Designation: D 2084 – 01

Standard Test Method for

Rubber Property—Vulcanization Using Oscillating Disk Cure
Meter1
This standard is issued under the fixed designation D 2084; 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 (e) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

1. Scope 3. Terminology
1.1 This test method describes the use of the oscillating disk 3.1 Definitions of Terms Specific to This Standard:
cure meter for determining selected vulcanization characteris- 3.1.1 The following measurements may be taken from the
tics of vulcanizable rubber compounds. curve of torque versus time (see Fig. 1).
1.2 The values stated in SI units are to be regarded as the 3.1.2 cure rate index—measure of rate of vulcanization
standard. The values given in parentheses are for information based on the difference between optimum vulcanization and
only. incipient scorch time.
1.3 ISO 3417 is very similar to this test method. It has minor 3.1.3 maximum, plateau, or highest torque—measure of
technical differences that are not considered to be significant. stiffness or shear modulus of the fully vulcanized test specimen
1.4 This standard does not purport to address all of the at the vulcanization temperature.
safety concerns, if any, associated with its use. It is the 3.1.4 minimum torque—measure of the stiffness of the
responsibility of the user of this standard to establish appro- unvulcanized test specimen taken at the lowest point of the
priate safety and health practices and determine the applica- curve.
bility of regulatory limitations prior to use. 3.1.5 time to incipient cure (scorch time)—measure of the
time at which vulcanization begins.
2. Referenced Documents 3.1.6 time to a percentage of full cure—measure of opti-
2.1 ASTM Standards: mum cure based on the time to develop some percentage of the
D 1349 Practice for Rubber—Standard Temperatures for highest torque or difference in torque from the minimum.
Testing2 3.1.7 torque—for an oscillating shear cure meter, the value
D 3185 Test Methods for Rubber—Evaluation of SBR measured by a torque transducer at the peak strain amplitude of
(Styrene-Butadiene Rubber) Including Mixtures With Oil2 the oscillating cycle.
D 3186 Test Methods for Rubber—Evaluation of SBR
(Styrene-Butadiene Rubber) Mixed With Carbon Black or 4. Summary of Test Method
Carbon Black and Oil2 4.1 A test specimen of vulcanizable rubber compound is
D 3187 Test Methods for Rubber—Evaluation of NBR inserted into the cure meter test cavity and after a closure
(Acrylonitrile-Butadiene Rubber)2 action is contained in a sealed cavity under positive pressure.
D 3190 Test Methods for Rubber—Evaluation of Chloro- The cavity is maintained at some elevated vulcanization
prene Rubber (CR)2 temperature. The rubber totally surrounds a biconical disk after
D 4483 Practice for Determining Precision for Test Method the dies are closed (see Fig. 2). The disk is oscillated through
Standards in the Rubber and Carbon Black Industries2 a small rotational amplitude (1° or 3°) and this action exerts a
2.2 ISO Standard: shear strain on the test specimen. The force required to oscillate
ISO 3417 Rubber—Measurement of Vulcanization Charac- or rotate the disk to maximum amplitude is continuously
teristics With the Oscillating Disk Rheometer3 recorded as a function of time, with the force being propor-
tional to the shear modulus (stiffness) of the test specimen at
1
This test method is under the jurisdiction of ASTM Committee D11 on Rubber
the test temperature. This stiffness first decreases as it warms
and is the direct responsibility of Subcommittee D11.12 on Processability Tests. up; then it increases due to vulcanization. The test is completed
Current edition approved Aug. 10, 2001. Published October 2001. Originally when the recorded torque either rises to an equilibrium or
published as D 2084 – 71 T, replacing Methods D 2705 and D 2706. Last previous maximum value, or when a predetermined time has elapsed.
edition D 2084 – 95.
2
Annual Book of ASTM Standards, Vol 09.01.
The time required to obtain a cure curve is a function of the
3
Available from American National Standards Institute, 25 W. 43rd St., 4th
Floor, New York, NY 10036.

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

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 D 2084

Left Curve: Cure to Equilibrium Torque.

Middle Curve: Cure to a Maximum Torque with Reversion.
Right Curve: Cure to No Equilibrium in Maximum Torque.
FIG. 1 Types of Cure Curve

