1、Designation: E1363 13E1363 16Standard 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
2、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 Scope*1.1 This test method describes the temperature calibration of thermomechanical analyzers from 50from 50 to1100C.1500C. (
3、See Note 1.)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 is similar to ISO 113591 but addresses a larger temperature range and utilizes additional calibrationmaterials.1.4 This standard does not purpor
4、t 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. Specific precautionary statements are given in Se
5、ction 7 and Note 1011.2. Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rheology2.2 Other Standards:3ISO 113591 Thermomechanical Analysis (TMA)-Part 1: General Principles3. Terminology3.1 Definitions:3.1.1 The terminology relating to thermal analysis appear
6、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 the experimentally observed program temperature and the actualmelting temperature for known melting standards. This is accomplished through the u
7、se of a thermomechanical analyzer with apenetration probe to obtain the onset temperatures for two melting point standards. An alternate, one-point method of temperaturecalibration,calibration is also given for use over very narrow temperature ranges. (See Note 2.)NOTE 1This test method may be used
8、for calibrating thermomechanical analyzers at temperatures outside this range of temperature. However, theaccuracy of the calibration will be no better than that of the temperature standards used.NOTE 2It is possible to develop a more elaborate method of temperature calibration using multiple (more
9、than two) fusion standards and quadraticregression analysis. Since most modern instruments are capable of heating rates which are essentially linear in the region of use, the procedure given hereis limited to a two-point calibration.5. Significance and Use5.1 Thermomechanical analyzers are employed
10、in their various modes of operation (penetration, expansion, flexure, etc.) tocharacterize a wide range of materials. In most cases, the value to be assigned in thermomechanical measurements is thetemperature of the transition (or event) under study. Therefore, the temperature axis (abscissa) of all
11、 TMA thermal curves must1 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 April 1, 2013Dec. 1, 2016. Published May 2013January
12、 2017. Originally approved in 1990. Last previous edition approved in 20082013 asE1363 08.E1363 13. DOI: 10.1520/E1363-13.10.1520/E1363-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume
13、information, refer to the standards Document Summary page on the ASTM website.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM sta
14、ndard an indication of what changes have been 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 AS
15、TM is to be considered the official document.*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 accurately calibrated either by direct reading of a temperature sensor or
16、 by adjusting the programmer temperature to match theactual temperature over the temperature range of interest.6. Apparatus6.1 Thermomechanical Analyzer (TMA), The essential instrumentation required to provide the minimum thermomechanicalanalytical or thermodilatometric capability for this method in
17、cludes:6.1.1 A Rigid Specimen Holder or Platform, of inert, low expansivity material (1 m m-1 K-1) to center the specimen in thefurnace and to fix the specimen to mechanical ground.6.1.2 A Rigid (expansion compression, flexure, tensile, etc.) Probe, of inert, low expansivity material (1 m m-1 K-1) t
18、hatcontacts with the specimen with an applied compressive or tensile force. For this test method, the use of a penetration probe isrecommended.6.1.3 A Sensing Element, linear over a minimum range of 2 mm 2 mm to measure the displacement of the rigid probe to 650nm resulting from changes in the lengt
19、h/height of the specimen.6.1.4 A Weight or Force Transducer, to generate a constant force of 50 6 5 mN (5.0 6 0.5 g) that is applied through the rigidprobe to the specimen.NOTE 3The recommendation of a 5.0 g load (or a force of 50 mN) is based on the use of penetration probes commonly used in the co
20、mmerciallyavailable thermomechanical analyzers. These probes have tip diameters ranging from 0.89 to 2.0 mm and lead to pressures from 80 to 16 kPa when usingthe recommended 5.0 g load. The use of probes which differ greatly from this range of tip diameters may require different loading (or force).6
