1、Designation: E 2254 03Standard 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 Electronic instrumentation or automatic data analysissystems or treatments equivalent to this test method may beused.1.3 SI units are the standard.1.4 Th
4、ere is no ISO standard equivalent to this test method.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility
5、of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:E 473 Terminology Relating to Thermal Analysis2E 1142 Terminology Relating to Thermophysical Proper-ties23. Terminology3.1 DefinitionsSpecific technical terms used in this testmethod are defined in Terminologies E 473 a
6、nd 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 storage modulus for that referencematerial. A linear relationship is used to correlate the experi-mental storage modulus signal wi
7、th 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 This test method calibrates or demonstrates conformityof a dynamic mechanical analyzer at an isothermal temperaturewithin the rang
8、e 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 storage modulus.5.3 A calibration factor may be required to obtain correctedstorage modulus values.5.4 This method may be used in res
9、earch 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 methodincludes:6.1.1 Drive Motor, to apply force (or displacement) to thespecimen in a periodic ma
10、nner. 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 the specimen.6.1.3 Clamping System(s), to fix the specimen between thedrive shaft and the stationary clamp(s).6.1.4 Position Senso
11、r, 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, to provide an indication of thespecimen temperature to 6 1 C.6.1.7 Furnace, to provide controlled heating or cooling of aspecimen
12、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 operating the furnace between-100 and +300 C.6.1.9 Recording Device, capable of recording and display-ing the
13、 measured signal as a change in specimen stress (force)or position on the y-axis and temperature or time on the x-axis.6.2 Auxiliary instrumentation considered necessary in con-ducting this method near or below ambient room temperature.1This test method is under the jurisdiction of ASTM Committee E3
14、7 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.01 on ThermalAnalysis Test Methods.Current edition approved Jan. 10, 2003. Published February 2003.2Annual Book of ASTM Standards, Vol 14.02.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohoc
15、ken, PA 19428-2959, United States.6.2.1 Cooling capability to sustain a constant temperatureat or below ambient room temperature or to provide controlledcooling.7. Reagents and Materials7.1 A reference material of known storage modulus, formedto the shape suitable for characterization by the particu
16、lardynamic 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
17、test apparatus 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 strip
18、s.NOTE 2It 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 Perfo
19、rm any storage 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.
20、) to be used for the characterization of the testspecimens. Unless otherwise indicated, the temperature condi-tion shall be isothermal between 20 and 22 C.10.2 Ensure that the storage modulus signal is less than 1MPa with no test specimen loaded and at an oscillation testfrequency of 1 Hz.NOTE 3Alte
21、rnatively, a thin specimen of a low modulus material (forexample, a thin piece of paper) may be used. The dimensions of the testspecimen (see 10.3) shall be used rather than the true dimensions of thethin low modulus material.10.3 Open the apparatus, place the reference material intothe specimen hol
22、der, and reassemble the apparatus. Equilibratethe reference material at the test conditions. Unless otherwiseindicated, the test frequency shall be 1 Hz and the temperatureshall be isothermal between 20 and 22 C. Ensure that theapplied strain (or stress) amplitude is within the linear regionsof the
23、sample.10.4 Record the storage modulus observed by the apparatusas Eo.10.5 Record the storage modulus of the reference materialfrom its certificate or from Table 1 as Es.10.6 Calculate and report the value of the slope (S) andpercent conformity (C) of the measurement using Eq 2 and 3.11. Calculation
24、11.1 For the purpose of this test method, it is assumed thatthe relationship between observed storage modulus (Eo) andthe reference storage modulus (Es) is linear and governed bythe slope (S)ofEq1.Es 5 Eo 3 S (1)11.2 By using the storage modulus values taken from 10.4and 10.5 calculate and report S
25、using Eq 2 to four decimalplaces.S 5 Es / Eo (2)11.3 The percent conformity (C) (that is, the percent differ-ence between the experimental slope and unity) of the instru-ment storage modulus scale is calculated using the value of Sfrom 11.2 and Eq 3.C 5 S 2 1.0000! 3 100 % (3)11.3.1 Conformity may b
26、e estimated to one significantfigure using the following criteria:11.3.1.1 If the value of S is between 0.9990 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 0.9900 and 0.9990 orbetween 1.0010 and 1.0100, then conformity is bette
27、r than 1 %.11.3.1.3 If the value of S is between 0.9000 and 0.9900 orbetween 1.0100 and 1.1000, then conformity is better than10 %.11.4 Report the value of S and the percent conformity, (C).11.5 Using the slope (S) from Eq 2, the observed storagemodulus (Eo) can provide a corrected storage modulus (
28、E)using Eq 4.E 5 Eo 3 S (4)12. Report12.1 The report shall include the following information:12.1.1 Details and description, including the manufacturerand instrument model number, where applicable, of the dy-namic mechanical analyzer. Also report the test mode, strainamplitude, and applied static lo
29、ad.12.1.1.1 Whether or not the instrument calibration includescompliance correction.TABLE 1 Reference Material ModulusA,B,CModulus, GPaTemperature,CCarbonSteelDMonelECopperFAluminum UHMWPE-198 207 185 121 77.9 . . .-101 201 182 116 75.8 . . .-46 198 180 114 74.5 . . .21 192 179 114 73.1 1.2693 191 1
30、79 112 71.7 . . .149 189 178 112 70.3 . . .204 186 177 110 65.5 . . .260 182 175 . . . . . . . . .316 177 170 . . . . . . . . .AAmerican Society of Mechanical Engineers, New York, NY, B31.5a, Refrigera-tion Piping, page 45 (1992).BPerrys Chemical Engineers Handbook, R.H. Perry, D.W. Green, J.O. Mal-
31、oney (eds.), 6th Edition, McGraw-Hill, New York, NY, page 6-92 (1984).CUltra High Molecular Weight Polyethylene Standard Reference Material SRM8456, National Institute of Standards and Technology, Gaithersburg, MD 20899(2000).D3.5 % Ni, 0.30 C.E67 % Ni, 30 % Cu.F99.90 % Cu, Alloy C12000, C12200.E225
32、403212.1.2 The value of S determined in 11.2, reported to at leastfour decimal places.12.1.3 The percent conformity (C), as determined in 11.3.12.1.4 The specific dated version of this method used.13. Precision and Bias13.1 An interlaboratory study is planned for 20032004 togenerate precision and bi
33、as information for this method.Anyone wishing to participate in this study may contact theE37 Staff Manager at ASTM Headquarters.13.2 Precision:13.2.1 The intralaboratory repeatability standard deviationfor S for a single instrument using carbon steel and was foundto be 0.67 %.13.3 Bias:13.3.1 The m
34、easurement of conformity in this test method isa comparison of the calibration constant S with the theoreticalvalue of 1.0000 and provides an indication of bias.13.3.2 The intralaboratory conformity for C for a singleinstrument using ultra high molecular weight polyethylenefollowing calibration with
35、 carbon steel was 4.0 %.14. Keywords14.1 calibration; conformity; dynamic mechanical analysis;storage modulusASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised
36、that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reap
37、proved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you
38、 feel that your comments have not received a fair hearing you shouldmake your views known 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).E2254033
