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
21、d 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 3Alternatively,
22、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 Measure and record the dimension of the test specimento a precision of 6 0.01 mm
23、. Open the apparatus, place thereference material into the specimen holder, and reassemble theapparatus. Equilibrate the reference material at the test condi-tions. Unless otherwise indicated, the test frequency shall be 1Hz and the temperature shall be isothermal between 2 and23 C. Ensure that the
24、applied strain (or stress) amplitude iswithin the linear viscoelastic regions of the sample.NOTE 4Typical specimen size is 50x9x1mm.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
25、Calculate and report the value of the slope (S) andpercent conformity (C) of the measurement using Eq 2 and 3.11. Calculation11.1 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
26、 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 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
27、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 be 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 b
28、etter 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 better 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 c
29、onformity, (C).TABLE 1 Reference Material ModulusA,B,CStorage Modulus, 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 191 179 112 71.7 . . .149 189 178 112 70.3 . . .204 186 177 110 65
30、.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-oney (eds.), 6th Edition, McGraw-Hill, New York, NY, page 6-9
31、2 (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.E225408211.5 Using the slope (S) from Eq 2, the observed storagem
32、odulus (Eo) can provide a corrected storage modulus (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
33、the test mode, strainamplitude, and applied static load.12.1.1.1 Whether or not the instrument calibration includescompliance correction.12.1.2 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 date
34、d version of this method used.13. Precision and Bias13.1 An interlaboratory study is planned for 20092010 togenerate precision and bias 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 intralaborat
35、ory repeatability standard deviationfor S for a single instrument using carbon steel and was foundto be 0.67 %.13.3 Bias:13.3.1 The measurement 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
36、 The intralaboratory conformity for C for a singleinstrument using ultra high molecular weight polyethylenefollowing calibration with carbon steel was 4.0 %.14. Keywords14.1 calibration; conformity; dynamic mechanical analysis;storage modulusASTM International takes no position respecting the validi
37、ty of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised 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 subjec
38、t to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarte
39、rs. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you 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
40、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).E2254083
