1、Designation: E1867 16E1867 18Standard 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 la
2、st revision. 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 calibration of dynamic mechanical analyzers (DMA) from 100C to300C.100 C t
3、o 300 C.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 does 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 est
4、ablish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.Specific precautionary statements are given in Note 10.1.4 This international standard was developed in accordance with internationally recognized princip
5、les on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal
6、 Analysis and RheologyE1142 Terminology Relating to Thermophysical PropertiesE1970 Practice for Statistical Treatment of Thermoanalytical DataE1640 Test Method for Assignment of the Glass Transition Temperature By Dynamic Mechanical AnalysisE2161 Terminology Relating to Performance Validation in The
7、rmal Analysis and RheologyE3142 Test Method for Thermal Lag of Thermal Analysis Apparatus3. Terminology3.1 Definitions:3.1.1 The technical terms used in these test methods are defined in Terminologies E473, E1142, and E2161, including dynamicmechanical analysis, frequency, stress, strain, and storag
8、e modulus.4. Summary of Test MethodMethods4.1 In dynamic mechanical analysis, often large (for example, 1 g to 10 g), low thermal conductivity test specimens arecharacterized while being mechanically supported using high thermal conductivity materials, while a temperature sensor isfree-floating in t
9、he atmosphere near the test specimen. Under temperature programming conditions, where the atmospheresurrounding the test specimen is heated or cooled at rates up to 5C/min, 5 C/min, the temperature of the test specimen may leador lag that of the nearby temperature sensor. It is the purpose of this s
10、tandard to calibrate the dynamic mechanical analyzertemperature sensor so that the indicated temperature more closely approximates that of the test specimen. This In Methods A, B,and C, this is accomplished by separating the test specimen calibration specimen (with its first order transition) from i
11、ts mechanicalsupports and from the surrounding atmosphere using a low thermal conductivity material. Three test methods of providing thisseparation are provided.In Method D, the thermal lag between the temperature sensor and the test specimen is determined as afunction of heating rate. This value is
12、 then used to adjust the indicated temperature following calibration under isothermal ambientconditions.1 These test methods are under the jurisdiction of ASTM Committee E37 on Thermal Measurements and are the direct responsibility of Subcommittee E37.10 onFundamental, Statistical and Mechanical Pro
13、perties.Current edition approved Feb. 15, 2016Aug. 1, 2018. Published April 2016August 2018. Originally approved in 1997. Last previous edition approved in 20132016 asE1867 13.E1867 16. DOI: 10.1520/E1867-16.10.1520/E1867-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or con
14、tactASTM Customer Service at serviceastm.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 be
15、en made to the previous version. Becauseit 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 documen
16、t.*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 States14.2 An equation is developed for the linear correlation of experimentally observed program or sensor temperature and th
17、e actualmelting temperature for known melting reference materials.or glass transition of the reference material. This is accomplished inMethod A by a melting point reference materialsmaterial loaded into a polymer tube, or in Method B by wrapping the calibrationmaterial with polymer tape or in Metho
18、d C by placing the calibration material between glass or ceramic plates and subjecting thistest specimen to a mechanical oscillation at either fixed or resonant frequency. The extrapolated onset of melting is identified bya rapid decrease in the ordinate signal (the apparent storage modulus, stress,
19、 inverse strain or probe position). This onset is usedfor temperature calibration with two melting point reference materials.5. Significance and Use5.1 Dynamic mechanical analyzers monitor changes in the viscoelastic properties of a material as a function of temperature andfrequency, providing a mea
20、ns to quantify these changes. In most cases, the value to be assigned is the temperature of the transition(or event) under study. Therefore, the temperature axis (abscissa) of all DMA dynamic mechanical analysis thermal curves mustbe accurately calibrated by adjusting the apparent temperature scale
