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    ASTM E1824-2018 Standard Test Method for Assignment of a Glass Transition Temperature Using Thermomechanical Analysis Tension Method.pdf

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    ASTM E1824-2018 Standard Test Method for Assignment of a Glass Transition Temperature Using Thermomechanical Analysis Tension Method.pdf

    1、Designation: E1824 13E1824 18Standard Test Method forAssignment of a Glass Transition Temperature UsingThermomechanical Analysis: Tension Method1This standard is issued under the fixed designation E1824; the number immediately following the designation indicates the year oforiginal adoption or, in t

    2、he case of revision, the year of 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 coversdescribes a procedure for the assignment of a glass transition

    3、 temperature (Tg) of materials onheating using thermomechanical measurements in tension.1.2 This test method may be used as a complement to Test Method E1545 and is applicable to amorphous or to partiallycrystalline materials in the form of films, fibers, wires, etc., that are sufficiently rigid to

    4、inhibit extension during loading at ambienttemperature.1.3 The generally applicable temperature range for this test method is 100 C to 600C. 600 C. This temperature range maybe altered depending upon the instrumentation used.1.4 The values stated in SI units are to be regarded as standard. No other

    5、units of measurement are included in this standard.1.5 There is no ISO method equivalent to this standard.1.5 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 establish appropriate safety sa

    6、fety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development

    7、 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 Analysis and RheologyE1142 Terminology Relating to Thermophysical PropertiesE1545

    8、Test Method for Assignment of the Glass Transition Temperature by Thermomechanical AnalysisE2602 Test Methods for the Assignment of the Glass Transition Temperature by Modulated Temperature Differential ScanningCalorimetry3. Terminology3.1 Definitions:3.1.1 The following terms are applicable to this

    9、 test method and can be found in Terminology E473 and Terminology E1142:thermomechanical analysis (TMA), thermodilatometry, glass transition, and glass transition temperature.4. Summary of Test Method4.1 This test method uses thermomechanical analysis equipment (thermomechanical analyzer, dilatomete

    10、r, or similar device)with the test specimen in tension to determine the change in dimension of a thin specimen observed when the material is subjectedto a constant heating rate through the glass transition region. This change in dimension associated with the change from vitreoussolid to amorphous li

    11、quid is observed as movement of a sensing probe in direct contact with the specimen and is recorded as a1 This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,Statistical and Mechanical Propert

    12、ies.Current edition approved Aug. 1, 2013Aug. 1, 2018. Published August 2013August 2018. Originally approved in 1996. Last previous edition approved in 20092013 asE1824 09E1824 13.1. DOI: 10.1520/E1824-13.10.1520/E1824-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contac

    13、tASTM 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 been

    14、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 document.C

    15、opyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1function of temperature. The intersection of the extrapolation of the slope of the probe displacement curve before and after thetransition is used to determine a temperature that is assig

    16、ned as the glass transition temperature.5. Significance and Use5.1 The glass transition is dependent on the thermal history, softening agents or additives of the material to be tested. Foramorphous and semicrystalline materials the assignment of a glass transition temperature may lead to important i

    17、nformation aboutthermal history, processing conditions, stability, progress of chemical reactions, and mechanical and electrical behavior.5.2 Thermomechanical analysis provides a rapid means of detecting changes in hardness or linear dimensional changeassociated with the glass transition. Dimensiona

    18、l changes measured as a specimen is heated over the glass transition region mayinclude the interaction of several effects: an increase in the coefficient of expansion, a decrease in the modulus, which under aconstant stress leads to increased extension, stress relief leading to irreversible dimensio

    19、nal change (shrinkage in one dimension,expansion in another dimension), and physical aging effects which change the kinetics of the dimensional change.5.3 This test method is useful for research and development, quality control, and specification acceptance testing; particularlyof films and fibers.6

    20、. Interferences6.1 This test method may be used for materials having a glass transition at or below ambient temperature providing care is takento avoid exposing the specimen to a tensile force prior to cooling the specimen below its glass transition. Applying a tensile loadon a specimen that is abov

