2 Discussion—The total heat flow is equal to the sum other low conductivity) purge gas at a rate of 20 mL/min to 60
of the reversing and nonreversing heat flows. mL/min constant to within 610 %.
NOTE 1—The temperature range of interest depends upon the tempera-
4. Summary of Test Method
ture of the glass transition. The apparatus need only address the tempera-
ture region from 50 °C below to 50 °C above the anticipated glass
4.1 The determination of the glass transition by differential
transition temperature.
scanning calorimetry using Test Method E1356 is difficult
6.1.2 A temperature controller, capable of executing a
when kinetic events such as the cure exotherm of a thermoset
specific temperature program by (1) operating the furnace
resin occur at or near the glass transition. In MTDSC, the total
between selected temperature limits at a rate of temperature
heat flow signal is separated into reversing and nonreversing
change of 7 °C/min 6 0.1 °C/min, (2) holding at an isothermal
components. The heat capacity change that indicates the glass
temperature within the temperature range of –120 °C to +600
transition appears in the reversing heat flow signal, while
°C within 60.1 °C, and (3) for Test Method A, varying
kinetic events (for example, curing, enthalpy of recovery, etc.)
temperature sinusoidally with an amplitude of 60.9 °C to 1.1
appear in the nonreversing heat flow signal. The separation of
°C and a period of 50 s to 71 s (frequency of 14 mHz to 20
these two signals permits the determination of the enthalpy of
mHz) or applying a 60.5 °C pulse at intervals between 15 s
reaction and the assignment of the glass transition in a single
and 30 s.
experiment.
6.1.3 A calculating device, capable of transforming the
4.1.1 This MTDSC method involves the continuous moni-
experimentally determined modulated temperature and modu-
toring of the reversing and nonreversing heat flow into or out
lated specimen heat flow signals into the required continuous
ofatestspecimenasitisheatedatacontrolledratethroughthe
output forms of reversing and nonreversing heat flow and
glass transition region.
average test temperature to the required accuracy and preci-
sion.
5. Significance and Use
6.1.4 A data collection device, to provide a means of
5.1 Materials undergo an increase in molecular mobility at
acquiring, storing and displaying measured or calculated sig-
the glass transition seen as a sigmoidal step increase in the heat
nalsorboth.TheminimumoutputsignalsrequiredforMTDSC
capacity.Thismobilityincreasemayleadtokineticeventssuch
are heat flow, reversing heat flow, nonreversing heat flow,
as enthalpic recovery, chemical reaction or crystallization at
elapsed time and average specimen temperature signals.
temperatures near the glass transition.The heat flow associated
6.2 Acoolant system to provide cooling at rates of at least 2
with the kinetic events may interfere with the determination of
°C/min.
the glass transition.
6.3 Inert nitrogen or other low conductivity purge gas
5.2 The glass transition is observed in differential scanning
flowingatarateof20mL/minto60mL/minconstanttowithin
calorimetry as a sigmoidal or step change in specific heat
610 %.
capacity.
NOTE 2—Helium, a commonly used purge gas with high thermal
5.3 MTDSC provides a test method for the separation of the conductivity, may result in reduced temperature range, precision and
accuracy. Follow the manufacturers recommendation when using helium.
heat flow due to heat capacity and that associated with kinetic
events making it possible to determine the glass transition in
6.4 A balance with a range of at least 200 mg to weigh
the presence of interfering kinetic event. specimens or containers, or both to 60.01 mg.
5.4 These test methods are useful in research and
6.5 A Sapphire disk calibration material,10mgto30mg
development, quality assurance and control and specification for heat capacity calibration.
acceptance.
6.6 Indium metal of >99.99 % purity for temperature and
5.5 Other methods for assigning the glass transition tem- enthalpy calibration.
peratureincludedifferentialscanningcalorimetry(TestMethod
6.7 Containers (pans, crucibles, etc.) that are inert to the
E1356), thermomechanical analysis (Test Method E1545) and
specimen and are of suitable structural shape and integrity to
dynamic mechanical analysis (Test Method E1640).
contain the specimen in accordance with the specific require-
ments of these test methods.
