1、Designation: E1953 07 (Reapproved 2013)Standard Practice forDescription of Thermal Analysis and Rheology Apparatus1This standard is issued under the fixed designation E1953; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、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 practice covers generic descriptions of apparatusused for thermal analysis or rheometry measurements and itspu
3、rpose is to achieve uniformity in description of thermalanalysis and rheometry instrumentation throughout standardtest methods. These descriptions are intended to be used astemplates for inclusion in any test method where the thermalanalysis instrumentation described herein is cited.1.2 Each descrip
4、tion contains quantifiable instrument per-formance requirements to be specified for each test method.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if
5、 any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis a
6、nd Rhe-ologyE1142 Terminology Relating to Thermophysical PropertiesIEEE/ASTM SI 10 Standard for Use of the InternationalSystem of Units (SI): The Modern Metric System3. Terminology3.1 Technical terms used in this document are found inTerminologies E473 and E1142 and Standard IEEE/ASTM SI 10.4. Signi
7、ficance and Use4.1 Section 5 identifies essential instrumentation and acces-sories required to perform thermal analysis or rheometry for avariety of different instruments. The appropriate generic instru-ment description should be included in any test methoddescribing use or application of the therma
8、l analysis orrheometry instrumentation described herein.4.2 Units included in these descriptions are used to identifyneeded performance criteria and are considered typical. Otherunits may be used when including these descriptions in aspecific test method. Items underlined constitute requiredinputs s
9、pecifically established for each test method (forexample, sensitivity of temperature sensor).4.3 Additional components and accessories may be added asneeded, with the appropriate performance requirements speci-fied. Items listed in these descriptions but not used in a testmethod (for example, vacuum
10、 system) may be deleted.5. Apparatus5.1 Differential Scanning Calorimeter (DSC)The essen-tial instrumentation required to provide the minimum differen-tial scanning calorimetric capability for this method includes:5.1.1 DSC Test Chamber composed of:5.1.1.1 A furnace(s) to provide uniform controlled
11、heatingor cooling of a specimen and reference to a constant tempera-ture or at a constant rate within the applicable temperaturerange of this method.5.1.1.2 A temperature sensor to provide an indication of thespecimen temperature to 6 _ K.5.1.1.3 Differential sensors to detect a heat flow (power)dif
12、ference between the specimen and reference with a range of_ mW and a sensitivity of 6 _ W.5.1.1.4 Ameans of sustaining a test chamber environment of_ at a purge rate of mL/min 6 _ mL/min.NOTE 1Typically, _ % pure nitrogen, argon, or helium isemployed when oxidation in air is a concern. Unless effect
13、s of moistureare to be studied, use of dry purge gas is recommended and is essential foroperation at subambient temperatures.5.1.2 A temperature controller, capable of executing aspecific temperature program by operating the furnace(s)between selected temperature limits at a rate of temperaturechang
14、e of _ K/min constant to 6 _ K/min (list1This practice is under the jurisdiction of Committee E37 on Thermal Measure-ments and is the direct responsibility of Subcommittee E37.10 on Fundamental,Statistical and Mechanical Properties.Current edition approved March 1, 2013. Published April 2013. Origin
15、allyapproved in 2002. Last previous edition approved in 2007 as E1953 07. DOI:10.1520/E1953-07R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Docu
16、ment Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1cooling requirements separately if different) or at an isothermaltemperature constant to 6 _ K.5.1.3 A data collection device, to provide a means ofa
17、cquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required for DSCare heat flow, temperature, and time.5.1.4 Containers (pans, crucibles, vials, lids, closures, seals,etc.) that are inert to the specimen and reference materials andthat are of suitab
18、le structural shape and integrity to contain thespecimen and reference in accordance with the specific require-ments of this test method including:5.1.5 Pressure/Vacuum System consisting of:5.1.5.1 Apressure vessel or similar means of sealing the testchamber at any applied pressure within the pressu
