Feature Article

Rheometers: Which Type Is Right For You?

Capillary and torque rheometers are good for simulating processing conditions, troubleshooting, and QC. But dynamic rotational
instruments can tell you more about a resin's molecular structure.
By Lilly Manolis Sherman

http://www.ptonline.com/articles/200405fa2.html

Long used by materials suppliers to characterize the viscoelastic properties of polymer melts, Company Info
rheometers are also becoming more popular among plastics compounders. Both groups use
rheometers to assess resin processability for routine quality control and also as R&D tools to C.W. Brabender
help determine which material best fits a process or application. Instruments, Inc.
Hackensack, N.J.
One reason for the broader use of rheometers in plastics is their declining prices, which is partly (201) 343-8425
a result of the improving cost/performance trend in computer power. While six-figure tabs were
typical in the past, instruments can now be had for under $40,000. The latest instruments also Brookfield Engineering
boast improved accuracy and both software and hardware accessories that expand the range of Laboratories
testing capabilities. Middleboro, Mass.
(800) 628-8139
There are three main types of rheometers: capillary, torque, and
dynamic rotational, and each serves a different purpose. For Ceast USA
example, if you are looking for a more sophisticated version of a Charlotte, N.C.
melt indexer, a capillary rheometer may be the instrument to (704) 423-0042
consider. A melt indexer measures only one point on the shear-
rate/viscosity curve, which offers only a crude indicator of
Dynisco Polymer Test
flowability or average molecular weight. A capillary rheometer
Morgantown, Pa.
measures multiple points on the curve to give a more realistic
(508) 541-9400
picture of flow at the higher-shear conditions of injection molding
(10,000 to 100,000 sec-1) or extrusion (100 to 1000 sec-1).
Capillary rheometers can range in price from $30,000 to $45,000 Goettfert
for entry-level, benchtop QC units up to $100,000 for more Rock Hill, S.C.
advanced models. (803) 324-3883

Torque rhoemeters Malvern Instruments, Inc.

There are also on-line capillary rheometers that measure viscosity
simulate real-world Southboro, Mass.
of material as it passes through an extruder. They typically cost
processing conditions. (508) 480-0200
$100,000 to $150,000, though a couple of companies have
Here, Thermo-Electron's
introduced versions priced around $50,000.
modular PolyLab system
TA Instruments
is running with extruder
Torque rheometers are essentially small mixers or extruders. They New Castle, Del.
and blown film
measure the torque on the mixing screws or rotors, which reflects (302) 427-4000
attachments.
how hard it is to mix the material. Machine torque, which can be
correlated to viscosity, is one of the primary ways that a processor can characterize materials’ Thermo Electron
processability. Torque rheometers can range in price from $35,000 to $40,000 for a basic Newington, N.H.
batch-mixing model up to $150,000 for a unit with a twin-screw extruder. (800) 258-0830

