ASTM E2918-2018a Standard Test Method for Performance Validation of Thermomechanical Analyzers.pdf
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1、Designation: E2918 18aStandard Test Method forPerformance Validation of Thermomechanical Analyzers1This standard is issued under the fixed designation E2918; 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 test method provides procedures for validatingtemperature and length change measurements of thermome-chanical analyzers (TMA)
3、and analytical methods based uponthe measurement of temperature and length change. Perfor-mance parameters include temperature repeatability, linearity,and bias; and dimension change repeatability, detection limit,quantitation limit, linearity, and bias.1.2 Validation of apparatus performance and an
4、alyticalmethods is a necessary requirement for quality initiatives.Results may also be used for legal purposes.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 co
5、ncerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance wit
6、h internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards
7、:2E473 Terminology Relating to Thermal Analysis and Rhe-ologyE1142 Terminology Relating to Thermophysical PropertiesE1363 Test Method for Temperature Calibration of Thermo-mechanical AnalyzersE1970 Practice for Statistical Treatment of ThermoanalyticalDataE2113 Test Method for Length Change Calibrat
8、ion of Ther-momechanical AnalyzersE2161 Terminology Relating to Performance Validation inThermal Analysis and Rheology3. Terminology3.1 Technical terms used in this test method are defined inTerminologies E473, E1142, and E2161, including termsanalyte, bow, Celsius, coeffcient of linear thermal expa
9、nsion,detection limit, linearity, quantification limit, relative standarddeviation, repeatability, standard deviation,thermodilatometry, thermomechanical analysis, and valida-tion.4. Summary of Test Method4.1 Temperature and time are the primary independentparameters and length change is the primary
10、 dependent experi-mental parameters provided by thermomechanical analysis.4.2 Temperature, a measured value, is validated by perform-ing a measurement of the penetration in sharply meltingmaterials at three (or more) different known melting tempera-tures.4.3 Length change, a measured value, is valid
11、ated byperforming a measurement of the linear thermal expansion forthree (or more) test materials.4.4 Validation of a thermomechanical test method basedupon length change may be performed using the test specimenas the analyte.4.5 The length change of three (or more) specimens (nomi-nally representin
12、g the maximum, midpoint and minimum ofthe range of the test method) are measured in triplicate (ormore). A fourth blank specimen, containing no analyte, ismeasured in triplicate (or more).NOTE 1Repeatability is determined by performing a sufficient numberof determinations to calculate valid estimate
13、s of the standard deviation orrelative standard deviation of the measurement.4.5.1 Temperature and length change measurement linearityand bias are determined from the linear regression correlationof the results from measurements of the three (or more)specimens.1This test method is under the jurisdic
14、tion ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.10 onFundamental, Statistical and Mechanical Properties.Current edition approved Dec. 1, 2018. Published January 2019. Originallyapproved in 2013. Last previous edition approved in 2018 as E2918 18.
15、 DOI:10.1520/E2918-18A.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 Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr
16、 Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recomme
17、ndations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14.5.2 Length change detection limit and quantitation limitare determined from the standard deviation of the blankdetermination with no analyte present.4.5.3 Temperature and length change repeatability are de
18、-termined from the repeatability measurements of three (ormore) specimens.4.5.4 Length change validation is independent of the tem-perature validation. The respective validations need not in-volve consistent ranges.5. Significance and Use5.1 This test method may be used to determine and validatethe
19、performance of a particular thermomechanical analyzerapparatus.5.2 This test method may be used to determine and validatethe performance of a particular method based upon thermome-chanical analyzer temperature or length change measurements.5.3 This test method may be used to determine the repeat-abi
20、lity of a particular apparatus, operator, or laboratory.5.4 This test method may be used for specification andregulatory compliance purposes.6. Apparatus6.1 Thermomechanical Analyzer (TMA)The essential in-strumentation required to provide the minimum thermome-chanical analytical or thermodilatometri
21、c capability for this testmethod include:6.1.1 A rigid specimen holder of an inert, low expansivitymaterial ( 0.6 m/m C) to center the specimen in a furnaceand to fix the specimen to mechanical ground.NOTE 2Apparatus capable of higher temperature operation may beconstructed of materials with greater
22、 expansivity. Additionally, a correc-tion for expansion of the material of construction is included in dimen-sional change measurements.6.1.2 A rigid expansion probe of inert low expansivitymaterial (0.6 m/m K) that contacts the specimen with anapplied compressive force (see Note 2). The circular ar
23、ea incontact with the test specimen shall have a diameter between0.5 mm and 1.1 mm.NOTE 3Expansion probes of other diameters may be used but shall bereported.6.1.3 A sensing element, linear over a minimum range of 2mm, to measure the displacement of the rigid expansion probewith a minimum resolution
24、 of 650 nm due to resultant changesin length of the specimen.6.1.4 A force transducer or weight to generate a constantforce of 1.0 mN to 100 mN (0.1 g to 10 g) 6 2.5 % that isapplied through the rigid expansion probe to the specimen.6.1.5 A furnace to provide uniform and controlled heatingor cooling
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