Rubber Testing

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Eschborn, Germany Montreal, Canada Rubber Testing
Rubber Process Analyzer 4
Brussels, Belgium
Moving Die Rheometer 8
Mooney Viscometer 10
Technology 12
Sample Cutter 17
Automation 18
Density 20
Hardness 22
Software 24
Applications 26
Rubber Testing
TA Instruments introduces a complete line of new instruments for the measurement of rheological and physical
properties of polymers, rubber and rubber compounds at all stages of manufacture. The new rubber testing
instruments include a Rubber Process Analyzer (RPA), Moving Die Rheometer (MDR), Mooney Viscometer,
Automated Density Tester and Automated Hardness Tester.

All TA Instruments rubber testing systems are manufactured to exacting mechanical standards and with the latest
measurement technology for the most accurate, reliable, and reproducible data available. Available automation
systems allow for maximum unattended laboratory productivity in all test environments. Relevant ASTM, DIN, and
ISO standards are easily met, as are demands for advanced testing, making these instruments the ideal choice
for quality control, analytical, and research needs.

As the world leader in viscoelastic measurements for over forty years, TA Instruments brings technical expertise
in making the most accurate physical property measurements and provides a world-renowned global support
network.

3
 MDR one
Moving Die Rheometer

The MDR one Moving Die Rheometer (MDR) is a reliable, accurate, and easy-to-operate rotorless curemeter perfect for routine and Features
standards-driven testing of rubber curing. The MDR one is configured for measuring curing profiles of rubber compounds under • Unmatched data precision, accuracy, and reproducibility
isothermal and non-isothermal test conditions at constant strain and frequency. The MDR one employs sealed biconical dies
•Robust, field-proven torque transducer for high stability,
meeting all relevant ASTM, ISO, and DIN standards. The unique design includes an ultra-rigid test frame, direct drive motor, precision reliable torque measurements
temperature control with optional cooling, available Autosampler, and intuitive Scarabaeus Software for control and analysis
• Extremely rigid test frame for accurate compliance-free data
making it the ideal platform for QC or R&D environments.
•Available autosampler for simple unattended operation
•Pneumatic locking cylinders for repeatable sample sealing
•Powerful and Intuitive Scarabaeus Software available in multiple
languages & compatible with other manufacturers’ instruments

• User calibration and user-replaceable seals

Specifications
Frequency Fixed: 1.67 Hz (100 cpm)
Amplitude ±0.2°, 0.5°, 1.0°, 3.0° arc
Strain ±2.–8 %, 7 %, 14 %, 42 %
Torque 0.1 to 20 N.m
Temperature Ambient to 230 °C
18 °C to 230 °C with Enhanced Cooling Option
Maximum Ramp Rate 80°C/min (1.33°C/s)
Die Type Sealed bicone, 0.48 mm gap
Sample volume 4.5 cm3
Platen Sealing Pressure Fixed: 4.5 bar
Test Modes Curemeter/Vulcanization both isothermal and temperature ramp
Measured Data Torque, Temperature, Frequency, Amplitude, Sample Pressure (optional)
Calculated Data Process parameters including: ts1, TC10, TC50, TC90, S’min, S’max, scorch time, cure rate,
and viscoelastic properties including: G’, G”, G*, S’, S”, S*, tan δ, η’, η”, η*
Standards ASTM D5289, ISO 6502, DIN 53529

8 Moving Die Rheometer 9

 technology

Direct Drive Motor

Powerful direct drive motors apply precise
deformation in all TA Instruments rubber rheometers
and viscometers. A high quality rheological or
dynamic measurement relies on the precise
application of a constant rate, step, or periodic
TA Instruments is the world’s leading supplier of analytical
deformation. In a direct drive system the start-up
instrumentation for the measurement of viscosity and
delays, compliance, and translational losses seen in
viscoelastic properties. The new rubber testing instruments
clutch or belt-driven configurations are eliminated.
are uniquely designed to deliver the highest quality of torque,
The superior TA Instruments motor design
amplitude, frequency, temperature, and pressure measurement
ensures that the most accurate and repeatable
and control. TA Instruments is the CLEAR CHOICE for testing
deformations are always applied to the sample.
rubber products at all stages of manufacture.