One popular single-bore
capillary rhoemeter for
plastics is Goettfert's
Rheotester 500, a unit
that is both a rheometer
and a melt indexer
(inset).
A stretching device such
as this one from Ceast
USA can be used with a
capillary rheometer to
determine extensional
viscosity through melt-
tension analysis.
Major suppliers of capillary
Instruments (which
(formerly Thermo Haake).
Although capillary
owing to its release of
Ceast USA. Likewise,
hygroscopic materials,
However, with on-line
hygroscopic materials
capillary instruments but
cannot be cleaned out.
Capillary rheometers can
Both capillary and torque rheometers typically provide data on viscosity and melt flow as material
passes through the instrument. In contrast, the purpose of dynamic rotational or oscillatory rheo-
meters is to probe into a polymer’s molecular structure and viscoelastic properties. These
instruments place the plastic sample between two components, one stationary and one that turns
back and forth at adjustable speed. These instruments operate at relatively low shear rates. They
provide information related to how a resin will process and have proved vital to material suppliers in
both R&D and QC functions. The cost range of rotational instruments used for plastics is $40,000 to
$90,000.
High-shear viscosity data from capillary rheometers and low-shear data from dynamic rotational
rheometers can be compared because they both measure “true” or absolute viscosity. That is not
true of torque rheometers, which provide only a relative measure of viscosity through correlation
with torque.
Instrument suppliers generally agree that compounders and processors looking for a QC tool with
some level of research capability are likely to opt first for a capillary rheometer. Next up the scale is
a torque rheometer, which allows you to troubleshoot flow in an extrusion die or injection mold and
also can be used for QC. In addition, torque rheometers can mix batches of materials for testing
and development, which is not possible with the other two rheometer types.
When processing problems cannot be diagnosed with either capillary or torque rheometers, the
solution may require insight into molecular structure, which can be provided by a dynamic rotational
rheometer.
(Not discussed here is another class of instruments known as viscometers, which measure only
viscous flow properties—not viscoelastic properties—of liquids. Viscometers are used with liquid
thermoset resins and rubbers.)
Capillary Rheometers
A high-shear, controlled-stress capillary rheometer consists of a heated
barrel and a piston that drives molten material through a calibrated die,
applying pressure either at a constant speed or a constant shear rate.
Die geometry can be changed to measure rheological properties under
different conditions. In addition to the most widely used single-bore
configuration, there are also twin bore (dual-barrel) instruments that
can perform two simultaneous tests under different conditions. There
are also on-line capillary rheometers, which are mounted on an
extruder.
rheometers include Ceast, Dynisco Polymer Test, Goettfert, Malvern
acquired Bohlin Instruments/Rosand in 2003), and Thermo Electron
Dual-bore capillary
rheometers such as
Malvern Instruments' rheometers can test a wide range of plastics, PVC poses difficulties
RH2200 model can run corrosive hydrochloric acid, notes Gerard Nelson, sales manager for
two test simultaneously corrosion from water is a problem with PET, nylon, and other
using dies of the same according to Alberto Correa, product manager at Thermo Electron.
diameter but different capillary rheometers, oxygen is excluded from the testing process, so
lengths. It automatically present no problem. Thermosets also can be processed in on-line
calculates the Bagley not in benchtop capillary models because the resins cure quickly and
correction to provide a
truer measure of absolute
viscosity. measure how a material’s viscosity changes as a function of
temperature and pressure. One test can cycle through 10 different piston speeds at a controlled temperature and track how the
viscosity changes relative to shear rate (rate of flow) and shear stress (force applied). The result is a rheology curve that plots
shear stress, measured in Pascals (Pa), on the X axis and shear rate (in sec-1) on the Y axis. The ratio of the two is the
viscosity in millipascal-seconds (mPas). One mPas equals 1 centipoise (cp), which is the viscosity of water at room
temperature.

Benchtop capillary rheometers for quality control have a lower force range of 5 to 10 kN, compared with 50 to 60 kN for mid-
range and higher level units. Benchtop QC models also typically provide piston-speed ranges of 20,000:1 vs. a 200,000:1 range
for more advanced units used by R&D departments.

The most widely used capillary rheometers are single-bore models. Popular examples include Goettfert’s Rheotester 500
extrusion plastomer, which is both a rheometer and a melt indexer; Dynisco’s LCR 7001; Ceast’s Rheologic 2500; Malvern
Instruments’ (Rosand) RH2100; and Thermo Electron’s (Haake) RheoCap S20.

A newer alternative is twin-bore capillary rheometers, some of which can be had for around $50,000. They save testing time by
allowing you to get two results in one test cycle. Their other key advantage is that they can automatically calculate Bagley or
other corrections, which translates into a truer measure of absolute viscosity. This is accomplished by using dies of the same
diameter but different lengths, resulting in different shear stresses at the same shear rate.

According to Ceast’s Nelson, twin-bore units can also be very useful in detecting slip-wall effects.
High slip at the wall may result from lubricants, pigments, or other additives. Excessive slip can
indicate the need to reduce additive levels, which will save formulation cost and improve processing.

Popular twin-bore capillary rheometers include Ceast’s Rheologic 5000, Goettfert’s Rheotester 2000,
Dynisco Polymer Test’s LCR 7002, Malvern Instruments’ (Rosand) RH 2200, and Thermo Electron’s Dynisco's ViscoSensor is
(Haake) RheoCap T100. said to be the smallest
return-streat on-line
Viscoelastic properties, too rheometer. It reportedly
offers the capabilities of
Relatively new to capillary rheometers are hardware and software that enable them to measure or units that cost more than
derive mathematically some viscoelastic properties such as extensional viscosity, die swell, and melt twice as much.
strength. Says Tim Haake, general manager at Goettfert, “Extensional or elongational viscosity is important for film, fiber, and
foam processing as well as blow molding and is not obtainable with a typical rheometer.” Patented several years ago,
Goettfert’s Rheotens is an extensional rheometer that sells for $60,000. Since then, other suppliers have come up with different
ways to accomplish the same end, in some cases by means of software correlations or special
hardware accessories.