FIG. 2 Cure Meter Assembly

characteristics of the rubber compound and of the test tempera- dies is shown in Fig. 3 and Fig. 4 with dimensions and
ture (see Fig. 1 for typical cure curves). tolerances (see Table 1). The top and bottom surfaces of the die
cavity shall contain rectangularly shaped grooves arranged
5. Significance and Use radially about the center and spaced at 20° intervals. Each die
5.1 This test method is used to determine the vulcanization shall have a well or hole drilled from the side to accommodate
characteristics of (vulcanizable) rubber compounds. a temperature sensor inserted through the platen. The lower
5.2 This test method may be used for quality control in dies shall have a hole in the center to allow for the insertion of
rubber manufacturing processes, for research and development the disk shaft. A suitable low-friction seal shall be provided in
testing of raw-rubber compounded in an evaluation formula- this hole to prevent material leaking from the cavity.
tion, and for evaluating various raw materials used in preparing 6.2.3 Disk—The biconical disk (see Fig. 5) shall be fabri-
(vulcanizable) rubber compounds. cated from tool steel having a minimum Rockwell Hardness of
HRC 50. The disk shall be fitted with a stem that fits into the
6. Apparatus torque shaft. The disk is shown in Fig. 5 (see Table 2).
6.1 Cure meter, consists of the following major compo- 6.2.3.1 Disk wear will affect test results. A disk worn to such
nents: specimen chamber and closure mechanism, temperature an extent that the disk diameter is less than the minimum
control system, rotor drive and torque measuring system (see diameter shown in this procedure shall not be used.
Fig. 2 for a detailed drawing of cure meter assembly). 6.2.3.2 The standard frequency of the rotary oscillation of
6.2 Specimen Chamber—Consists of platens, dies, and a the disk shall be constant at 1.7 Hz (100 cpm). Other
biconical disk. frequencies may be used, if required.
6.2.1 Platens—Two platens made of aluminum alloy, each
6.2.3.3 A rotary drive system shall be provided for oscilla-
containing an electric heater, and each having in the center, a
tory rotation of the disk. The amplitude of oscillation of the
cavity to accommodate a die and from the side, a well for
unloaded disk shall be constant at 61.00° with a tolerance of
inserting a temperature sensor.
60.03° about the center position, that is, a total amplitude of
6.2.2 Dies—Two which form a cavity when closed and
2°. Other amplitudes may be used, if specified.
which shall be fabricated from tool steel having a minimum
Rockwell Hardness HRC 50. The geometry of the standard NOTE 1—Where the effect of surface contamination on the disk is not

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FIG. 3 Lower Die

a problem, greater sensitivity in determining curing characteristics may be

obtained using 63° angle of oscillation.
6.2.4 Die Closing Mechanism—A pneumatic cylinder or FIG. 4 Upper Die
other device shall close the dies and hold them closed during
the test with a force of 11.0 6 0.5 kN (2500 6 100 lbf). TABLE 1 Die Dimensions
Dimension, Tolerance,
NOTE 2—The manufacturer recommends the source air pressure be Code
mm mm
adjusted to 345 kPa (50 psi). Provisions are made for this adjustment in
the instrument. Therefore, 345 kPa acting on the instrument’s 203-mm A 55.88 60.13
B 10.64 60.25
(8-in.) diameter air cylinder will produce a force of 11 kN (2500 lbf) on
C 7.94 60.13
the die per the following equation: D 18.26 60.13

F5P S DpD2
4 (1)
E
F
G
1.57
0.8
4.76
60.13
60.1
60.13
H 24.07 60.06
where: I 12.70 60.40
F = closure force on die, J 2.38 60.40
P = source air pressure, and K 54.61 60.05
D = diameter of piston in pneumatic cylinder. L 41.91 60.03
M 5.35 60.01
To calculate maximum cavity pressure, the effect of this force acting on
N 1.65 60.03
the surface area of the upper die may be calculated per the following O 4.57 60.13
equation: P 15.38 60.03
Q 5.08 60.05
4F
Pc 5 (2) R 41.91 60.03
pd 2

where:
Pc = pressure on sample in upper die cavity, and
d = diameter of upper die cavity (55.9 mm (2.2 in.)). 10 000
5 12.06
~For example, Pc 5 Pc S 5 829 psi. D (3)
~4!~2500!
5 6.3 Temperature Controlling System—A temperature con-
~3.14!~2.2!2
10 000 troller shall be provided for maintaining the dies within
5
~3.14!~4.84! 60.5°C (61°F) of the specified test temperature.

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 D 2084
use of any suitable data collection device, including printers, plotters, and
computers.
NOTE 4—Direct proportionality between torque and stiffness cannot be
expected under all test conditions, particularly in higher torque ranges,
because elastic deformation of the disk shaft and driving device must be
taken into account. However, for routine quality control test purposes
corrections are not necessary.