21、.1.5 A Furnace, capable of providing uniform controlled heating (cooling) at a rate of 1 1C min-1 to 10 6 1C min-1 of aspecimen to a constant temperature within the applicable temperature range of this method.NOTE 4The temperature range of operation of commercial thermomechanical analyzers vary by m
22、anufacturer and mode. The complete range oftemperature of an instrument is sometimes achieved by the use of two different furnaces. In this case, temperature calibration must be carried out for eachfurnace.6.1.6 A Temperature Controller, capable of executing a specific temperature program by operati
23、ng the furnace between selectedtemperature limits at a rate of temperature change of 10 6 1C min-1.6.1.7 A Temperature Sensor, that may be positioned in close proximity to the test specimen to provide an indication of thespecimen/furnace temperature to within 60.1C min-1.6.1.8 Ameans of sustaining a
24、n environment around the specimen with an inert purge gas (for example, nitrogen, helium, argon,etc.) at a purge gas flow rate of 20 20 mL min-1 to 50 mLmin-1.6.1.9 A Data Collection Device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.The minimum
25、output signals required for TMA are a change in linear dimension, temperature, and times.7. Hazards7.1 This test method may involve the use of hazardous materials, operations, and equipment. It is the responsibility of the userof this test method to establish appropriate safety practice and to deter
26、mine the applicability of regulatory limitations prior to use.(WarningToxic or corrosive effluents, or both, may be released when heating some materials and could be harmful to personneland the apparatus.)7.2 Once this calibration procedure has been executed as described in 10.1.2.1 10.1.2.7 of this
27、 test method, the measuringtemperature sensor position should not be changed, nor should it be in contact with the sample or sample holder in a way that wouldimpede movement. If for some reason the temperature sensor position is changed or the temperature sensor is replaced, then theentire calibrati
28、on procedure should be repeated.8. Calibration8.1 For the temperature range covered by many applications, the melting transition of 99.99 % pure materials may be used forcalibration. (See Table 1.)NOTE 5The values in Table 1 were determined using special 99.9999 % pure materials and highly accurate
29、steady-state conditions that are notattainable with this method. The actual precision of this test method is given in Section 13.NOTE 6The melting temperatures of these materials have been selected as primary fixed points (see Table 1) for the International PracticalTemperature Scale of 1990.4NOTE 7
30、Some materials have different crystalline forms (for example, tin) or may react with the container. Such calibration materials should bediscarded after their initial melt.9. Assignment of the Penetration Onset Temperature9.1 The assignment of the TMA penetration onset temperature is an important pro
31、cedure since, when using this method,temperature calibration of the thermomechanical analyzer is directly dependent upon it. The temperature standards given in Table4 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E37-1011. Con
32、tact ASTM CustomerService at serviceastm.org.E1363 1621 will give a downward deflection on the thermal curve, similar to that shown in Fig. 1, when placed under a weighted TMApenetration probe and heated to their respective melting temperatures.9.2 The extrapolated onset temperature for such a penet
33、ration thermal curve is obtained by extending the pretransitionpre-transition portion of the thermal curve to the point of intersection with a line drawn tangent to the steepest portion of the curvewhich describes the probe displacement. The temperature corresponding to this point of intersection is
34、 the penetration onsettemperature. This is shown graphically in Fig. 1. There are some materials (for example, aluminum metal) which showpretransitionpre-transition probe displacement prior to the sharper downward deflection observed on melting. In this case, thepretransitionpre-transition baseline
35、is extended from the point which represents the highest temperature the material reaches priorto exhibiting significant or measurable softening under the conditions of the experiment. Fig. 2 describes the assignment of theextrapolated onset temperature for a specimen which exhibits pretransitionpre-
