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 service@astm.org. 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)

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 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.

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 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.

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 D5289 − 19a

FIG. 3 (a) and (b)—Typical Unsealed Torsion Shear Rotorless Curemeter

6.5.1 For calibrating torsion shear curemeters, either a 6.5.1.1 A displacement transducer for checking angular
displacement transducer and wire-mass calibration or a torque displacement shall be coupled by a knife-edge bearing in
standard shall be used. contact with a rod fixed to one of the dies (see Fig. 5). The

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 D5289 − 19a

FIG. 6 Typical Torque Standard Calibration Device for Torsion

Shear Curemeters

force measuring system shall be checked by loading a wire,

attached to the die or block by a pulley, with masses corre-
sponding to the full-scale force being measured. The torque
shall be calculated in this case from the product of the applied
FIG. 4 Typical Sealed Torsion Shear Rotorless Curemeter force 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 a
reference steel torsion rod to the oscillating die and the torque
measuring die of the torsion shear cure meter (see Fig. 6). The
reference values for angular displacement and corresponding
torque have been established by the manufacturer for each
torque standard.
6.6 Temperature Controlling System—The method of tem-
perature control shall maintain the following process param-
eters: heating up time, curing temperature, temperature
distribution, and reference temperature, which are necessary
for reproducible measurement of the vulcanization curve. The
temperature control system shall permit the reference tempera-
ture to be varied between 110°C and 200°C with an accuracy
of 60.3°C or better.
6.6.1 Die shall heat up in 1.5 min or less from closure of the
die cavity.
6.6.2 Once heating up time hs been completed, die tempera-
ture shall not vary by more than 60.3°C for the rest of the test.
6.6.3 The temperature distribution within the test specimen
shall be as uniform as possible. Within the deformation zone,
a tolerance of 61°C of the average test specimen temperature
shall not be exceeded.
6.6.4 The reference temperature is determined by a tempera-
ture sensor used for control. The difference between the
reference temperature and the average test specimen tempera-
FIG. 5 Displacement Transducer and Wire-Mass Calibration ture shall not be more than 2°C.
Equipment for Torsion Shear Curemeters
6.6.5 Temperature measurement accuracy shall be
60.3°C for the reference temperature sensor.

