ASTM E1867-22

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Designation: E1867 − 18 E1867 − 22
Standard Test Methods for
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
2.1 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
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.
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.
*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
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 accomplished in Method A by a melting
point reference material loaded into a polymer tube, or in Method B by wrapping the calibration material with polymer tape or
in Method C by placing the calibration material between glass or ceramic plates and subjecting this test specimen 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).
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 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.
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, nor shall it be in contact with the specimen or specimen holder in a way that would impede movement. If the temperature
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
be repeated in the geometry matching that of specimen testing.
6.4 These test methods do not apply to calibration for shear or compressive geometries of deformation.
7. Apparatus
7.1 The function of the apparatus is to hold a specimen of uniform dimension so that the specimen acts as the elastic and
dissipative element in a mechanically oscillated system. Dynamic mechanic analyzers typically operate in one of several modes
as outlined in Table 1.
TABLE 1 Dynamic Mechanical Analyzer Modes of Operation
Mechanical Response
Mode
Tension Flexural Torsion Compression
A
Free/dec . . . . . . X . . .
A
Forced/res/CA . . . X X . . .
A
Forced/fix/CA X X X X
A
Forced/fix/CS X X . . . X
A
Free = free oscillation; dec = decaying amplitude; forced = forced oscillation;
CA = constant amplitude; res = resonant frequency; fix = fixed frequency;
CS = controlled stress.
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7.1.1 The apparatus shall consist of the following:
7.1.1.1 Clamps—A clamping arrangement that permits gripping of the specimen. This may be accomplished by clamping at both
ends (most systems), one end (for example, torsional pendulum) or neither end (for example, free bending between knife edges).
7.1.1.2 Device to Apply Oscillatory Stress or Strain—A device for applying an oscillatory deformation (strain) or oscillatory stress
to the specimen. The deformation may be applied and then released, as in freely vibrating devices, or continually applied, as in
forced vibration devices.
7.1.1.3 Detector—A device or devices for determining the dependent and independent experimental parameters, such as force
(stress), deformation (strain), frequency, and temperature. Temperature shall be readable to within 60.1 °C, force to within 61 %
and frequency to within 61 %.
7.1.1.4 Temperature Controller and Oven—A device for controlling the specimen temperature, either by heating, cooling (in steps
or ramps), or by maintaining a constant experimental environment. The temperature programmer shall be stable to within 60.1
°C.
7.1.1.5 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 dynamic mechanical analysis are storage modulus, loss modulus, tangent delta,
temperature, and time.
NOTE 1—Some instruments, suitable for this test, may display only linear or logarithmic storage modulus while others may display both linear or
logarithmic storage modulus. Care must be taken to use the same modulus scale when comparing unknown specimens, and in the comparison of results
from one instrument to another.
7.2 For Method A, high-temperature polymer tubing such as PTFE (Polytetrafluoroethylene) or PEEK (Polyetherether-
ketone), of 3-mm outside diameter and wall thickness of 0.5-mm (0.002 in.) (1) may be used for low temperature standards (that
is, less than 160 °C). The tubing may be sealed with suitable melting temperature wax plugs, or similar sealant. (See Appendix
X2.)
NOTE 2—PTFE tubing is selected for its flexibility and inert nature for the solvents in use at the temperatures of interest. Furthermore, its transitions should
not produce any interference in the dynamic mechanical analyzer signal within the range of the suggested calibrant materials. PEEK provides increased
stiffness for ease of loading. For other temperature ranges, a suitable replacement for the high temperature polymer tubing may be used.
7.2.1 Calibration Materials—One or more suitable materials presented in Table 2.
7.3 For Method B, PTFE tape, to be used for wrapping metal point standards.
7.3.1 Calibration Materials—One or more suitable materials presented in Table 2.
TABLE 2 Calibration Materials
A
Transition Temperature
Material Reference
°C K
n-Heptane –90.56 182.65 (2)
Cyclohexane –87.06 186.09 (3)
n-Octane –56.76 216.39 (4)
n-Decane –26.66 246.49 (4)
n-Dodecane –9.65 263.5 (4)
Water 0.01 273.16 (5)
Cyclohexane 6.54 279.69 (3)
Indium 156.5985 495.7485 (5)
Tin 231.928 505.078 (5)
A
The values in this table were determined under special, highly accurate test
conditions that are not attainable or applicable to these test methods. The actual
precision of these test methods is given in Section 14.
The boldface numbers in parentheses refer to a list of references at the end of this standard.
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7.4 For Method C, sheet stock or coupons composed of one of the materials in Table 3, approximately 0.5 mm in thickness, and
length and width similar to that of an unknown test specimen to be used.