    21、e its glass transition will result in elongation of the specimen which may introduce orientation andresidual stresses that will alter the specimen thermal history and may yield erroneous results during the heating cycle.6.2 Specimens of thickness less than 0.2 mm may be difficult to handle.6.3 Speci

    22、mens of thickness greater than 5 mm may develop temperature nonuniformities of sufficient extent as to yielderroneously high values for an assigned glass transition temperature using this test method.7. Apparatus7.1 The essential equipment required to provide the minimum instrument capability for th

    23、is test method includes:7.1.1 A Thermomechanical Analyzer (TMA) or Thermodilatometer, consisting of:7.1.1.1 Rigid Specimen Holder, of inert, low expansivity material (20 mm-C), usually quartz, to center the specimen in thefurnace and to fix the specimen to mechanical ground.NOTE 1Use of rigid specim

    24、en holders and tension probes constructed of lower thermal expansivity (20 m m-C) materials or corrections forhardware expansivity may be necessary if very small changes in specimen dimensions are encountered with this test method.7.1.1.2 Rigid Tension Probe, of inert, low expansivity material ( 5 m

    25、m-C), usually quartz, which contacts the specimen withan applied in-plane tensile force.7.1.1.3 Sensing Element, with a dynamic range of at least 5 mm, a linearity of 1 % or better, and sufficient sensitivity to measurethe displacement of the rigid tension probe within 61 m resulting from changes in

    26、 length of the specimen.7.1.1.4 Weight or Force Transducer, to generate a constant force between 0 mN and 50 m50 mN 6 2 %N 6 2 % that is appliedthrough the rigid tension probe to the specimen.7.1.1.5 Furnace and Temperature Controller, capable of executing a temperature program of uniform controlled

    27、 heating of aspecimen at a constant rate of 5 6 0.2C5min C/min 6 0.2 C/min between required temperature limits to 60.5C.60.5 C.7.1.1.6 Temperature Sensor, that can be positioned reproducibly in close proximity to the specimen to measure its temperaturebetween 100 and 600C C and 600 C readable with a

    28、 resolution of 60.1C.60.1 C.7.1.1.7 Means of Providing a Specimen Environment, of an inert gas at a purge rate of 10 mL/min to 50 mLmin 6 5 %. Thetypical purge gas rate is usually given by the instrument manufacturer.NOTE 2Typically 99.99 % pure nitrogen, argon, or helium is employed when oxidation

    29、in air is a concern. Unless effects of moisture are to be studied,use of dry purge gas is recommended; especially for operation at subambient temperatures. Calibration shall be performed using the same purge gas tobe used with test specimens.7.1.1.8 Data Collection Device, provide a means of acquiri

    30、ng, storing, and displaying measured or calculated signals, or both.The minimum output signals required for thermomechanical analysis are dimension change, temperature and time.7.1.2 Rigid Specimen Clamps, (clamps, grips, pins, or split shot) of inert, low expansivity material ( 20 mm-C) that grip t

    31、hespecimen between the rigid specimen holder and the rigid tension probe without distortion (1 %) or slippage (1 %).7.2 Auxiliary equipment considered useful in conducting this test method includes:7.2.1 Coolant System, that can be coupled directly to the furnace/temperature controller to hasten rec

    32、overy from elevatedtemperatures, to provide controlled cooling rates constant to 61.0C/min, 61.0 C/min, and to sustain a subambient temperatureto 60.5C.60.5 C.7.2.2 Calipers, or other measuring device to determine specimen dimensions to 60.01 mm.7.2.3 Balance, to determine the specimen mass to 60.1

    33、mg.E1824 1828. Sampling8.1 Analyze samples as received or after a prescribed pretreatment. If some treatment is applied to a specimen prior to analysis,note this treatment and any resulting changes in mass or appearance in the report. For samples with a glass transition belowambient, it may be desir

    34、able to form the glass with a known thermal history by using a controlled constant cooling rate to thestarting temperature. Film samples may undergo stress relief related dimensional change that depends on whether the sample isprepared and measured parallel to the machine direction of manufacture or

    35、 perpendicular to the machine direction.9. Calibration9.1 Perform temperature calibration in accordance with the apparatus manufacturer operators manual using the same heatingrate, purge, and temperature sensor position to be used with the test method.10. Procedure10.1 Attach a pair of rigid specime

