ASTM D1646-19a

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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: D1646 − 19a

Standard Test Methods for


Rubber—Viscosity, Stress Relaxation, and Pre-Vulcanization
Characteristics (Mooney Viscometer)1
This standard is issued under the fixed designation D1646; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope 1.5 The values stated in SI units are to be regarded as the


1.1 These test methods cover procedures for measuring a standard. The values given in parentheses are for information
property called Mooney viscosity. Mooney viscosity is defined only.
as the shearing torque resisting rotation of a cylindrical metal 1.6 This standard does not purport to address all of the
disk (or rotor) embedded in rubber within a cylindrical cavity. safety concerns, if any, associated with its use. It is the
The dimensions of the shearing disk viscometer, test responsibility of the user of this standard to establish appro-
temperatures, and procedures for determining Mooney viscos- priate safety, health, and environmental practices and deter-
ity are defined in these test methods. mine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accor-
1.2 When disk rotation is abruptly stopped, the torque or
dance with internationally recognized principles on standard-
stress on the rotor decreases at some rate depending on the
ization established in the Decision on Principles for the
rubber being tested and the temperature of the test. This is
Development of International Standards, Guides and Recom-
called “stress relaxation” and these test methods describe a test
mendations issued by the World Trade Organization Technical
method for measuring this relaxation.
Barriers to Trade (TBT) Committee.
NOTE 1—Viscosity as used in these test methods is not a true viscosity
and should be interpreted to mean Mooney viscosity, a measure of 2. Referenced Documents
shearing torque averaged over a range of shearing rates. Stress relaxation
is also a function of the test configuration and for these test methods the 2.1 ASTM Standards:2
results are unique to the Mooney viscometer. D1349 Practice for Rubber—Standard Conditions for Test-
1.3 When compounded rubber is placed in the Mooney ing
viscometer at a temperature at which vulcanization may occur, D1418 Practice for Rubber and Rubber Latices—
the vulcanization reaction produces an increase in torque. Nomenclature
These test methods include procedures for measuring the initial D1485 Practice for Rubber from Natural Sources—
rate of rubber vulcanization. Sampling and Sample Preparation
D3182 Practice for Rubber—Materials, Equipment, and Pro-
1.4 ISO 289 Parts 1 and 2 also describes the determination cedures for Mixing Standard Compounds and Preparing
of Mooney viscosity and pre-vulcanization characteristics. In Standard Vulcanized Sheets
addition to a few insignificant differences there are major D3185 Test Methods for Rubber—Evaluation of SBR
technical differences between ISO 289 and this test method in (Styrene-Butadiene Rubber) Including Mixtures With Oil
that ISO 289 does not provide for sample preparation on a mill, D3186 Test Methods for Rubber—Evaluation of SBR
while this test method allows milling sample preparation in (Styrene-Butadiene Rubber) Mixed With Carbon Black or
some cases prior to running a Mooney viscosity test. This can Carbon Black and Oil
result in different viscosity values for some rubbers. D3896 Practice for Rubber From Synthetic Sources—
Sampling
1
These test methods are under the jurisdiction of ASTM Committee D11 on
Rubber and Rubber-like Materials and are the direct responsibility of Subcommittee
2
D11.12 on Processability Tests. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2019. Published November 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1959. Last previous edition approved in 2019 as D1646 – 19. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D1646-19A. the ASTM website.

