1、Designation: E2509 08E2509 14Standard Test Method forTemperature Calibration of Rheometers in Isothermal Mode1This standard is issued under the fixed designation E2509; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st 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 temperature calibration or conformance of rheometers. The applicable temperature range is
3、0 to 80C however other ranges may be selected for the purpose at hand.1.2 The values stated in SI units are the standard. to be regarded as standard. No other units of measurement are included inthis standard.1.3 There are no ISO equivalents to this standard.1.4 This standard does not purport to add
4、ress all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E473 Terminolog
5、y Relating to Thermal Analysis and RheologyE1142 Terminology Relating to Thermophysical Properties3. Terminology3.1 DefinitionsSpecific technical terms found in this standard are defined in Terminologies E473 and E1142, includingrheometer and rheometryrheometry.4. Summary of Test Method4.1 An electr
6、onic thermometer of known characteristics is placed in the center of a dummy test specimen in contact with thetorque applying instrument plates of a rheometer at constant (isothermal) temperature. The difference between the rheometer settemperature and that indicated by the thermometer is used to ca
7、librate the rheometer temperature signal.5. Significance and Use5.1 Rheological properties such as viscosity and storage and loss modulus change rapidly with temperature. High qualitydeterminations of these properties depend upon a stable and well-known temperature of the measuring apparatus.6. Inte
8、rferences6.1 In many rheological experiments, temperature is varied with time. The calibration in this test method is made under stableand isothermal temperature conditions. Thus the effects of changes in temperature with time are not addressed. This isothermalcalibration does not provide any inform
9、ation about the specimen under temperature scanning conditions.7. Apparatus7.1 An Electronic Thermometerelectronic thermometer that includes:7.1.1 Temperature Sensor,sensor, (such as a thermocouple, platinum resistance thermometer, thermistor, etc.) with an accuracy(traceable to a known absolute sta
10、ndard) and resolution of 60.1C and a range of 0 to 80C.1 This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.08 on Rheology.Current edition approved Feb. 1, 2008Aug. 1, 2014. Published April 2008August 2014. Or
11、iginally approved in 2008. Last previous edition approved in 2008 as E2509 08.DOI: 10.1520/E2509-08.10.1520/E2509-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to
12、the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes
13、accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United
14、 States1NOTE 1Sensors with other temperature ranges may be used at the operators convenience.NOTE 2Some sensors are available already affixed with dummy test specimens from section 7.27.1.2 Temperature indicator, to convert the signal presented by the temperature sensor into a digital electronic tem
15、peraturedisplay with the accuracy and precision indicated in section 7.1.1.7.2 Dummy Test Specimen,test specimen, Two two polymer sheets each 1mm 1 mm in thickness of such a diameter to fill thespace (i.e. (that is, gap) between the instrument plates.NOTE 3The dummy test specimen may be composed of
16、the material to be tested or some other representative polymer material. Polydimethylsiloxane(PDMS) (e.g. (for example, “Silly Putty”3) may be used for this purpose.NOTE 4Polydimethylsiloxane may leave a residue of silicone oil on the surfaces of the instrument plates. This oil should be removed pri
17、or tosubsequent use.7.3 Rheometer, Thethe essential instrumentation required providing the minimum rheological analytical capabilities for this testmethod include:7.3.1 A drive actuator, to apply torque or displacement to the specimen in a periodic manner capable of frequencies ofoscillation from 0.
