1、Designation: E 1953 07Standard Practice forDescription of Thermal Analysis and Rheology Apparatus1This standard is issued under the fixed designation E 1953; 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 (e) 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 ach
3、ieve 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 description contains q
4、uantifiable instrument per-formance requirements to be specified for each test method.1.3 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 and health practices a
5、nd determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 473 Terminology Relating to Thermal Analysis and Rhe-ologyE 1142 Terminology Relating to Thermophysical PropertiesSI 10 Standard for Use of the International System of Units(SI): The M
6、odern Metric System3. Terminology3.1 Technical terms used in this document are found inTerminologies E 473 and E 1142 and Practice SI 10.4. Significance and Use4.1 Section 5 identifies essential instrumentation and acces-sories required to perform thermal analysis or rheometry for avariety of differ
7、ent instruments. The appropriate generic instru-ment description should be included in any test methoddescribing use or application of the thermal analysis orrheometry instrumentation described herein.4.2 Units included in these descriptions are used to identifyneeded performance criteria and are co
8、nsidered typical. Otherunits may be used when including these descriptions in aspecific test method. Items underlined constitute requiredinputs specifically established for each test method (for ex-ample, sensitivity of temperature sensor).4.3 Additional components and accessories may be added asnee
9、ded, with the appropriate performance requirements speci-fied. Items listed in these descriptions but not used in a testmethod (for example, vacuum system) may be deleted.5. Apparatus5.1 Differential Scanning Calorimeter (DSC)The essen-tial instrumentation required to provide the minimum differen-ti
10、al 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 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.
11、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)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
12、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 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 controll
13、er , capable of executing aspecific temperature program by operating the furnace(s)between selected temperature limits at a rate of temperaturechange of _ K/min constant to 6 _ K/min (listcooling requirements separately if different) or at an isothermaltemperature constant to 6 _ K.1This practice is
14、 under the jurisdiction of Committee E37 on Thermal Measure-ments and is the direct responsibility of Subcommittee E37.01 on Thermal TestMethods and Practices.Current edition approved April 1, 2007. Published May 2007. Originallyapproved in 2002. Last previous edition approved in 2005 as E 1953 05.2
15、For 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 Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C
16、700, West Conshohocken, PA 19428-2959, United States.5.1.3 A data collection device, 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, vial
17、s, lids, closures, seals,etc.) that are inert to the specimen and reference materials 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
18、.5.1 Apressure vessel or similar means of sealing the testchamber at any applied 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 tran
19、sducer or similar device to measurethe pressure inside the test chamber to 6_ %, 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 du
20、ring testing.5.1.5.4 A pressure regulator or similar device to adjust theapplied 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 env
21、ironment inthe test chamber or to isolate components of the pressure/vacuum system, 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,
22、 or tosustain an isothermal subambient temperature.5.1.6.2 A balance to weigh specimens 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-strumenta
23、tion required to provide the minimum thermome-chanical analytical or thermodilatometric 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 (expansi
24、on, compression, flexure, tensile, etc.)probe of inert low expansivity material _ 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 ri
25、gid probe without distortion_ or slippage_ for tensile or flexure mode only.5.2.4 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 const
26、antforce of _6 _ or between _ and _6_ that is applied through the rigid _probe to 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 contro
27、ller 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 6 _ K/min list coolingrequirements separately if different or at an isothermal tem-perature constant to 6 _ K.5.2.8 A temperatur
28、e sensor to provide an indication of thespecimen/furnace temperature to 6 _ K.5.2.9 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 moistu
29、reare to be studied, use of dry purge gas is recommended and is essential foroperation 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 i
30、n linear dimension, temperature, and time.5.2.11 Auxiliary instrumentation considered 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
31、.5.2.11.2 Micrometer or other measuring device to determinespecimen dimensions of _ 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 thermogr
32、avi-metric analytical capability for this method includes:5.3.1 A thermobalance composed 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 sens
33、or to provide an indication of thespecimen/furnace temperature to 6 _ K.5.3.1.3 A 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
34、apurge rate of _ L/min 6 _.NOTE 4Excessive purge rates should be avoided as this may intro-duce interferences due to turbulance effects and temperature gradients.5.3.2 A temperature controller capable of executing a spe-cific temperature program by operating the furnace betweenE1953072selected tempe
35、rature limits at a rate of temperature change of_ K/min constant to within 6 _ K/min (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 meas
36、ured or calculatedsignals, or both. The minimum output signals required for TGAare 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 instrumentatio
37、n considered necessary oruseful in conducting this method includes:5.3.5.1 A cooling 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 requ
38、ired to provide the minimum dynamicmechanical analytical capability for this method 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 spe
39、cimen.5.4.2 A coupling shaft, or other means to transmit the forceor displacement 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 dynami
40、c 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 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 ratew
41、ithin the applicable temperature range of the method.5.4.8 A temperature controller, 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 differe
42、nt) or at an isothermal temperature constantto 6_K.5.4.9 A data collection device, 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, tempera-ture, and time.5.4.10 Au
43、xiliary instrumentation considered necessary oruseful in conducting this method includes: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 st
44、orage modu-lus, loss modulus, tangent angle delta, or other useful param-eters derived 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
45、 thespecimen in a periodic manner capable of frequencies ofoscillation from _ to _ rad/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 ge
46、ometry or tool to fix the specimen between thedrive shaft and a stationary position.5.5.4 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 the
47、specimen temperature to 6 _ C.5.5.6 6 A furnace, or heating/cooling element to providecontrolled 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 tempe
48、rature 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 programbetween selected stress or strain limits at a rate of stress orstrain change of _ (units) constant to within 6 _ (units)or at an iso-stress or iso-strain constant to within 6 _(units).5.5.