7. Sampling
7.1 The sample shall be taken from a vulcanizable rubber
compound as required by the mixing method or other sampling
instructions.
7.2 The sample shall be in sheeted form, at room tempera-
ture, and as free of air as possible.
8. Test Specimen
8.1 A circular test specimen taken from a sample shall be 30
6 2 mm (1.2 6 0.1 in.) in diameter and 11.5 6 1.5 mm (0.45
6 0.05 in.) in thickness or equivalent to a volume of 9 cm3 (0.5
in.3).
8.2 The test specimen is considered to be of proper size
when a small bead of compound is extruded uniformly around
the periphery of the die as it is closed. This is achieved when
the specimen volume is between 8 and 11 cm3(9 to 13 g of
rubber compound with a specific gravity of 1.15). Undersized
specimens can cause low cavity pressure and low torque
readings. Oversized specimens cool the dies excessively during
the early part of the test cycle affecting the vulcanization
characteristics.
9. Test Temperatures
FIG. 5 Biconical Disk
9.1 The standard test temperature shall be 160°C (320°F).
9.2 The test temperature tolerance shall be 60.5°C
TABLE 2 Disk Dimensions
(61.0°F).
Code Dimension, mm Tolerance, mm
9.3 Tests may be carried out at other temperatures, if
S Diameter 35.55 60.01 required. They should be selected in accordance with Practice
T Radius 0.80 60.03
U 6.28° 60.08° D 1349.
VA Groove width 0.80 60.05
Groove depth 0.8 60.1 10. Calibration
Groove lengths, min 7.5
12.5
10.1 The cure meter shall be calibrated mechanically in
WA Groove width 0.80 60.05 accordance with the manufacturer’s instructions.
Groove depth 0.8 60.1 10.2 Provisions shall be made for electronic verification of
Groove lengths, min 7.5
9.5 the recorder and for torque transducer calibration by means of
X Diameter 9.50 60.02 a resistor incorporated in the torque measuring circuit that
−0.00 simulates an applied torque of specified value.
A
Grooves on top and bottom surfaces should be displaced 5°. 10.3 The cure meter shall be calibrated with the torque
standard supplied by the manufacturer any time the results are
suspected of being inaccurate, after any repairs, any change in
6.4 Torque Measuring System—The torque measuring sys-
arc, or frequently enough to ensure the maintenance of proper
tem shall consist of a device, such as a torque transducer,
calibration. The cure meter shall read zero when running empty
producing a signal that is directly proportional to the torque
and read the certified value with the torque standard inserted.
required to oscillate the disk. A recorder to record the maxi-
mum amplitude signal from the torque transducer shall be 11. Procedure
provided. The recorder shall have a full-scale deflection
11.1 Preparation for Test:
response on the torque scale of 1 s or less and be capable of
11.1.1 Bring the temperature of both dies to the temperature
recording the torque with accuracy of 60.5 % of the torque
of test with the disk in place and the dies in the closed position.
range. Four torque ranges shall be provided; 0 to 25, 0 to 50,
Set recorder range to zero and adjust the recorder pen to zero
0 to 100, and 0 to 200 dN·m (or 0 to 25, 0 to 50, 0 to 100, and
torque and zero time position on the chart. Select the correct
0 to 200 lbf· in.)
running time and choose the torque range to give maximum
NOTE 3—The term “recorder” as used in this test method implies the torque in the upper half of the recorder chart.

