1、Designation: D 5289 07aStandard Test Method forRubber PropertyVulcanization Using Rotorless CureMeters1This standard is issued under the fixed designation D 5289; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. A number 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 covers a method for the measurementof selected vulcanization characteristics of rubber compoundsusing unseal
3、ed and sealed torsion shear cure meters. The twotypes of instruments may not give the same results.NOTE 1An alternative method for the measurement of vulcanizationcharacteristics is given in Test Method D 2084.1.2 The values stated in SI units are to be regarded as thestandard. The values given in p
4、arentheses are for informationonly.1.3 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-priate safety and health practices and determine the applica-bility of regulatory limit
5、ations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1349 Practice for RubberStandard Temperatures forTestingD 1566 Terminology Relating to RubberD 2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD 4483 Practice for Evaluating Precision for Test MethodSt
6、andards in the Rubber and Carbon Black ManufacturingIndustries3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 rotorless cure meter, na name for a class of curemeters that uses one of the two specimen shaping members ordies to sense the torque or stress during strain applicatio
7、n.Rotorless cure meters do not have a third member in the formof a rotor (see definitions of cure meter in Terminology D 1566and Test Method D 2084).3.1.2 S torque, nfor an oscillating shear rotorless curemeter, the value measured by a torque transducer at the peakstrain amplitude of the oscillating
8、 cycle; represents the elasticresponse of the test material.3.1.3 The following measurements may be taken from therecorded curve of torque as a function of time (see Fig. 1):3.1.3.1 minimum S torquemeasure of the elastic stiffnessof the unvulcanized test specimen at the specified vulcanizingtemperat
9、ure, taken at the lowest point in the vulcanizationcurve.3.1.3.2 maximum, plateau, or highest S torquemeasureof the elastic stiffness of the vulcanized test specimen at thespecified vulcanizing temperature, measured within a specifiedperiod of time.3.1.3.3 time to a percentage of full curemeasure of
10、 curebased on the time to develop some percentage of the differencein S torque from the minimum to the maximum.3.1.3.4 time to incipient cure (scorch time)measure of thetime at which a specified small increase in S torque hasoccurred; it indicates the beginning of vulcanization.3.1.4 S” torque, nfor
11、 an oscillating shear rotorless curemeter, the value measured by a torque transducer at zero strainamplitude of the oscillating cycle; represents the viscousresponse of the test material (see Fig. 2).3.1.5 S* torque, nfor an oscillating shear rotorless curemeter, the maximum value measured by a torq
12、ue transducerduring the oscillating cycle (see Fig. 2).3.1.6 The relationship between S*, S, and S” for anyoscillating cycle is:S* 5 =S !21 S ”!2(1)3.1.7 phase angle d, nfor an oscillating shear cure meter,the angle of shift between the sinusoidal strain and thesinusoidal S* torque during the oscill
13、ating cycle (see Fig. 2).3.1.8 Tan d, nfor an oscillating shear rotorless curemeter, the tangent of the phase angle d.3.1.8.1 DiscussionThe relationship between Tan d, S,and S” is:Tan d5S ”S (2)1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibilit
14、y of Subcommittee D11.12 on Processability Tests.Current edition approved Nov. 1, 2007. Published December 2007. Originallyapproved in 1992. Last previous edition approved in 2007 as D 5289 07.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at se
15、rviceastm.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, United States.Copyright by ASTM Intl (all rights reserved); Tue Mar
16、 24 01:59:40 EDT 2009Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.3.1.9 The following measurements may be taken from therecorded S” and Tan d curves as a function of time (see Fig. 1):3.1.9.1 S” MLvalue of S” torque when the minimum Storque
17、 is taken.3.1.9.2 Tan d MLvalue of Tan d when the minimum Storque is measured.3.1.9.3 S” MHvalue of S” torque when the maximumS torque is taken.FIG. 1 Typical Vulcanization CurvesFIG. 2 Example of Torque Responses for an Oscillation CycleD 5289 07a2Copyright by ASTM Intl (all rights reserved); Tue M
18、ar 24 01:59:40 EDT 2009Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.3.1.9.4 Tan d MHvalue of Tan d when the maximum Storque is measured.4. Summary of Test Method4.1 A rubber test piece is contained in a die cavity whichmay be closed or almo
