ASTM E2254-08
(Test Method)Standard Test Method for Storage Modulus Calibration of Dynamic Mechanical Analyzers
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 SI units are the 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:E2254–08
Standard Test Method for
Storage Modulus Calibration of Dynamic Mechanical
1
Analyzers
This standard is issued under the fixed designation E2254; 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 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 SI units are the standard. that change in temperature on the storage modulus.
1.3 This standard does not purport to address all of the 5.3 Acalibration factor may be required to obtain corrected
safety concerns, if any, associated with its use. It is the storage modulus values.
responsibility of the user of this standard to establish appro- 5.4 This method may be used in research and development,
priate safety and health practices and determine the applica- specification acceptance, and quality control or assurance.
bility of regulatory limitations prior to use.
6. Apparatus
2. Referenced Documents
6.1 The essential instrumentation required to provide the
2
2.1 ASTM Standards: minimum dynamic mechanical capability for this test method
E473 Terminology Relating to Thermal Analysis and Rhe- includes:
ology 6.1.1 Drive Motor, to apply force (or displacement) to the
E1142 Terminology Relating to Thermophysical Properties specimeninaperiodicmanner.Thismotormayalsobecapable
of providing static force or displacement on the specimen.
3. Terminology
6.1.2 Coupling Shaft, or other means to transmit the force
3.1 Definitions—Specific technical terms used in this test
from the motor to the specimen.
method are defined in Terminologies E473 and E1142. 6.1.3 Clamping System(s), to fix the specimen between the
drive shaft and the stationary clamp(s).
4. Summary of Test Method
6.1.4 Position Sensor, to measure the change in position of
4.1 The storage modulus signal measured by a dynamic
the specimen during dynamic motion, or,
mechanical analyzer for an elastic reference material is com-
6.1.5 Force Sensor, to measure the force developed by the
pared to the reported storage modulus for that reference
specimen.
material. A linear relationship is used to correlate the experi-
6.1.6 Temperature Sensor, to provide an indication of the
mental storage modulus signal with the reported value of the
specimen temperature to 6 1 °C.
reference material.
6.1.7 Furnace, to provide controlled heating or cooling of a
4.2 The mode of deformation (for example, tensile, flexure,
specimen at a constant temperature or at a constant rate within
compression, etc.) shall be reported.
the applicable temperature range of -100 to +300 °C.
6.1.8 Temperature Controller, capable of executing a spe-
1
cific temperature program by operating the furnace between
This test method is under the jurisdiction ofASTM Committee E37 onThermal
Measurements and is the direct responsibility of Subcommittee E37.10 on Funda-
-100 and +300 °C.
mental, Statistical and Mechanical Properties.
6.1.9 A Data Collection Device, to provide a means of
Current edition approved Feb. 1, 2008. Published March 2008. Original
acquiring, storing and displaying measured or calculated sig-
approved in 2003. Last previous edition approved in 2003 as E2254–03. DOI:
nals, or both.The minimum output signals required are storage
10.1520/E2254-08.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
modulus, loss modulus, tangent delta, temperature and time.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.2 Auxiliary instrumentation considered necessary in con-
Standards volume information, refer to the standard’s Document Summary page on
ducting this method near or below ambient room temperature.
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
E2254–08
6.2.1 Cooling capability to sustain a constant temperature 10.2 Ensure that the storage modulus signal is less than 1
at or below ambient room temperature or to provide controlled MPa with no test specimen loaded and at an oscillation test
cooling. frequency of 1 Hz.
6.3 M
...
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:E2254–03 Designation:E2254–08
Standard Test Method for
Storage Modulus Calibration of Dynamic Mechanical
1
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
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.
1.2Electronic instrumentation or automatic data analysis systems or treatments equivalent to this test method may be used.
1.3SI units are the standard.
1.4There is no ISO standard equivalent to this test method.
1.5
1.2 SI units are the 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
E 473 Terminology Relating to Thermal Analysis and Rheology
E 1142 Terminology Relating to Thermophysical Properties
3. Terminology
3.1 Definitions—Specific technical terms used in this test method are defined in Terminologies E 473 and E 1142.
4. Summary of Test Method
4.1 The storage modulus signal measured by a dynamic mechanical analyzer for an elastic reference material is compared to
thereportedstoragemodulusforthatreferencematerial.Alinearrelationshipisusedtocorrelatetheexperimentalstoragemodulus
signal with the reported value of the reference material.
4.2 The mode of deformation (for example, tensile, flexure, compression, etc.) shall be reported.
5. Significance and Use
5.1 This test method calibrates or demonstrates conformity of a dynamic mechanical analyzer at an isothermal temperature
within the range of -100 to 300 °C.
5.2 Dynamic mechanical analysis experiments often use temperature ramps. This method does not address the effect of that
change in temperature on the storage modulus.
5.3 A calibration factor may be required to obtain corrected storage modulus values.
5.4 This method may be used in research and development, specification acceptance, and quality control or assurance.
6. Apparatus
6.1 Theessentialinstrumentationrequiredtoprovidetheminimumdynamicmechanicalcapabilityforthistestmethodincludes:
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal
Analysis Test Methods.
Current edition approved Jan. 10, 2003. Published February 2003.
1
This test method is under the jurisdiction ofASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal Test
Methods and Practices.
Current edition approved Feb. 1, 2008. Published March 2008. Original approved in 2003. Last previous edition approved in 2003 as E 2254–03.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 14.02.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.
1
---------------------- Page: 1 ----------------------
E2254–08
6.1.1 Drive Motor, to apply force (or displacement) to the specimen in a periodic manner. This motor may also be capable of
providing static force or displacement on the specimen.
6.1.2 Coupling Shaft, or other means to transmit the force from the motor to the specimen.
6.1.3 Clamping System(s), to fix the specimen between the drive shaft and the stationary clamp(s).
6.1.4 Position Sensor, to measure the change in position of the specimen during dynamic motion, or,
6.1.5 Force Sensor, to measure the force developed by the specimen.
6.1.6 Temperature Sensor, to provide an indication of the specimen temperature to 6 1 °C.
6.1.7 Furnace, to provide controlled heating or cooling of a specimen at a constant temperature or at a constant rate within the
applicable temperature range of -100 to +300 °C.
6.1.8 Temperature Controller, capable of executing a sp
...
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