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11.1.2 “Running Zero” may be checked at this point and 12.2.3.1 tS1 is equal to the time to 1 dN·m (or lbf·in.) rise
should be off no more than 0.5 dN·m (or 0.5 lbf·in.). If in above ML; is used with 1° amplitude.
excess of this, check the cure meter for frictional drag that 12.2.3.2 tS2 is equal to the time to 2 dN·m (or 2 lbf·in.) rise
could be caused either by bad bearings, by improper friction above ML; is used with 3° (and 5°) amplitudes.
seal (6.2.2), by rotor misalignment, or by sample “build-up” 12.2.4 Cure time, min.
around the rotor shaft. If the error persists, consult the 12.2.4.1 t8 x is equal to the time to x % of torque increase
manufacturers manual. or t8x = minutes to ML + x(MH − ML)/100 torque.
11.2 Loading the Cure Meter:
NOTE 7—This test method of determining the cure times is considered
11.2.1 Open the dies, place the test specimen (Note 5 and the standard test method.
Note 6) on top of the disk and close the dies. This operation
must be completed within 20 s. 12.2.4.2 tx is equal to the time to x % of maximum torque,
11.2.2 Start the recorder at the instant the dies are closed. or t x = minutes to x MH/100 torque.
The disk may be oscillating at zero time or oscillation may be NOTE 8—This is an alternative test method for cure time determination.
started not later than 1 min after the dies are closed. In the latter The most commonly used values of x are 50 and 90.
case, report preheat as required in 12.1.8. 12.2.5 Cure Rate Index = 100/(cure time − scorch time).
NOTE 5—When testing sticky rubber compounds, cellophane, or other 13. Precision and Bias
thin film that will not melt at the test temperature, may be inserted below
and above the test specimen, but not against the rotor. This prevents the 13.1 This precision and bias section has been prepared in
rubber from sticking to the dies. Suitable film materials are Dupont 600 accordance with Practice D 4483. Refer to Practice D 4483 for
PD/001,4 Avisco 300P1,5 or Polyester Film Mylar Type A-100.6 terminology and other statistical calculation details.
NOTE 6—A deposit of material from the rubber compounds under test 13.2 All precision data were obtained using the diaphragm
may build up on the disk and dies. This may affect the final torque values. upper die shown in Fig. 4. The use of the alternative solid die
It is suggested that stable vulcanizable rubber compound be tested daily to shown in Fig. A1.1 may cause different results.
detect this occurrence. If such contamination develops, it may be removed
by cleaning with a noncorrosive compound or solution that does not
13.3 Both Type 1 and Type 2 precision results are given in
degrade the aluminum insert contained in the upper die of most cure Table 3. For both types of precision repeatability and repro-
meters. After solvent cleaning one or two runs on a nonessential rubber ducibility are short term; a period of a few days separates
compound are required to eliminate solvent or residue completely. replicate test results. A test result is the test value, as specified
Abrasive cleaning may be used with caution. The recommended cleaner is by this test method, obtained on one determination or measure-
220 grit aluminum oxide. ment of the property or parameter in question.
12. Report 13.4 For the Type 1 precision, four compounds (or materi-
als) were used; these were tested in eleven laboratories on two
12.1 Report the following information on the sample and different days (see Table 3).
instrument used: 13.5 For the Type 2 precision, the precision results reported
12.1.1 Sample or specimen identification, or both, in Table 3 represent pooled average values obtained from four
12.1.2 Method of specimen preparation (for example, (other) rubber evaluation standards; Test Methods D 3185
amount of milling), (SBR, OE-SBR) and Methods D 3186 (SBR-BMB), D3187
12.1.3 Make and model of the cure meter, (NBR), and D3190 (CR). These precision values are derived
12.1.4 Temperature of the dies, from interlaboratory programs with two different types of
12.1.5 Amplitude of oscillation used, reported as half of materials (for each rubber as listed above), in seven laborato-
total amplitude, ries with the mixing and testing both conducted on two
12.1.6 Frequency of oscillation, Hz (or cpm), different days essentially one week apart.
12.1.7 Recorder range, 13.6 The precision of this test method may be expressed in
12.1.8 Full-scale recorder time, and the format of the following statements that use what is called
12.1.9 Preheat time, if not zero. an “appropriate value” of r, R, (r), or (R), that is, that value
12.2 Test results reported are normally chosen from the obtained from Table 3, to be used in decisions about test results
following parameters (refer to Fig. 1 for guidance). The (obtained with the test method).
conversion from dN·m to lbf·in. is: 1.13 (dN·m) = 1.00 13.7 Repeatability—The repeatability, r, of this test method
(lbf·in.). has been established as the appropriate value for any parameter
12.2.1 ML—Minimum torque, dN·m (lbf·in.). as tabulated in Table 3. Two single test results, obtained under
12.2.2 Maximum torque—All in dN·m (or lbf·in.). normal test method procedures, that differ by more than this
12.2.2.1 MHF—Maximum torque where curve plateaus. tabulated r must be considered as derived from different or
12.2.2.2 MHR—Maximum torque of reverting curve. nonidentical sample populations.
12.2.2.3 MH—Highest torque attained during specified pe- 13.8 Reproducibility—The reproducibility, R, of this test
riod of time when no plateau or maximum torque is obtained. method has been established as the appropriate value for any
12.2.3 Scorch time, min. parameter as tabulated in Table 3. Two single test results
obtained in two different laboratories, under normal test
4
Dupont 600 PD/001 is suitable for this purpose.
method procedures, that differ by more than the tabulated R
5
Avisco 300P1 is suitable for this purpose. must be considered to have come from different or nonidentical
6
Polyester Film Mylar Type A-100 is suitable for this purpose. sample populations.

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TABLE 3 Precision

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). (R) = reproducibility (in percent).
Range of Mean Within Laboratory Between Laboratory
Test Parameter
Values Value Sr r (r)A SR R (R)A
Type 1 Precision:
ML(dN·m) 7.1 to 9.7 8.4 0.158 0.45 5.4 1.36 3.85 45.8
MH(dN·m) 28.4 to 38.9 33.7 0.181 0.51 1.5 1.98 5.60 16.6
tsl (min) 2.3 to 5.3 3.8 0.12 0.34 9.0 0.25 0.71 18.7
t8 50 (min) 3.9 to 8.8 6.4 0.15 0.43 6.7 0.34 0.96 15.0
t8 90 (min) 6.4 to 14.0 10.2 0.20 0.57 5.6 0.60 1.70 16.7
Type 2 Precision:
ML(dN·m) 7.6 to 9.8 8.7 0.215 0.61 7.0 0.735 2.08 23.9
MH(dN·m) 32.0 to 47.7 39.9 0.35 0.99 2.5 2.60 7.36 18.4
tsl (min) 4.4 to 5.8 5.1 0.12 0.34 6.7 0.37 1.05 20.6
t8 50 (min) 7.7 to 9.9 8.8 0.18 0.51 5.8 0.90 2.55 29.0
t8 90 (min) 15.9 to 18.0 17.0 0.19 0.54 3.2 1.50 4.25 25.0
A
These are estimated values, using the mid-point of the range for the parameter mean value.
Type 1 precision is obtained from fully prepared test specimens (compounds mixed in one laboratory); these are circulated to all participating laboratories.
Type 2 precision is obtained by circulating all compounding materials (drawn from a common source) to each participating laboratory. The mixing to prepare the
compound is done in each laboratory and therefore mixing variation is part of the “total test” variation or test precision.