Dynisco Polymer Test, for example, has developed new software routines that allow users to derive
some viscoelastic properties, such as elongational viscosity, from shear-rate and shear-stress
measurements. According to company president Rich Pavero, Dynisco also has developed software
that provides excellent correlation of standard capillary data to the intrinsic viscosity (I.V.) of PET, a
feature that reportedly has generated interest among PET compounders and processors.

Randy Byrne, v.p. of marketing at Malvern Instruments, says both the company’s mid-level RH2000
(Rosand) and high-level RH10 series (Bohlin) rheometers now can measure die swell through a
combination of special software and hardware. The latter involves a high-resolution laser that
measures the diameter of the polymer stream as it exits the die.
C.W. Brabender's new
Malvern’s Rosand line of capillary rheometers measures extensional viscosity using a melt-strength ATR PlastiCorder is an
device. These rheometers perform other processing-related measurements such as wall-slip advanced torque
velocity, melt fracture, thermal degradation, and stress relaxation. Similarly, Ceast’s rheometers rheometer with lower
can now be equipped with stretching units to carry out melt-tension analysis that provides horsepower and a lower
extensional viscosity. Laser die-swell measurement systems are also available. price tag than previous
units.
Ceast also now offers an equilibrium stress prediction (ESP) algorithm as standard software. Says Nelson, “Instead of waiting
for the rheological curve to stabilize at each piston speed (shear rate), indicating the attainment of equilibrium stress, this
algorithm can predict it early on, saving up to 60% of the testing time. We have generated data that shows a very good
correlation between a full test and early ESP prediction.”

On-line models

Compounders and resin suppliers need not wait for lab test results on production samples every few hours: They can maintain
almost real-time control of product quality with an on-line rheometer On-line rheometers process a side stream of melt diverted
from the extruder. After testing, the melt is either discarded or returned to the extruder. Thermo Electron’s Correa notes that
the company’s on-line Process Control Rheometer (PCR 630) is used by major resin producers whose extruders run 60,000
lb/hr. Clearly, they can’t wait to find out whether their material is on- or off-spec. The hurdle for other processors has been the
cost of these units—over $100,000. Recently, two suppliers have introduced on-line models priced at around $50,000. Dynisco’s
ViscoSensor is said to be the smallest return-stream on-line capillary rheometer, one that reportedly matches the capabilities of
higher-end units. Says Pavero, “We have had compounders using it, as well as PET and polyolefin sheet and film extruders,
higher-end PET recyclers, and extruders of nylon shapes and rods. A maker of PET sheet for thermoformed trays is using it as a
viscosity and moisture analyzer, as they can monitor the I.V. number and quickly respond if dryers are not functioning
adequately.”

Meanwhile, Thermo Electron developed an on-line system in Germany that is now being made
available here. The ProFlow rheometer sells for a base price of $50,000, but it does not return the
material to the main stream.

Among high-end models, Goettfert’s smaller on-line unit, the MBR, is used most often by PET
processors to monitor I.V. during processing. The company’s Real Time Rheometer (RTR) is a
return-stream system that has seen some use in plastics. “It can take up to one-half hour for some
very viscous materials to go through an extrusion die, which means you can be making off-spec
material for that half-hour. The RTR has an extra circulation pump that transports the material
sample [to the rheometer] in 5 min,” says Tim Haake.

Torque Rheometers
Patented SMT technology
featured in TA The heart of a torque rheometer is a special motor that can measure the torque on its shaft. Its
Instruments' Ares 2000 drive system can be coupled to interchangeable accessories like a miniature laboratory mixer or
dynamic rotational single- or twin-screw extruder. Suppliers of these instruments include C.W. Brabender and Thermo
rheometers separates Electron.
torque measurement
from the drive system,
The torque rheometer is connected to data-acquisition software that tracks the process torque,
eliminating the need for drive speed, temperature, and pressure. These data indicate how easily materials process and how
multiple calibrations.
readily different additives disperse. In the polymers industry, torque rheometers got their start with
PVC and rubbers because of all the additives that go into these formulations. For example, a torque rheometer helps assess the
sensitivity of a formulation to degradation. “This will show up as an increase in the torque curve of PVC as the material starts
crosslinking,” explains Scott Martin, senior product specialist at Thermo Electron.