6. Apparatus
6.8 Ameans, tool or device to close, encapsulate or seal the
6.1 The instrumentation required to provide the capability
container of choice.
for these test methods includes a MTDSC composed of:
6.1.1 A differential scanning calorimeter (DSC) test cham-
7. Calibration and Standardization
ber of (1)a furnace or furnaces to provide uniform controlled
7.1 Calibrate the temperature signal from the MTDSC
heating or cooling of a specimen and reference to a constan
...
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: E2602 − 09 (Reapproved 2015) E2602 − 22
Standard Test Methods for
the Assignment of the Glass Transition Temperature by
Modulated Temperature Differential Scanning Calorimetry
This standard is issued under the fixed designation E2602; 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 describe the assignment of the glass transition temperature of materials using modulated temperature
differential scanning calorimetry (MTDSC) over the temperature range from –120 °C to +600°C. +600 °C. The temperature range
may be extended depending upon the instrumentation used.
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 There are no ISO equivalents to 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 safety, health, and healthenvironmental 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
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E967 Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers
E968 Practice for Heat Flow Calibration of Differential Scanning Calorimeters
E1142 Terminology Relating to Thermophysical Properties
E1356 Test Method for Assignment of the Glass Transition Temperatures by Differential Scanning Calorimetry
E1545 Test Method for Assignment of the Glass Transition Temperature by Thermomechanical Analysis
E1640 Test Method for Assignment of the Glass Transition Temperature By Dynamic Mechanical Analysis
3. Terminology
3.1 Definitions—Specific technical terms found in these test methods are defined in Terminologies E473 and E1142 including
differential scanning calorimetry, extrapolated onset, glass transition, glass transition temperature, non-reversing, reversing,
specific heat capacity, and thermal curve.
These test methods are under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Calorimetry
and Mass Loss.
Current edition approved May 1, 2015Feb. 1, 2022. Published May 2015May 2022. Originally approved in 2009. Last previous edition approved in 20092015 as E2602
– 09. 09 (2015). DOI: 10.1520/E2602-09R15.10.1520/E2602-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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 the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2602 − 22
3.2 Definitions of Terms Specific to This Standard:
3.2.1 extrapolated end temperature (Te), n—the point of intersection of the tangent drawn at the point of greatest slope (that is,
the inflection point) in the transition region with the extrapolated baseline following the transition.
3.2.2 extrapolated onset temperature (Tf), n—the point of intersection of the tangent drawn at the point of greatest slope (that is,
the inflection point) in the transition region with the extrapolated baseline prior to the transition.
3.2.3 midpoint temperature (Tm), n—the point on the thermal curve corresponding to the average of the extrapolated onset and
extrapolated end temperatures.
3.2.4 modulated, n—a prefix indicating that a parameter changes in a periodic manner during the experiment.
3.2.5 modulated heat flow, n—the heat flow resulting from an applied modulated temperature program.
3.2.6 modulated temperature differential scanning calorimetry (MTDSC),n—a method of differential scanning calorimetry (DSC)
that varies the temperature sinusoidally or with a periodic step-and-hold or pulse program to the test specimen over a traditional
isothermal or temperature ramp program. Results from the experiment include reversing and nonreversing heat flow and specimen
temperature.
3.2.7 nonreversing heat flow, n—the kinetic component of the total heat flow. That is, the portion of the heat flow that responds
to temperature and not to the temperature rate of change.
3.2.8 reversing heat flow, n—the portion of the total heat flow that responds to the temperature rate of change.
3.2.7 total heat flow, n—the value of the modulated heat flow averaged over one modulation period or impulse.
3.2.7.1 Discussion—
The total heat flow is equivalent to the heat flow signal of conventional differential scanning calorimetry.
3.2.7.2 Discussion—
The total heat flow is equal to the sum of the reversing and nonreversing heat flows.