19、st closed and maintained at an elevatedtemperature. The cavity is formed by two dies, one of which isoscillated through a small rotary amplitude. This action pro-duces a sinusoidal alternating torsional strain in the test pieceand a sinusoidal shear torque which depends on the stiffness(shear modulu
20、s) of the rubber compound.4.2 The stiffness of the rubber test piece increases asvulcanization proceeds. The test is completed when the re-corded torque rises to either an equilibrium or maximum value,or when a predetermined time has elapsed (see Fig. 1).Acurverepresenting the torque at peak strain
21、in one direction of theoscillation cycle is continuously recorded as a function of time.5. Significance and Use5.1 This test method is used to determine the vulcanizationcharacteristics of (vulcanizable) rubber compounds.5.2 This test method may be used for quality control inrubber manufacturing pro
22、cesses, for research and developmenttesting of raw-rubber compounded in an evaluation formula-tion, and for evaluating various raw materials used in preparing(vulcanizable) rubber compounds.5.3 The test specimen in a rotorless cure meter approachesthe test temperature in a shorter time and there is
23、a bettertemperature distribution in the test specimen due to theelimination of the unheated rotor found in oscillating disk curemeters.5.4 Several manufacturers produce rotorless cure meterswith design differences that may result in different torqueresponses and cure times for each design. Correlati
24、ons of testresults between cure meters of different designs should beestablished for each compound tested, and for each set of testconditions.6. Apparatus6.1 Rotorless cure meters of two types can be used. In eachcase, an oscillation of small amplitude is applied to one die.6.1.1 Unsealed Torsion St
25、rain Rotorless Cure MeterThistype of cure meter measures the torque produced by an angularstrain of constant amplitude in a cavity that is not completelyclosed (see Fig. 3(a).6.1.2 Sealed Torsion Strain Rotorless Cure MeterThistype of cure meter measures the torque produced by an angularstrain of co
26、nstant amplitude in a cavity that is completelyclosed and sealed (see Fig. 4(a).6.2 Die CavityThe die cavity is formed by two dies. In themeasuring position, the two dies are fixed a specified distanceapart so that the cavity is almost closed (see Fig. 3(b), orclosed and sealed (see Fig. 4(a).6.2.1
27、The dimensions for typical torsional shear curemetersinclude biconical-shaped dies having a diameter of 40 6 2mm(1.57 6 0.08 in.), and an angle of separation ranging from 7 to18, depending on the manufacturers design. In the center ofthe dies, a separation equal to 0.5 mm (0.02 in.) plus the diegap
28、should be maintained (see Fig. 3(b) or Fig. 4(b). Manu-facturers guidelines should be followed to determine if thedies have been excessively worn and should be replaced.6.2.2 Die GapThe gap between the edges of the dies inthe closed position shall be between 0.05 and 0.20 mm (0.002to 0.008 in.), pre
29、ferably 0.1 mm (0.004 in.) for unsealedcavities. For sealed cavities, no gap should exist at the edges ofthe dies.6.2.3 Die Closing MechanismA pneumatic cylinder orother device shall close the dies and hold them closed duringthe test with a force of not less than 8.0 kN (1820 lbf).6.3 Die Oscillatin
30、g SystemThe die oscillating systemimparts a torsional oscillating movement to one of the dies, inthe plane of the cavity.6.3.1 The amplitude of the oscillation should be 60.1 to63.0, preferably 60.5 of arc for torsional shear cure meters.6.3.2 The frequency of oscillation should be between 0.5and 2
31、Hz, preferably 1.7 6 0.1 Hz.6.4 Torque Measuring SystemA torque measuring systemshall measure the resultant torque.6.4.1 The torque measuring device shall be rigidly coupledto one of the dies and any deformation shall be negligibly smalland shall generate a signal which is proportional to the torque
32、.The total error resulting from zero point error, sensitivity error,linearity, and reproducibility errors shall not exceed 1 % of themeasuring range selected.NOTE 2The elastic deformation of the oscillating and measuringsystem should not be more than 1 % of the oscillating amplitude;otherwise, the c
33、uremeter curves must be corrected.6.4.2 The torque recorder device shall be used to record thesignal from the torque measuring device. It shall record the Storque at maximum oscillation as a function of time.6.4.3 The torque recorder device shall be used to record thesignal from the torque measuring
34、 device. It shall record thetorque at maximum oscillation continuously as a function oftime (see Fig. 1) and shall have a response time for full-scaledeflection on the torque scale of1sorless. The torque shall berecorded with an accuracy of 60.5 % of the range. Torquerecording devices may include an