13.9 Repeatability and reproducibility expressed as a per- the appendix for details and a full report on the precision
centage of the mean level, (r) and (R), have equivalent results.
application statements as 13.7 and 13.8 for r and R. For the (r) 13.11 Bias—In test method terminology, bias is the differ-
and (R) statements, the difference in the two single test results ence between an average test value and the reference (or true)
is expressed as a percentage of the arithmetic mean of the two test property value. Reference values do not exist for this test
test results. method since the value (of the test property) is exclusively
13.10 Precision (International Interlaboratory Testing)— defined by the test method. Bias, therefore, cannot be deter-
The Appendix gives precision results obtained in an interna- mined.
tional interlaboratory program conducted in ISO Technical
Committee 45 on Rubber/Rubber Products in 1984/1985. 14. Keywords
These results are given for additional background on a broad- 14.1 compounds; ODR oscillating disk cure meter; vulca-
based comprehensive interlaboratory program. Please refer to nization characteristics

ANNEX

(Mandatory Information)

A1. ALTERNATIVE UPPER DIE

A1.1 This annex describes an alternative upper die for use and then to maintain essentially constant pressure on the
in the oscillating disk cure meter (ODC). This die does not specimen as it shrinks slightly in volume during vulcanization.
contain a diaphram as shown in the die in Fig. 4.
A1.4 The precision and bias observed with the alternative
A1.2 Some manufacturers of ODC instruments furnish solid upper die as well as any differences in observed results
upper dies with a diaphram while others do not. have not been determined.
A1.3 The stated purpose of the diaphram die is to allow the A1.5 The solid upper die is shown in Fig. A1.1. Dimensions
diaphram to be flexed when the dies are closed on a specimen are listed in Table 1.

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FIG. A1.1 Alternative Upper Die

APPENDIXES

(Nonmandatory Information)

X1. INTERNATIONAL INTERLABORATORY TESTING

X1.1 This appendix gives the precision results of an TABLE X1.1 Compound Formulations (ISO 3417-ITP)
international interlaboratory Oscillating Disc Cure Meter Formulations Used
Material
(ODC) test program conducted in ISO TC-45 in 1984 and A B C D
1985. It is added as an appendix to this test method to give SBR 1502 100.0 ... ... 100.0
additional information on the precision of ODC testing. The SBR 1712A ... 68.8 137.5 ...
ISO/TC45 standard that is analogous to Test Method D 2084 is BR (CB441)B ... 68.8 ... ...
Zinc oxide 5.0 5.0 5.0 5.0
ISO 3417. Stearic acid 1.0 1.5 1.5 1.5
IRB Number 5C ... 80.0 60.0 ...
X1.2 The practice for analysis and expression of precision N330 45.0 ... ... ...
results for ISO TC45 is equivalent in its basic fundamentals Process OilD ... 8.8 5.0 5.0
DPPDE ... 1.5 1.5 1.5
and format to Practice D 4483. AntiozonantF ... 1.5 1.5 1.5
TBBSG ... 1.2 1.0 1.0
X1.3 Test Details: TMTDH 3.0 ... ... ...
Sulfur ... 2.0 2.0 2.0
X1.3.1 An interlaboratory test program (ITP) was organized __ __ __ __
in late 1984 to obtain precision results. Four compounds with Specific Gravity 1.13 1.16 1.16 0.98
a range of cure properties were mixed and prepared in one A
37.5 (phr) oil extended SBR.
B
laboratory, sealed in metal foil packets, and distributed to 37.5 (phr) oil extended, BR rubber.
C
ASTM Committee D-24 Industry Reference Carbon Black Number 5.
laboratories located in 19 countries in Europe, Asia, and North D
Sundex 7260T or equivalent.
and South America. Tests were conducted in late January and E
Dimethyl-butylphenyl-phenylene diamine.
F
early February 1985 according to the following schedule: Trimethyl-dihydroquinoline.
G
N-tert-butyl-2-benzothiazole-sulfenamide.
X1.3.1.1 Part I of 160C—One test (determination) on each H
Tetramethylthiuram disulfide.
of two days, one week apart, for all four compounds.
X1.3.1.2 Part II of 150C—One test on each of two days, pound D is a gum compound with a conventional cure system.
one week apart, for all four compounds. X1.3.3 A Type 1 precision was measured in the ITP (no
X1.3.2 The formulations for the four compounds are listed processing operations required on the circulated materials in
in Table X1.1. Compound A has a moderate black level with a any given laboratory). The time period for repeatability and
non-free sulfur (TMTD) cure system. Compounds B and C are reproducibility is on a scale of days.
relatively high black with conventional cure systems. Com- X1.3.4 A test result is (the test value) obtained from one