The RPA elite and RPA flex provide continuously

variable strain and frequency ranges for
flexible testing. The RPA elite applies the highest
combination of frequency and amplitude in any
rubber rheometer. This provides important material
information such as:

Rigid Testing Platform • The linear viscoelastic response of highly filled

All TA Instruments rubber rheometers and viscometers are built with an ultra-stiff testing frame and crosshead which eliminates rubbers at low strains
the effects of instrument compliance on test data. Instrument compliance, or instrument deformation, produces erroneously • Behavior at extreme processing and use
low values of measured properties such as modulus and torque, irregular strain and torque waveform signals, and other errors. conditions characterized by high strains
• Terminal material behavior exhibited at low
Large diameter steel rods and a thick crosshead brace in the H-shaped load frame provide unmatched rigidity to resist frequencies
instrument deflection while the motor deforms the sample. This special design ensures that the commanded strain is achieved • Response to high speed deformations measured
with each cycle of deformation, even for highly filled, fully cured rubbers. Additionally, a non-compliant system allows for truly at high frequencies
sinusoidal strain profiles under all conditions. This can be verified by continuous Fourier Transform analysis of the deformation
and measured torque signals which is available in the Scarabaeus Software. The superior design also guarantees smooth travel,
proper alignment, and precise application of vertical load.

High-Stiffness Torque Transducer

The RPA elite and RPA flex benefit from a proprietary wide range ultra-stiff torque transducer. This rugged, non-compliant device
measures the widest range of torques accurately and precisely. This greatly improves the accuracy and precision of measured torque,
modulus, and viscosity values.

Advanced Data Processing

The complex deformations and stress-strain response common to rubber testing demand the most advanced data processing
techniques. TA Instruments rubber rheometers utilize a state-of-the-art 20-bit encoder and advanced data sampling technique to
perform calculations based on a Fast Fourier Transform (FFT) analysis using 90 data points for each cycle of oscillation.

The RPA elite and RPA flex are capable of measuring and reporting non-linearities in torque and displacement. Higher harmonics that
indicate non-linearity in the applied displacement or measured torque are reported for each data point, alerting the operator with a
simple indicator if test conditions are not ideal and storing this information for subsequent data validation.

12 Technology 13
 technology

Crosshead Bearing
Testing Dies and Rotors

High Pressure Pneumatic System The MDR one, RPA flex, and RPA elite rotorless shear rheometers employ the industry-standard sealed cavity biconical die design. The dies are
constructed from durable, high-stiffness, low thermal expansion stainless steel to minimize system compliance and prevent gap changes
All TA Instruments rotorless rheometers and curemeters employ a
with temperature. The test fixtures are connected directly in line with the motor below for precision deformation control and the torque
high pressure pneumatic system to seal the sample properly and
transducer above for accurate measurement.
reproducibly. The high capacity pneumatic system applies up to
8 bar nominal pressure to the sample during gap closure. Proper
Direct contact electric heaters mounted within the dies provide exceptional temperature control and stability under isothermal, step and
alignment and the use of mechanical bearings ensure efficient
temperature ramp conditions. This highly responsive system returns rapidly to the programmed test temperature upon the addition of a cold
transfer of load from the system to the sample without load frame
sample, providing the most representative values for scorch time and other cure characteristics. Extremely durable user-replaceable seals
losses. Actual sealing pressure is measured directly and recorded.
provide absolute sample containment at all temperatures and conditions.
This high pressure automated sample containment removes
operator dependence and tightly contains the test specimen.
This sealing process is particularly important for materials that
undergo positive or negative volumetric changes with curing and
highly stiff materials such as carbon-filled fluoroelastomers.

Cooling Options
All rotorless rheometers are compatible with either the Air Cooling System or Enhanced Cooling System. The Air Cooling System uses ambient
air to expedite temperature changes above ambient conditions and improve temperature stability near room temperature.

The Enhanced Cooling System is a mechanical device that employs pressurized air to cool the test environment, allowing characterization
of rubbers at temperatures as low as 18 °C and greatly accelerating cooling time between non-isothermal experiments. The system has no
moving parts, making it extremely reliable and easy to use.