21、to match the actual specimen temperature over the temperaturerange of interest.5.2 This test method is useful for research, quality assurance, and specification acceptance.6. Interferences6.1 An increase or decrease in heating rates or change in purge gas type or rate from those specified may alter
22、results.6.2 Once the temperature calibration procedure has been executed, the measuring temperature sensor position shall not bechanged, nor shall it be in contact with the specimen or specimen holder in a way that would impede movement. If the temperaturesensor position is changed or is replaced, t
23、hen the entire calibration procedure shall be repeated.6.3 Once the temperature calibration has been executed, the geometry deformation (bending study, versus tensile, and the like)shall not be changed. If the specimen testing geometry differs significantly from that of the calibrants, then the cali
24、bration shallbe repeated in the geometry matching that of specimen testing.6.4 These test methods do not apply to calibration for shear or compressive geometries of deformation.7. Apparatus7.1 The function of the apparatus is to hold a specimen of uniform dimension so that the specimen acts as the e
25、lastic anddissipative element in a mechanically oscillated system. Dynamic mechanic analyzers typically operate in one of several modesas outlined in Table 1.7.1.1 The apparatus shall consist of the following:7.1.1.1 ClampsAclamping arrangement that permits gripping of the specimen.This may be accom
26、plished by clamping at bothends (most systems), one end (for example, torsional pendulum) or neither end (for example, free bending between knife edges).7.1.1.2 Device to Apply Oscillatory Stress or StrainA device for applying an oscillatory deformation (strain) or oscillatorystress to the specimen.
27、 The deformation may be applied and then released, as in freely vibrating devices, or continually applied,as in forced vibration devices.7.1.1.3 DetectorA device or devices for determining the dependent and independent experimental parameters, such as force(stress), deformation (strain), frequency,
28、and temperature. Temperature shall be measurable with an accuracy of 60.1C, readableto within 60.1 C, force to within 61 % and frequency to within 61 %.7.1.1.4 Temperature Controller and OvenA device for controlling the specimen temperature, either by heating, cooling (insteps or ramps), or by maint
29、aining a constant experimental environment. The temperature programmer shall be sufficiently stableto permit measurement of specimen temperature to 0.1C.stable to within 60.1 C.7.1.1.5 A Data Collection Device, to provide a means of acquiring, storing, and displaying measured or calculated signals,
30、orboth. The minimum output signals required for dynamic mechanical analysis are storage modulus, loss modulus, tangent delta,temperature, and time.NOTE 1Some instruments, suitable for this test, may display only linear or logarithmic storage modulus while others may display both linear orTABLE 1 Dyn
31、amic Mechanical Analyzer Modes of OperationMode Mechanical ResponseTension Flexural Torsion CompressionFree/decA . . . . . . X . . .Forced/res/CAA . . . X X . . .Forced/fix/CAA X X X XForced/fix/CSA X X . . . XA Free = free oscillation; dec = decaying amplitude; forced = forced oscillation;CA = cons
32、tant amplitude; res = resonant frequency; fix = fixed frequency;CS = controlled stress.E1867 182logarithmic storage modulus, or both. modulus. Care must be taken to use the same modulus scale when comparing unknown specimens, and in thecomparison of results from one instrument to another.7.2 For Met
33、hod A, high-temperature polymer tubing such as PTFE (Polytetrafluoroethylene) or PEEK(Polyetheretherketone),(Polyetherether-ketone), of 3-mm outside diameter and wall thickness of 0.5-mm (0.002 in.) (1)3 may be used for low temperature standards (thatis, less than 160C). 160 C). The tubing may be se
34、aled with suitable melting temperature wax plugs, or similar sealant. (SeeAppendix X3X2.)NOTE 2PTFE tubing is selected for its flexibility and inert nature for the solvents in use at the temperatures of interest. Furthermore its transitionsshould not produce any interference in the DMAdynamic mechan