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 D5289 − 19a
6.7 Reference Test Temperature—The standard reference 9.2 Loading the Curemeter:
test temperature shall be 160°C (320°F). Tests may be carried 9.2.1 Open the dies, unload the previous sample (if
out at other temperatures if required. Temperatures should be necessary), place the test piece in the cavity, and close the dies
selected in accordance with Practice D1349. within 20 s.
9.2.2 The test time shall be counted from the instant that the
7. Sampling dies are closed. Oscillation of the movable die shall be started
7.1 The sample shall be taken from a vulcanizable rubber at zero time or before.
compound as required by the mixing method or other sampling 10. Report
instructions.
10.1 Report the following information:
7.2 The sample shall be homogeneous, in sheeted form, at 10.1.1 A full description of the sample, its origin and
room temperature, and as free of air as possible. compound details,
7.3 The temperature of the sample and its heat history can 10.1.2 Test method and test details,
significantly affect test results. For referee testing and for 10.1.2.1 Reference to this test method,
testing under controlled circumstances, the sample shall be 10.1.2.2 Type and model curemeter used (sealed or unsealed
conditions at 23 6 1°C (73 6 2°F) for at least 1 h before rotorless, manufacturer, die options, if any),
testing. 10.1.2.3 Amplitude of the die oscillation, in degrees,
7.4 In production control testing, samples may be tested 10.1.2.4 Frequency of oscillation,
without the conditioning period, but care should be taken to 10.1.2.5 Torque range selected, in deci Newton metres
minimize temperature and heat history variations prior to (dN·m). (The equation for conversion from dN·m to lbf·in. is
testing. 1.13 (dN·m) = 1.00 (lbf·in.)),
10.1.2.6 Time scale of the recording device,
8. Test Specimen 10.1.2.7 Curing temperature in degrees Celsius,
10.1.2.8 Date of the test, and
8.1 The recommended test specimen volume is between 3 10.1.2.9 Type of film used, if any.
and 6 cm3, depending on the instrument model being used.
10.2 Test results reported are normally chosen from the
8.2 The test specimen should be circular, with a diameter following parameters (refer to Fig. 1 for guidance):
smaller than the test chamber of the instrument to be used. 10.2.1 ML—Minimum S’ torque, in dN·m (lbf·in.).
8.3 The test specimen is considered to be of proper size 10.2.2 Maximum S’ Torque—All in dN·m (lbf·in.).
when a small bead of rubber compound is extruded uniformly 10.2.2.1 MHF—Maximum S’ torque where curve plateaus.
around the periphery of the dies as they are closed (116 to 10.2.2.2 MHR—Maximum S’ torque of reverting curve.
160 % of the test cavity volume). For an instrument with a test 10.2.2.3 MH—Highest S’ torque attained during a specified
cavity volume of 3.44 cm3, this is achieved when the test period of time when no plateau or maximum torque is
specimen volume is between 4.0 and 5.5 cm3 (4.6 to 6.3 g of obtained.
rubber compound with a specific gravity of 1.15). Undersized 10.2.3 tsx—Scorch time, in minutes (time to an increase of
test specimens can cause low cavity pressure and low torque x units of S’ torque from the ML value). The preferred scorch
readings. Oversized test specimens cool the dies excessively time for tests at an oscillation amplitude of 60.5° is ts1 (1.0 S’
during the early part of the test period, affecting the vulcani- torque unit rise).
zation characteristics.
NOTE 3—The value of ts1 is different if the units of S’ torque rise are
8.4 When testing low viscosity or sticky materials, materials in lbf·in instead of dN·m.
that may adhere to metal, to minimize contamination of the 10.2.4 Cure Time, in minutes.
dies, or to allow for automated removal of the tested specimen, 10.2.4.1 t'x—equal to the time to x % of S’ torque increase
it is permissible to insert between the specimen and the dies a or t'x = minutes to (ML + x(MH − ML) ⁄100) S’ torque. This
layer of film approximately 0.025 mm (0.001 in.) thick. The test result may also be called TCx.
film selected should not react with the test specimen or melt at
test temperatures. Film materials that have been found suitable NOTE 4—This method of determining the cure times is considered the
standard method. The most commonly used values of x are 50 and 90. A
include polyester, heat-stabilized nylon, and similar materials. cure time of t'10 is sometimes used as a measure of scorch time.
For referee testing such compounds a 0.025 6 0.001 mm
(0.001 6 0.00004 in.) thick polyester film from the same 10.2.4.2 tx—equal to the time to x % of S’ torque increase or
source could be used. Test results obtained when film is used tx = minutes to (x(MH)/100) S’ torque.
may be different from results obtained without film, but tests NOTE 5—This is an alternate method for cure time determination.
run using film may be more repeatable by reducing contami- 10.2.5 Cure Rate Index—equal to 100/(cure time − scorch
nation from previous tests. time).
10.2.6 PCR (Peak Cure Rate)—Maximum slope of the S’
9. Procedure torque curve as a function of time, in dN·m/min. This value is
9.1 Preparation for Test—Bring the temperature of both usually measured with the aid of computer data recording.
dies to the reference temperature with the cavity closed. Adjust 10.2.7 PCR Time—test time at which the Peak Cure Rate is
the zero of the force or torque measuring device, if necessary. reached, in minutes.

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 D5289 − 19a
10.2.8 “t10 % Rise” is the time for the torque to rise to both programs. Both ITPs evaluated Type 1 precision, with
110 % of the minimum value. This may be used to measure fully prepared test specimens sent to all participants.
scorch in some cases. 11.1.3 The data generated in Precision Programs I and II
10.2.9 S” @ML—The value of S” torque when the ML were collected from tests run on instruments from a single
value of S’ torque is taken. manufacturer. This is due to most participants in both inter-
10.2.10 Tan δ @ML—The value of Tan δ when the ML laboratory studies having similar equipment. This test method
value of S’ torque is taken. is intended to cover use of a wide range of rotorless curemeter
10.2.11 S” @MH—The value of S” torque when the MH designs, and the fact that the data reported is from a single
value of S’ torque is measured. manufacturer’s instrument is not to be considered an endorse-
10.2.12 Tan δ @MH—The value of Tan δ when the MH ment of that instrument over the use of other manufacturer’s
value of S’ torque is measured. instruments. Each manufacturer’s rotorless curemeter design
has unique characteristics that may cause some shifts in test
11. Precision and Bias results. As noted in the report section of this test method,
11.1 This precision and bias section has been prepared in reports of test results should include notation of the instrument
accordance with Practice D4483. Refer to Practice D4483 for used to obtain the results.
terminology and other statistical calculation details. 11.2 Precision Program 1—In this ITP three compounds
11.1.1 The precision results in this precision and bias based on SBR and SBR/NR polymers with sulfenamide cure
section give an estimate of the precision of this test method systems and carbon black reinforcement were carefully mixed
with the materials (rubbers, etc.) used in the particular inter- and prepared for testing. Precut specimens were sent to 11
laboratory test programs (ITPs) as described below. The laboratories along with instructions to test duplicate samples of
precision parameters should not be used for acceptance or each compound in one day, and repeat the testing, after
rejection testing of any group of materials without documen-
tation that they are applicable to those particular materials and
the specific testing protocols that include this test method.
11.1.2 The precision has been evaluated in two separate
interlaboratory test programs: Program 1 in 1989 and Program
2 in 2000. Each program is described below and then repeat-
ability and reproducibility statements are given that apply to