14 Technology 15
 test fixtures vs
Volumetric Sample Cutter

Rotorless Rheometer Sample Preparation

RPA and MDR die surfaces feature an optimized arrangement of Sample preparation for RPA, MDR, and Mooney instruments is
radial serrations to guarantee constant sample contact at even made safe and simple with the VS Volumetric Sample Cutter.
the highest strain values. Polyester or polyamide films may be This dual-action pneumatic system allows for the preparation of
used to facilitate sample release and avoid the need to clean uncured rubber specimens of a user-defined volume.
dies between experiments.
Preparing samples in this well-controlled fashion reduces
Torque calibration is made simple with a certified torque operational variability, greatly improving overall experimental
Die Surfaces calibration standard.This allows the user to calibrate the instrument precision.
directly, increasing data confidence and operation time,
and reducing the reliance on service engineers for calibration. The VS comes standard with a closing pressure of 6 bar.
The sample is first compressed to the user-prescribed thickness,
then cut to the die diameter. The closing pressure, and sample
Torque Calibration Standard
volume are user-adjustable. An optional booster is available
to increase operating pressure to 8 bar for highly filled and stiff
materials. Two-handed operation and lateral guards guarantee
Mooney Viscometer safe operation at all times.

The MV one Mooney Viscometer includes both large (38.1 mm)

and small (30.48 mm) diameter rotors. Both rotors are endorsed by
international standards and can be selected for measurement of
low or high viscosity rubbers or polymers. Both rotor types can be
used in conjunction with polyester or polyamide films to simplify
instrument cleaning and reduce time between runs. Rotors
are designed with low mass to optimize thermal response and
transient speed changes at the beginning and end of shearing
steps.

Calibration is software-driven and does not require the use of

external weights, fixtures, or reference materials. A weight of known
mass is connected by a well-defined radius, creating a constant
torque value. The software-driven torque calibration routine uses
this internal standard to ensure utmost data accuracy.
Sample Cutting Dies
Sample dies for either the Mooney Viscometer
or rotorless rheometers and curemeters can be
removed and exchanged quickly and easily.
The MV one Mooney Viscometer uses two
40 mm diameter samples, one above and one
below the rotor. A hole is punched in the center
of the sample to ease insertion. Standard RPA and
MDR samples are single piece discs cut to meet
volume specifications per ASTM, DIN, and ISO
standards.

Mooney Viscometer Rotors Integrated Torque Calibration

16 Sample Cutter 17
 reliable automation
RPA and MDR

All TA Instruments rotorless curemeters and rheometers are compatible with the highly reliable
rubber automation system. This carousel-based autosampler allows for the unattended testing
of rubber samples. Coupled with the Scarabaeus Software automated analysis, statistics, and
control chart generation, the automated rheometer becomes a highly integrated part of the
manufacturing control process. This improved data throughput is also invaluable for screening
multiple formulations in a research or product development environment.

Samples are moved from the

autosampler tray to the test position
using a suction transfer system. This
system is highly tolerant of non-ideal
sample geometries, so uncured rubber
from many sources can be used.
Samples are loaded on a carousel and
more specimens may be added while
another test is in progress, allowing for
uninterrupted productivity.

An automated film transfer system removes

the previously tested specimen and advances
the film roll to prepare for the next experiment.
An integrated sensor alerts the operator at the
end of the roll so it can be replaced in a timely
manner.

