1、Designation: E2254 11E2254 13Standard 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
2、last revision. 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 performance confirmation for the storage modulus scale of a commercial o
3、rcustom built dynamic mechanical analyzer (DMA) over the temperature range of -100100 to 300 C300C using referencematerials in the range of 1 to 200 GPa.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard doe
4、s not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standa
5、rds:2E473 Terminology Relating to Thermal Analysis and RheologyE698 Test Method for Arrhenius Kinetic Constants for Thermally Unstable Materials Using Differential Scanning Calorimetryand the Flynn/Wall/Ozawa MethodE1142 Terminology Relating to Thermophysical PropertiesE2425 Test Method for Loss Mod
6、ulus Conformance of Dynamic Mechanical AnalyzersD638 Test Method for Tensile Properties of Plastics3. Terminology3.1 DefinitionsSpecific technical terms used in this test method are defined in Terminologies E473 and E1142 includingCelsius, dynamic mechanical analysis, and storage modulus.4. Summary
7、of Test Method4.1 The storage modulus signal determined by a dynamic mechanical analyzer for an elastic reference material is compared tothe reported storage modulus for that reference material.Alinear relationship is used to correlate the experimental storage modulussignal with the reported value o
8、f the reference 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 conformity of a dynamic mechanical analyzer at an isothermal temperaturewithin the range of -100100 to 300
9、C.300C.5.2 Dynamic mechanical analysis experiments often use temperature ramps. This method does not address the effect of thatchange in temperature on the storage modulus.5.3 A calibration factor may be required to obtain corrected storage modulus values.5.4 This method may be used in research and
10、development, specification acceptance, and quality control or assurance.1 This test method is under the jurisdiction ofASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,Statistical and Mechanical Properties.Current edition approved Aug.
11、 1, 2011Aug. 1, 2013. Published August 2011August 2013. Originally approved in 2003. Last previous edition approved in 20092011 asE2254 09.E2254 11. DOI: 10.1520/E2254-11.10.1520/E2254-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at servicea
12、stm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Beca
13、useit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 B
14、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Apparatus6.1 The essential instrumentation required to provide the minimum dynamic mechanical capability for this test method includes:6.1.1 Drive Motor, to apply force (or displacement) to the specimen in a periodic m
15、anner. This motor may also be capable ofproviding static force or displacement on the specimen.6.1.2 Coupling Shaft, or other means to transmit the force from the motor to the specimen.6.1.3 Clamping System(s), to fix the specimen between the drive shaft and the stationary clamp(s).6.1.4 Position Se
16、nsor, to measure the change in position of the specimen during dynamic motion, or,6.1.5 Force Sensor, to measure the force applied to the specimen.6.1.6 Temperature Sensor, to provide an indication of the specimen temperature to 61 C.61C.6.1.7 Furnace, to provide controlled heating or cooling of a s
17、pecimen at a constant temperature or at a constant rate within theapplicable temperature range of 100 to +300 C.+300C.6.1.8 Temperature Controller, capable of executing a specific temperature program by operating the furnace between 100 and+300 C.6.1.9 A Data Collection Device, to provide a means of
18、 acquiring, storing and displaying measured or calculated signals, or both.The minimum output signals required are storage modulus, loss modulus, tangent delta, temperature and time.6.2 Auxiliary instrumentation considered necessary in conducting this method near or below ambient room temperature.6.
19、2.1 Cooling capability to sustain a constant temperature at or below ambient room temperature or to provide controlledcooling.6.3 Micrometer, calipers or other length measuring device capable of measuring length of 1.0 to 100 mm with a precision of60.01 mm.7. Reagents and Materials7.1 Areference mat
20、erial of known storage modulus, formed to the shape suitable for characterization by the particular dynamicmechanical analyzer (see Table 1).NOTE 1The storage modulus of the calibration materials used in this standard is often similar to that of the construction materials of the test apparatus.Thus
21、the examination of high modulus materials may result in instrument compliance during testing. The test apparatus calibration procedure (see 9.1)should include a compliance correction. The user of this standard shall verify whether or not such compliance corrections are included prior to its use.TABL
22、E 1 Reference Material ModulusA,B,Ccolwidth=“0.46in“ colwidth=“0.46in“ colwidth=“0.46in“ colwidth=“0.46in“ colwidth=“0.46in“Storage Modulus, GPaTemperature,CCarbonSteelD MonelE CopperF Aluminum 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
23、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 . . . . . . . . .TABLE 1 Reference Material ModulusA,B,CStorage Modulus, GPaTemperature,CCarbonSteelD MonelE CopperF Aluminum UHMWPE Nimonic 75(BCR-661)G,H198 207 185 121 77.9 .