TABLE 1 Precision Program 1A

NOTE 1—
Sr = within laboratory standard deviation,
r = repeatability (in measurement units),
(r) = repeatability (in percent),
SR = between-laboratory standard deviation,
R = reproducibility (in measurement units), and
(R) = reproducibility (in percent).
Compound, Mean Within Labs Between Labs
Test Parameter Value Sr r (r) SR R (R)
Compound A:
ML (dN·m) 1.35 0.007 0.02 1.4 0.071 0.20 14.8
MH (dN·m) 13.60 0.025 0.07 0.5 0.608 1.72 12.7
ts1 (min) 1.55 0.009 0.02 1.6 0.065 0.18 11.8
t'50 (min) 3.10 0.007 0.03 0.8 0.061 0.17 5.6
t'90 (min) 4.93 0.015 0.04 0.9 0.147 0.42 8.5
Gr. Avg. 0.013 0.036 1.04 0.190 0.538 10.68
Compound B:
ML (dN·m) 1.00 0.008 0.02 2.2 0.048 0.14 13.6
MH (dN·m) 10.17 0.024 0.07 0.7 0.478 1.35 13.3
ts1 (min) 2.22 0.008 0.02 1.0 0.076 0.21 9.6
t'50 (min) 3.55 0.007 0.02 0.6 0.098 0.28 7.8
t'90 (min) 5.74 0.023 0.06 1.1 0.156 0.44 7.7
Gr. Avg. 0.014 0.036 1.12 0.171 0.484 10.40
Compound C:
ML (dN·m) 1.50 0.011 0.03 2.1 0.076 0.22 14.3
MH (dN·m) 12.30 0.045 0.13 1.0 0.571 1.62 13.1
ts1 (min) 1.80 0.011 0.03 1.7 0.063 0.18 9.9
t'50 (min) 3.34 0.009 0.03 0.8 0.098 0.28 8.3
t'90 (min) 5.73 0.018 0.05 0.9 0.156 0.44 7.7
Gr. Avg. 0.019 0.054 1.30 0.193 0.548 10.66
A
These values are Type I precision values, obtained from fully prepared test specimens (compounds mixed in one laboratory) which were circulated to all participating
laboratories.

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 D5289 − 19a
TABLE 2 Precision Program 2
NOTE 1—
Sr = within laboratory standard deviation,
r = repeatability (in measurement units),
(r) = repeatability (in percent of mean level),
SR = between-laboratory standard deviation (for total between-laboratory variation in measurement units),
R = reproducibility (in measurement units), and
(R) = reproducibility (in percent of mean level).
Compound, Mean Within Labs Between Labs No.
Test Parameter Value Sr r (r) SR R (R) LabsA,B
Compound A:
ML (dN·m) 2.13 0.025 0.071 3.34 0.076 0.210 10.0 17
MH (dN·m) 14.43 0.176 0.49 3.42 0.548 1.53 10.6 17
ts1 (min) 3.14 0.055 0.15 4.90 0.095 0.270 8.47 16
t'10 (min) 3.26 0.048 0.14 4.14 0.085 0.240 7.29 16
t'50 (min) 5.37 0.091 0.25 4.73 0.204 0.572 10.7 19
t'90 (min) 10.34 0.172 0.48 4.66 0.586 1.64 15.9 19
Gr. Avg. 0.079 0.222 4.11 0.202 0.564 9.39
Compound B:
ML (dN·m) 2.00 0.021 0.059 2.93 0.067 0.19 9.3 18
MH (dN·m) 16.32 0.122 0.341 2.09 0.635 1.78 10.9 17
ts1 (min) 2.78 0.023 0.066 2.37 0.069 0.19 6.9 14
t'10 (min) 3.00 0.027 0.077 2.55 0.086 0.24 8.0 16
t'50 (min) 4.61 0.032 0.091 1.97 0.090 0.25 5.4 16
t'90 (min) 8.10 0.081 0.226 2.79 0.303 0.85 10.5 18
Gr. Avg. 0.045 0.127 2.38 0.189 0.530 8.1
Compound C:
ML (dN·m) 2.23 0.026 0.074 3.30 0.063 0.18 7.9 17
MH (dN·m) 10.68 0.118 0.329 3.08 0.391 1.10 10.3 17
ts1 (min) 6.25 0.126 0.359 5.75 0.228 0.64 10.2 17
t'10 (min) 5.81 0.106 0.297 5.12 0.157 0.44 7.56 18
t'50 (min) 5.37 0.091 0.254 4.73 0.204 0.57 10.7 19
t'90 (min) 10.31 0.156 0.438 4.25 0.583 1.63 15.8 19
Gr. Avg. 0.093 0.263 4.40 0.209 0.586 9.3
Compound D:
ML (dN·m) 2.19 0.0098 0.027 1.25 0.034 0.100 4.4 9
MH (dN·m) 31.52 0.245 0.685 2.17 0.536 1.50 4.8 9
ts1 (min) 2.56 0.027 0.076 2.97 0.107 0.300 11.7 9
t'10 (min) 3.76 0.065 0.183 4.87 0.082 0.230 6.1 10
t'50 (min) 4.98 0.061 0.170 3.42 0.119 0.333 6.7 11
t'90 (min) 7.32 0.117 0.327 4.47 0.322 0.901 12.3 8
Gr. Avg. 0.103 0.288 3.73 0.233 0.65 8.3
A
The final number of laboratories remaining in the ITP after (Option 1) deletion of outliers. Compounds A, B, and C had a total of 20 labs participating in the ITP.
B
Compound D had a total of 12 labs participating in the ITP.
ML = minimum torque; MH = maximum torque; ts1 = time to 1 unit torque rise; t’10, t’50, and t’90 = times to 10, 50, and 90 %, respectively, of full cure time.

