1、Designation: E1867 16Standard Test Methods forTemperature Calibration of Dynamic Mechanical Analyzers1This standard is issued under the fixed designation E1867; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 These test methods describes the temperature calibrationof dynamic mechanical analyzers (DMA) from 100C to300C.1.2 The values s
3、tated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 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
4、and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Note 10.2. Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rhe-ologyE1142 Terminology Relating to Thermophysical Pro
5、pertiesE2161 Terminology Relating to Performance Validation inThermal Analysis and Rheology3. Terminology3.1 Definitions:3.1.1 The technical terms used in these test methods aredefined in Terminologies E473, E1142, and E2161, includingdynamic mechanical analysis, frequency, stress, strain, andstorag
6、e modulus.4. Summary of Test Method4.1 In dynamic mechanical analysis, often large (forexample, 1 to 10 g), low thermal conductivity test specimensare characterized while being mechanically supported usinghigh thermal conductivity materials, while a temperature sen-sor is free-floating in the atmosp
7、here near the test specimen.Under temperature programming conditions, where the atmo-sphere surrounding the test specimen is heated or cooled atrates up to 5C/min, the temperature of the test specimen maylead or lag that of the nearby temperature sensor. It is thepurpose of this standard to calibrat
8、e the dynamic mechanicalanalyzer temperature sensor so that the indicated temperaturemore closely approximates that of the test specimen. This isaccomplished by separating the test specimen from its me-chanical supports and from the surrounding atmosphere usinga low thermal conductivity material. Th
9、ree test methods ofproviding this separation are provided.4.2 An equation is developed for the linear correlation ofexperimentally observed program or sensor temperature andthe actual melting temperature for known melting referencematerials. This is accomplished in MethodAby a melting pointreference
10、 materials loaded into a polymer tube, or in Method Bby wrapping the calibration material with polymer tape or inMethod C by placing the calibration material between glass orceramic plates and subjecting this test specimen to a mechani-cal oscillation at either fixed or resonant frequency. Theextrap
11、olated onset of melting is identified by a rapid decreasein the ordinate signal (the apparent storage modulus, stress,inverse strain or probe position). This onset is used fortemperature calibration with two melting point reference ma-terials.5. Significance and Use5.1 Dynamic mechanical analyzers m
12、onitor changes in theviscoelastic properties of a material as a function of tempera-ture and frequency, providing a means to quantify thesechanges. In most cases, the value to be assigned is thetemperature of the transition (or event) under study. Therefore,the temperature axis (abscissa) of all DMA
13、 thermal curvesmust be accurately calibrated by adjusting the apparent tem-perature scale to match the actual temperature over thetemperature range of interest.6. Interferences6.1 An increase or decrease in heating rates or change inpurge gas type or rate from those specified may alter results.6.2 O
14、nce the temperature calibration procedure has beenexecuted, the measuring temperature sensor position shall not1These test methods are under the jurisdiction of ASTM Committee E37 onThermal Measurements and are the direct responsibility of Subcommittee E37.10 onFundamental, Statistical and Mechanica
15、l Properties.Current edition approved Feb. 15, 2016. Published April 2016. Originallyapproved in 1997. Last previous edition approved in 2013 as E1867 13. DOI:10.1520/E1867-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. Fo
16、r Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1be cha
17、nged, nor shall it be in contact with the specimen orspecimen holder in a way that would impede movement. If thetemperature sensor position is changed or is replaced, then theentire calibration procedure shall be repeated.6.3 Once the temperature calibration has been executed, thegeometry deformatio
18、n (bending study, versus tensile, and thelike) shall not be changed. If the specimen testing geometrydiffers significantly from that of the calibrants, then thecalibration shall be repeated in the geometry matching that ofspecimen testing.6.4 These test methods do not apply to calibration for shearo
19、r compressive geometries of deformation.7. Apparatus7.1 The function of the apparatus is to hold a specimen ofuniform dimension so that the specimen acts as the elastic anddissipative element in a mechanically oscillated system. Dy-namic mechanic analyzers typically operate in one of severalmodes as
20、 outlined in Table 1.7.1.1 The apparatus shall consist of the following:7.1.1.1 ClampsAclamping arrangement that permits grip-ping of the specimen. This may be accomplished by clampingat both ends (most systems), one end (for example, torsionalpendulum) or neither end (for example, free bending betw
21、eenknife edges).7.1.1.2 Device to Apply Oscillatory Stress or StrainAdevice for applying an oscillatory deformation (strain) oroscillatory stress to the specimen. The deformation may beapplied and then released, as in freely vibrating devices, orcontinually applied, as in forced vibration devices.7.
