ASTM E3433-24 Standard Practice for Glass Transition Temperature Reference Values

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Designation: E3433 24
Standard Practice for
Glass Transition Temperature Reference Values
1
This standard is issued under the fixed designation E3433; 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 It is the purpose of this practice to provide accepted
reference values for the glass transition temperature that may
be used for evaluation of dynamic mechanical analysis
methods, apparatus, and software.
NOTE 1—Suggested additional or alternative reference materials or
values are requested and may be submitted to the E37 Staff Manager at
ASTM International, West Conshohocken PA for consideration.
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 appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
D4092 Terminology for Plastics: Dynamic Mechanical
Properties
E473 Terminology Relating to Thermal Analysis and Rhe-
ology
E1142 Terminology Relating to Thermophysical Properties
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
3. Terminology
3.1 Definitions:
3.1.1 Specific technical terms used in this practice are
defined in Terminologies D4092,E473,E1142, and E2161
including: bias,calibration,Celsius,certified reference
material,differential scanning calorimetry,dynamic mechani-
cal analysis,dynamic mechanical measurement,extrapolated
onset value,frequency,glass transition,glass transition
temperature,loss modulus,peak,storage modulus,reference
material,standard reference material,tan delta,tangent delta,
and temperature.
3.1.2 accepted reference value, n—a value that serves as an
agreed upon reference for comparison and which is derived as
either a theoretical or established value, based on scientific
principles or an assigned value based on experimental work.
4. Summary of Practice
4.1 The glass transition, where an amorphous material
changes from an amorphous solid state into a liquidy or
rubbery one, takes place over a temperature range. The glass
transition temperature is a temperature taken to represent that
temperature range. The glass transition temperature is a func-
tion of the thermal history, test frequency, the heating rate, and
position on thermal curve assigned (see Test Method E3142
and Appendix X1).
4.2 In dynamic mechanical analysis, the glass transition
temperature may be assigned in at least three ways—as the
extrapolated onset in the sigmoidal change in storage modulus,
as the peak of the loss modulus signal, or as the peak of the
tangent delta signal (see Test Method E1640). Each of these
temperatures are offset from each other.
4.3 Temperature calibration of dynamic mechanical analyz-
ers may be performed using known glass transition values.
1
This practice is under the jurisdiction of ASTM Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.02 on Refer-
ence Materials.
Current edition approved Aug. 1, 2024. Published August 2024. DOI: 10.1520/
E3433-24.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at www.astm.org/contact. 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
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.
1
4.4 There are no known certified reference materials for
glass transition temperature.
4.5 It is the purpose of this practice to provide best estimate
(accepted reference value(s)) for the storage modulus onset, the
loss modulus peak, and tangent δfor the glass transition of a
commonly available material(s) such as polycarbonate.
5. Significance and Use
5.1 The bias or offset temperature value provided by this
practice may be used to calibrate or to evaluation the perfor-
mance of standard, apparatus, technique, or software.
NOTE 2—Calibration or calibration verification is recommended for all
signals at least annually.
5.2 The glass transition temperature is a function of heating
rate. The observed values at a heating rate different from that
of the calibration need to be assessed using thermal lag (see
Test Method E3142).
6. Procedure
6.1 Using a standard, apparatus, technique, or software to be
evaluated, obtain an experimentally observed glass transition
temperature (T
o
) for a material listed in Table 1. Report this
value.
6.2 Obtain a corresponding reference glass transition refer-
ence temperature (T
t
) from Table 1.
6.3 Determine the bias or offset temperature (T
b
) using Eq 1.
NOTE 3—For measurements other than dynamic mechanical analysis,
use the value for storage modulus extrapolated onset temperature from
Table 1.
7. Calculation
7.1
T
b
5T
r
2T
o
(1)
where:
T
b
= temperature bias, °C,
T
r
= reference temperature, °C, and
T
o
= observed temperature, °C.
8. Report
8.1 Identification of the glass transition method being ex-
amined.
