This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5289 − 19a

Standard Test Method for

Rubber Property—Vulcanization Using Rotorless Cure
Meters1
This standard is issued under the fixed designation D5289; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 3. Terminology
1.1 This test method covers a method for the measurement 3.1 Definitions of Terms Specific to This Standard:
of selected vulcanization characteristics of rubber compounds 3.1.1 rotorless cure meter, n—a name for a class of cure
using unsealed and sealed torsion shear cure meters. The two meters that uses one of the two specimen shaping members or
types of instruments may not give the same results. dies to sense the torque or stress during strain application.
NOTE 1—An alternative method for the measurement of vulcanization Rotorless cure meters do not have a third member in the form
characteristics is given in Test Method D2084. of a rotor (see definitions of cure meter in Terminology D1566
1.2 The values stated in SI units are to be regarded as the and Test Method D2084).
standard. The values given in parentheses are for information 3.1.2 S’ torque, n—for an oscillating shear rotorless cure
only. meter, the value measured by a torque transducer at the peak
1.3 This standard does not purport to address all of the strain amplitude of the oscillating cycle; represents the elastic
safety concerns, if any, associated with its use. It is the response of the test material.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- 3.1.3 The following measurements may be taken from the
mine the applicability of regulatory limitations prior to use. recorded curve of torque as a function of time (see Fig. 1):
1.4 This international standard was developed in accor- 3.1.3.1 minimum S’ torque—measure of the elastic stiffness
dance with internationally recognized principles on standard- of the unvulcanized test specimen at the specified vulcanizing
ization established in the Decision on Principles for the temperature, taken at the lowest point in the vulcanization
Development of International Standards, Guides and Recom- curve.
mendations issued by the World Trade Organization Technical 3.1.3.2 maximum, plateau, or highest S’ torque—measure of
Barriers to Trade (TBT) Committee. the elastic stiffness of the vulcanized test specimen at the
specified vulcanizing temperature, measured within a specified
2. Referenced Documents
period of time.
2.1 ASTM Standards:2 3.1.3.3 time to a percentage of full cure—measure of cure
D1349 Practice for Rubber—Standard Conditions for Test- based on the time to develop some percentage of the difference
ing
in S’ torque from the minimum to the maximum.
D1566 Terminology Relating to Rubber
D2084 Test Method for Rubber Property—Vulcanization 3.1.3.4 time to incipient cure (scorch time)—measure of the
Using Oscillating Disk Cure Meter time at which a specified small increase in S’ torque has
D4483 Practice for Evaluating Precision for Test Method occurred; it indicates the beginning of vulcanization.
Standards in the Rubber and Carbon Black Manufacturing 3.1.4 S” torque, n—for an oscillating shear rotorless cure
Industries meter, the value measured by a torque transducer at zero strain
amplitude of the oscillating cycle; represents the viscous
1
response of the test material (see Fig. 2).
This test method is under the jurisdiction of ASTM Committee D11 on Rubber
and Rubber-like Materials and is the direct responsibility of Subcommittee D11.12 3.1.5 S* torque, n—for an oscillating shear rotorless cure
on Processability Tests. meter, the maximum value measured by a torque transducer
Current edition approved Nov. 1, 2019. Published November 2019. Originally
approved in 1992. Last previous edition approved in 2019 as D5289 – 19. DOI: during the oscillating cycle (see Fig. 2).
10.1520/D5289-19A.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 3.1.6 The relationship between S*, S’, and S” for any
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM oscillating cycle is:
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. S* 5 =~ S ’ ! 2 1 ~ S ” ! 2 (1)

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D5289 − 19a

FIG. 1 Typical Vulcanization Curves

FIG. 2 Example of Torque Responses for an Oscillation Cycle

3.1.7 phase angle δ, n—for an oscillating shear cure meter, 3.1.8.1 Discussion—The relationship between Tan δ, S’, and
the angle of shift between the sinusoidal strain and the S” is:
sinusoidal S* torque during the oscillating cycle (see Fig. 2). S”
3.1.8 Tan δ, n—for an oscillating shear rotorless cure meter, Tan δ 5 (2)
S’
the tangent of the phase angle δ.