35、ical analyzer signal within the range of the suggested calibrant materials. PEEK providesincreased stiffness for ease of loading. For other temperature ranges, a suitable replacement for the high temperature polymer tubing may be used.7.2.1 Calibration MaterialsOne or more suitable materials present
36、ed in Table 2.7.3 For Method B, PTFE tape, to be used for wrapping metal point standards.7.3.1 Calibration MaterialsOne or more suitable materials presented in Table 2.7.4 For Method C, sheet stock or coupons composed of one of the materials in Table 3, approximately 0.5 mm in thickness,and length a
37、nd width similar to that of an unknown test specimen to be used.7.4.1 Calibration MaterialsOne or more suitable materials presented in Table 2.7.5 Calibration MaterialsFor Method D: One or more suitable materials presented in Table 2.7.5.1 Calibration MaterialA high temperature polymer sheet stock o
38、r coupons, 0.5 mm to 1.0 mm in thickness with lengthand width similar to that of the unknown test specimen, with a well-defined glass transition.NOTE 3Polycarbonate or a fully cured thermoset composite have been found suitable.7.5.2 Thermometer, calibrated digital or analog, capable of measuring tem
39、perature over the range of 15 C to 30 C readableto within 0.1 C.7.6 Calipers or other length measuring device capable of measuring dimensions (or length) readable to within 610 m.8. Reagents and Materials8.1 Dry nitrogen, helium, or other inert gas supplied for purging purposes and especially to ens
40、ure that moisture condensationand ice formation is avoided when measurements involve temperatures below the dew point.NOTE 4The same purge gas shall be used for calibration as for the determination of unknown specimens.3 The boldface numbers in parentheses refer to a list of references at the end of
41、 this standard.TABLE 2 Calibration MaterialsMaterial Transition TemperatureAReferenceC Kn-Heptane 90.56 182.65 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.
42、4Tin 231.928 505.078 X1.4TABLE 2 Calibration MaterialsMaterial Transition TemperatureAReferenceC Kn-Heptane 90.56 182.65 (2)Cyclohexane 87.06 186.09 (3)n-Octane 56.76 216.39 (4)n-Decane 26.66 246.49 (4)n-Dodecane 9.65 263.5 (4)Water 0.01 273.16 (5)Cyclohexane 6.54 279.69 (3)Indium 156.5985 495.7485
43、(5)Tin 231.928 505.078 (5)A The values in this table were determined under special, highly accurate testconditions that are not attainable or applicable to these test methods. The actualprecision of these test methods is given in Section 1314.E1867 1839. Calibration and Standardization9.1 Prepare th
44、e instrument for operation as described by the manufacturer in the operations manual.10. ProcedurePrecedureMethods A, B, or C10.1 Two Point CalibrationFor the purposes of this procedure, it is assumed that the relationship between observedextrapolated onset temperature (Too) and actual specimen temp
45、erature (Ttt) is a linear one governed by the equation:Tt5To3S!1I (1)where: S and I are the slope and intercept of a straight line, respectively.10.2 Select two calibration standards near the temperature range of interest. The standards should be as close to the upper andlower temperature limits use
46、d for the subsequent test materials as practical.NOTE 5The purpose of the polymer encapsulation is to provide thermal resistance between the test specimen and the environment similar to thatoffered by polymer test specimens. In some testing geometries it may be possible to perform the test directly
47、on the metal melting point reference materialswithout encapsulation. (See Appendix X2X1.)10.3 Method ACalibration Using Materials that are Liquids at Ambient Temperature and where the melting temperature doesnot exceed 100C. 100 C. (See Appendix X3X2.)10.3.1 Fill the polymer tubing with the calibrat
48、ion material. Calibrant must extend to the ends of the clamping geometry andmust have uniform dimensions with respect to width.10.3.2 Mount the specimen in accordance with the procedure recommended by the manufacturer.NOTE 6For specimen clamping arrangements where the specimen is not gripped on eith
49、er end (for example, free bending between knife edges) thespecimen must be rigid enough at the test start temperature to sustain initial loading. Alternatively, the calibration specimen, without encapsulation, canbe placed between the knife edge and a substrate.10.3.3 Maximum strain amplitude shall be within the linear viscoelastic range of the specimens to be subsequently analyzed.Strains of less than 1 % are recommended and shall not exceed 3 %.10.3.4 Equilibrate the test specimen for 5 min at a temperature 30 C below the a