19、re limitsrequired for this method.5.1.5.2 A source of pressurized gas or vacuum capable ofsustaining a regulated gas pressure in the test chamber ofbetween _ Pa and _ Pa.5.1.5.3 A pressure transducer or similar device to measurethe pressure inside the test chamber to 6_ %, includingany temperature d
20、ependence of the transducer.NOTE 2The link between test chamber and pressure transducer shouldallow fast pressure equilibration to ensure accurate recording of thepressure above the specimen during testing.5.1.5.4 A pressure regulator or similar device to adjust theapplied pressure in the test chamb
21、er to 6 _ % of thedesired value.5.1.5.5 A ballast or similar means to maintain the appliedpressure in the test chamber constant to 6 _ Pa or 6_ %.5.1.5.6 Valves to control the gas or vacuum environment inthe test chamber or to isolate components of the pressure/vacuum system, or both.5.1.6 Auxiliary
22、 instrumentation considered necessary oruseful for conducting this method includes:5.1.6.1 A cooling capability to hasten cool down fromelevated temperatures, to provide constant cooling rates, or tosustain an isothermal subambient temperature.5.1.6.2 A balance to weigh specimens or containers (pans
23、,crucibles, vials, etc.), or both, to 6 _ mg.5.1.6.3 A means, tool, or device to close, encapsulate, orseal the container of choice.5.2 Thermomechanical Analyzer (TMA)The essential in-strumentation required to provide the minimum thermome-chanical analytical or thermodilatometric capability for this
24、method includes:5.2.1 A rigid specimen holder of inert low expansivitymaterial _ m/(m-K) to center the specimen in thefurnace and to fix the specimen to mechanical ground.5.2.2 A rigid (expansion, compression, flexure, tensile, etc.)probe of inert low expansivity material _ m/(m-K)which contacts the
25、 specimen with an applied compressive ortensile force.5.2.3 Rigid specimen clamps of inert low expansivity ma-terial _ m/(m-K) that grip the specimen between therigid specimen holder and the rigid probe without distortion_ or slippage_ for tensile or flexure mode only.5.2.4 A sensing element linear
26、over a minimum rangeof_ mm to measure the displacement of the rigid _probe to 6 _ m resulting from changes in length/height ofthe specimen.5.2.5 A weight or force transducer to generate a constantforce of _6 _ or between _ and _6_ that is applied through the rigid _probe to thespecimen.5.2.6 A furna
27、ce to provide uniform controlled heating orcooling of a specimen to a constant temperature or at a constantrate within the applicable temperature range of this method.5.2.7 A temperature controller capable of executing a spe-cific temperature program by operating the furnace betweenselected temperat
28、ure limits at a rate of temperature change of_ K/min constant to 6 _ K/min list coolingrequirements separately if different or at an isothermal tem-perature constant to 6 _ K.5.2.8 A temperature sensor to provide an indication of thespecimen/furnace temperature to 6 _ K.5.2.9 A means of sustaining a
29、n environment around thespecimen of _ at a purge rate of _ mL/min 6_.NOTE 3Typically, _ % pure nitrogen, argon, or helium isemployed when oxidation in air is a concern. Unless effects of moistureare to be studied, use of dry purge gas is recommended and is essential foroperation at subambient temper
30、atures.5.2.10 A data collection device, to provide a means ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required forTMA are a change in linear dimension, temperature, and time.5.2.11 Auxiliary instrumentation considered necessary oruseful in
31、 conducting this method includes:5.2.11.1 A cooling capability to hasten cool down fromelevated temperatures, to provide constant cooling rates or tosustain an isothermal subambient temperature.5.2.11.2 Micrometer or other measuring device to determinespecimen dimensions of _ mm 6 _ mm.5.2.11.3 A ba
32、lance with a minimum capacity of _ mg toweigh specimens or clamps, or both, to 6 _ mg.5.3 Thermogravimetric Analyzer (TGA)The essential in-strumentation required to provide the minimum thermogravi-metric analytical capability for this method includes:5.3.1 A thermobalance composed of:5.3.1.1 A furna
33、ce to provide uniform controlled heating orcooling of a specimen to a constant temperature or at a constantrate within the applicable temperature range of this method.5.3.1.2 A temperature sensor to provide an indication of thespecimen/furnace temperature to 6 _ K.5.3.1.3 A continuously recording ba
34、lance to measure thespecimen mass with a minimum capacity of _ mg and asensitivity of 6 _ g.5.3.1.4 A means of maintaining the specimen/containerunder atmospheric control of _ of _ % purity at apurge rate of _ L/min 6 _.NOTE 4Excessive purge rates should be avoided as this may introduceinterferences