    36、n clamps to a specimen with a minimum spacing of 5 mm between the contact points. Weighthe specimen and clamps and record this value.NOTE 3Use of between-clamp distances of less than 5 mm may impart erroneous results because of end effects introduced by the clamp pressure.Refer to the Precautions Se

    37、ction, if a thickness outside the range of 0.2 mm to 5 mm is to be used.10.2 Suspend the specimen with clamps between the contact points of the specimen holder and the tension probe. BE SURETHE POSITION OF THE TEMPERATURE SENSOR IS UNCHANGED FROM THAT USED IN THE CALIBRATIONPROCEDURE.10.3 Move the f

    38、urnace to enclose the specimen and clamps. Start the inert gas purge and equilibrate the specimen and clampsat the desired starting temperature.NOTE 4Cool or heat the specimen, clamps and furnace to a temperature equivalent to at least 3 min of heating below the first temperature of interestto ensur

    39、e stable heater control; for example, 15C 15 C for a 5C/min 5 C/min rate. The coolant used to lower the temperature should not come incontact with the specimen or clamps.10.4 Apply a constant tensile force to the specimen in the range of either 5 mN to 10 m10 mNN (to observe shrinkage) or of20 mN to

    40、 50 m50 mNN (to observe elongation).NOTE 5The observed inflection temperature will be dependent upon the applied stress. Therefore, the applied force should be adjusted for specimencross-section area to ensure the same stress level is applied to all specimens.10.5 Heat the specimen and clamps at a c

    41、onstant rate of 5C/min 5 C/min over the desired temperature range.NOTE 6Other forces and heating rates may be used if applied both in the calibration and throughout the testing. The test conditions shall be notedin the report.FIG. 1 Determination of TgE1824 18310.6 Note the occurrence of an abrupt c

    42、hange in slope (positive for shrinkageelongation and negative for elongation)shrinkage)of the length versus temperature curve that indicates a transition of the material from one state to another.10.7 Upon reaching the upper temperature limit of the heating program, remove the applied tensile force

    43、and restore the furnace,specimen, and clamps to ambient temperature.10.8 Reweigh the specimen and clamps reporting any change in mass.NOTE 7Weighing of the specimen and clamps is required to determine whether changes such as loss of solvent or plasticizer which may alter theassigned glass transition

    44、 temperature have occurred.11. Calculation11.1 Derive a glass transition temperature as follows using graphics or software:11.1.1 Construct a tangent to the lower temperature portion of the thermal curve,11.1.2 Construct a tangent to the steepest portion of the slope beyond the transition, and11.1.3

    45、 The temperature at which these tangents intersect is the derived glass transition temperature, Tg.11.2 Apply any temperature correction determined from the instrument temperature calibration to Tg to obtain the assignedglass transition temperature, Tg. (See Fig. 1.) Note, there are three cases illu

    46、strated, namely, a sample that exhibits shrinkage (overthe Tg region under the conditions utilized), a sample that exhibits elongational reorientation, and a sample with no apparentstress-relied induced dimensional change. Because Tg is an assigned parameter its value may depend on experimental cond

    47、itions,namely on the applied stress on the sample, and in the case of a film, the direction of the applied stress relative to the vector ofthe stress relief.12. Report12.1 Report the following information:12.1.1 Acomplete identification and description of the material tested including specimen dimen

    48、sions, clamp distance, and anypretreatment,12.1.2 Description of the instrument used for the test including tensile force,12.1.3 Test conditions including temperature program executed, purge gas composition and flow rate, and cooling medium ifused,12.1.4 Description of the temperature calibration pr

    49、ocedure,12.1.5 The thermomechanical analysis curves,12.1.6 The assigned glass transition temperature, Tg, and12.1.7 Any change in mass associated with the test.13. Precision and Bias313.1 An interlaboratory test was conducted in 2007 on a polystyrene film. Ten laboratories participated in the test using twoinstrument models from a single manufacturer.13.2 Precision:13.2.1 Within laboratory variability may be describe using the repeatability value (r) obtained by multiplying the repeatabilitystandard deviation by 2.8. The r


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