18 Automation 19
 scarabaeus software

The Scarabaeus Software for instrument control and data analysis is a powerful and versatile system for programming experiments, providing
quick feedback of results, and managing data from all rubber testing instruments. The Scarabaeus Software was developed with customers
Advanced Data Analysis and Modeling: Curing Kinetics
from the rubber industry and is designed to meet the specific need of production and research. Isothermal curing data at multiple temperatures can be analyzed according to a rubber-specific methodology to determine curing kinetics
parameters. This modeling system can determine:
Pre-cure Non-Isothermal Final
Viscoelaastic Curing Viscoelaastic • Reaction Rate • Reaction Order, n • Rate Constant, k • Incubation Time, ti • Arrhenius Activation Energy, Ea
Simple Instrument Control, Properties Properties

Frequency
Flexible Programming 100
24.0
Instrument control software is preloaded with test programs 22.0 90

for the most common experiment types, enabling simple 20.0 80

18.0 70
operation by new users. Multi-step tests can be easily

Strain
16.0

Conversion (%)
programmed to collect many types of data from a single 60

s’ (dn.m)
14.0
180˚C 50
specimen, or to mimic an industrial curing or other 12.0
170˚C

Temperature
processing sequence. 10.0 40
160˚C
8.0 30
150˚C
6.0 140˚C experiment
20
4.0 Model
Time 2.0 10
0.0
Quick Operator Feedback 0.0 5.0 10.0 15.0 20.0 25.0 30.0
0
0 2 3 5 6 8
Qualification of multiple lots of similar materials is made easy with quick operator feedback. Predefined test parameters with tolerances Time (min) Time (min)
can be assigned for a given material. Upon completion of a test, a simple pass/fail indicator shows whether the specimen falls within the
acceptable limits for the selected material, allowing meaningful decisions to be made quickly and easily.

MDR one
Statistical Process Control 30.0
39.30
Moving Die
Rheometer
Test data is readily converted into actionable information

Reaction Rate (dn.m/min)

31.50
for process control and manufacturing. Automated
data analysis can be programmed based on typical 20.0
s’ (dn.m)

24.70
ADT
performance metrics, such as minimum and maximum MV one
torque, scorch times, conversion times, and more. These 17.90 Automated
Mooney
Density
data are compared against user-defined limits and are 10.0 11.10 Designed for Integration Viscometer
used to track processes using histograms, control charts, Tester
The Scarabaeus Software system for instrument
and summary reports. 4.30
control and analysis integrates and organizes
0.0 -2.50 data from multiple instruments and historical
0.0 1.6 3.2 4.8 6.4 8.0 tests. Data from RPA, MDR, Mooney Viscometer, Scarabaeus
Time (min) Hardness, and Density tests can be organized, Software
35.00 30 -3σ -2σ -1σ +1σ +2σ +3σ compared, and analyzed by material type,
inventory order, date, and more. Advanced
24 integration with even greater capability is also RPA elite AHT
30.00
Rubber Automated
Relative Frequency (%)

available.
Process Hardness
s’max (dn.m)

18
25.00 Analyzer Tester
12

20.00
6
and more
15.00 0
1.20 1.30 1.40 1.50 1.60 1.70 1.80 1.90 2.00
12/13
12/27
1/10
1/15
1/23
2/2
2/27
3/7
3/14
3/21
3/28
4/2
4/4
4/10
4/12
4/18
4/23
4/24
4/28
5/3

TC 90 (min)
Date

24 Scarabaeus Software 25
 applications 160

140 ML (1+4)
15 rpm
120 2 rpm

Mooney Viscosity (Mu)

0.2 rpm
100
0.02 rpm
80

60

Mooney Viscosity 80.0 40

The Mooney Viscosity test is a well-established method for

20 Mooney Viscosity at Multiple Rates
64.0 0
characterizing uncured rubber materials. Following well- In addition to the viscosity at a single rate and temperature,

Mooney Viscosity (Mu)

Polymer A 0 200 400 600 800 1000 1200
defined standard procedures, the sample is preheated for a the MV one Mooney Viscometer can measure viscosity at a
48.0 Polymer b Time (s)
defined period, then sheared at a constant rate. The Mooney range of shear rates and temperatures. This range of rates
Polymer C
Viscosity is recorded from the end of this deformation stage. 100 allows a more complete understanding of the polymer
32.0
In the present example, the outstanding precision of the behavior, especially a tendency for shear thinning. Low rates
MV one Mooney Viscometer is demonstrated. Three polymer in Mooney Viscosity experiments can also be beneficial
16.0