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 D 2084
measurement or determination with the ODC at any tempera- results for the temperature nearest to the actual test temperature
ture. under consideration.
X1.3.5 A total of 50 laboratories participated in Part I, and X1.5.1.2 Enter the Summary Precision Result section of
45 laboratories participated in Part II in addition to their either Table X1.2 or X1.3 at an average material value nearest
participation in Part I. to the test data average under consideration. This will give the
applicable r, (r), R, and (R) for use in the decision process.
X1.4 Precision Results:
X1.5.1.3 With these r and (r) values the following general
X1.4.1 The precision results for both Parts I and II are given
repeatability statements may be used to make decisions. For an
for five ODC cure parameters. These five parameters are as
absolute difference, the difference, | x1 − x2 |, between two
follows:
measured ODC parameters values, found on (presumed) iden-
X1.4.1.1 ML—Minimum torque (N·m).
tical material samples under normal and correct ODC operation
X1.4.1.2 MHF—Maximum torque (N·m).
conditions, will exceed the tabulated r, on average not more
X1.4.1.3 ts—Scorch time, (minutes).
X1.4.1.4 t1c (50)—50 % cure time, (minutes). than once in 20 cases. For a percentage difference, the percent
X1.4.1.5 t1c (90)—90 % cure time, (minutes). difference, | x1 − x2 | /(x1 + x2)/2]100, between two measured
X1.4.2 For Part I of 160C, the precision results are given in ODC parameter values, found on (presumed) identical material
Table X1.2. samples under normal and correct ODC operation conditions,
X1.4.3 For Part II of 150C, the precision results are given in will exceed the tabulated (r), on average not more than once in
Table X1.3. 20 cases.
X1.5.1.4 With these R and (R) values the following general
X1.5 Use of Precision Results: reproducibility statements may be used to make decisions. For
X1.5.1 The general procedure for using precision results is an absolute difference, the difference | x1 − x2 |, between two
with the symbol | x1 − x2 | designating a positive difference, that independently measured ODC parameter values, found in two
is, without regard to sign. The symbol x refers to any parameter laboratories using normal and correct ODC procedures on
value. identical test material samples, will exceed the tabulated
X1.5.1.1 Select the ODC parameter on which decisions are reproducibility R, not more than once in 20 cases. For a
to be made. Find in Table X1.2 (160C) or Table X1.3 (150C) percentage difference, the percent difference, | x1 − x2 |
the Summary section for this parameter. If the tests and data /(x1 + x2)/2]100, between two independently measured ODC
under consideration are not at 150 or 160C, select the summary parameter values, found in two laboratories using normal and

TABLE X1.2 ISO 3417: Type 1—Precision of 160 °C

Parameter 1—Min torque, ML (N-M) 160 °C
Final Summary Table: Precision Values
Averages given in increasing order
Within Laboratories Between Laboratories
Material Average
Sr r (r) SR R (R)
4. Compound D 0.39 0.0315 0.0892 23.040 0.1404 0.3973 102.649
3. Compound C 0.70 0.0316 0.0893 12.700 0.1997 0.5652 80.380
2. Compound B 0.99 0.0339 0.0960 9.652 0.4399 1.2448 125.147
1. Compound A 1.65 0.0656 0.1857 11.249 0.1442 0.4081 24.715
Pooled values 0.92 0.0432 0.1223 13.298 0.2645 0.7486 81.422
Parameter 2—Max torque, MHF (N-M) 160 °C
Final Summary Table: Precision Values
Averages given in increasing order
Within Laboratories Between Laboratories
Material Average
Sr r (r) SR R (R)
4. Compound D 2.21 0.0582 0.1646 7.447 0.1996 0.5648 25.550
3. Compound C 2.71 0.0511 0.1446 5.328 0.2207 0.6246 23.007
2. Compound B 3.26 0.0750 0.2123 6.521 0.2625 0.7430 22.820
1. Compound A 4.26 0.0546 0.1544 3.621 0.3628 1.0266 24.073
Pooled Values 3.11 0.0605 0.1713 5.506 0.2686 0.7602 24.432
Parameter 3—Scorch time, (min) 160 °C
Final Summary Table: Precision Values
Averages given in increasing order
Within Laboratories Between Laboratories
Material Average
Sr r (r) SR R (R)
1. Compound A 1.41 0.1028 0.2910 20.580 0.1547 0.4377 30.957
4. Compound D 5.04 0.2017 0.5708 11.324 0.7011 1.9842 39.364
2. Compound B 5.08 0.1836 0.5197 10.222 0.7278 2.0598 40.512
3. Compound C 5.57 0.2302 0.6515 11.689 0.6752 1.9109 34.284
Pooled Values 4.32 0.1854 0.5247 12.140 0.6234 1.7642 40.822

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TABLE X1.3 ISO 3417: Type 1—Precision of 150 °C