4. Summary of Test Method
4.1 The determination of the glass transition by differential scanning calorimetry using Test Method E1356 is difficult when kinetic
events such as the cure exotherm of a thermoset resin occur at or near the glass transition. In MTDSC, the total heat flow signal
is separated into reversing and nonreversing components. The heat capacity change that indicates the glass transition appears in
the reversing heat flow signal, while kinetic events (for example, curing, enthalpy of recovery, etc.) appear in the nonreversing heat
flow signal. The separation of these two signals permits the determination of the enthalpy of reaction and the assignment of the
glass transition in a single experiment.
4.1.1 This MTDSC method involves the continuous monitoring of the reversing and nonreversing heat flow into or out of a test
specimen as it is heated at a controlled rate through the glass transition region.
5. Significance and Use
5.1 Materials undergo an increase in molecular mobility at the glass transition seen as a sigmoidal step increase in the heat
capacity. This mobility increase may lead to kinetic events such as enthalpic recovery, chemical reaction or crystallization at
temperatures near the glass transition. The heat flow associated with the kinetic events may interfere with the determination of the
glass transition.
5.2 The glass transition is observed in differential scanning calorimetry as a sigmoidal or step change in specific heat capacity.
5.3 MTDSC provides a test method for the separation of the heat flow due to heat capacity and that associated with kinetic events
making it possible to determine the glass transition in the presence of interfering kinetic event.
E2602 − 22
5.4 These test methods are useful in research and development, quality assurance and control and specification acceptance.
5.5 Other methods for assigning the glass transition temperature include differential scanning calorimetry (Test Method E1356),
thermomechanical analysis (Test Method E1545) and dynamic mechanical analysis (Test Method E1640).
6. Apparatus
6.1 The instrumentation required to provide the capability for these test methods includes a MTDSC composed of:
6.1.1 A differential scanning calorimeter (DSC) test chamber of (1) a furnace or furnaces to provide uniform controlled heating
or cooling of a specimen and reference to a constant temperature or at a constant rate within the range from –120 °C to +600°C,
+600 °C, (2) a temperature sensor to provide an indication of the specimen temperature readable to 60.01°C, 60.02 °C, (3) a
differential sensor to detect a heat flow difference between specimen and reference equivalent to 1 μW and (4) a means of
sustaining a test chamber environment of inert nitrogen (or other low conductivity) purge gas at a rate of 20 mL/min to 60 mL/min
constant to within 610 %.
NOTE 1—The temperature range of interest depends upon the temperature of the glass transition. The apparatus need only address the temperature region
from 50°C 50 °C below to 50°C 50 °C above the anticipated glass transition temperature.
6.1.2 A temperature controller, capable of executing a specific temperature program by (1) operating the furnace between selected
temperature limits at a rate of temperature change of 7 °C/min 6 0.1°C/min, 0.1 °C/min, (2) holding at an isothermal temperature
within the temperature range of –120 °C to +600°C within 60.1°C, +600 °C within 60.1 °C, and (3) for Test Method A, varying
temperature sinusoidally with an amplitude of 60.9 °C to 1.1°C 1.1 °C and a period of 50 s to 71 s (frequency of 14 mHz to 20
mHz) or applying a 60.5°C 60.5 °C pulse at intervals between 15 s and 30 s.
6.1.3 A calculating device, capable of transforming the experimentally determined modulated temperature and modulated
specimen heat flow signals into the required continuous output forms of reversing and nonreversing heat flow and average test
temperature to the required accuracy and precision.
6.1.4 A data collection device, to provide a means of acquiring, storing and displaying measured or calculated signals or both. The
minimum output signals required for MTDSC are heat flow, reversing heat flow, nonreversing heat flow, elapsed time and average
specimen temperature signals.
6.2 A coolant system to provide cooling at rates of at least 2°C/min.2 °C/min.
6.3 Inert nitrogen or other low conductivity purge gas flowing at a rate of 20 mL/min to 60 mL/min constant to within 610 %.
NOTE 2—Helium, a commonly used purge gas with high thermal conductivity, may result in reduced temperature range, precision and accuracy. Follow
the manufacturers recommendation when using helium.
6.4 A balance with a range of at least 200 mg to weigh specimens or con
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