2
 D5289 − 19a
3.1.9 The following measurements may be taken from the 6.2 Die Cavity—The die cavity is formed by two dies. In the
recorded S” and Tan δ curves as a function of time (see Fig. 1): measuring position, the two dies are fixed a specified distance
3.1.9.1 S” @ML—value of S” torque when the minimum S’ apart so that the cavity is almost closed (see Fig. 3(b)), or
torque is taken. closed and sealed (see Fig. 4(a)).
3.1.9.2 Tan δ @ML—value of Tan δ when the minimum S’ 6.2.1 The dimensions for typical torsional shear curemeters
torque is measured. include biconical-shaped dies having a diameter of 40 6 2 mm
3.1.9.3 S” @MH—value of S” torque when the maximum (1.57 6 0.08 in.), and an angle of separation ranging from 7 to
S’ torque is taken. 18°, depending on the manufacturer’s design. In the center of
3.1.9.4 Tan δ @MH—value of Tan δ when the maximum S’ the dies, a separation equal to 0.5 mm (0.02 in.) plus the die
torque is measured. gap should be maintained (see Fig. 3(b) or Fig. 4(b)). Manu-
facturer’s guidelines should be followed to determine if the
4. Summary of Test Method dies have been excessively worn and should be replaced.
4.1 A rubber test piece is contained in a die cavity which 6.2.2 Die Gap—The gap between the edges of the dies in the
may be closed or almost closed and maintained at an elevated closed position shall be between 0.05 and 0.20 mm (0.002 to
temperature. The cavity is formed by two dies, one of which is 0.008 in.), preferably 0.1 mm (0.004 in.) for unsealed cavities.
oscillated through a small rotary amplitude. This action pro- For sealed cavities, no gap should exist at the edges of the dies.
duces a sinusoidal alternating torsional strain in the test piece 6.2.3 Die Closing Mechanism—A pneumatic cylinder or
and a sinusoidal shear torque which depends on the stiffness other device shall close the dies and hold them closed during
(shear modulus) of the rubber compound. the test with a force of not less than 8.0 kN (1820 lbf).
4.2 The stiffness of the rubber test piece increases as 6.3 Die Oscillating System—The die oscillating system
vulcanization proceeds. The test is completed when the re- imparts a torsional oscillating movement to one of the dies, in
corded torque rises to either an equilibrium or maximum value, the plane of the cavity.
or when a predetermined time has elapsed (see Fig. 1). A curve 6.3.1 The amplitude of the oscillation should be 60.1 to
representing the torque at peak strain in one direction of the 63.0°, preferably 60.5° of arc for torsional shear cure meters.
oscillation cycle is continuously recorded as a function of time. 6.3.2 The frequency of oscillation should be between 0.5
and 2 Hz, preferably 1.7 6 0.1 Hz.
5. Significance and Use
6.4 Torque Measuring System—A torque measuring system
5.1 This test method is used to determine the vulcanization shall measure the resultant torque.
characteristics of (vulcanizable) rubber compounds. 6.4.1 The torque measuring device shall be rigidly coupled
5.2 This test method may be used for quality control in to one of the dies and any deformation shall be negligibly small
rubber manufacturing processes, for research and development and shall generate a signal which is proportional to the torque.
testing of raw-rubber compounded in an evaluation The total error resulting from zero point error, sensitivity error,
formulation, and for evaluating various raw materials used in linearity, and reproducibility errors shall not exceed 1 % of the
preparing (vulcanizable) rubber compounds. measuring range selected.
5.3 The test specimen in a rotorless cure meter approaches NOTE 2—The elastic deformation of the oscillating and measuring
the test temperature in a shorter time and there is a better system should not be more than 1 % of the oscillating amplitude;
temperature distribution in the test specimen due to the otherwise, the curemeter curves must be corrected.
elimination of the unheated rotor found in oscillating disk cure 6.4.2 The torque recorder device shall be used to record the
meters. signal from the torque measuring device. It shall record the S’
5.4 Several manufacturers produce rotorless cure meters torque at maximum oscillation as a function of time.
with design differences that may result in different torque 6.4.3 The torque recorder device shall be used to record the
responses and cure times for each design. Correlations of test signal from the torque measuring device. It shall record the
results between cure meters of different designs should be torque at maximum oscillation continuously as a function of
established for each compound tested, and for each set of test time (see Fig. 1) and shall have a response time for full-scale
conditions. deflection on the torque scale of 1 s or less. The torque shall be
recorded with an accuracy of 60.5 % of the range. Torque
6. Apparatus recording devices may include analog chart recorders, printers,
6.1 Rotorless cure meters of two types can be used. In each plotters, or computers.
case, an oscillation of small amplitude is applied to one die. 6.5 Torque calibration equipment is required to measure the
6.1.1 Unsealed Torsion Strain Rotorless Cure Meter—This angular strain amplitude and to calibrate the torque measuring
type of cure meter measures the torque produced by an angular device. Examples of calibration equipment are shown in Fig. 5
strain of constant amplitude in a cavity that is not completely and Fig. 6. The amplitude of oscillation of the device shall be
closed (see Fig. 3(a)). checked with no test specimen in it. A displacement transducer
6.1.2 Sealed Torsion Strain Rotorless Cure Meter—This shall be used to measure the amplitude and torque measure-
type of cure meter measures the torque produced by an angular ments shall be checked against standard masses using a device
strain of constant amplitude in a cavity that is completely as shown in Fig. 5. An alternate technique shall use a torque
closed and sealed (see Fig. 4(a)). standard.