1、Designation: E 2206 06Standard Test Method forForce Calibration Of Thermomechnical Analyzers1This standard is issued under the fixed designation E 2206; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A n
2、umber 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 test method describes the calibration or perfor-mance confirmation of the electronically applied force signalfor thermomechanical
3、analyzers over the range of 0 to 1 N.1.2 SI units are the standard.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, associated with its use. It is theresponsibility of the user of this standard to establish appro-
4、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 MachinesE 473 Terminology Relating to Thermal Analysis and Rhe-ologyE 617 Specification for Laboratory
5、Weights and PrecisionMass StandardsE 831 Test Method for Linear Thermal Expansion of SolidMaterials by Thermomechanical AnalysisE 1142 Terminology Relating to Thermophysical PropertiesE 1363 Test Method for Temperature Calibration of Ther-momechanical AnalyzersE2113 Test Method for Length Change Cal
6、ibration ofThermomechanical Analyzers3. Terminology3.1 The technical terms used in this standard are defined inTerminologies E 473 and E 1142.4. 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. The
7、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 s
8、ome 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 control
9、, manufacturing or regulatory applications.5.4 Other thermomechanical analyzer calibration functionsinclude temperature by Test Method E 1363 and length changeby Test Method E2113.6. Apparatus6.1 Thermomechanical AnalyzerThe essential instrumen-tation required to provide a minimum thermomechanical a
10、naly-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 beused
11、 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 displacement of the rigid prob
12、e to 6 1mresulting from changes in length of the specimen.6.1.4 Programmable Force Transducer, to generate a con-stant force (6 1.0 %) of up to 1.0 N that is applied through therigid probe to the specimen.NOTE 2Other force ranges may be used but shall be reported.6.1.5 Furnace, capable of providing
13、uniform controlledheating (cooling) of the specimen to a constant temperature orat a constant rate within the temperature range of 100 to 600C.1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.01 on ThermalTes
14、t Methods and Practices.Current edition approved March 1, 2006. Published April 2006. Originallyapproved in 2002. Last previous edition approved in 2002 as E 2206 02.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual B
15、ook 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, United States.NOTE 3Other temperature ranges may be used but shall be reported.6.1.6 Temperatu
16、re Controller, capable of executing a spe-cific temperature program by operating the furnace betweenselected temperature limits at a rate of change of up to 10C/min constant to 0.1 C/min or at an isothermal temperatureconstant to 6 0.5 C.NOTE 4Other heating rates may be used but shall be reported.6.
17、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 6 0.1 C.6.1.8 A means of sustaining an environment around thespecimen of inert purge gas with a purge gas rate of 10 to
18、 1006 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.6.1.9 Recording Device, capable of record
19、ing and display-ing any fraction of the specimen dimension (TMA curve) orforce, including signal noise, on the Y-axis as a function oftemperature or time, including signal noise, on the X-axis.6.2 50 to 100 g 6 0.002 % Class 4 or better mass (traceableto a national reference laboratory) in complianc
20、e with Speci-fication E 617.7. 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 procedures which may be used, butwhich are not required
21、in this standard include Test MethodsE 1363, E 831 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.NOTE 6The means for determining “no load” condition is
22、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)mass of the standard as M1in g.Apply a countering for
23、ce 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 the equations of Section 9.9. Calculations9.1 For the
24、 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 force exerted by the standard mass in airusing Eq 2:F1
25、5 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.9.3 Calculate the calibration constant (S) using the
26、valuesfrom 8.2 and 9.2 and Eq 2.S 5F1F2(3)9.4 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 conformity is usually a very small number andexpressing it as a percent may be inconsistent with SI n
27、otation. 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 criteria:9.4.1.1 If S lies:(1) Between 0.9999 and 1.0001, the conformity is betterthan 0.01 %,(2) Betw
28、een 0.9990 and 0.9999, or between 1.001 and1.0010, then conformity is better than 0.1 %,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 3500)1
29、067 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 0.999
30、6 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.E2206062(3) Between 0.9900 and 0.9990 or between 1.0010 and1.0100, then conformity is better than 1 %, and(4) Between 0.9000 and 0.9900 or between 1.0100 and1.100, then conf
31、ormity 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 thermomechanicalanalyzer included manufacturer and model number,10
32、.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 Bias311.1 An interlaboratory test was conducted in 2005 in
33、 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 standard deviation by 2.8. The repeatabilityvalue estimates
34、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 standarddeviation for the measurement of slope (S) was found to
35、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 estimates the 95 % confidence limit. That is, tworesults f
36、rom 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) was found tobe 2.8 % with 48 degrees of experimental
37、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 be used toassess the performance of other instrument
38、s.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 of this standard are expressly advised that determina
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