24、. . . . .101 201 182 116 75.8 . . . . . .46 198 180 114 74.5 . . . . . .21 192 179 114 73.1 1.26 210.0 1.593 191 179 112 71.7 . . . . . .149 189 178 112 70.3 . . . . . .204 186 177 110 65.5 . . . . . .260 182 175 . . . . . . . . . . . .316 177 170 . . . . . . . . . . . .A American Society of Mechani
25、cal Engineers, New York, NY, B31.5a, Refrigeration Piping, B31.5a, New York, NY, 1992, p. 45.B Perrys Chemical Engineers Handbook, R.H. Perry, D.W. Green, J.O. Maloney (eds.), 6th Edition, McGraw-Hill, New York, NY, page 6-92 (1984).1984, pp. 692.C Ultra High Molecular Weight Polyethylene Standard R
26、eference Material SRM 8456, National Institute of Standards and Technology, Gaithersburg, MD 20899(2000).20899, 2000.D 3.5 % Ni, 0.30 C.E 67 % Ni, 30 % Cu.F 99.90 % Cu, Alloy C12000, C12200.G Available from Institute of Reference Materials and Measurements, Retieseweg 111, B-2440 Geel, Belgium.H Lor
27、d, J. D., and Morrell, R., “Elastic Modulus Measurement,” Measurement Good Practice Guide No. 98, National Physical Laboratory, Teddington, Middlesex, UK, 2006.E2254 1328. Sampling8.1 Test specimens are typically prepared in the form of a rectangular test bars or film strips.NOTE 2It is common pract
28、ice to bevel or “break” edges of machined parts. This practice shall not be followed in the preparation of test specimensfor this method. The measured storage modulus of such test specimens reads low due to imperfect sample geometry.9. Calibration and Standardization9.1 Perform any storage modulus s
29、ignal calibration procedures recommended by the manufacturer of the dynamic mechanicalanalyzer as described in the operations manual.10. Procedure10.1 Prepare the dynamic mechanical analyzer for operation under the test conditions (for example, specimen clamps, purgegas, etc.) to be used for the cha
30、racterization of the test specimens. Unless otherwise indicated, the temperature condition shall beisothermal between 20 and 22 C.22C.10.2 Ensure that the storage modulus signal is less than 1 MPa with no test specimen loaded and at an oscillation test frequencyof 1 Hz.NOTE 3Alternatively, a thin sp
31、ecimen of a low modulus material (for example, 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 the thin low modulus material.10.3 Measure and record the dimension of the test specimen to a precision of 60.01 mm.10.4 O
32、pen the apparatus, place the reference material into the specimen holder, and reassemble the apparatus. Equilibrate thereference material at the test conditions. Unless otherwise indicated, the test frequency shall be 1 Hz and the temperature shall beisothermal between 2 and 23 C.23C. Ensure that th
33、e applied strain (or stress) amplitude is within the linear viscoelastic regionsof the sample typically less than 1 % strain.NOTE 4Typical specimen size is 50 9 1 mm. The specimen should have a length-to-thickness ratio greater than 10-to-1.10.5 Record the storage modulus observed by the apparatus a
34、s Eo.10.6 Record the storage modulus of the reference material from its certificate or from Table 1 as Es.10.7 Calculate and report the value of the slope (S) and percent conformity (C) of the measurement using Eq 2 and 3.11. Calculation11.1 For the purpose of this test method, it is assumed that th
35、e relationship between observed storage modulus (Eo) and thereference storage modulus (Es) is linear and governed by the slope (S) of Eq 1.Es5Eo3S (1)11.2 By using the storage modulus values taken from 10.5 and 10.6 calculate and report S using Eq 2 to four decimal places.S 5Es/Eo (2)11.3 The percen
36、t conformity (C) (that is, the percent difference between the experimental slope and unity) of the instrumentstorage modulus scale is calculated using the value of S from 11.2 and Eq 3.C 5S 21.0000!3100% (3)11.3.1 Conformity may be estimated to one significant figure using the following criteria:11.
37、3.1.1 If the value of S is between 0.9990 and 0.9999 or between 1.0001 and 1.0010, then the conformity is better than 0.1 %.11.3.1.2 If the value of S is between 0.9900 and 0.9990 or between 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
38、 or between 1.0100 and 1.1000, then conformity is better than 10 %.11.4 Report the value of S and the percent conformity, (C).11.5 Using the slope (S) from Eq 2, the observed storage modulus (Eo) can provide a corrected storage modulus (E) using Eq4.E 5Eo3S (4)12. Report12.1 The report shall include
39、 the following information:12.1.1 Details and description, including the manufacturer and instrument model number, where applicable, of the dynamicmechanical analyzer. Also report the test mode, strain amplitude, and applied static load.12.1.1.1 Whether or not the instrument calibration includes com
40、pliance correction.12.1.2 The value of S determined in 11.2, reported to at least four 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.E2254 13313. Precision and Bias13.1 An interlaboratory study was conducted in 2010 that
41、 included 15 laboratories using 7 instrument models from 4manufacturers using a single ultra-high molecular weight polyethylene sample.313.2 Precision:13.2.1 Within laboratory variability may be described using the repeatability value (r) obtained by multiplying the repeatabilitystandard deviation b
42、y 2.8.The repeatability value estimates the 95 % confidence limit.That is, two results from the same laboratoryshould be considered suspect (at the 95 % confidence level) if they differ by more than the repeatability value.13.2.2 The within laboratory repeatability standard deviation was 0.041 GPa r
43、esulting 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 described using the reproducibility value (R) obtained by multiplying thereproducibility standard deviatio
44、n by 2.8. The reproducibility value estimates the 95 % confidence limit. That is, results obtainedfrom two different laboratories, operators or apparatus should be considered suspect (at the 95 % confidence level) if they differby more than the reproducibility value.13.2.4 The between laboratory rep
45、roducibility standard deviation was 0.16 GPa resulting in a reproducibility relative standarddeviation of 14 %. The reproducibility value R thus is 0.45 GPa13.3 Bias:13.3.1 Bias is the difference between the mean value obtained and an acceptable reference value for the same material.13.3.2 The Young
46、s modulus calculated from the storage modulus (E) value determined by this standard and the loss modulus(E”) value determined by Test Method E2425 may be compared to the Youngs modulus (E) obtained by Test Method E698 bythe equation:E5E22E”2#1/213.3.3 The value for Youngs modulus determined for this
47、 material by Test Method D638 is 1.256 GPa.13.3.4 The mean value for storage modulus (E) determined by this standard is 1.184 GPa.13.3.5 The mean value for loss modulus (E”) for this material determined by Test Method E2425 was 62.0 MPa.13.3.6 Based upon the Students “t” test, these values for Young
48、s 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 rights asserted in connection with any item mentionedin this standard. Users of this
49、 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 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 comments will receive careful
