1、Designation: E1363 18Standard Test Method forTemperature Calibration of Thermomechanical Analyzers1This standard is issued under the fixed designation E1363; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. 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 This test method describes the temperature calibrationof thermomechanical analyzers from 50 C to 1500 C. (SeeNote 1.)1.2 The value
3、s stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 WarningMercury has been designated by many regu-latory agencies as a hazardous substance that can causeserious medical issues. Mercury, or its vapor, has beendemonstrated to be hazardou
4、s to health and corrosive tomaterials. Use caution when handling mercury and mercury-containing products. See the applicable product Safety DataSheet (SDS) for additional information. The potential existsthat selling mercury or mercury-containing products, or both,is prohibited by local or national
5、law. Users must determinelegality of sales in their location.1.4 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, health, and environmental practices and deter-
6、mine the applicability of regulatory limitations prior to use.Specific precautionary statements are given in Section 7 andNote 11.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for
7、theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rhe-ologyE3142 Test Method for Thermal Lag of Thermal
8、AnalysisApparatus3. Terminology3.1 Definitions:3.1.1 The terminology relating to thermal analysis appear-ing in Terminology E473 shall be considered applicable to thisdocument.4. Summary of Test Method4.1 An equation is developed for the linear correlation of theexperimentally observed program tempe
9、rature and the actualmelting temperature for known melting standards. This isaccomplished through the use of a thermomechanical analyzerwith a penetration probe to obtain the onset temperatures fortwo melting point standards.An alternate, one-point method oftemperature calibration is also given for
10、use over very narrowtemperature ranges. (See Note 2.)NOTE 1This test method may be used for calibrating thermomechani-cal analyzers at temperatures outside this range of temperature. However,the accuracy of the calibration will be no better than that of thetemperature standards used.NOTE 2It is poss
11、ible to develop a more elaborate method oftemperature calibration using multiple (more than two) fusion standardsand quadratic regression analysis. Since most modern instruments arecapable of heating rates which are essentially linear in the region of use,the procedure given here is limited to a two
12、-point calibration.5. Significance and Use5.1 Thermomechanical analyzers are employed in theirvarious modes of operation (penetration, expansion, flexure,etc.) to characterize a wide range of materials. In most cases,the value to be assigned in thermomechanical measurements isthe temperature of the
13、transition (or event) under study.Therefore, the temperature axis (abscissa) of all TMA thermal1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.10 onFundamental, Statistical and Mechanical Properties.Current
14、edition approved Dec. 1, 2018. Published January 2019. Originallyapproved in 1990. Last previous edition approved in 2016 as E1363 16. DOI:10.1520/E1363-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of AST
15、MStandards 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 StatesThis international standard
16、 was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1curves mu
17、st be accurately calibrated either by direct reading ofa temperature sensor or by adjusting the programmer tempera-ture to match the actual temperature over the temperature rangeof interest.6. Apparatus6.1 Thermomechanical Analyzer (TMA)The essential in-strumentation required to provide the minimum
18、thermome-chanical analytical or thermodilatometric capability for this testmethod includes:6.1.1 A Rigid Specimen Holder or Platform, of inert, lowcoefficient of expansion material (1 m m-1K-1) to center thespecimen in the furnace and to fix the specimen to mechanicalground.6.1.2 A Rigid (expansion
19、compression, flexure, tensile, etc.)Probe, of inert, low coefficient of expansion material (1 mm-1K-1) that contacts with the specimen with an appliedcompressive or tensile force. For this test method, the use of apenetration probe is recommended.6.1.3 A Sensing Element, linear over a minimum range