NOTE 1—Sr = repeatability standard deviation. r = repeatability = 2.83 (square root of the repeatability variance). (r) = repeatability (as percentage of
material average). SR = reproducibility standard deviation. R = reproducibility = 2.83 (square root of the reproducibility variance). (R) = reproducibility
(as percentage of material average).
Parameter 1—Min torque, ML (N-M) 150 °C
Final Summary Table: Precision Values
Averages given in increasing order
Within Laboratories Between Laboratories
Material Average
Sr r (r) SR R (R)
4. Compound D 0.40 0.0300 0.0848 21.000 0.1286 0.3639 90.135
3. Compound C 0.69 0.0403 0.1141 16.448 0.1025 0.2901 41.798
2. Compound B 0.77 0.0258 0.0730 9.511 0.0743 0.2101 27.376
1. Compound A 1.74 0.0517 0.1463 8.399 0.1616 0.4574 26.250
Pooled Values 0.90 0.0384 0.1086 12.098 0.1221 0.3457 38.505
Parameter 2—Max torque, MHF (N-M) 150 °C
Final Summary Table: Precision Values
Averages given in increasing order
Within Laboratories Between Laboratories
Material Average
Sr r (r) SR R (R)
4. Compound D 2.31 0.0324 0.0916 3.960 0.1942 0.5495 23.768
3. Compound C 2.82 0.0684 0.1937 6.861 0.2431 0.6878 24.364
2. Compound B 3.39 0.0642 0.1818 5.354 0.2654 0.7511 22.124
1. Compound A 4.34 0.0787 0.2228 5.134 0.2464 0.6972 16.066
Pooled Values 3.20 0.0633 0.1793 5.594 0.2397 0.6783 21.169
Parameter 3—Scorch time, (min) 150 °C
Final Summary Table: Precision Values
Averages given in increasing order
Within Laboratories Between Laboratories
Material Average
Sr r (r) SR R (R)
1. Compound A 1.99 0.1141 0.3230 16.265 0.2471 0.6992 35.214
2. Compound B 8.61 0.4932 1.3958 16.213 1.2572 3.5577 41.325
4. Compound D 8.77 0.2524 0.7143 8.149 0.6697 1.8951 21.621
3. Compound C 9.73 0.3233 0.9150 9.406 1.3838 3.9161 40.257
Pooled Values 7.31 0.3266 0.9243 12.650 0.9867 2.7924 38.217
Parameter 4—50 % cure time, (min) 150 °C
Final Summary Table: Precision Values
Averages given in increasing order
Within Laboratories Between Laboratories
Material Average
Sr r (r) SR R (R)
1. Compound A 5.56 0.2100 0.5943 10.691 0.4654 1.3172 23.696
2. Compound B 13.34 0.5602 1.5852 11.882 0.9905 2.8032 21.011
3. Compound C 17.20 0.3975 1.1250 6.539 1.1619 3.2883 19.113
4. Compound D 17.56 0.3393 0.9603 5.470 1.1049 3.1269 17.812
Pooled Values 13.46 0.3983 1.1272 8.374 0.9726 2.7525 20.448
Parameter 5—90 % cure time, (min) 150 °C
Final Summary Table: Precision Values
Averages given in increasing order
Within Laboratories Between Laboratories
Material Average
Sr r (r) SR R (R)
1. Compound A 11.91 0.6954 1.9680 16.521 1.2683 3.5894 30.133
2. Compound B 19.90 0.7055 1.9964 10.031 1.4111 3.9934 20.065
3. Compound C 30.07 0.6387 1.8075 6.010 2.1003 5.9439 19.763
4. Compound D 33.52 0.9787 2.7699 8.264 2.5473 7.2088 21.507
Pooled Values 23.91 0.7671 2.1708 9.080 1.9092 5.4030 22.599

correct ODC procedures on identical material samples, will

exceed the tabulated reproducibility (R), not more than once in
20 cases.