22、1.1.3 DetectorA device or devices for determining thedependent and independent experimental parameters, such asforce (stress), deformation (strain), frequency, and temperature.Temperature shall be measurable with an accuracy of 60.1C,force to 61 % and frequency to 61%.7.1.1.4 Temperature Controller
23、and OvenA device forcontrolling the specimen temperature, either by heating, cool-ing (in steps or ramps), or by maintaining a constant experi-mental environment. The temperature programmer shall besufficiently stable to permit measurement of specimen tempera-ture to 0.1C.7.1.1.5 A Data Collection D
24、evice, to provide a means ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required fordynamic mechanical analysis are storage modulus, lossmodulus, tangent delta, temperature, and time.NOTE 1Some instruments, suitable for this test, may display
25、 onlylinear or logarithmic storage modulus while others may display linear orlogarithmic storage modulus, or both. Care must be taken to use the samemodulus scale when comparing unknown specimens, and in the compari-son of results from one instrument to another.7.2 For MethodA, high-temperature poly
26、mer tubing such asPTFE (Polytetrafluoroethylene) or PEEK(Polyetheretherketone), of 3-mm outside diameter and wallthickness of 0.5-mm (0.002 in.) (1)3may be used for lowtemperature standards (that is, less than 160C). The tubingmay be sealed with suitable melting temperature wax plugs, orsimilar seal
27、ant. (See Appendix X3.)NOTE 2PTFE tubing is selected for its flexibility and inert nature forthe solvents in use at the temperatures of interest. Furthermore itstransitions should not produce any interference in the DMA signal withinthe range of the suggested calibrant materials. PEEK provides incre
28、asedstiffness for ease of loading. For other temperature ranges, a suitablereplacement for the high temperature polymer tubing may be used.7.3 For Method B, PTFE tape, to be used for wrappingmetal point standards.7.4 For Method C, sheet stock or coupons composed of oneof the materials in Table 3, ap
29、proximately 0.5 mm in thickness,and length and width similar to that of an unknown testspecimen to be used.7.5 Calibration MaterialsOne or more suitable materialspresented in Table 2.7.6 Calipers or other length measuring device capable ofmeasuring dimensions (or length) within 610 m.8. Reagents and
30、 Materials8.1 Dry nitrogen, helium, or other inert gas supplied forpurging purposes and especially to ensure that moisture con-densation and ice formation is avoided when measurementsinvolve temperatures below the dew point.9. Calibration and Standardization9.1 Prepare the instrument for operation a
31、s described by themanufacturer in the operations manual.3The boldface numbers in parentheses refer to a list of references at the end ofthis standard.TABLE 1 Dynamic Mechanical Analyzer Modes of OperationModeMechanical ResponseTension Flexural Torsion CompressionFree/decA. . X .Forced/res/CAA. X X .
32、Forced/fix/CAAXX XForced/fix/CSAX X . XAFree = free oscillation; dec = decaying amplitude; forced = forced oscillation;CA = constant amplitude; res = resonant frequency; fix = fixed frequency;CS = controlled stress.TABLE 2 Calibration MaterialsMaterialTransition TemperatureAReferenceC Kn-Heptane 90.