Andrew Yacykewych, applications laboratory manager at C.W. Brabender, says torque rheometers are now testing all types of
thermoplastics, including nanocomposites and wood-filled plastics. Applications now also encompass thermosets, particularly
unsaturated polyesters and phenolics, where the instrument is used to study curing behavior.

Processors using torque rheometers are primarily extruders of film, sheet, tubing, and coatings, according to Yacykewych.
These small, precisely controlled extruders have also been used for small-volume production of products such as catheters.

Newer developments in torque rheometers include special sensors that are used by compounders and masterbatch suppliers to
measure thermal and electrical conductivity as a QC check on dispersion quality or the performance of additives like carbon
black, according to Thermo Electron’s Martin.

Compounders also use torque rheometers to simulate their twin-screw extrusion lines on a small
scale. Thermo Electron’s new PolyLab system is a modular torque rheometer designed for process
simulation in the lab or pilot plant. According to Martin, many compounders start with the small
batch-mixer module for formulation work. “Once you have the base formulation, then you want to
make the compound in a continuous fashion using the twin-screw extruder module. Material can be
run through a pelletizer and then the torque-rheometer drive is attached to a single screw extruder
that will process those pellets through a miniature blown film line and make actual bags.”

The company’s PolyDrive line includes less expensive rheometers with a dedicated mixer or extruder
attachment that cannot be interchanged. For example, a PVC compounder who wants a unit to
perform only PVC fusion tests may be satisfied with a dedicated PolyDrive mixer. PolyDrive systems Thermo Electron's
with software cost in the range of $35,000 to $45,000. Rheostress 600 dynamic
rotational rheometer has
C.W. Brabender’s top-of-the-line unit is the four-year-old Intelli-Torque Plasti-Corder, which an ultra-low-mass motor
features a precision digital servo drive with a torque range of 1 to 400 Nm over the entire speed that reduces the inertial
range of 0.2 to 150 rpm. More recently, the company introduced the ATR Plasti-Corder, which has a effects on torque
smaller drive (2.5 hp) and costs about half as much as the Intelli-Torque. The ATR can apply up to measurements.
160 Nm of torque and can accommodate any Brabender mixer or single-screw extruder attachment.

New torque rheometer software from Brabender includes Winmix for batch mixers, which features evaluation routines for PVC,
elastomers, polyolefins, thermosets, and engineering resins. Tests include plasticizer or liquid absorption, flow and cure
behavior, heat and shear stability, fusion behavior of rigid PVC, and carbon-black incorporation time. Also new is Winext
software for extrusion. It can assess a polymer’s viscosity under conditions similar to an actual processing environment.

Dynamic Rotational Rheometers

The primary components of a dynamic rotational rheometer are a motor, optical encoder, torque-sensing mechanism, and (for
plastics applications) a means of applying force along the rotor axis. Another critical component is an air bearing that allows the
rotor and torque sensor to “float” and minimize friction. Major suppliers of this type of rheometer include Thermo Electron
(Haake), TA Instruments (including the former Rheometric line), and Malvern Instruments (Bohlin).

These instruments operate in continuous rotation and oscillation modes. Oscillation at a narrow
angle is most often used for plastics. This small-strain oscillation provides information on
viscoelastic properties, including melt viscosity, molecular weight, MW distribution, and polymer
relaxation—all of which can affect how the material processes. These instruments’ software can plot
elastic modulus and viscous modulus against oscillation frequency in radians/sec. This low-shear
test runs a scan sequence from very short turns back and forth to wider-amplitude oscillations to
simulate processing shear conditions.