35、 due to turbulance effects and temperature gradients.E1953 07 (2013)25.3.2 A temperature controller capable of executing a spe-cific temperature program by operating the furnace betweenselected temperature limits at a rate of temperature change of_ K/min constant to within 6 _ K/min (list coolingreq
36、uirements separately if different) or to an isothermal tem-perature which is maintained constant to 6 _ K .5.3.3 A data collection device, to provide a means ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required for TGAare mass, temperature,
37、 and time.5.3.4 Containers (pans, crucibles, etc.) that are inert to thespecimen and that will remain gravimetrically stable within thetemperature limits of this method.5.3.5 Auxiliary instrumentation considered necessary oruseful in conducting this method includes:5.3.5.1 A cooling capability to ha
38、sten cool down fromelevated temperatures, to provide constant cooling rates, or tosustain an isothermal subambient temperature.5.4 Dynamic Mechanical Analyzer (DMA)- the essentialinstrumentation required to provide the minimum dynamicmechanical analytical capability for this method includes:5.4.1 A
39、drive motor, to apply force or displacement to thespecimen in a periodic manner capable of frequencies from_ to _Hz. This motor may also be capable of providingstatic force or displacement on the specimen.5.4.2 A coupling shaft, or other means to transmit the forceor displacement from the motor to t
40、he specimen.5.4.3 A clamping system(s), to fix the specimen between thedrive shaft and the stationary clamp(s).5.4.4 A position sensor, to measure the changes in positionof the specimen during dynamic motion to 6_m,or5.4.5 A force sensor, to measure the force of _N devel-oped by the specimen.5.4.6 A
41、 temperature sensor, to provide an indication of thespecimen temperature to 6_K.5.4.7 A furnace, to provide controlled heating or cooling ofa specimen at a constant temperature or at a constant ratewithin the applicable temperature range of the method.5.4.8 A temperature controller, capable of execu
42、ting aspecific temperature program by operating the furnace betweenselected temperature limits at a rate of temperature change of_K/min constant to 6_K (list cooling requirementsseparately if different) or at an isothermal temperature constantto 6_K.5.4.9 A data collection device, to provide a means
43、 ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required forDMA are storage modulus, loss modulus, tan delta,temperature, and time.5.4.10 Auxiliary instrumentation considered necessary oruseful in conducting this method includes:5.4.10.1 A coo
44、ling capability, to hasten cool down fromelevated temperatures, to provide constant cooling rates, or tosustain an isothermal subambient temperature.5.4.10.2 Data analysis capability, to provide storagemodulus, loss modulus, tangent angle delta, or other usefulparameters derived from the measure sig
45、nals.5.5 RheometerThe essential instrumentation required pro-viding the minimum rheological analytical capabilities for thismethod include:5.5.1 A drive motor, to apply force or displacement to thespecimen in a periodic manner capable of frequencies ofoscillation from _ to _ rad/s or Hz. This motor
46、may alsobe capable of providing static force or displacement on thespecimen.5.5.2 A coupling shaft, or other means to transmit the forceor displacement from the motor to the specimen.5.5.3 A geometry or tool to fix the specimen between thedrive shaft and a stationary position.5.5.4 Either a force se
47、nsor to measure the force of _ Ndeveloped by the specimen or a position sensor to measure thedisplacement of _ nm of the test specimen.5.5.5 A temperature sensor to provide an indication of thespecimen temperature to 6 _ C.5.5.6 6 A furnace, or heating/cooling element to providecontrolled heating or
48、 cooling of a specimen at a constanttemperature or at a constant rate within the applicable tempera-ture range of the method.5.5.7 A temperature controller, capable of executing aspecific temperature program by operating the furnace orheating/cooling element between selected temperature limits ata rate of temperature change of _ C/min constant to 6_C/min (list cooling requirements separate if different) or atan isothermal temperature constant to 6 _ C.5.5.8 A stress or strain controller, capable of executing aspecific unidirectional or oscillatory stress or strain programbe
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