Mooney Viscosity (Mu)

samples were tested in duplicate. The outstanding run-to-run for measuring highly elastic materials that are otherwise
reproducibility and the ease of distinguishing one polymer inaccessible to Mooney Viscosity measurements.
0.0
from another is clear.
0.0 1.6 3.2 4.8 6.4 8.0 80˚C
100˚C
Time (min)
130˚C
150˚C

10
100 0.001 0.01 0.1 1 10 100
Mooney Stress Relaxation
Rotor speed (rpm)
While the Mooney Viscosity experiment is typically indicative
Mooney Relaxation (Mu)

of polymer viscosity, stress relaxation can be used to

identify elasticity. Upon completion of the Mooney Viscosity 14 1.9
Isothermal Cure
buna s’max
measurement, the rotor is stopped immediately and the 1.8
10 CARiFLeX 12 TC90 Isothermal cure experiments are critical for rubber and
torque decay is observed. The slope of this decay is indicative HiPRen 1.7
elastomer processing. The TA Instruments rubber rheometers
10
of polymer elasticity, which may be related to a branched inTOL 1.6 provide high precision data that is simple to analyze. All the
architecture and correlates well with extrudate swell in rubber KOsYn
8 important characteristics, such as minimum and maximum

s’ (dnm)
1.5

s”(dnm)
KRALeX TC50
processing.
6 1.4 viscosity, scorch time, and conversion time can be calculated
1 1.3 easily and automatically. The data can also be handled in
0.1 1 10 100 4 ts2 its complete graphical form for comparison or alternative
1.2
Time (s) ts1 analyses.
2
1.1
s’min
0 1
0 2 4 6 8 10 12 14

100 Time (min)

Mooney Scorch 80 14 180

Non-isothermal Cure
Mooney Viscosity (Mu)

The Mooney Viscometer can also be used to measure 160

12 In addition to the industry-standard isothermal cure
60
the initial rate of vulcanization. In this example, a styrene 140
methods, the RPA and MDR can perform non-isothermal
10
butadiene rubber (SBR) was tested for prevulcanization

Temperature (˚C)
120 cure experiments. These experiments can be programmed
40
characteristics at 150°C using the small rotor. For this simple 8
s’ (dn.m) 100 to follow virtually any temperature profile and are especially
experiment the initial Mooney viscosity, minimum viscosity, valuable when simulating manufacturing processes that
6 80
20
scorch times, and cure index are the most commonly are not isothermal. Non-isothermal curing experiments may
60
reported values. 4 also be coupled with isothermal tests such as strain and
0 40
0 2 4 6 8 10 12 14 2 frequency sweeps before or after cure to provide a more
20
complete material data set before, through, and after cure.
Time (min) 0 0
0 2 4 6 8 10 12 14

Time (min)

26 Applications 27
 applications
xxxxxxx

Isothermal Curing at Variable Strain 4.0 300

High Strain Non-Linear Behavior
While standard test methods often call for a single strain 0.5° 200 The viscoelastic response of a branched material at very
and frequency value to be used for all materials (0.5°, 1.67 3.0 high strains differs not only in magnitude from its linear
0.4°

shear stress (kPa)

100
Hz), these are not always the ideal conditions for every 0.3° counterpart, but also in type. The careful examination of a
material. In the present example, the sample material is polymer’s stress-strain response at high strains reveals features

s’ (n.m)
2.0 0
tested by isothermal cure at three deformation amplitudes, associated with filler content and structure, as well as polymer
five times each. At the standard of 0.5° and 0.4° the -100 architecture. In the present example, qualitatively different
experimental variability is extremely broad. This is because 1.0 Linear features are observed at large strains for two EPDM materials:
branched
these experiments are performed at strains beyond the -200 a linear polymer and a branched polymer. Both exhibit
linear viscoelastic limit for this material. Testing at a smaller identical Mooney viscosities, but markedly different high strain
0.0 -300
amplitude (0.3°) produces valid data with greatly improved -40 -30 -20 -10 0 10 20 30 40 behavior. Both the uncorrelated data, and the FT analysis of
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 0.8 2.0
reproducibility. periodic data are available through the Scarabaeus Software
Time (min) shear Rate (s ) -1

to allow in-depth analysis of this new type of data.