20、of2 mm to measure the displacement of the rigid probe to 650nm resulting from changes in the length/height of the speci-men.6.1.4 A Weight or Force Transducer, to generate a constantforce of 50 6 5 mN (5.0 6 0.5 g) that is applied through therigid probe to the specimen.NOTE 3The recommendation of a
21、5.0 g load (or a force of 50 mN) isbased on the use of penetration probes commonly used in the commer-cially available thermomechanical analyzers. These probes have tipdiameters ranging from 0.89 mm to 2.0 mm and lead to pressures from 80kPa to 16 kPa when using the recommended 5.0 g load. The use o
22、f probeswhich differ greatly from this range of tip diameters may require differentloading (or force).6.1.5 A Furnace, capable of providing uniform controlledheating (cooling) at a rate of 1 C min-1to 10 6 1Cmin-1ofa specimen to a constant temperature within the applicabletemperature range of this t
23、est method.NOTE 4The temperature range of operation of commercial thermo-mechanical analyzers vary by manufacturer and mode. The completerange of temperature of an instrument is sometimes achieved by the use oftwo different furnaces. In this case, temperature calibration must becarried out for each
24、furnace.6.1.6 A Temperature Controller, capable of executing aspecific temperature program by operating the furnace betweenselected temperature limits at a rate of temperature change of10 6 1Cmin-1.6.1.7 A Temperature Sensor, that may be positioned in closeproximity to the test specimen to provide a
25、n indication of thespecimen/furnace temperature to within 60.1 C min-1.6.1.8 A means of sustaining an environment around thespecimen with an inert purge gas (for example, nitrogen,helium, argon, etc.) at a purge gas flow rate of 20 mL min-1to50 mL min-1.6.1.9 A Data Collection Device, to provide a m
26、eans ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required forTMAare a change in linear dimension, temperature, and times.7. Hazards7.1 This test method may involve the use of hazardousmaterials, operations, and equipment. It is the responsi
27、bility ofthe user of this test method to establish appropriate safetypractice and to determine the applicability of regulatorylimitations prior to use. (WarningToxic or corrosiveeffluents, or both, may be released when heating some mate-rials and could be harmful to personnel and the apparatus.)7.2
28、Once this calibration procedure has been executed asdescribed in 10.1.2.1 10.1.2.7 of this test method, themeasuring temperature sensor position should not be changed,nor should it be in contact with the sample or sample holder ina way that would impede movement. If for some reason thetemperature se
29、nsor position is changed or the temperaturesensor is replaced, then the entire calibration procedure shouldbe repeated.8. Calibration8.1 For the temperature range covered by manyapplications, the melting transition of 99.99 % pure materialsmay be used for calibration. (See Table 1.)NOTE 5The values
30、in Table 1 were determined using special99.9999 % pure materials and highly accurate steady-state conditions thatare not attainable with this test method. The actual precision of this testmethod is given in Section 13.NOTE 6The melting temperatures of these materials have beenselected as primary fix
31、ed points (see Table 1) for the InternationalPractical Temperature Scale of 1990.3NOTE 7Some materials have different crystalline forms (for example,tin) or may react with the container. Such calibration materials should bediscarded after their initial melt.3Supporting data have been filed at ASTM I
32、nternational Headquarters and maybe obtained by requesting Research Report RR:E37-1011. ContactASTM CustomerService at serviceastm.org.TABLE 1 Recommended Melting Temperature ReferenceMaterialsCalibration MaterialAMelting Temperature(C) (K)Mercury 38.8344 234.3156Water 0.01 273.16Gallium 29.7646 302
33、.9146Indium 156.5985 429.7485Tin 231.928 505.078Bismuth 271.402 544.552Cadmium 321.069 594.219Lead 327.462 600.612Zinc 419.527 692.677Antimony 630.628 903.778Aluminum 660.323 933.473Silver 961.78 1234.93Gold 1064.18 1337.33Copper 1084.62 1357.77Nickel 1455 1728Cobalt 1495 1768ADella Gatta, G., Richa
34、rdson, M. J., Sarge, S. M., and Stolen, S., “Standards,Calibration, and Guidelines in Microcalorimetry, Part 2: Calibration Standards forDifferential Scanning Calorimetry,” Pure and Applied Chemistry, Vol 78, No. 7,2006, pp. 14551476.E1363 1829. Assignment of the Penetration Onset Temperature9.1 The
