1、Designation: E2254 11Standard Test Method forStorage Modulus Calibration of Dynamic MechanicalAnalyzers1This standard is issued under the fixed designation E2254; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 cust
3、om 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 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport t
4、o 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 of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E473 Ter
5、minology Relating to Thermal Analysis and Rhe-ologyE698 Test Method for Arrhenius Kinetic Constants forThermally Unstable Materials Using Differential ScanningCalorimetry and the Flynn/Wall/Ozawa MethodE1142 Terminology Relating to Thermophysical PropertiesE2425 Test Method for Loss Modulus Conforma
6、nce ofDynamic Mechanical AnalyzersD638 Test Method for Tensile Properties of Plastics3. Terminology3.1 DefinitionsSpecific technical terms used in this testmethod are defined in Terminologies E473 and E1142 includ-ing Celsius, dynamic mechanical analysis, and storage modu-lus.4. Summary of Test Meth
7、od4.1 The storage modulus signal determined 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 with the reported value of theref
8、erence 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 range of -100 to 300 C.5.2 Dynamic
9、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 research and development,specifica
10、tion 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 manner. This motor may also be ca
11、pableof 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 Sensor, to measure the change in pos
12、ition ofthe specimen during dynamic motion, or,6.1.5 Force Sensor, to measure the force applied to thespecimen.6.1.6 Temperature Sensor, to provide an indication of thespecimen temperature to 61 C.6.1.7 Furnace, to provide controlled heating or cooling of aspecimen at a constant temperature or at a
13、constant rate withinthe applicable temperature range of 100 to +300 C.1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.10 on Funda-mental, Statistical and Mechanical Properties.Current edition approved Aug. 1
14、, 2011. Published August 2011. Originallyapproved in 2003. Last previous edition approved in 2009 as E2254 09. DOI:10.1520/E2254-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inform
15、ation, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.1.8 Temperature Controller, capable of executing a spe-cific temperature program by operating the furnace betwee
16、n100 and +300 C.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 required are storagemodulus, loss modulus, tangent delta, temperature and time.6.2 Auxiliary instrumentation considered necessar
17、y 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 controlledcooling.6.3 Micrometer, calipers or other length measuring devicecapable of measuring length of 1.0 to 100 mm wit
18、h a precisionof 60.01 mm.7. Reagents and Materials7.1 A reference material of known storage modulus, formedto the shape suitable for characterization by the particulardynamic mechanical analyzer (see Table 1).NOTE 1The storage modulus of the calibration materials used in thisstandard is often simila
19、r to that of the construction materials of the testapparatus. Thus the examination of high modulus materials may result ininstrument compliance during testing. The test apparatus calibrationprocedure (see 9.1) should include a compliance correction. The user ofthis standard shall verify whether or n
20、ot 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 is common practice to bevel or “break” edges of machinedparts. This practice shall not be followed in the preparation of test
21、specimens for this method. The measured storage modulus of such testspecimens reads low due to imperfect sample geometry.9. Calibration and Standardization9.1 Perform any storage modulus signal calibration proce-dures recommended by the manufacturer of the dynamicmechanical analyzer as described in
22、the operations manual.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 testspecimens. Unless otherwise indicated, the temperature condi-tion shall be isothermal b
23、etween 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, a thin specimen of a low modulus material (forexample, a thin piece of paper) may be used. The dimensions of the testspecimen
24、 (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 60.01 mm.10.4 Open the apparatus, place the reference material intothe specimen holder, and reassemble the apparatus. Equilibratethe r
25、eference material at the test conditions. Unless otherwiseindicated, the test frequency shall be 1 Hz and the temperatureshall be isothermal between 2 and 23 C. Ensure that theapplied strain (or stress) amplitude is within the linear vis-coelastic regions of the sample typically less than 1 % strain
26、.NOTE 4Typical specimen size is 50 3 9 3 1 mm. The specimenshould have a length-to-thickness ratio greater than 10-to-1.10.5 Record the storage modulus observed by the apparatusas Eo.10.6 Record the storage modulus of the reference materialfrom its certificate or from Table 1 as Es.10.7 Calculate an
27、d 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 bythe slope
28、 (S)ofEq1.Es 5 Eo 3 S (1)11.2 By using the storage modulus values taken from 10.5and 10.6 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 storage modu
29、lus 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 better than0.
30、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 %.TABLE 1 Reference Material ModulusA,B,CStorage Modulus,
31、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 65.5 . . .260 182 175 . . . . . . . . .316 177 170 . . . . . . . . .AAmer
32、ican Society of Mechanical Engineers, New York, NY, B31.5a, Refrigera-tion Piping, 1992, p. 45.BPerrys Chemical Engineers Handbook, R.H. Perry, D.W. Green, J.O. Malo-ney (eds.), 6th Edition, McGraw-Hill, New York, NY, page 6-92 (1984).CUltra High Molecular Weight Polyethylene Standard Reference Mate
33、rial 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.E2254 11211.4 Report the value of S and the percent conformity, (C).11.5 Using the slope (S) from Eq 2, the observed storagemodulus (Eo) ca
34、n 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 the test mode,
35、 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 dated version of t
36、his method used.13. Precision and Bias13.1 An interlaboratory study was conducted in 2010 thatincluded 15 laboratories using 7 instrument models from 4manufacturers using a single ultra-high molecular weightpolyethylene sample.313.2 Precision:13.2.1 Within laboratory variability may be described usi
37、ngthe repeatability value (r) obtained by multiplying the repeat-ability standard deviation by 2.8. The repeatability valueestimates the 95 % confidence limit. That is, two results fromthe same laboratory should be considered suspect (at the 95 %confidence level) if they differ by more than the repe
38、atabilityvalue.13.2.2 The within laboratory repeatability standard devia-tion was 0.041 GPa resulting in a repeatability relative standarddeviation of 4.8 % with 48 degrees of experimental freedom.The repeatability value r thus 0.11 GPa,13.2.3 The between laboratory variability may be describedusing
39、 the reproducibility value (R) obtained by multiplying thereproducibility standard deviation by 2.8. The reproducibilityvalue estimates the 95 % confidence limit. That is, resultsobtained from two different laboratories, operators or apparatusshould be considered suspect (at the 95 % confidence leve
40、l) ifthey differ by more than the reproducibility value.13.2.4 The between laboratory reproducibility standard de-viation was 0.16 GPa resulting in a reproducibility relativestandard deviation of 14 %. The reproducibility value R thus is0.45 GPa13.3 Bias:13.3.1 Bias is the difference between the mea
41、n value ob-tained and an acceptable reference value for the same material.13.3.2 The Youngs modulus calculated from the storagemodulus (E) value determined by this standard and the lossmodulus (E”) value determined by Test Method E2425 may becompared to the Youngs modulus (E) obtained by Test Method
42、E698 by the equation:E 5 E2 E”2#1/213.3.3 The value for Youngs modulus determined for thismaterial by Test Method D638 is 1.256 GPa.13.3.4 The mean value for storage modulus (E) determinedby this standard is 1.184 GPa.13.3.5 The mean value for loss modulus (E”) for thismaterial determined by Test Me
43、thod E2425 was 62.0 MPa.13.3.6 Based upon the Students “t” test, these values forYoungs modulus are equivalent. That is, no bias is detected.14. Keywords14.1 calibration; conformity; dynamic mechanical analysis;storage modulusASTM International takes no position respecting the validity of any patent
44、 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 subject to revision at
45、 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 Headquarters. Your comment
46、s 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 is copyrighted b
47、y 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:E37-1041.E2254 113