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X2. HISTORY OF THE OSCILLATING DISK CURE METER

X2.1 Oscillating disk cure meters were first made commer- dies and rotor. Higher strain leads to higher torques, and the
cially available in 1963. The first units oscillated at a frequency smaller specimen (10 to 12 g for a stock with a specific gravity
of three cycles per minute, typically at 63° of arc. The dies of 1.15) gives a cure curve with a significantly different shape,
(SCD) for these early cure meters were commonly a 2-in. as shown in Fig. X2.2. Higher torques have been shown to
square cavity 0.4 in. high, with a biconical rotor centered in the cause slippage at the surface of the rotor for many stocks, and
cavity. A typical rubber sample of 1.15 specific gravity that slippage is a potential source of variation in test results.
weighed 22 g, and was loaded in two pieces, above and below Studies conducted with the smaller dies and rotor indicated
the rotor. A20 to 60-s preheat was required after closure before slippage due to rotor contamination was common above 50
collecting data. The strain on the sample at 3° arc was 21 %. in.·lbs of torque. As a result, Test Method D 2084 specifies a 1°
arc of oscillation as standard, with a 16 % shear strain.
X2.2 Frequencies of oscillation of 10, 100, and 900 cpm
were made available over the next five years. These created X2.5 The curves obtained with MPC dies at 1° arc were
different curve shapes due to the heat energy added to the used as standards until 1987, when further reductions in the
cavity in working the rubber, breakdown of polymer structure temperature recovery time became possible due to improved
when curing under dynamic conditions, and the shear rate temperature controllers.
dependence of the rubber flow resistance. Fig. X2.1 compares
the cure meter curves for the various speeds of oscillation using X2.6 Another improvement introduced at this time was the
the square dies and an arc of 63°. reduction of the mechanical compliance of the rotor drive
system for improved reproducibility between instruments. The
X2.3 When the oscillating disk cure meter was first improved mechanical design increased maximum torques, but
proposed as an ASTM standard in 1968, a smaller, production- lowered minimum torques by reducing friction. Faster tem-
sized table model of the cure meter was introduced along with perature recovery has two advantages: first, the cure is closer to
a new die that was 2 in. in diameter (LPC dies). This circular the desired cure temperature of the test for more accurate
die had the same height and used the same rotor as the square results; second, the potential for variation in results due to
dies. The LPC die produced similar torque values for minimum cooling of the rotor during loading and unloading is greatly
and maximum torques as the SCD die. The sample could be reduced. Table X2.1 illustrates the potential operator effects.
loaded as one piece on top of the rotor for most stocks. The
X2.7 As part of the continuing evolution in cure meter
practice of adding a preheat, as commonly used with the SCD
design, a number of manufacturers have introduced rotorless
die, was eliminated. The elimination of the preheat time led to
cure meters. These cure meters use a sample of 3 to 5 g, with
slightly faster cures for the LPC die. Another advantage of this
a thinner cross section to obtain more rapid temperature
die was the flat lower die surface which allowed easier removal
recovery and more uniform temperature throughout the speci-
of the cured sample for most stocks.
men. The dies are usually directly heated, and smaller in mass
X2.4 In 1971, a smaller version of the LPC die, called the than for the oscillating disk cure meters, so that faster tem-
MPC die, was adopted in conformance with Test Method perature recovery can be achieved. By eliminating the rotor,
D 2084. The MPC die used a rotor with a different conical the surface area under load is reduced so that smaller torque
angle. At 3° of arc, the strain is 48 % versus 21 % for the larger values are achieved. Faster temperature recovery leads to faster
cure times. Fig. X2.3 compares typical cure curves for an SBR
stock from the rotorless and oscillating disk cure meters.

FIG. X2.1 Comparison of Oscillation Frequencies Using the

Square Die and 63° Arc FIG. X2.2 Comparison of Cure Meter Dies

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TABLE X2.1 Operator Effects on ODR Cure Meter Tests
Cure Times, min
Sample Loading Variable
TS2 T850 T890
Slow Temperature Recovery:
Optimum loading time (20 s) 2.01 3.51 5.86
2-min loading time 2.33 3.90 6.33
% change with loading time 15.9 11.1 8.0
Rapid Temperature Recovery:
Optimum loading time (20 s) 1.71 3.06 5.40
2-min loading time 1.86 3.23 5.60
% change with loading time 8.8 5.6 3.7

FIG. X2.3 Comparison of Cure Meters Using SBR Stock

X3. ALTERNATIVE BICONICAL DISK

X3.1 This appendix describes an alternative biconical disk biconical disk show in Fig. 5. This modification has provisions
for use in the oscillating disk cure meter (ODC). The alterna- for directly controlling the disk temperature, as shown in Fig.
tive disk described in this appendix is directly heated for the X3.2. In this example, an electrical heater and temerature
purpose of maintaining the temperature of the disk at the sensor are located in a metal tube, which is inserted in the disk
specified test temperature during the total testing interval. throught a vertical well in the disk shaft. The well is typically
33 cm (0.130 in.) in diameter and extends to within 0.25 cm
X3.2 Some manufactures of ODC instruments offer a
(0.100 in.) of the disk apex. The insertion tube diameter is
heated rotor, while others do not. If the disk is heatd, both
typically 0.1 cm (0.005 in.) less than the well diameter,
torque values and cure times may be signifcantly altered. Fig.
allowing easy tube removal for cleaning.
X3.1 shows an example of the difference in cure curves. Test
results between ODC tests using heated and unheated disks X3.4 A temperature controller shall be provided for main-
canot be compared without taking the differences in heating taining the disk temperature within 6 0.5°C (6 1.0°F) of the
into account. When a heated rotor is used, it shall be reported specified test temperature.
with the test results.
X3.3 The alternative heated disk is a modification of the

FIG. X3.1 Comparison of Cure Curves With Heated and Unheated

Rotors FIG. X3.2 Example of an ODC Rotor With Provision for Heating

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X3.5 The precision and bias of ODC tests run with the
alternative heated biconical disk have not been statistically
determined.

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