There are three different types of stress-sensor attachments: cone and plate, plate and plate, or
concentric cylinder. The last is used mainly for adhesives and coatings. Plate-and-plate (or parallel-
plate) geometry is used to characterize thermoplastic melts and thermosets (disposable plates are
necessary). Cone-and-plate is used primarily for steady-shear and normal-force testing, the latter of
which correlates with die swell of thermoplastics. Creep studies on solid plastics can also be
For less than $4000, performed with parallel-plate or cone-and-plate sensors. In a creep test, a constant stress is applied
Brookfield's New DV-III to the sample and the strain is monitored. “Creep allows direct measurement of the equilibrium
Ultra dymanic rotational recoverable compliance and zero-shear viscosity,” explains Russ Ulbrich, product manager at TA
rheometer reportedly Instruments.
provides some of the
same viscoelastic data as Among the popular dynamic rheometers for plastics is the AR series from TA Instruments. It uses
instruments costing 10 CMT (combined motor and transducer) technology. More expensive, but still quite popular for
times as much. plastics, is TA Instruments’ patented SMT (separate motor and transducer) construction, which
measures torque independently from the drive motor, greatly reducing calibration requirements. “With CMT devices, there is a
need to correct for inertia of the system,” says Ulbrich. His firm’s Rheometric Ares SMT rheometers decouple torque sensing
from the motor, thus overcoming the problem of inertia contribution, Ulbrich explains.

For example, CMT rheometers can have difficulty measuring very low viscosities because the inertia of the rotor and sensor
becomes very large in relation to the resistance offered by the materials. Problems also can occur in analyzing materials like
thermosets that show large changes in viscosity during processing. Users may encounter inertia limitations on CMT rheometers
as the polymer cures. But Ares rheometers with SMT technology reportedly can measure the whole range of viscosities
accurately.

CMT devices measure controlled stress but not controlled strain. “Traditionally, CMT devices have been only able to control
strain in oscillation using iterative feedback loops, which required several oscillation cycles to achieve the programmed strain.
This lengthened the testing time. SMT devices never had this limitation,” says Ulbrich. Advances in CMT devices now allow a
user to hit the programmed strain within the first oscillation, like a SMT device, but additional calibrations are then needed. An
example is TA Instruments’ AR Mobius Drive 2000 system, which can be equipped with accessories such as an oven for
thermoset cure studies. Says Ulbrich, “This system can directly control strain and stress in oscillation and do controlled strain-
rate/stress-relaxation tests on one platform.”

Similar benefits are claimed for Malvern’s Bohlin Gemini and C-Vor CMT instruments, whose Rotonetic drive can make both
controlled stress and strain measurements. Thermo Electron’s two-year-old RheoStress 600 has an ultra-low-mass motor that
reduces inertial effects during testing. Another interesting feature is the measurement of normal force (along the rotor axis).
Says applications engineer Jenni Briggs, “Forces acting perpendicular to the direction of flow play an important role in many
rheological applications. With RheoStress 600, the normal force can be used as a set parameter as well as a measured variable.
The normal-stress differences induced by shearing a viscoelastic sample are measured by the normal-force sensor integrated in
the air bearing.”

The instrument’s MFC (Micro Force Correction) feature extends the measurable force range down to 0.01 N (0.002 lb). In the
FLC (Forced-Controlled-Loading) mode, samples are loaded under a preset normal force in order to increase reproducibility.

A low-cost alternative

A very different type of dynamic rotational rheometer is sold by Brookfield Engineering Laboratories. Its “cone spindle” (cone-
and-plate) instruments rotate continuously and have mechanical bearings. While they are not as sensitive as air-bearing
instruments and do not perform oscillation tests, they are significantly less costly. They are recommended for QC and some
types of polymer characterization. Explains marketing director Bob McGregor, “The air-bearing instruments tell you more
precisely the yield value of the material and provide greater detail on its elastic modulus, which is important for analytical
studies. But for more basic characterization our instruments may be very suitable.”

Brookfield’s R/S controlled-stress rheometer, which sells for $12,000 to $20,000, applies constant or ramped speeds and also
can vary the amount of normal force to permit direct measurement of yield and creep behavior.

Brookfield recently introduced the DV-III Ultra, which sells for just $3995. It replaces the former DV-III+ model, a controlled-
rate instrument that measures how a material behaves at constant shear rate. The upgraded Ultra version combines the
capabilities of the DV-III+ with the yield-stress measurement capability of Brookfield’s YR-1 yield-test rheometer. McGregor
says the DV-III Ultra, when used with vane spindles and Brookfield’s EZ-Yield software, can provide viscoelastic data on storage
and loss moduli comparable to that obtained with higher-end air-bearing rheometers. Adds McGregor, “We are now developing
a method that will allow us to determine the phase angle—something that is now only provided by instruments that perform
oscillation tests.”

PT Home | Research Zones | Suppliers | Materials Database | Machinery Database | Articles | Resin Prices | News | Subscribe

The Definitive Web Resource For Plastics Processors

© 2008 Gardner Publications, Inc