35、 assignment of the TMA penetration onset tempera-ture is an important procedure since, when using this testmethod, temperature calibration of the thermomechanical ana-lyzer is directly dependent upon it. The temperature standardsgiven in Table 1 will give a downward deflection on thethermal curve, s
36、imilar to that shown in Fig. 1, when placedunder a weighted TMA penetration probe and heated to theirrespective melting temperatures.9.2 The extrapolated onset temperature for such a penetra-tion thermal curve is obtained by extending the pre-transitionportion of the thermal curve to the point of in
37、tersection with aline drawn tangent to the steepest portion of the curve whichdescribes the probe displacement. The temperature correspond-ing to this point of intersection is the penetration onsettemperature. This is shown graphically in Fig. 1. There aresome materials (for example, aluminum metal)
38、 which showpre-transition probe displacement prior to the sharper down-ward deflection observed on melting. In this case, the pre-transition baseline is extended from the point which representsthe highest temperature the material reaches prior to exhibitingsignificant or measurable softening under t
39、he conditions of theexperiment. Fig. 2 describes the assignment of the extrapolatedonset temperature for a specimen which exhibits pre-transitionpenetration.10. Procedure10.1 Two-Point CalibrationFor the purposes of thisprocedure, it is assumed that the relationship between observedextrapolated onse
40、t temperature (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.10.1.1 Select two calibration reference materials near thetemperature range of interest. The standards should be
41、as closeto the upper and lower temperature limits used in the actualanalysis runs as is practical.10.1.2 Determine the apparent extrapolated onset tempera-ture for the calibration reference material chosen, using apenetration-type probe with the TMA instrument.10.1.2.1 Place a 10-mg to 20-mg specime
42、n of one of thecalibration reference materials on the sample platform (orholder, whichever is applicable).NOTE 8The specimen should have a smooth surface on both top andbottom. Avoid the use of specimens with sharp ridges and irregularsurfaces. These can lead to false values for the onset temperatur
43、es.Powdered or liquid standards may be placed into a stable, inert container,if necessary.10.1.2.2 Place a probe loaded with 5 g (or force of 50 mN)in contact with the test specimen.10.1.2.3 Purge the specimen chamber area with inert gas ata flow rate that is appropriate to the dimensions of theappa
44、ratus throughout the experiment. Typical flow rates arefrom 20 mLmin to 50 mL/min. The same purge gas and flowrate should be maintained in both calibration runs and analysisruns.10.1.2.4 Heat the calibration sample specimen to a tempera-ture about 50 C below the calibration temperature and allowthe
45、TMA furnace to equilibrate for at least 1 min.10.1.2.5 Heat the calibration specimen at 5 C/min throughthe transition allowing the probe to reach a point of maximumpenetration. (See Fig. 1.)NOTE 9Temperature calibration may be affected by heating rate,purge gas flow rate, and choice of purge gas.NOT
46、E 10Other heating rates may be used but shall be reported. SeeTest Method E3142 for the determination and application of thermal lag.10.1.2.6 From the TMA thermal curve obtained, assign theextrapolated onset temperature (see Fig. 1) to the requiredprecision.NOTE 11Retain all available digits.10.1.2.
47、7 Repeat the procedure described in 10.1.2 10.1.2.5using the second calibration reference material that was cho-sen.11. Calculation11.1 Using the reference material temperature values fromTable 1 and the corresponding onset temperatures obtainedexperimentally, determine the slope and intercept using
48、 thefollowing equations:FIG. 1 Assignment of the Extrapolated Onset Temperature (To)from TMA Thermal CurveFIG. 2 Assignment of Extrapolated Onset Temperature (To) fromTMA Thermal Curve for Specimen ExhibitingPre-Transition SofteningE1363 183S 5 Ta12 Ta2#/T012 T02# (2)I 5 T013Ta2! 2 Ta13T02!#/T012 T0
49、2! (3)where:S = slope (nominal value = 1.00),I = intercept,Ta1= reference transition temperature for Reference Mate-rial 1 taken from Table 1,Ta2= reference transition temperature for Reference Mate-rial 2 taken from Table 1,T01= experimentally observed transition onset temperaturefor Reference Material 1, andT02= experimentally observed transition onset temperaturefor Reference Material 2.(WarningThe slope S is a dimensionless number whosevalue is independent of which temperature scale is used for Iand T. In all cases, I must have the sa