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

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D1646 − 19a
D4483 Practice for Evaluating Precision for Test Method 5. Significance and Use
Standards in the Rubber and Carbon Black Manufacturing 5.1 Viscosity—Viscosity values determined by this test
Industries method depend on molecular structure, molecular weight, and
2.2 ISO Standard:3 non-rubber constituents that may be present. Since rubber
ISO 289 Rubber, Unvulcanized—Determinations Using the behaves as a non-Newtonian fluid, no simple relationship
Shearing Disk Viscometer, exists between the molecular weight and the viscosity.
Part 1 Determination of Mooney Viscosity, and Therefore, caution must be exercised in interpreting viscosity
Part 2 Determination of Prevulcanization Characteristics. values of rubber, particularly in cases where molecular weight
is very high. For example, as the molecular weight increases,
3. Terminology the viscosity values for IIR polymers (butyl rubbers) reach an
3.1 Definitions of Terms Specific to This Standard: upper limit of about 80, at 100°C (212°F) using a large rotor at
a rotation speed of 2 r/min, and may then decrease to
3.1.1 Mooney viscosity, n—measure of the viscosity of a
considerably lower values. For these higher molecular weight
rubber or rubber compound determined in a Mooney shearing
rubbers, better correlation between viscosity values and mo-
disk viscometer; viscosity is indicated by the torque required to
lecular weight is obtained if the test temperature is increased.
rotate a disk embedded in a rubber specimen and enclosed in
the die cavity under specified conditions. 5.2 Stress Relaxation—The stress relaxation behavior of
rubber is a combination of both an elastic and a viscous
3.1.2 pre-vulcanization characteristics, n—for a vulcaniz-
response. Viscosity and stress relaxation behavior do not
able compound, a measure of the time to the incipient
depend on such factors as molecular weight and non-rubber
vulcanization and the rate of cure during the early stages of
constituents in the same way. Thus both of these tests are
vulcanization.
important and complement each other. A slow rate of relaxation
3.1.3 stress relaxation, n—response of a raw or com- indicates a higher elastic component in the overall response,
pounded rubber to a rapid cessation of flow or a sudden while a rapid rate of relaxation indicates a higher viscous
deformation; specific to the use of the shearing disk component. The rate of stress relaxation has been found to
viscometer, it takes the form of a decaying level of stress correlate with rubber structure characteristics such as molecu-
initiated by suddenly stopping the rotation of the disk. lar weight distribution, chain branching, and gel content.
3.1.4 test temperature, n—steady-state temperature of the 5.3 Pre-Vulcanization Characteristics—The onset of vulca-
closed dies with rotor in place and the cavity empty; this nization can be detected with the Mooney viscometer as
steady-state temperature shall be measured within the dies as evidenced by an increase in viscosity. Therefore, this test
described in 6.1.3. method can be used to measure incipient cure (scorch) time and
the rate of cure during very early stages of vulcanization. This
4. Summary of Test Methods test method cannot be used to study complete vulcanization
4.1 These test methods are divided into three parts: because the continuous rotation of the disk will result in
4.1.1 Part A: Viscosity—This test method describes the slippage when the specimen reaches a stiff consistency.
measurement of the Mooney viscosity. The Mooney viscosity
is measured by a metal disk embedded in a rubber specimen 6. Apparatus
contained in a rigid cylindrical cavity maintained at a specified 6.1 Mooney Viscometer—An instrument consisting of a
pressure and temperature. The disk is slowly and continuously motor-driven rotating disk within a cylindrical die cavity
rotated in one direction for a specified time. The resistance to formed by two dies maintained at specified conditions of
this rotation offered by the rubber is measured in arbitrary temperature and die closure force. The Mooney viscometer
torque units as the Mooney viscosity of the specimen. measures the effect of temperature and time on the viscosity of
4.1.2 Part B: Stress Relaxation—This test method describes rubbers. If the stress relaxation test is to be performed, the
the procedure to measure stress relaxation. At the end of a instrument must be capable of quickly stopping the rotation of
Mooney viscosity test, the rotation of the metal disk is the disk and monitoring the relaxation of stress versus time.
suddenly stopped and the rate of decrease of torque is The die-rotor relationship of an example design is shown in
monitored as a function of time. Fig. 1. The Mooney viscometer shall incorporate the following
4.1.3 Part C: Pre-Vulcanization Characteristics—This test components:
method describes how pre-vulcanization properties may be 6.1.1 Dies—The dies and die holders forming the die cavity
measured. The viscosity of vulcanizable rubber compounds is shall be fabricated from a nondeforming tool steel, shall have
recorded during heating at a specified temperature. The mini- an unplated finish, and shall be hardened to a Rockwell
mum viscosity and the times for the viscosity to increase by hardness of 60 HRC minimum. The dimensions of the die
specified amounts are used as arbitrary measures of the start cavity, measured from the highest surfaces, shall be 50.93 6
and rate of vulcanization. 0.13 mm (2.005 6 0.005 in.) in diameter and 10.59 6 0.03 mm
(0.417 6 0.001 in.) in depth. The surfaces of the die cavity
shall either be serrated or contain V-grooves to minimize
3
slippage of the specimen.
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036. NOTE 2—The two types of dies may not give the same results.