33、56 182.65 X1.2Cyclohexane 87.06 186.09 X1.3n-Octane 56.76 216.39 X1.1n-Decane 26.66 246.49 X1.1n-Dodecane 9.65 263.5 X1.1Water 0.01 273.16 X1.4Cyclohexane 6.54 279.69 X1.3Indium 156.5985 495.7485 X1.4Tin 231.928 505.078 X1.4AThe values in this table were determined under special, highly accurate tes
34、tconditions that are not attainable or applicable to these test methods. The actualprecision of these test methods is given in Section 13.E1867 16210. Procedure10.1 Two Point CalibrationFor the purposes of thisprocedure, it is assumed that the relationship between observedextrapolated onset temperat
35、ure (To) and actual specimen tem-perature (Tt) is a linear one governed by the equation:Tt5 To3S!1I (1)where: S and I are the slope and intercept of a straight line,respectively.10.2 Select two calibration standards near the temperaturerange of interest. The standards should be as close to the upper
36、and lower temperature limits used for the subsequent testmaterials as practical.NOTE 3The purpose of the polymer encapsulation is to providethermal resistance between the test specimen and the environment similarto that offered by polymer test specimens. In some testing geometries itmay be possible
37、to perform the test directly on the metal melting pointreference materials without encapsulation. (See Appendix X2.)10.3 Method ACalibration Using Materials that are Liq-uids at Ambient Temperature and where the melting tempera-ture does not exceed 100C. (See Appendix X3.)10.3.1 Fill the polymer tub
38、ing with the calibration material.Calibrant must extend to the ends of the clamping geometryand must have uniform dimensions with respect to width.10.3.2 Mount the specimen in accordance with the proce-dure recommended by the manufacturer.NOTE 4For specimen clamping arrangements where the specimen i
39、snot gripped on either end (for example, free bending between knife edges)the specimen must be rigid enough at the test start temperature to sustaininitial loading. Alternatively, the calibration specimen, withoutencapsulation, can be placed between the knife edge and a substrate.10.3.3 Maximum stra
40、in amplitude shall be within the linearviscoelastic range of the specimens to be subsequently ana-lyzed. Strains of less than 1 % are recommended and shall notexceed 3 %.10.3.4 Conduct the calibration experiments at the heatingrate of interest, preferably 1C/min but no greater than 5C/minand a frequ
41、ency of 1 Hz. Other heating rates and frequenciesmay be used but shall be reported. (See Appendix X2.)NOTE 5Calibration for temperature shall be performed under theconditions of heating rate and frequency at which the unknown specimenswill be tested. This test method does not address the issues of f
42、requencyaffects for polymeric transitions (such as the upwards shift of glasstransition temperature with increasing frequency), and will only compen-sate for thermal lag within the measuring device.10.3.5 Measure and record the ordinate signal, from 30Cbelow to 20C above the melting point of the ref
43、erencematerial. The calibration specimen may be equilibrated aminimum of 50C below the melting transition, but adequatetime to achieve thermal equilibrium in the specimen must beallowed.TABLE 3 Insulating Sheet StockMaterialThermalConductivityat 25C,W/(m-K)ReferenceRoomTemperatureThermalDiffusivity
44、at25 C,mm2/sMaximumTemperature, CPolytetrafluorothylene 0.25 (2) 260 (2)Polyimide 0.120.35C(3)Polyetheretherketone 0.25 (4) 400 (4)MacorA1.460.840.73Soda Lime Glass 0.94 0.51 250PyrexBGlass 1.45 (5)AMacor is a registered trademark of Corning, Inc., Corning, NY.BPyrex is a registered trademark of Cor
45、ning, Inc., Corning, NY.CAt 40C.FIG. 1 Transition TemperatureE1867 16310.4 Method BCalibration Where the Material is a Solidat Ambient Temperature:10.4.1 The calibration material must extend to the ends ofthe clamping geometry and must have uniform dimensionswith respect to the width and thickness.
46、Wrap the calibrationmaterial with polytetrafluoroethylene tape to a thickness of 0.5mm. Other thicknesses may be used but shall be reported.10.4.2 Mount the wrapped specimen into the apparatusaccording to the procedure recommended by the manufactureras described in the operations manual.NOTE 6For sp
47、ecimen clamping arrangements where the specimen isnot gripped on either end (for example, free bending between knife edges)the specimen must be rigid enough at the test start temperature to sustaininitial loading. Alternatively, the calibration specimen, withoutencapsulation, can be placed between t
48、he knife edge and a substrate.10.4.3 Maximum strain amplitude shall be within the linearviscoelastic range of the specimen. Strain of less than1%isrecommended and shall not exceed 3 %.10.4.4 Conduct the calibration experiments at the heatingrate of interest, preferably 1C/min but no greater than 5C/
49、minand a frequency of 1 Hz. Other heating rates and frequenciesmay be used but shall be reported.NOTE 7Calibration for temperature shall be performed under theconditions of heating rate and frequency at which the unknown specimenswill be tested. This test method does not address the issues of frequencyaffects for polymeric transitions (such as the upwards shift of glasstransition temperature with increasing frequency), and will only compen-sate for thermal lag within the measuring device.10.4.5 Measure and record the ordinate signal, from