18、01 to 10 rad/s (0.0016 to 1.6 Hz). This actuator may also be capable of providing static force or transient stepor displacement of the test specimen.7.3.2 A coupling shaft, or other means to transmit the torque or displacement from the actuator to the specimen.7.3.3 A geometry, tools or plates, to f
19、ix the specimen between the coupling shaft and a stationary position. For the purposes ofthis test, parallel plates are the preferred configuration7.3.4 Either a torque sensor, to measure force developed by the specimen or a position sensor to measure the angulardisplacement , either one being capab
20、le of measuring within limits appropriate to the specimen and test being performed.7.3.5 A temperature sensor, to provide an indication of the specimen temperature readable to within 6 0.1 C.60.1C.7.3.6 A furnace or heating/cooling element, to provide controlled heating or cooling of a specimen to a
21、 constant temperatureconstant to within +/- 0.1 C 60.1C over the temperature range of interest.7.3.7 Atemperature controller, capable of executing a specific temperature program by operating the furnace or heating/coolingelement between selected temperature limits constant to within 60.1C.7.3.8 A st
22、ress or stain controller, capable of executing a specific unidirectional or oscillatory stress or strain program betweenselected stress or strain limits capable of controlling within limits appropriate to the specimen and test being performed.7.3.9 A recording data collecting device, capable of reco
23、rding all signals and displaying on the Y-axis any subset of themeasured signal (such as to provide a means of acquiring, storing, and displaying measured or calculated signals, or both. Theminimum output signals required include applied force, position or frequency)frequency or calculated signal (s
24、uch as viscosity,storage modulus, loss modulus, or tangent delta) using a linear or logarithmic scale as a function of any subset of and theindependent experimental parameterparameters (such as temperature, time, stress, strain, or frequency of oscillation.) on theX-axis. oscillation).7.3.10 Auxilia
25、ry instrumentation considered necessary or useful in conducting this test method includes:7.3.10.1 A cooling capability to hasten cool down from elevated temperatures, to provide constant cooling rates, or to sustainan isothermal subambient temperature.7.3.10.2 Data analysis capability, to provide d
26、etermined signals (such as viscosity, storage, or loss modulus) or other usefulparameters derived from the measured signals.8. Preparation of Apparatus8.1 Turn on the rheometer and allow it to equilibrate for at least 30 minutes prior to temperature calibration.8.2 Assemble the rheometer with the in
27、strument plates to be used during subsequent tests.9. Calibration and Standardization9.1 Perform any temperature calibration procedures recommended by the rheometer manufacturer as described in theinstruments operations manual.10. Procedure10.1 Insert the temperature sensor so that it is located at
28、the vertical and radial center of the dummy test specimen.NOTE 5This may be accomplished by placing the sensor between two sheets of the dummy test specimen.10.2 Mount the dummy test specimen between the instrument plates. Close the gap to the dimension to be used for the testspecimen, keeping the t
29、emperature sensor centered vertically and radially.NOTE 6Other gaps and plate diameters may be used but shall be reported.NOTE 7It is not necessary to trim the dummy test specimen but a large excess of material beyond the edges of the plates should be avoided.3 The trademark Silly Putty is registere
30、d to Crayola Properties, inc., Easton, PA, 18042.E2509 14210.3 Heat (or cool) the plates to the desired calibration temperature and equilibrate until the indicated temperature changes byless than 60.1C in 5 min.10.4 Measure and record the temperature indicated by the thermometer as To and that of se
31、t temperature of the rheometer asTs.10.5 Determine the temperature calibration value according to section 11.NOTE 8Depending upon the needs of the user, a single point single-point temperature calibration may be adequate. In this case, a single offsetcalibration value is determined. Others may prefe
32、r a two-point temperature calibration where the temperature values of interest are selected to encompassall test temperatures. Here, a linear interpolation of results between the two temperature calibration points may be used. Some users may wish to calibratethe apparatus at temperature intervals ov
33、er the full range of the temperature range. In this case, a working curve composed of offset values as a functionof temperature should be created.11. Calculation or Interpretation of Results11.1 The temperature response of the apparatus is assumed to be linear and is described by the equation:To 5S
