1、Designation: E2206 11 (Reapproved 2015)Standard Test Method forForce Calibration of Thermomechanical Analyzers1This standard is issued under the fixed designation E2206; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast 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 describes the calibration or perfor-mance confirmation of the electronically applied force signalfor t
3、hermomechanical analyzers over the range of 0 to 1 N.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 There is no ISO method equivalent to this standard.1.4 This standard does not purport to address all of thesafety conce
4、rns, if 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:2E4 Practices for Force Verification of T
5、esting MachinesE473 Terminology Relating to Thermal Analysis and Rhe-ologyE617 Specification for Laboratory Weights and PrecisionMass StandardsE831 Test Method for Linear Thermal Expansion of SolidMaterials by Thermomechanical AnalysisE1142 Terminology Relating to Thermophysical PropertiesE1363 Test
6、 Method for Temperature Calibration of Thermo-mechanical AnalyzersE2113 Test Method for Length Change Calibration of Ther-momechanical AnalyzersE2161 Terminology Relating to Performance Validation inThermal Analysis and Rheology3. Terminology3.1 The technical terms used in this standard are defined
7、inTerminologies E473, E1142, and E2161 including calibration,conformance, precision, relative standard deviation,repeatability, reproducibility, and thermomechanical analyzer.4. Summary of Test Method4.1 The electronic force signal generated by a thermome-chanical analyzer is compared to that exerte
8、d by gravity on aknown mass. The thermomechanical analyzer may be said tobe in conformance if the performance is within establishedlimits, typically 1 %. Alternatively, the force signal may becalibrated using a two-point calibration method.5. Significance and Use5.1 Most thermomechanical analysis ex
9、periments are car-ried out with some force applied to the test specimen. Thisforce is often created electronically. It may be constant orchanged during the experiment.5.2 This method demonstrates conformance or calibrates theelectronically applied force signal.5.3 This method may be used for researc
10、h and development,quality control, manufacturing or regulatory applications.5.4 Other thermomechanical analyzer calibration functionsinclude temperature by Test Method E1363 and length changeby Test Method E2113.6. Apparatus6.1 Thermomechanical AnalyzerThe essential instrumen-tation required to prov
11、ide a minimum thermomechanical analy-sis or thermodilatometric capability for this method includes:6.1.1 Rigid Specimen Holder, inert, low expansivity mate-rial typically 0.6 m(m K) to center the specimen in thefurnace and to fix the specimen to mechanical ground.NOTE 1Materials of construction with
12、 greater expansivity may beused but shall be reported.6.1.2 Rigid (Expansion or Compression) Probe, inert, lowexpansivity material typically 0.6 m(m K) which con-tacts the specimen with an applied compressive force (see Note1).6.1.3 Sensing Element, linear over a minimum range of2 mm to measure the
13、displacement of the rigid probe to 61mresulting from changes in length of the specimen.6.1.4 Programmable Force Transducer, to generate a con-stant force (61.0 %) of up to 1.0 N that is applied through therigid probe to the specimen.1This test method is under the jurisdiction ofASTM Committee E37 on
14、 ThermalMeasurements and is the direct responsibility of Subcommittee E37.10 onFundamental, Statistical and Mechanical Properties.Current edition approved Oct. 1, 2015. Published October 2015. Originallyapproved in 2002. Last previous edition approved in 2011 as E2206 11. DOI:10.1520/E2206-11R15.2Fo
15、r 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 Harbor Drive, PO Box C700
16、, West Conshohocken, PA 19428-2959. United States1NOTE 2Other force ranges may be used but shall be reported.6.1.5 Furnace, capable of providing uniform controlledheating (cooling) of the specimen to a constant temperature orat a constant rate within the temperature range of 100 to600C.NOTE 3Other t
17、emperature ranges may be used but shall be reported.6.1.6 Temperature Controller, capable of executing a spe-cific temperature program by operating the furnace betweenselected temperature limits at a rate of change of up to10C/min constant to 0.1C/min or at an isothermal tempera-ture constant to 60.
18、5C.NOTE 4Other heating rates may be used but shall be reported.6.1.7 Temperature Sensor, that can be attached to, in contactwith, or reproducibly positioned in close proximity to thespecimen to provide an indication of the specimen temperatureto 60.1C.6.1.8 A means of sustaining an environment aroun
19、d thespecimen of inert purge gas with a purge gas rate of 10 to100 6 5 mLmin.NOTE 5Typically, 99.9+ % pure nitrogen, argon, or helium is em-ployed when oxidation in air is a concern. Unless effects of moisture areto be studied, use of dry purge gas is recommended and is essential foroperation at sub
20、ambient temperatures.6.1.9 Data Collection Device, to provide a means ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required forthermomechanical analysis are a change in linear dimension,temperature, and time.6.2 50 to 100 g 6 0.002 % Class 4
21、 or better mass (traceableto a national reference laboratory) in compliance with Speci-fication E617.7. Calibration7.1 Prepare the thermomechanical analyzer for operationaccording to procedures recommended by the manufacturer ofthe thermomechanical analyzer as described in the OperationsManual.7.2 O
22、ther calibration procedures which may be used, butwhich are not required in this standard include Test MethodsE1363, E831, and E2113.8. Procedure8.1 With no specimen present, lower the probe so that itcontacts the specimen holder. Zero the device so that no force(load) is applied by the probe to the
23、 specimen holder.NOTE 6The means for determining “no load” condition is specific tothe instrument used. The user of this method should check the InstrumentOperations Manual for this information.)8.2 Apply a Class 4 or better (that is, Class 1, 2, 3, or 4)mass standard of 50 to 100 g to the probe. Re
24、cord the(traceable) mass of the standard as M1in g.Apply a counteringforce to the force transducer so that no force is applied by theprobe to the specimen holder. Record this force as F2in mN.NOTE 7Other masses may be used but shall be reported.8.3 Calculate the force calibration constant (S) and co
25、nfor-mity (C) using the equations of Section 9.9. Calculations9.1 For the purpose of this test method, it is assumed that therelationship between observed force (F2) and the actual force(F1) is linear and is governed by Eq 1:F15 F2S (1)where:S = force calibration constant (nominal value of 1.00000).