36、transition penetration.10. Procedure10.1 Two-Point CalibrationFor the purposes of this procedure, it is assumed that the relationship between observedextrapolated onset temperature (To) and actual specimen temperature (Tt) is a linear one governed by the equation:Tt 5To 3S!1I (1)TABLE 1 Recommended
37、Melting Temperature ReferenceMaterialsACalibration MaterialB Melting Temperature(C) (K)Mercury 38.8344 234.3156Water 0.01 273.16Gallium 29.7646 302.9146Indium 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 90
38、3.778Aluminum 660.323 933.473Silver 961.78 1234.93Gold 1064.18 1337.33Copper 1084.62 1357.77Nickel 1455 1728Cobalt 1495 1768A The values in Table 1 were determined using special, 99.9999 % pure materials,and highly accurate steady state steady-state conditions that are not attainable orapplicable to
39、 thermal analysis techniques. The actual precision of this test methodis given in Section 1213.B B. W. Mangnum and G. T. Furukawa, “Guidelines for Realizing the InternationalTemperature Scale of 1990 (ITS-90),” National Institute ofDella Gatta, G.,Richardson, M. J., Sarge, S. M., and Stolen, S., “St
40、andards, Calibration, andGuidelines in Microcalorimetry, Part 2: Calibration Standards for DifferentialScanning Calorimetry,” StandardsPure and Technology TechnicalAppliedChemistry, Note 1265, 1990, p. 8.Vol 78, No. 7, 2006, pp.14551476.FIG. 1 Assignment of the Extrapolated Onset Temperature (To) fr
41、om TMA Thermal CurveE1363 163where S and I are the slope and intercept of a straight line, respectively.10.1.1 Select two calibration reference materials near the temperature range of interest. The standards should be as close to theupper and lower temperature limits used in the actual analysis runs
42、 as is practical.10.1.2 Determine the apparent extrapolated onset temperature for the calibration reference material chosen, using apenetration-type probe with the TMA instrument.10.1.2.1 Place a 1010-mg to 20-mg specimen of one of the calibration reference materialmaterials on the sample platform (
43、orholder, whichever is applicable).NOTE 8The specimen should have a smooth surface on both top and bottom. Avoid the use of specimens with sharp ridges and irregular surfaces.These can lead to false values for the onset temperatures. Powdered or liquid standards may be placed into a stable, inert co
44、ntainer, 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 at a flow rate that is appropriate to the dimensions of the apparatusthroughout the experiment. Typical flow rates are from 2020
45、mLmin to 50 mL/min. The same purge gas and flow rate should bemaintained in both calibration runs and analysesanalysis runs.10.1.2.4 Heat the calibration sample specimen to a temperature about 50C below the calibration temperature and allow theTMA furnace to equilibrate.equilibrate for at least 1 mi
46、n.10.1.2.5 Heat the calibration specimen at 5C/min5 Cmin through the transition allowing the probe to reach a point ofmaximum penetration. (See Fig. 1.)NOTE 9Temperature calibration may be affected by heating rate, purge gas flow rate, and choice of purge gas.NOTE 10Other heating rates may be used b
47、ut shall be reported.10.1.2.6 From the TMAthermal curve obtained, assign the extrapolated onset temperature (see Fig. 1) to the required precision.NOTE 11Retain all available digits.10.1.2.7 Repeat the procedure described in 10.1.2 10.1.2.5 using the second calibration reference material that was ch
48、osen.11. Calculation11.1 Using the reference material temperature values from Table 1 and the corresponding onset temperatures obtainedexperimentally, determine the slope and intercept using the following equations:S 5Ta12Ta2 #/T012T02 # (2)I 5T013Ta2!2Ta13T02!#/T012T02! (3)where:S = slope (nominal
49、value = 1.00),I = intercept,Ta1 = reference transition temperature for Reference Material 1 taken from Table 1,Ta2 = reference transition temperature for Reference Material 2 taken from Table 1,T01 = experimentally observed transition onset temperature for Reference Material 1, andT02 = experimentally observed transition onset temperature for Reference Material 2.(WarningThe slope S is a dimensionless number whose value is independent of which temperature scale is used for I andT.I,T. inIn all cases, I must have the same units as