checking calibration, for day 2 one week later. The testing was Precut specimens were sent to 20 laboratories for compounds
conducted using a sealed torsion type rotorless curemeter,3 A, B, and C and 12 laboratories for compound D, along with
with typical dies as illustrated in Fig. 4, at 175°C and 60.5° instructions to test duplicate samples of each compound in one
arc. The duplicate test values for each day were averaged to get day, and repeat the testing, after checking calibration, for day
a single value for each day and the analysis was conducted on 2 one week later. The testing was conducted using a sealed
these day 1–day 2 test results. The precision output for torsion type rotorless curemeter,3 with typical dies as illus-
Program 1 is listed in Table 1. trated in Fig. 4, at 160°C and 60.5° arc. The duplicate test
11.3 Precision Program 2—In this ITP four compounds values for each day were averaged to get a single value for each
were used for testing. Compounds A, B, and C were based on day and the analysis was conducted on these day 1–day 2 test
SBR with a sulfenamide cure system and carbon black rein- results. The precision output for Program 2 is listed in Table 2.
forcement with increasing sulfur content for A, B, and C. 11.3.1 The analysis of the ITP data for Program 2 was
Compound D was a Fluoroelastomer compound that required conducted after Practice D4483 was revised (see 2004 pub-
the use of film between the sample and the dies for testing. All lished version). This Practice D4483 revision has improved
compounds were carefully mixed and prepared for testing. procedures for outlier identification and subsequent deletion.
The 2004 version of Practice D4483 permits identifying the
3
The MDR-2000 from Alpha Technologies, 3030 Gilchrist Road, Akron, OH core group of laboratories in any ITP that have good control
44305 was used by all participants in both Interlaboratory Test Programs. There are over their testing operations and thus represent the industry
several other manufacturers of rotorless cure meters, but not enough participants benchmark for high quality testing. Note the last column of
using other instruments were available to generate meaningful statistics for this
precision and bias statement. No endorsement of any instrument is implied in this Table 2 that indicates the number of laboratories used for
study. precision calculation after deletion of outliers.

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 D5289 − 19a
11.4 The precision may be expressed in the format of the 11.4.3 Repeatability and reproducibility expressed as a per-
following statements that use an appropriate value of r, R, (r), centage of the mean level, (r) and (R), have equivalent
or (R), that is, that value obtained from Table 1 or Table 2 for application statements as cited above for r and R. For the (r)
any of the measured properties, to be used in decisions about and (R) statements, the difference in the two single test results
results obtained for that property, with the test method. is expressed as a percentage of the arithmetic mean of the two
11.4.1 Repeatability—The repeatability, r, of this test test results.
method has been established as the appropriate value for any
parameter as tabulated in Table 1 or Table 2. Two single test 11.5 Bias—In test method terminology, bias is the difference
results, obtained under normal test method procedures that between an average test value and the reference (or true) test
differ by more than this tabulated r must be considered as property value. Reference values do not exist for this test
derived from different or non-identical sample populations. method since the value (of the test property) is exclusively
11.4.2 Reproducibility—The reproducibility, R, of this test defined by the test method. Bias, therefore, cannot be deter-
method has been established as the appropriate value for any mined.
parameter as tabulated in Table 1 or Table 2. Two single test
results obtained in two different laboratories, under normal test 12. Keywords
method procedures, that differ by more than the tabulated R
12.1 compounds; rheometer; rotorless cure meter; vulcani-
must be considered to have come from different or non-
zation characteristics
identical sample populations.

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