106
1400
Time Dependent Structure
Breakdown
Isothermal Frequency Sweep MWD–
1200
The van der Waals interactions that lead to increased
Measuring the frequency-dependent viscoelastic properties 1000
modulus in carbon black filled rubber are highly sensitive to
g’ and g’’ (Pa)

of a material is a powerful way to understand its molecular

g’ (kPa)
105 800 processing. In this example, identical samples are subjected
gc
structure. A frequency sweep as shown can reveal information
Mixer +1 min mill
to different lengths of milling after being removed from
600
about the average molecular weight (crossover frequency) Mixer + 2 min mill the mixer. Carbon network structure is reduced with each
and molecular weight distribution (crossover modulus). 400 Mixer + 4 min mill
MWD+
Mixer + 8 min mill increase in milling time up to 8 minutes, after which the
200 Mixer + 15 min mill modulus was unchanged with increased milling.This provides
AMW+ ωc AMW–
104 critical information about the amount of milling needed to
0
0.1 1 10 100 0.01 0.1 1 create a consistent workable material.

Angular Frequency (rad/s) Amplitude (°)

500
Strain Sweep for Filler Loading 10 phr
15 1800
Cure with Blowing Reaction
20 phr 1500 Final product density and mechanical performance are
The strain-dependent modulus is particularly important as an 400
indicator of the amount and type of rubber filler dispersion 40 phr often enhanced through the use of blowing agents to create
10 1200
60 phr a cellular architecture. These blowing agents generate gas

Pressure (kPa)
and interaction. In the present example, the impact of 300
g* (kPa)

s’ (dn.m)
carbon black addition at five different levels is seen in the during decomposition in parallel with the curing reaction.
900
low strain region. High strain behavior is generally insensitive Monitoring sample pressure through the curing reaction is
200
to filler addition, as it is less sensitive to filler-filler interaction 5 600 an effective way to quantify the blowing reaction, allowing

and more dependent on polymer molecular weight, and 100

for the characterization of curing and blowing in a single
300 experiment. These two processes must be balanced in order
polymer-filler interactions.
to form the desired cell architecture in the finished product.
0 0 0
0.1 1 10 100 1000 0.0 0.5 1.0 1.5 2.0 2.5 3.0

strain (%) Time (min)

28 Applications 29
 specifications

Feature Summary
MDR one RPA flex RPA elite

Torque Transducer High-Stiffness Proprietary Ultra-High-Stiffness Proprietary Ultra-High-Stiffness

Torque Range 0.01 to 25 N.m 0.01 to 25 N.m 0.1 to 20 N.m

Motor Direct Drive Direct Drive Direct Drive

Strain

0.2°, 0.5°, 1.0°, 3.0°

0.1° to 7° (continuous) —

0.005° to 360° (continuous),

—
Strain Sweep, Offset, LAOS

Frequency

1.67 Hz (100 cpm)

0.001 Hz to 50 Hz, Frequency Sweep —

Sealing Pressure

Fixed: 4.5 bar

Variable: 1 to 8 bar —

Sample Pressure Measurement —

Air Cooling System (ambient to 230°C)

Enhanced Cooling System (18°C to 230°C)

Isothermal and Non-Isothermal Curing

Non-Linearity Measurements —

Stress Relaxation —

Advanced Oscillation
—
(arbitrary wave, multi-frequency)

Autosampler

Included

Optional

— Not Available

30
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DSC TGA DMA Dielectric Thermal Conductivity Rheometers

• Curing profiles and kinetics • Compositional analysis • Final viscoelastic properties • Dieletric Properties • Highly accurate, simple measurement • High sensitivity rheology
• Residual cure • Thermal Stability • Finished part analysis • Filler networks • Heat dissipation • Solutions, polymers, coatings
• Phase transitions • Evolved Gas Analysis by • Phase Transitions • High frequency relaxation • Cure process modeling • -160 ˚C to 600 ˚C
Mass Spec or FTIR
• Oxidation Induction Time • Filler effects • Phase transitions • Many sample types
• Decomposition kinetics • Compatible with DMA or • Complementary accessories
rheometer systems

32
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