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D1646 − 19a

FIG. 1 Relationship of Platens, Dies, and Rotor in a Typical Shearing Disk Viscometer

6.1.1.1 Serrated Dies—When the cavity is formed from four holding them closed during a test. During a test it is extremely
pieces of steel, serrations on the surfaces of the dies and die important that the die cavity be held closed with the correct
holders are used. These serrations consist of rectangular force. To obtain the correct closing force for the mechanical-
grooves 0.8 6 0.02 mm (0.031 6 0.0008 in.) wide with a type closures, follow explicitly either the manufacturer’s rec-
uniform depth of not less than 0.25 mm (0.010 in.) nor more ommendation or other procedure of equal reliability.4 Pneu-
than 0.38 mm (0.015 in.). The grooves shall be vertical and matically closed dies shall be held closed during the test with
shall be cut on 1.6 6 0.04 mm (0.063 6 0.002 in.) centers. The a force of 11.5 6 0.5 kN (2585 6 115 lbf). A greater force may
serrations of the dies shall consist of two sets of such grooves be required to close the dies when testing extremely tough
at right angles to each other. stocks. At least 10 s before the motor is started, the force
6.1.1.2 Radial Grooved Dies—When the die cavity is should be set to 11.5 6 0.5 kN. The die closure shall be such
formed from two pieces of steel, radial V-grooves are used only that a piece of thin soft tissue (with a thickness not greater than
on the flat surfaces of the die cavity. The grooves shall be 0.04 mm (0.0015 in.)) placed between the meeting surfaces
spaced at 20° intervals and shall form a 90° angle in the die will retain a continuous pattern of uniform intensity when the
surfaces with the bisector of the angle perpendicular to the dies are closed upon it. A nonuniform pattern indicates wear of
surface. They shall extend from the 7-mm (0.281-in.) circle to the die holder surface, misalignment, or distortion of dies and
the 47-mm (1.875-in.) circle in the upper die and from the die holders. Any of these situations will result in undue leakage
12-mm (0.472-in.) circle to the 47-mm circle in the lower die. and erroneous results.
The grooves shall be 1 6 0.1 mm (0.04 6 0.004 in.) wide at NOTE 4—For mechanical-type closure viscometers, the pressure on the
the surface. die cavities may change if the viscometer is used at a different temperature
NOTE 3—Die wear can affect test results, usually to a lesser extent than than that at which it is adjusted.
rotor wear. As a general practice, many users replace dies every second 6.1.2 Rotors—Two rotors are specified, differing only in
time they replace worn rotors (see 6.1.2.1). This practice may not apply to their diameter. They shall be fabricated from a nondeforming
all materials tested, as wear is material dependent. The ultimate way to
determine if die wear has affected test results is to replace the dies with a
tool steel, shall have an unplated finish and shall be hardened
new set and determine if the test results are changed. to a Rockwell hardness of 60 HRC minimum. The large rotor
shall be 38.10 6 0.03 mm (1.500 6 0.001 in.) in diameter and
6.1.1.3 Mounting of Dies—The dies shall be an integral part
5.54 6 0.03 mm (0.218 6 0.001 in.) in thickness as measured
of or mounted on platens equipped with a heating device and
from the highest points. The small rotor shall conform to the
controls capable of maintaining the die cavity at the specified
large rotor except the diameter shall be 30.48 6 0.03 mm
test temperature with a tolerance of 60.5°C (61°F) at equi-
librium conditions.
6.1.1.4 Die Closure—The viscometer shall have a suitable 4
Decker, G. E., “Note on the Adjustment of the Mooney Viscometer Die
device for opening and closing the platens and dies and for Closure,” ASTM Bulletin, No. 195, January 1954, p. 51.

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