7.4.1 Calibration Materials—One or more suitable materials presented in Table 2.
7.5 For Method D:
7.5.1 Calibration Material—A high temperature polymer sheet stock or coupons, 0.5 mm to 1.0 mm in thickness with length and
width similar to that of the unknown test specimen, with a well-defined glass transition.
NOTE 3—Polycarbonate or a fully cured thermoset composite have been found suitable.
7.5.2 Thermometer, calibrated digital or analog, capable of measuring temperature over the range of 15 °C to 30 °C readable to
within 0.1 °C.
7.6 Calipers or other length measuring device capable of measuring dimensions (or length) readable to within 610 μm.
8. Reagents and Materials
8.1 Dry nitrogen, helium, or other inert gas supplied for purging purposes and especiallyspecially to ensure that moisture
condensation and ice formation is avoided when measurements involve temperatures below the dew point.
NOTE 4—The same purge gas shall be used for calibration as for the determination of unknown specimens.
9. Calibration and Standardization
9.1 Prepare the instrument for operation as described by the manufacturer in the operations manual.
10. Precedure—MethodsProcedure—Methods A, B, or C
10.1 Two Point Calibration—For the purposes of this procedure, it is assumed that the relationship between observed extrapolated
onset temperature (T ) and actual specimen temperature (T ) is a linear one governed by the equation:
o t
T 5 ~T 3S!1I (1)
t o
where: S and I are the slope and intercept of a straight line, respectively.
10.2 Select two calibration standards near the temperature range of interest. The standards should be as close to the upper and
lower temperature limits used for the subsequent test materials as practical.
TABLE 3 Insulating Sheet Stock
Room
Thermal Temperature
Conductivity Thermal Maximum
Material Reference
at 25 °C, Diffusivity at Temperature, °C
W/(m-K) 25 °C,
mm /s
Polytetrafluorothylene 0.25 (6) 260 (6)
Polytetrafluoroethylene
0.25 (6) 260 (6)
Polyimide 0.12
(7)
C
0.35
Polyetheretherketone 0.25 (8) 200 (8)
A
Macor 0.84
1.46
0.73
Soda Lime Glass 0.94 0.51 250
B
Pyrex Glass 1.45 (9)
A
Macor is a registered trademark of Corning, Inc., Corning, NY.
B
Pyrex is a registered trademark of Corning, Inc., Corning, NY.
C
At 40 °C.
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NOTE 5—The purpose of the polymer encapsulation is to provide thermal resistance between the test specimen and the environment similar to that offered
by polymer test specimens. In some testing geometries it may be possible to perform the test directly on the metal melting point reference materials
without encapsulation. (See Appendix X1.)
10.3 Method A—Calibration Using Materials that are Liquids at Ambient Temperature and where the melting temperature does
not exceed 100 °C. (See Appendix X2.)
10.3.1 Fill the polymer tubing with the calibration material. Calibrant must extend to the ends of the clamping geometry and must
have uniform dimensions with respect to width.
10.3.2 Mount the specimen in accordance with the procedure recommended by the manufacturer.
NOTE 6—For specimen clamping arrangements where the specimen is not gripped on either end (for example, free bending between knife edges) the
specimen must be rigid enough at the test start temperature to sustain initial loading. Alternatively, the calibration specimen, without encapsulation, can
be placed between the knife edge and a substrate.
10.3.3 Maximum strain amplitude shall be within the linear viscoelastic range of the specimens to be subsequently analyzed.
Strains of less than 1 % are recommended and shall not exceed 3 %.
10.3.4 Equilibrate the test specimen for 5 min at a temperature 30 °C below the anticipated transition temperature.
10.3.5 Conduct the calibration experiments at the heating rate of interest, preferably 11 °C °C/min ⁄min but no greater than 55 °C
°C/min ⁄min and a frequency of 1 Hz from 30 °C 30 °C below to 20 °C 20 °C above the anticipated melting temperature of the
calibration material. Other heating rates and frequencies may be used but shall be reported. (See Appendix X1.)
NOTE 7—Calibration for temperature shall be performed under the conditions of heating rate and frequency at which the unknown specimens will be
tested. This test method does not address the issues of frequency affects for polymeric transitions (such as the upwards shift of glass transition temperature
with increasing frequency), and will only compensate for thermal lag within the measuring device.
10.4 Method B—Calibration Where the Material is a Solid at Ambient Temperature:
10.4.1 The calibration material must extend to the ends of the clamping geometry and must have uniform dimensions with respect
FIG. 1 Transition Temperature
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to the width and thickness. Wrap the calibration material with polytetrafluoroethylene tape to a thickness of 0.5 mm. 0.5 mm. Other
thicknesses may be used but
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