1、Designation: E1953 14Standard 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 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. Scope1.1 This practice covers generic descriptions of apparatusused for thermal analysis or rheometry measurements and itspurpose is to achiev
3、e uniformity in description of thermalanalysis, rheometry, and viscometer instrumentation through-out standard test methods. These descriptions are intended tobe used as templates for inclusion in any test method where thethermal analysis instrumentation described herein is cited.1.2 Each descriptio
4、n 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 an
5、y, 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 and
6、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. Signific
7、ance and Use4.1 Section 5 identifies essential instrumentation and acces-sories required to perform thermal analysis, rheometry, orviscometry for a variety of different instruments. The appro-priate generic instrument description should be included in anytest method describing use or application of
8、the thermalanalysis, rheometry, or viscometry instrumentation describedherein.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 const
9、itute requiredinputs specifically 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 testmetho
10、d (for example, vacuum 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 provi
11、de uniform controlled 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
12、a heat flow (power)difference 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
13、concern. Unless effects 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 ra
14、te of temperaturechange 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, 2014. Publis
15、hed March 2014. Originallyapproved in 2002. Last previous edition approved in 2013 as E1953 07 (2013).DOI: 10.1520/E1953-14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, r
16、efer to the standards Document 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 devi
17、ce, to provide a means ofacquiring, 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 mater
18、ials andthat are of suitable 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
19、pressure within the pressure 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_ %,
20、includingany temperature dependence 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
21、pressure in the test chamber 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 syste
22、m, or both.5.1.6 Auxiliary 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 spe
23、cimens or containers (pans,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 thermodilato
24、metric capability for thismethod 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 _
25、 m/(m-K)which contacts the 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
26、 A sensing element linear 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
27、 thespecimen.5.2.6 A furnace 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 furnac
28、e betweenselected temperature 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
29、.9 A means of sustaining an 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 foroper
30、ation at subambient temperatures.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 consid
31、ered necessary oruseful in 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
32、 _ mm 6 _ mm.5.2.11.3 A balance 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 c
33、omposed of:5.3.1.1 A furnace 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
34、 continuously recording balance 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
35、may introduceinterferences due to turbulance effects and temperature gradients.E1953 1425.3.2 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/m
36、in (list coolingrequirements 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
37、 mass, temperature, 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 cooli
38、ng capability to hasten 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 metho
39、d, includes:5.4.1 A 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
40、 from the motor to the 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
41、the specimen.5.4.6 A 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 controll
42、er, capable of executing 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
43、, to provide a means 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 inc
44、ludes:5.4.10.1 A cooling 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
45、from the measure signals.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/
46、s or Hz. This motor 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
47、.4 Either a force sensor 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 providec
48、ontrolled heating or 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
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