26、9.2 Calculate the force exerted by the standard mass in airusing Eq 2:F15 Maf (2)where:M = mass of the weight, g,a = standard acceleration due to gravity, (= 9.8065 m s-2),f = correction factor for local values of gravity and airbuoyancy taken from Table 1, dimensionless, andF1= force exerted by the
27、 standard mass, mN.9.3 Calculate the calibration constant (S) using the valuesfrom 8.2 and 9.2 and Eq 2.S 5F1F2(3)TABLE 1 Unit Force Exerted by a Unit Mass in Air at Various LatitudesALatitude,()Elevation Above Sea Level, m (ft)30.5 to 152(100 to 500)152 to 457(500 to 1500)457 to 762(1500 to 2500)76
28、2 to 1067(2500 to 3500)1067 to 1372(3500 to 4500)1372 to 1676(4500 to 5500)20 0.9978 0.9977 0.9976 0.9975 0.9975 0.997425 0.9981 0.9980 0.9979 0.9979 0.9978 0.997730 0.9985 0.9984 0.9983 0.9982 0.9982 0.998135 0.9989 0.9988 0.9987 0.9987 0.9986 0.998540 0.9993 0.9993 0.9992 0.9991 0.9990 0.998945 0.
29、9998 0.9997 0.9996 0.9996 0.9995 0.999450 1.0003 1.0002 1.0001 1.0000 0.9999 0.999955 1.0007 1.0006 1.0005 1.0005 1.0004 1.0003ATaken from Practice E4.E2206 11 (2015)29.4 Calculate the percent conformity (C) of the instrumentforce signal using the value for S from 9.3 and Eq 4.C 5 S 2 1.00000! 3100%
30、 (4)NOTE 8The percent conformity is usually a very small number andexpressing it as a percent may be inconsistent with SI notation. Becauseof common use and its effect on the experiment, however, it is expressedas a percent in this procedure.9.4.1 Conformity may be estimated to one significant figur
31、eusing the following criteria:9.4.1.1 If S lies:(1) Between 0.9999 and 1.0001, the conformity is betterthan 0.01 %,(2) Between 0.9990 and 0.9999, or between 1.001 and1.0010, then conformity is better than 0.1 %,(3) Between 0.9900 and 0.9990 or between 1.0010 and1.0100, then conformity is better than
32、 1 %, and(4) Between 0.9000 and 0.9900 or between 1.0100 and1.100, then conformity is better than 10 %.9.5 Using the determined value for S, Eq 1 may be used tocalculate the true force (F1) from an observed force value (F2).10. Report10.1 Report the following information:10.1.1 A unique identificati
33、on of the thermomechanicalanalyzer included manufacturer and model number,10.1.2 The calibration constant (S), as determined in 9.3,reported to at least five places to the right of the decimal point,10.1.3 Conformity (C) as determined in 9.4, and10.1.4 The specific dated version of this method used.
34、11. Precision and Bias311.1 An interlaboratory test was conducted in 2005 in which13 laboratories participated using four instrument models fromtwo manufacturers.11.2 Precision:11.2.1 Within laboratory variability may be described usingthe repeatability value (r) obtained by multiplying the repeat-a
35、bility relative standard deviation by 2.8. The repeatabilityvalue estimates the 95 % confidence limit. That is, two resultsfrom the same laboratory should be considered suspect (at the95 % confidence level) if they differ by more than the repeat-ability value.11.2.2 The within laboratory repeatabili
36、ty relative standarddeviation for the measurement of slope (S) was found to be0.10 % with 48 degrees of experimental freedom.11.2.3 Between laboratory variability (R) may be describedusing the reproducibility value (R) by multiplying the repro-ducibility relative standard deviation by 2.8. The repro
37、ducibil-ity value estimates the 95 % confidence limit. That is, tworesults from different laboratories should be considered suspect(at the 95 % confidence level) if they differ by more than thereproducibility value.11.2.4 The between laboratory reproducibility relative stan-dard deviation for the me
38、asurement of slope (S) was found tobe 2.8 % with 48 degrees of experimental freedom11.3 BiasThis is a calibration document. Bias is defined inthis standard by the value of percent conformity (C) deter-mined.11.3.1 The mean value of conformance was found to be+0.12 %.NOTE 9This value has no predictiv
39、e qualities. It shall not be used toassess the performance of other instruments.12. Keywords12.1 calibration; conformity; force; thermal analysis; ther-momechanical analysisASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentione
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