34、Ts1b (1)where:To = observed temperature in C,Ts = requested controller temperature in C,S = Slope of the plot of To vs. Ts, dimensionless, andS = slope of the plot of To versus Ts, dimensionless, andb = temperature offset or bias (intercept of the To vs. Ts plot) in C.b = temperature offset or bias
35、intercept of the To versus Ts plot) in C.11.2 Single Point Single-Point Temperature CalibrationCalibration:11.2.1 In a single pointsingle-point temperature calibration, it is assumed that the slope (S)(S) for the instrument calibration is1.00000 and that there is only an offset between the observed
36、 and requested temperature. This is a reasonable assumption wherethe temperature range to be used is narrow.11.2.2 The offset or bias (b)(b) is given by:b 5To 2Ts (2)11.2.3 The value for b is determined by entering the values for To and Ts measured according to section 10.4 into Eq 2.11.2.4 The true
37、 value for an instrument requested temperature is then given by:T 5Ts1b (3)where:T = true specimen temperature in CT = true specimen temperature in C.11.3 Two Point Two-Point Temperature CalibrationCalibration:11.3.1 In a two-point temperature calibration, the response of the instrument is assumed t
38、o be linear and the slope and offsetmay be used to describe the relationship between the requested temperature and that achieved.This is a reasonable assumption overa broad temperature range for well-designed instruments.11.3.2 The slope (S)(S) of the calibration plot is given by:S 5Tohi! 2Tolo!#/Ts
39、hi! 2Tslo!# 5To/Ts (4)where:To(hi) = High observed temperature in C,To(lo) = Low observed temperature in C,Ts(hi) = High set temperature in C,Ts(lo) = Low set temperature in C.To(hi) = high observed temperature in C,To(lo) = low observed temperature in C,Ts(hi) = high set temperature in C, andTs(lo)
40、 = low set temperature in C.are taken from measurements according to section 10.4.11.3.3 The offset (b)(b) is the intercept of the calibration plot and is given by:b 5$Tshi! 3Tolo!# 2Tslo! 3Tohi!#%/ Tshi! 2Tslo!# (5)E2509 143where:b = Calibration intercept in C.b = calibration intercept in C.11.3.4
41、The true temperature for an observed temperature measurement is then given by:T 5S Ts1b (6)11.4 Multi-Point Temperature Calibration:11.4.1 In the multi-point temperature calibration, the response of the apparatus is considered to be linear over the shortdifference interval between observation points
42、 but non-linear over the large temperature interval of the whole range of theapparatus.11.4.2 Prepare a Calibration Working Tablecalibration working table with three columns labeled observed temperature (T(To),requested controller temperature (T(Ts) and temperature difference (b) where:b 5To 2Ts (7
43、)where:To(hi) = High observed temperature in C,To(lo) = Low observed temperature in C,Ts(hi) = High set temperature in C,Ts(lo) = Low set temperature in C.To(hi) = high observed temperature in C,To(lo) = low observed temperature in C,Ts(hi) = high set temperature in C, andTs(lo) = low set temperatur
44、e in C.are taken from measurements according to section 10.4.11.4.3 Fill in the table with observed values measured according to section10.4 10.4 and calculated offset values from section11.4.2.11.4.4 The true temperature for a requested temperature is determined by interpolation of the adjacent tem
45、perature points in theCalibration Working Tablecalibration working table and Eq 3 where the value of b is the offset for the corresponding value of Ts.NOTE 9Alternatively, the results of the Calibration Working Tablecalibration working table may be plotted with To on the ordinate (Y-axis) and Tson t
46、he abscissa (X-axis). Moreover, the data may be fitted by a polynomial, cubic spline, or other mathematical curve fitting technique to obtain aCalibration Working Equation.calibration working equation. This equation may be used to determine the true temperature from an observed temperaturemeasuremen
47、t.12. Report12.1 Report the following information:12.1.1 Description of the instrument (manufacturer and model number) as well as the data-handling device used in the test.12.1.2 Description of the dimension, geometry, and material of the dummy test specimen.12.1.3 Method of Calibration:Calibration
48、Single Point, two Point or Multi-Point Calibrationsingle-point, two-point, ormulti-point temperature calibration.12.1.4 For the Single Point Method,single-point temperature calibration, the temperature of calibration and the value for the bias(b).12.1.5 For the Two Point Calibration,two-point temper
49、ature calibration, the high and low calibration temperatures (known asthe calibration temperature range) , and the values of calibration slope (S) and intercept (I).12.1.6 For the multipointmulti-point temperature calibration, the high and low calibration temperatures (known as thecalibration temperature range) and the Calibration Working Table.calibration working table.12.1.7 The specific dated version of this test method used.13. Precision and Bias13.1 The precision and bias of this test method will be determined in
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