1、Designation: E2206 11Standard 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 last revision. A nu
2、mber 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 thermomechanical an
3、alyzers 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 concerns, if any, assoc
4、iated 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 Testing MachinesE47
5、3 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 Method for Temper
6、ature Calibration of Ther-momechanical AnalyzersE2113 Test Method for Length Change Calibration ofThermomechanical AnalyzersE2161 Terminology Relating to Performance Validation inThermal Analysis3. Terminology3.1 The technical terms used in this standard are defined inTerminologies E473, E1142, and
7、E2161 including calibration,conformance, precision, relative standard deviation, repeat-ability, reproducibility, and thermomechanical analyzer.4. Summary of Test Method4.1 The electronic force signal generated by a thermome-chanical analyzer is compared to that exerted by gravity on aknown mass. Th
8、e 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 experiments are car-ried out with
9、 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 research and development,quality contr
10、ol, 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 provide a minimum thermomechanical
11、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 greater expansivity may beuse
12、d 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).1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the dir
13、ect responsibility of Subcommittee E37.10 on Funda-mental, Statistical and Mechanical Properties.Current edition approved Aug. 1, 2011. Published August 2011. Originallyapproved in 2002. Last previous edition approved in 2006 as E2206 06. DOI:10.1520/E2206-11.2For referenced ASTM standards, visit th
14、e 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 C700, West Conshohocken, PA 19428-2959,
15、United States.6.1.3 Sensing Element, linear over a minimum range of2 mm to measure the 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 pr
16、obe to the specimen.NOTE 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 to600 C.NOTE 3Other temperature ranges may be used
17、 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 to10 C/min constant to 0.1 C/min or at an isothermal tempera-ture constant to 60.5 C.NOTE 4Other heating rat
18、es 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 60.1 C.6.1.8 A means of sustaining an environment around thespecimen of inert pu
19、rge gas with a purge gas rate of 10 to100 6 5 mL/min.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 subambient temperatures.6.1
20、.9 Data Collection Device, to provide a means of acquir-ing, storing, and displaying measured or calculated signals, orboth. The minimum output signals required for thermome-chanical analysis are a change in linear dimension, tempera-ture, and time.6.2 50 to 100 g 6 0.002 % Class 4 or better mass (t
21、raceableto 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 Other calibration p
22、rocedures 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 specimen holder.N
23、OTE 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) massstandard of 50 to 100 g to the probe. Record the (traceable
24、)mass of the standard as M1in g.Apply a countering force to theforce transducer so that no force is applied by the probe to thespecimen 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 confor-mity (C) using
25、 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 F2 S (1)where:S = force calibration constant (nominal value of 1.00000).9.2 Calculate the
26、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 standard mass, mN
27、.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)762 to 1067(2500 to
28、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 0.9998 0.9997 0.9996
29、 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 1129.4 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! 3 100 % (4)NOTE 8The percent c
30、onformity 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 figureusing the following cr
31、iteria: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 1 %, and(4) Between 0.
32、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 identification of the thermomechani
33、calanalyzer 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.11. Precision and Bias3
34、11.1 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-ability relative standar
35、d 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 repeatability relative standarddev
36、iation 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 reproducibil-ity value estim
37、ates 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 measurement of slope (S)
38、was found tobe 2.8 % with 48 degrees of experimental freedom11.3 BiasThis is a calibration document. Bias is definedin this standard by the value of percent conformity (C)determined.11.3.1 The mean value of conformance was found to be+0.12 %.NOTE 9This value has no predictive qualities. It shall not
39、 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 mentionedin this standard. Users
40、of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every fi
41、ve years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical
42、committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
43、A 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:E37-1035.E2206 113
