ASTM E2254-03

Standard Test Method for Storage Modulus Calibration of Dynamic Mechanical Analyzers

SIGNIFICANCE AND USE
This test method calibrates or demonstrates conformity of a dynamic mechanical analyzer at an isothermal temperature within the range of -100 to 300 °C.
Dynamic mechanical analysis experiments often use temperature ramps. This method does not address the effect of that change in temperature on the storage modulus.
A calibration factor may be required to obtain corrected storage modulus values.
This method may be used in research and development, specification acceptance, and quality control or assurance.
SCOPE
1.1 This test method describes the calibration or performance confirmation for the storage modulus scale of a commercial or custom built dynamic mechanical analyzer (DMA) over the temperature range of -100 to 300—C using reference materials in the range of 1 to 200 GPa.
1.2 Electronic instrumentation or automatic data analysis systems or treatments equivalent to this test method may be used.
1.3 SI units are the standard.
1.4 There is no ISO standard equivalent to this test method.
1.5 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Jan-2003
• ICS: 17.020 - Metrology and measurement in general
• Technical Committee: E37 - Thermal Measurements
• Drafting Committee: E37.10 - Fundamental, Statistical and Mechanical Properties

Relations

• Replaced By: ASTM E2254-08 - Standard Test Method for Storage Modulus Calibration of Dynamic Mechanical Analyzers
• Effective Date: 01-Feb-2008
• Referred By: ASTM D4065-20 - Standard Practice for Plastics: Dynamic Mechanical Properties: Determination and Report of Procedures
• Effective Date: 10-Jan-2003
• Referred By: ASTM D8269-21 - Standard Guide for the Use of Geocells in Geotechnical and Roadway Projects
• Effective Date: 10-Jan-2003
• Referred By: ASTM E1640-23 - Standard Test Method for Assignment of the Glass Transition Temperature By Dynamic Mechanical Analysis
• Effective Date: 10-Jan-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:E2254–03
Standard Test Method for
Storage Modulus Calibration of Dynamic Mechanical
Analyzers
This standard is issued under the fixed designation E 2254; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Significance and Use
1.1 This test method describes the calibration or perfor- 5.1 This test method calibrates or demonstrates conformity
mance confirmation for the storage modulus scale of a com- ofadynamicmechanicalanalyzeratanisothermaltemperature
mercial or custom built dynamic mechanical analyzer (DMA) within the range of -100 to 300 °C.
over the temperature range of -100 to 300 °C using reference 5.2 Dynamic mechanical analysis experiments often use
materials in the range of 1 to 200 GPa. temperature ramps. This method does not address the effect of
1.2 Electronic instrumentation or automatic data analysis that change in temperature on the storage modulus.
systems or treatments equivalent to this test method may be 5.3 Acalibration factor may be required to obtain corrected
used. storage modulus values.
1.3 SI units are the standard. 5.4 This method may be used in research and development,
1.4 There is no ISO standard equivalent to this test method. specification acceptance, and quality control or assurance.
1.5 This standard does not purport to address all of the
6. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 6.1 The essential instrumentation required to provide the
minimum dynamic mechanical capability for this test method
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. includes:
6.1.1 Drive Motor, to apply force (or displacement) to the
2. Referenced Documents
specimeninaperiodicmanner.Thismotormayalsobecapable
2.1 ASTM Standards: of providing static force or displacement on the specimen.
E 473 Terminology Relating to Thermal Analysis 6.1.2 Coupling Shaft, or other means to transmit the force
E 1142 Terminology Relating to Thermophysical Proper- from the motor to the specimen.
ties 6.1.3 Clamping System(s), to fix the specimen between the
drive shaft and the stationary clamp(s).
3. Terminology
6.1.4 Position Sensor, to measure the change in position of
3.1 Definitions—Specific technical terms used in this test
the specimen during dynamic motion, or,
method are defined in Terminologies E 473 and E 1142. 6.1.5 Force Sensor, to measure the force developed by the
specimen.
4. Summary of Test Method
6.1.6 Temperature Sensor, to provide an indication of the
4.1 The storage modulus signal measured by a dynamic
specimen temperature to 6 1 °C.
mechanical analyzer for an elastic reference material is com-
6.1.7 Furnace, to provide controlled heating or cooling of a
pared to the reported storage modulus for that reference
specimen at a constant temperature or at a constant rate within
material. A linear relationship is used to correlate the experi-
the applicable temperature range of -100 to +300 °C.
mental storage modulus signal with the reported value of the
6.1.8 Temperature Controller, capable of executing a spe-
reference material.
cific temperature program by operating the furnace between
4.2 The mode of deformation (for example, tensile, flexure,
-100 and +300 °C.
compression, etc.) shall be reported.
6.1.9 Recording Device, capable of recording and display-
ing the measured signal as a change in specimen stress (force)
or position on the y-axis and temperature or time on the x-axis.
This test method is under the jurisdiction ofASTM Committee E37 onThermal
6.2 Auxiliary instrumentation considered necessary in con-
Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal
ducting this method near or below ambient room temperature.
Analysis Test Methods.
Current edition approved Jan. 10, 2003. Published February 2003.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E2254–03
NOTE 3—Alternatively, a thin specimen of a low modulus material (for
6.2.1 Cooling capability to sustain a constant temperature
example, a thin piece of paper) may be used. The dimensions of the test
at or below ambient room temperature or to provide controlled
specimen (see 10.3) shall be used rather than the true dimensions of the
cooling.
thin low modulus material.
10.3 Open the apparatus, place the reference material into
7. Reagents and Materials
the specimen holder, and reassemble the apparatus. Equilibrate
7.1 Areference material of known storage modulus, formed
the reference material at the test conditions. Unless otherwise
to the shape suitable for characterization by the particular
indicated, the test frequency shall be 1 Hz and the temperature
dynamic mechanical analyzer (see Table 1).
shall be isothermal between 20 and 22 °C. Ensure that the
NOTE 1—The storage modulus of the calibration materials used in this
applied strain (or stress) amplitude is within the linear regions
standard is often similar to that of the construction materials of the test
of the sample.
apparatus. Thus the examination of high modulus materials may result in
10.4 Record the storage modulus observed by the apparatus
instrument compliance during testing. The test apparatus calibration
as Eo.
procedure (see 9.1) should include a compliance correction. The user of
10.5 Record the storage modulus of the reference material
this standard shall verify whether or not such compliance corrections are
from its certificate or from Table 1 as Es.
included p
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