35、alog chart recorders, printers,plotters, or computers.6.5 Torque calibration equipment is required to measure theangular strain amplitude and to calibrate the torque measuringdevice. Examples of calibration equipment are shown in Fig. 5and Fig. 6. The amplitude of oscillation of the device shall bec
36、hecked with no test specimen in it.Adisplacement transducershall be used to measure the amplitude and torque measure-ments shall be checked against standard masses using a deviceas shown in Fig. 5. An alternate technique shall use a torquestandard.6.5.1 For calibrating torsion shear curemeters, eith
37、er adisplacement transducer and wire-mass calibration or a torquestandard shall be used.6.5.1.1 A displacement transducer for checking angulardisplacement shall be coupled by a knife-edge bearing incontact with a rod fixed to one of the dies (see Fig. 5). Theforce measuring system shall be checked b
38、y loading a wire,attached to the die or block by a pulley, with masses corre-sponding to the full-scale force being measured. The torqueD 5289 07a3Copyright by ASTM Intl (all rights reserved); Tue Mar 24 01:59:40 EDT 2009Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further
39、 reproductions authorized.shall be calculated in this case from the product of the appliedforce and the radius of the die block where the wire is attached.6.5.1.2 Torque standard calibration checks the torque mea-surement at the selected angular displacement by clamping aFIG. 3 (a) and (b)Typical Un
40、sealed Torsion Shear Rotorless CuremeterD 5289 07a4Copyright by ASTM Intl (all rights reserved); Tue Mar 24 01:59:40 EDT 2009Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.reference steel torsion rod to the oscillating die and the torquemeasu
41、ring die of the torsion shear cure meter (see Fig. 6). Thereference values for angular displacement and correspondingtorque have been established by the manufacturer for eachtorque standard.6.6 Temperature Controlling SystemThe method of tem-perature control shall maintain the following process para
42、m-eters: heating up time, curing temperature, temperature distri-bution, and reference temperature, which are necessary forreproducible measurement of the vulcanization curve. Thetemperature control system shall permit the reference tempera-ture to be varied between 110C and 200C with an accuracyof
43、60.3C or better.6.6.1 Die shall heat up in 1.5 min or less from closure of thedie cavity.6.6.2 Once heating up time hs been completed, die tempera-ture shall not vary by more than 60.3C for the rest of the test.6.6.3 The temperature distribution within the test specimenshall be as uniform as possibl
44、e. Within the deformation zone,a tolerance of 61C of the average test specimen temperatureshall not be exceeded.6.6.4 The reference temperature is determined by a tempera-ture sensor used for control. The difference between thereference temperature and the average test specimen tempera-ture shall no
45、t be more than 2C.6.6.5 Temperature measurement accuracy shall be60.3C for the reference temperature sensor.6.7 Reference Test TemperatureThe standard referencetest temperature shall be 160C (320F). Tests may be carriedout at other temperatures if required. Temperatures should beselected in accordan
46、ce with Practice D 1349.FIG. 4 Typical Sealed Torsion Shear Rotorless CuremeterFIG. 5 Displacement Transducer and Wire-Mass CalibrationEquipment for Torsion Shear CuremetersFIG. 6 Typical Torque Standard Calibration Device for TorsionShear CuremetersD 5289 07a5Copyright by ASTM Intl (all rights rese
47、rved); Tue Mar 24 01:59:40 EDT 2009Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.7. Sampling7.1 The sample shall be taken from a vulcanizable rubbercompound as required by the mixing method or other samplinginstructions.7.2 The sample shall
48、be homogeneous, at room temperature,and as free of trapped air as possible.8. Test Specimens8.1 The recommended test specimen volume is between 3and5cm3, depending on the model of instrument being used.The size of the test specimen should exceed the test chambervolume by a small amount, to be determ
49、ined by preliminarytests. Typically, specimen volume should be 130 to 190 % ofthe test chamber volume. Once a target weight is established,the weight of specimens should be controlled to within 60.5 gfor best repeatability.8.2 The test specimen taken from the sample should becircular, with a diameter smaller than the test chamber of theinstrument to be used.9. Procedure9.1 Preparation for TestBring the temperature of bothdies to the reference temperature with the cavity closed.Adjustthe zero of the force