8.2 A complete description of the reference material being
used for the comparison, including its source and physical
dimensions.
8.3 The bias (difference) between the measured and refer-
ence value.
9. Precision and Bias
9.1 This practice does not determine within or between
laboratory repeatability or reproducibility precision.
9.2 Bias is the difference between an observe value and that
of an accepted reference value. This standard determines that
bias for the applicable standard, apparatus, technique or
software. No additional bias is applicable.
10. Keywords
10.1 calibration; dynamic mechanical analysis; glass transi-
tion
TABLE 1 Meta-Analysis of the Glass Transition Temperature Determined by Dynamic Mechanical Analysis, Obtained at 1 Hz and
Extrapolated to 0 K/min Heating Rate
Material Heating Rate, °C/min Freq. Hz Storage Modulus
Onset Temperature,
°C
Loss Modulus Peak
Temperature, °C
Tangent δPeak
Temperature, °C
Ref.
Polycarbonate
A
0.0 1.0 146.7 ± 4.1 150.5 ± 3.2 154.8 ± 3.6
B
A
99+% purity with molecular weight greater than 50 000 g/mol (50 kDa).
B
A research report is pending at ASTM International.
E3433 − 24
2
ANNEX
(Mandatory Information)
A1. META-ANALYSIS OF THE POLYCARBONATE GLASS TRANSITION TEMPERATURE DETERMINED BY DYNAMIC
MECHANICAL ANALYSIS
APPENDIX
(Nonmandatory Information)
X1. THERMAL LAG
X1.1 In dynamic mechanical analysis, the temperature sen-
sor is not in direct contact with the test specimen leading to a
difference in temperature between the sensor and the specimen
that varies with heating/cooling rate. This effect requires that
temperature calibration be performed at the same heating/
cooling rate as that used for the test specimen.
X1.2 The temperature measurement performed at a heating/
cooling rate different from that of the calibration may not be
accurate.
X1.3 The effect of heating/cooling rate on the temperature
difference is known as thermal lag and is a characteristic of the
individual apparatus. Thermal lag can be assessed using Test
Method E3142.
X1.4 The known thermal lag of an apparatus and Test
Method E3142 can then be used to adjust the temperature
calibration obtained at one heating/cooling rate to that at
another.
REFERENCES
(1) Dunson, D., Characterization of Polymers using Dynamic Mechanical
Analysis (DMA), EAS Laboratories, San Luis Obespo CA [Accessed
2023].
(2) Chartoff, R.P., Thermoplasic Polymers, in Thermal Characterization
of Polymeric Materials, Turi, E.A., Editor, 1981, Academic Press,
New York, p. 483-744.
(3) Foreman, J.A., Sauerbrunn, S.R., and Marcozzi, C.L., Exploring the
Sensitivity of Thermal Analysis Techniques to the Glass Transition,
1997, TA Instruments, New Castle DE, TA082.
(4) Sehrawat, M., et al., Glass Transition Temperature Measurement of
Polycarbonate Specimen by Dynamic Mechanical Analyzer Towards
the Development of Reference Material, MAPAN—Journal of Me-
trology Society of India, 2022, 37 (2), p. 1-11.
(5) Anonymous, Polycarbonate, in Wikipedia, 2023.
(6) Dexit, M., et.al., Morphology, Miscibility and Mechanical Properties
of PMMA/PC Blends, Phase Transitions, 2009, 82 (12), p. 866-878.
(7) Kamykowski, G., Personal Communications, 2023, TA Instruments,
New Castle DE.
(8) Anonymous, LaCompte Francais d’Accrediutation (French Commit-
tee for Accreditation), AirBus DMA Calibration,Technical Definition,
2023, Blagnac, France [Accessed 2023].
(9) PTP, Technical Definition—PC and PES Calibrant specimens for
DMA, in Airbus DMA Calibration Kit 2018. 2023, Blagnac, France.
(10) Opliger, M.S., The Development of the Dynamic Mechanical Analy-
sis (DMA) Calibration and Testing Procedures in Aerospace
Engineering,2013, Wichita State University, p. 81.
TABLE A1.1 Meta-Analysis of the Polycarbonate Glass Transition Temperature Determined by Dynamic Mechanical Analysis
Heating Rate, °C/min Freq. Hz Storage Modulus
Onset Temperature, °C
Loss Modulus Peak
Temperature, °C
Tangent δPeak
Temperature, °C
Year Ref.
--- --- 149.5 154.3 158.7 --- 1
--- 1.0 148.0 150.6 151.4 1981 2
3.0 --- 152.2 153.4 157.9 ---
A
3.0 1.0 141.8 147.1 151.5 1997 3
2.0 1.0 142.13 ± 0.52 146.90 ± 0.68 156.15 ± 0.41 2022 4
--- --- '147 --- --- --- 5
--- --- --- --- 150.4 2009 6
3.0 1.0 157.5 ± 2.5 2023 7
148 ± 1 8
153 ± 1 2023 9
146.7 ± 0.32 10
0.0 1.0 148.4 ± 5.7 153.1 ± 7.9 159.6 ± 8.3 2023
A
mean 146.7 ± 4.1 150.5 ± 3.2 154.8 ± 3.6
A
A research report is pending at ASTM International.
E3433 − 24
3
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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
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http://www.copyright.com/
E3433 − 24
4
摘要:

ASTM E3433-2024 Standard Practice for Glass Transition Temperature Reference Values 玻璃化转变温度参考值的标准实施规程

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