1、Designation: E 2425 05Standard Test Method forLoss Modulus Conformance of Dynamic MechanicalAnalyzers1This standard is issued under the fixed designation E 2425; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revi
2、sion. 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 performance confirma-tion or measurement of conformance for the loss modulus scaleof a commerci
3、al or custom-built dynamic mechanical analyzer(DMA) at 21 C using poly(methylmethacrylate) as a referencematerial.1.2 SI units are the standard1.3 There is no ISO standard equivalent to this test method.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with
4、its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and to determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 473 Terminology Relating to Thermal AnalysisE 1142 Terminology Rel
5、ating to Thermophysical PropertiesE 1867 Test Method for Temperature Calibration of Dy-namic Mechanical Analyzers3. Terminology3.1 Definitions: Specific technical terms used in this testmethod are defined in Terminologies E 473 and E 1142.4. Summary of Test Method4.1 The loss modulus signal measured
6、 by a dynamic me-chanical analyzer for an elastic material is compared to thereported loss modulus for that reference material. A linearrelationship is used to correlate the experimental loss modulussignal with the reported value of the reference material.4.2 The mode of deformation (for example, te
7、nsile, flexure,compression, shear. etc.) shall be reported.5. Significance and Use5.1 This test method demonstrates conformity of a dynamicmechanical analyzer at an isothermal temperature of 21 C.5.2 Dynamic mechanical analysis experiments often uselinear temperature change. This method does not add
8、ress theeffect of that change in temperature on the loss modulus.5.3 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 mechanical capability for this test
9、 methodincludes:6.1.1 Drive Actuator, to apply force (or displacement) to thespecimen in a periodic manner. This actuator may also becapable of providing static force or displacement to thespecimen.6.1.2 Coupling Shaft, or other means to transmit the forcefrom the motor to the specimen.6.1.3 Clampin
10、g 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, or6.1.5 Force Sensor, to measure the force developed by thespecimen.6.1.6 Temperature Sensor, to provide an indication of
11、 thespecimen temperature to within 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 temperature program by
12、 operating the furnace between-100 and +300 C and at a constant temperature within thatrange.6.1.9 Recording Device, capable of recording and display-ing the loss modulus signal as a change in specimen stress(force) or position (displacement) on the Y-axis and tempera-ture or time on the X-axis.6.2
13、Auxiliary instrumentation considered necessary in con-ducting this method near or below ambient temperature:1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.01 Thermal andRheological Test Methods and Practice
14、s.Current edition approved Sept. 1, 2005. Published October 2005.2For 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 page onthe ASTM webs
15、ite.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2.1 Cooling capability to sustain a constant temperature ator below ambient temperature or to provide controlled cooling.6.2.2 Data Analysis capability to provide loss modulusinfo
16、rmation derived from measured signals.7. Reagents and Materials7.1 A reference material of known loss modulus, formed tothe shape suitable for characterization by the particular dy-namic mechanical analyzer (see Table 1).8. Sampling and Test Specimens8.1 Test specimens are typically prepared in the
17、form of arectangular test bars or film strips.NOTE 1It 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 loss modulus of such specimensreads low due to imperfect sample geometry.9. Cali
18、bration and Standardization9.1 Perform any loss modulus signal calibration procedurerecommended by the manufacturer of the dynamic mechanicalanalyzer as described in the operations manual.9.2 If not already done so, calibrate the temperature scale ofthe dynamic mechanical analyzer as near as is prac
19、tical to thetest temperature (see Table 1) using standard E 1867.10. Procedure10.1 Prepare the dynamic mechanical analyzer for operationunder the test conditions (for example, specimen clamps, purgegas, etc.) to be used for the characterization of the testspecimen(s). Unless otherwise indicated the
20、temperature con-dition shall be isothermal at 21 +/1C(i.e., between 20 and22 C).10.2 Ensure that the loss modulus signal is less than 1 MPawith no test specimen loaded and at an oscillation testfrequency to be used in this test (see Table 1).NOTE 2Alternatively, a thin specimen of a low modulus mate
21、rial (forexample, a thin piece of paper) may be used. The dimension of the testspecimen shall be used rather than the true dimensions of the thin, lowmodulus material.10.3 Open the apparatus, place the reference material intothe specimen holder, and reassemble the apparatus. Equilibratethe reference
22、 material at the test conditions. Unless otherwiseindicated, the test frequency shall be that indicated in table 1and the temperature shall be isothermal between 20 and 22 C.Ensure that the applied strain (or stress) amplitude is within thelinear viscoelastic region of the sample.10.4 Record the los
23、s modulus observed by the apparatus asEo.10.5 Record the loss modulus of the reference material fromits certificate or from Table 1 as Es.10.6 Calculate and report the value of the slope (S) andconformity (C) of the measurement using Eq 2 and Eq 3.11. Calculation11.1 For the purpose of this test met
24、hod, it is assumed thatthe relationship between the observed loss modulus (Eo) andthe reference loss modulus (Es) is linear and governed by theslope (S)ofEq1.Es5 Eo3 S (1)11.2 By using the loss modulus values taken from 10.4 and10.5, calculate and report S using Eq 2 to four decimal places.S 5 Es/ E
25、o(2)11.3 The conformity (C) (that is, the percent differencebetween the experimental slope and unity) of the instrumentloss modulus scale is calculated using the value of S from 11.2and Eq 3.C 5 S 2 1.0000! 3 100 % (3)11.3.1 Conformity may be estimated to one significantfigure using the following cr
26、iteria:11.3.1.1 If the value of S is between 0.990 and 0.9999 orbetween 1.0001 and 1.0010, then the conformity is better than0.1 %.11.3.1.2 If the value of S is between 0.9000 and 0.9990 orbetween 1.0010 and 1.0100, then conformity is better than 1 %.11.3.1.3 If the value of S is between 0.9000 and
27、0.9900 orbetween 1.0100 and 1.1000, then the conformity is better than10 %.11.4 Report the value of slope (S) and the conformity (C).12. Report12.1 The report shall include the following information:12.1.1 Details and description of the dynamic mechanicalanalyzer, including the manufacturer and inst
28、rument modelnumber, where applicable. Also report the test mode, strainamplitude, frequency and applied static load.12.1.1.1 Whether or not the instrument calibration includedcompliance corrections.12.1.2 The value of slope (S) determined in 11.2, reported toat least four decimal places.12.1.3 The c
29、onformity (C), as determined in 11.3.12.1.4 The specific dated version of this test method used.13. Precision and Bias13.1 An interlaboratory study is planned for 2007-2008 togenerate precision and bias information for this method.Anyone wishing to participate in this study may contact theE 37 Staff
30、 Manager at ASTM International Headquarters.13.2 Precision13.2.1 Replicate determinations on a single instrumentshows that the mean value and repeatability standard deviationTABLE 1 Reference Material Loss ModulusTemperature(C)Material FrequencyHzLoss Modulus(MPa)21 Poly(methylmethacrylate)A7 351AB.
31、E. Read and G.D. Dean, The Determination of Dynamic Properties ofPolymers and Composites, 1978, Chapter 8, pp. 180-202, Wiley and Sons, NewYorkE2425052for S using poly(methymethacrylate) to be 0.8217 6 0.033corresponding to a relative standard deviation of 6 4.1 % %.13.3 Bias13.3.1 The measurement o
32、f conformity in this test method isa comparison of the slope (S) with the theoretical value of1.0000 and provides an indication of bias.13.3.2 The intralaboratory conformity for a single instru-ment using poly(methymethacrylate) is -18 %.14. Keywords14.1 calibration; conformity; dynamic mechanical a
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36、 to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).E2425053
