ASTM E2254-2008 Standard Test Method for Storage Modulus Calibration of Dynamic Mechanical Analyzers.pdf
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1、Designation: E 2254 08Standard Test Method forStorage Modulus Calibration of Dynamic MechanicalAnalyzers1This standard is issued under the fixed designation E 2254; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r
2、evision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes the calibration or perfor-mance confirmation for the storage modulus scale of a com-mercial or c
3、ustom built dynamic mechanical analyzer (DMA)over the temperature range of -100 to 300 C using referencematerials 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 thesafety concerns, if any, associated with its use. It is theresponsibili
4、ty of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 473 Terminology Relating to Thermal Analysis and Rhe-ologyE 1142 Terminology Relating to Thermoph
5、ysical Properties3. Terminology3.1 DefinitionsSpecific technical terms used in this testmethod are defined in Terminologies E 473 and E 1142.4. Summary of Test Method4.1 The storage modulus signal measured by a dynamicmechanical analyzer for an elastic reference material is com-pared to the reported
6、 storage modulus for that referencematerial. A linear relationship is used to correlate the experi-mental storage modulus signal with the reported value of thereference material.4.2 The mode of deformation (for example, tensile, flexure,compression, etc.) shall be reported.5. Significance and Use5.1
7、 This test method calibrates or demonstrates conformityof a dynamic mechanical analyzer at an isothermal temperaturewithin the range of -100 to 300 C.5.2 Dynamic mechanical analysis experiments often usetemperature ramps. This method does not address the effect ofthat change in temperature on the st
8、orage modulus.5.3 A calibration factor may be required to obtain correctedstorage modulus values.5.4 This method may be used in research and development,specification acceptance, and quality control or assurance.6. Apparatus6.1 The essential instrumentation required to provide theminimum dynamic mec
9、hanical capability for this test methodincludes:6.1.1 Drive Motor, to apply force (or displacement) to thespecimen in a periodic manner. This motor may also be capableof providing static force or displacement on the specimen.6.1.2 Coupling Shaft, or other means to transmit the forcefrom the motor to
10、 the specimen.6.1.3 Clamping System(s), to fix the specimen between thedrive shaft and the stationary clamp(s).6.1.4 Position Sensor, to measure the change in position ofthe specimen during dynamic motion, or,6.1.5 Force Sensor, to measure the force developed by thespecimen.6.1.6 Temperature Sensor,
11、 to provide an indication of thespecimen temperature to 6 1 C.6.1.7 Furnace, to provide controlled heating or cooling of aspecimen at a constant temperature or at a constant rate withinthe applicable temperature range of -100 to +300 C.6.1.8 Temperature Controller, capable of executing a spe-cific t
12、emperature program by operating the furnace between-100 and +300 C.1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.01 on ThermalTest Methods and Practices.Current edition approved Feb. 1, 2008. Published Mar
13、ch 2008. Originalapproved in 2003. Last previous edition approved in 2003 as E 225403.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary
14、 page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.1.9 A Data Collection Device, to provide a means ofacquiring, storing and displaying measured or calculated sig-nals, or both. The minimum output signals requ
15、ired are storagemodulus, loss modulus, tangent delta, temperature and time.6.2 Auxiliary instrumentation considered necessary in con-ducting this method near or below ambient room temperature.6.2.1 Cooling capability to sustain a constant temperatureat or below ambient room temperature or to provide
16、 controlledcooling.6.3 Micrometer, calipers or other length measuring devicecapable of measuring length of 1.0 to 100 mm with a precisionof 6 0.01 mm.7. Reagents and Materials7.1 A reference material of known storage modulus, formedto the shape suitable for characterization by the particulardynamic
17、mechanical analyzer (see Table 1).NOTE 1The storage modulus of the calibration materials used in thisstandard is often similar to that of the construction materials of the testapparatus. Thus the examination of high modulus materials may result ininstrument compliance during testing. The test appara
18、tus calibrationprocedure (see 9.1) should include a compliance correction. The user ofthis standard shall verify whether or not such compliance corrections areincluded prior to its use.8. Sampling8.1 Test specimens are typically prepared in the form of arectangular test bars or film strips.NOTE 2It
19、is common practice to bevel or “break” edges of machinedparts. This practice shall not be followed in the preparation of testspecimens for this method. The measured storage modulus of such testspecimens reads low due to imperfect sample geometry.9. Calibration and Standardization9.1 Perform any stor
20、age modulus signal calibration proce-dures recommended by the manufacturer of the dynamicmechanical analyzer as described in the operations manual.10. Procedure10.1 Prepare the dynamic mechanical analyzer for operationunder the test conditions (for example, specimen clamps, purgegas, etc.) to be use
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