ASTM E2510-2007(2013) Standard Test Method for Torque Calibration or Conformance of Rheometers《流变仪的扭矩校准或一致性用标准试验方法》.pdf

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1、Designation: E2510 07 (Reapproved 2013)Standard Test Method forTorque Calibration or Conformance of Rheometers1This standard is issued under the fixed designation E2510; 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 conformance for the torque signal generated by com-mercial o

3、r custom-built rheometers. The specific range of thetest depends upon the torque range of the rheometer.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 standard equivalent to this test method.1.4 This sta

4、ndard 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 and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1

5、ASTM Standards:2E4 Practices for Force Verification of Testing MachinesE473 Terminology Relating to Thermal Analysis and Rhe-ologyE617 Specification for Laboratory Weights and PrecisionMass StandardsE1142 Terminology Relating to Thermophysical Properties3. Terminology3.1 Specific technical terms use

6、d in this test method aredefined in Terminologies E473 and E1142. These terms includeangular frequency, frequency, loss modulus, rheometer, storagemodulus, strain, stress, viscoelasticity, viscometer, viscometry,and viscosity.3.2 Definitions:3.2.1 torque, nforce applied through a moment arm thatprod

7、uces or tends to produce rotation (N m)4. Summary of Test Method4.1 A known force is applied to a rheometer coupling shaftthrough a moment arm to produce a torque. The torque thusapplied is measured and compared to the measured torque. Theratio between indicated and applied torque is used to create

8、acalibration coefficient that may be used in future determina-tions.4.2 The known force generated by suspended precisionmass or masses is transmitted to the rheometer coupling shaftby a line and an appropriate series of pulleys.4.3 Torque is mathematically defined by Eq 1: 5 dFsin (1)where: = torque

9、d = the length of the moment arm (m)F = the applied force (N) = the angle to the moment arm over which the force isapplied ()4.3.1 If the force is applied tangentially at right angles (thatis, = 90) to the moment arm, then sin = 1 and Eq 1 reducesto Eq 2: 5 dF (2)4.4 The moment arm in this test meth

10、od is created byattaching a fixture of known radius to the rheometer couplingshaft in lieu of a geometry, tool or plate. The radius of thefixture is the value of d in Eq 2.4.5 A force is applied to the fixture at a tangent by asuspended mass through a thin wire and a suitable pulleyarrangement (see,

11、 for example, Fig. 1).4.6 For a mass or masses of known value, the applied forceis given by Eq 3:F 5 Mgf (3)where:M = the suspended mass (kg)g = standard acceleration due to gravity (= 9.8065 m s2)f = correction factor for local gravity and air buoyancytaken from Table 1 (dimensionless)1This test me

12、thod is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.08 on Rheol-ogy.Current edition approved March 1, 2013. Published April 2013. Originallyapproved in 2007. Last previous edition approved in 2007 as E2510 07. DOI:10.1520/E2

13、510-07R13.2For 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 Harbor Drive

14、, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Significance and Use5.1 The test method calibrates or demonstrates conformityof the torque signal of a rheometer at ambient temperature.5.2 A calibration factor thus determined may be used toobtain correct torque values.5.3 This test

15、method may be used in research, development,specification acceptance, and quality control or assurance.6. Apparatus6.1 RheometerThe essential instrumentation required pro-viding the minimum rheological analytical capabilities include:6.1.1 Drive Actuator, to apply torque or angular displace-ment to

16、the specimen in a periodic manner capable of frequen-cies of oscillation from 0.001 to 100 rad/s. This actuator mayalso be capable of providing static torque or displacement onthe specimen.6.1.2 Coupling Shaft, or other means to transmit the torqueor displacement from the motor to the specimen.6.1.3

17、 Geometry or Tool, to fix the specimen between thedrive shaft and a stationary position.6.1.4 Sensor, to measure the torque developed by thespecimen, a position sensor to measure the angular displace-ment of 50 nanoradians of the test specimen, or both.FIG. 1 Example of Suspended MassTABLE 1 Unit Fo

18、rce Exerted by a Unit Mass in Air at Various Latitudes and ElevationsAElevation Above Sea Level, m (ft)Latitude, 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)1067 to 1372(3500 to 4500)1372 to 1676(4500 to 5500)20 0.9978 0.9977 0.9976 0.9975 0.9975 0.

19、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 0.9996 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

20、.0004 1.0003ATaken from Practice E4.E2510 07 (2013)26.1.5 Temperature Sensor, to provide an indication of thespecimen temperature to within 60.1C.6.1.6 Furnace, or Heating/Cooling Element, to providecontrolled heating or cooling of a specimen at a constanttemperature or at a constant rate within the

21、 temperature rangeof interest.6.1.7 Temperature Controller, capable of executing a spe-cific temperature program by operating the furnace or heating/cooling element between selected temperature limits constantto within 60.1C.6.1.8 Recording Device, capable of recording and display-ing on the Y-axis

22、any fraction of the measured signal (hereapplied torque) or calculated signal (such as viscosity, storageand loss modulus, etc.) including signal noise using a linear orlogarithmic scale as a function of any fraction of the indepen-dent experimental parameter (such as temperature, time) orcalculated

23、 signals (such as stress or strain) on the X-axisincluding signal noise.6.1.9 Auxiliary instrumentation considered necessary oruseful in conducting this method includes:6.1.9.1 Cooling Capability, to hasten cool down from el-evated temperatures, to provide constant cooling rates, or tosustain an iso

24、thermal sub-ambient temperature.6.1.9.2 Data Analysis Capability, to provide viscosity, stor-age and loss modulus, stress, strain, etc. or other usefulparameters derived from the measured signals.6.1.10 A test fixture of known radius to attach a tangentiallyapplied load to the coupling shaft in lieu

25、 of the geometry, tool,or plate.NOTE 1Test fixtures of appropriate design may be obtained from themanufacture of the rheometry apparatus.6.1.11 Mass or Masses, with a suspending hook, the massvalue for which are known to within 60.1 % (see E617). Thevalue of the required mass or masses depends upon

26、the nominaltorque range of the rheometer and is given by Eq 4:M 5 80 to 90% ofadng!(4)where:a= maximum measuring torque of the rheometerdn= nominal radius of the test fixture (m)6.1.12 Line or Lines, composed of a non-elastic materialsuch as monofilament line of suitable length to connect thecalibra

27、tion mass or masses to the test fixture at its tangent.6.1.13 An arrangement of pulleys over which the line maybe strung so that the force of the suspended mass is transmittedtangentially to the test fixture.NOTE 2The friction of the pulley(s) shall be sufficiently small that itwill not significantl

28、y contribute to the torque measurement.6.1.14 Calipers, or other length-measuring device with arange of up to 10 cm to determine length to within 60.1 m.7. Preparation of Apparatus7.1 Mount the test fixture to the coupling shaft in such a waythat a line or lines connected to a mass or masses transmi

29、ts theforce of the suspended mass or masses tangentially to the testfixture and coupling shaft. An illustrative example is shown inFig. 1.8. Calibration and Standardization8.1 Prepare the apparatus for testing according to themanufacturers recommendation as described in the operationsmanual.9. Proce

30、dure9.1 Measure the distance from the center of the connectingshaft to the edge of the test fixture to within 60.1 mm andrecord this value as d.NOTE 3The value of d is commonly 2.5 cm (= 0.025 m).9.2 With no torque applied to the test fixture, observe thetorque signal and ensure that it is less than

31、 0.1 % of the fullscale torque value.9.3 Select a precision mass the value for which is within themaximum range of the apparatus as defined by Eq 4.9.4 Apply the calibrating torque to the rheometer by con-necting one end of the line to the calibration fixture, over anyneeded pulleys to the suspended

32、 mass or masses. Ensure thatthe mass(es) is (are) free hanging without obstruction and thatthe mass is steady (without swinging from side-to-side).NOTE 4The friction of the pulley(s) shall be sufficiently small that itwill not significantly contribute to the torque measurement.9.5 Measure the applie

33、d torque and record this value as i.9.6 Calculate the calibration constant (S) using Eq 5.9.7 Calculate the percent conformance (C) using Eq 6.10. Calculation or Interpretation of Results10.1 For the purposes of this test method, it is assumed thatthe relationship between the indicated and applied r

34、eferencetorque is linear and governed by the slope (S)ofEq 5:S 5Mgdfi(5)where:S = slope of the torque calibration curve (dimensionless)i= the indicated torque (N m)10.2 The percent conformity (C) (that is, the percent differ-ence between the experimental slope and unity) of the instru-ments torque m

35、easurement is calculated using the value of Sfrom 10.1 and Eq 6:C 5 S 2 1.0000! 3100% (6)11. Report11.1 The report shall include the following information:11.1.1 Details and description of the rheometer includingthe manufacturer and model number.11.1.2 The value of calibration constant (S) determine

36、d insection 9.6 reported to within 60.0001.11.1.3 The conformity value (C) as described in section 9.7reported to at least two significant figures.11.1.4 The specific dated version of this method used.E2510 07 (2013)312. Precision and Bias12.1 Precision of the torque measurement depends upon theprec

37、ision of the moment arm, the mass and the acceleration dueto gravity. Maximum imprecision in the determination of thetorque may be estimated from the imprecisions in the indi-vidual measurements by the following equation:/ 5 d/d!21M/M!21g/g!2#1/2(7)where: = imprecision in the value for torque = torq

38、ued = imprecision in the measurement of the moment arm,mmd = moment arm, mmg = imprecision in the value for acceleration due togravity, m s2g = acceleration due to gravity, m s2M = imprecision in mass value, gM = mass, g12.1.1 Example:if:d = 60.5 mmd =25mmg = 6 0.0026 m s2g =9.8ms2M = 6 0.5 gM = 500

39、 gthen:/ 5 0.5 mm/25 mm!210.5 g/500 g!210.0026 m s22/9.8 m s22!2#1/2or expressed as percent:/ 5 2.0%!210.1%!210.27%!2#1/2562.0%12.2 An interlaboratory study is planned for 20072008 togenerate precision and bias information for this test method.Anyone wishing to participate in this study may contact

40、theE37 Staff Manager at ASTM International Headquarters.12.3 Precision:12.3.1 The intralaboratory repeatability standard deviationfor S for a single instrument was found to be 60.05.12.4 Bias:12.4.1 The measurement of conformance in this test methodis a comparison of the calibration constant S with

41、the theoreti-cal value of 1.000 and is an indicator of bias.12.4.2 Interlaboratory results indicate that the value for C isanticipated to be 65%.13. Keywords13.1 rheometer; calibration; torqueASTM International takes no position respecting the validity of any patent rights asserted in connection wit

42、h any item mentionedin this standard. Users 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 techn

43、ical committee and must be reviewed every five 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 considerati

44、on at a meeting of theresponsible technical 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 Har

45、bor Drive, PO Box C700, West Conshohocken, PA 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/).E2510 07 (2013)4