Tips and Tricks from Joe Flow

Rheometers: How and What Do They Measure?

To understand rheological measurements, it is often helpful to learn more about the rheometer
setup and how it works.

Rheometer design

Rotational and oscillatory rheometers are set up as

shown in Figure 1. The measuring head contains the
drive motor and encoder which measure and set the
torque, deflection angle and speed.

What is measured in rotational tests?

Let's imagine that the measuring gap contains

ketchup. The viscosity of the ketchup should be
measured with a shear-rate-controlled rotational test.
You set the shear rate profile. The viscosity is
calculated according to the viscosity law from the
quotients of the shear stress  and shear rate γ̇ .
η = τ / γ̇
As you already know, the shear stress correlates with
the torque. If you measure the ketchup with a large
To measure the rheological properties of your sample measuring system, a large torque is required because
with a rheometer requires determination of the torque the shear surface is large. If you use a small
and deflection angle of the measuring bob. Your measuring system, a smaller torque is needed to
sample provides resistance or a preset torque to the obtain the required speed.
presetting. The resulting deflection angle is then However, the viscosity of the ketchup is the same in
measured by the rheometer's encoder. The speed is both measuring systems. The rheological parameter
calculated from the deflection angle and the time. shear stress  is calculated from the torque in relation
However, as the user, you are usually more interested to the shearing surface. Therefore, the shear stress is
in the rheological parameters. How do you get these? independent of the used measuring system. It is
Rheological parameters are calculated from the easier to work with the rheological parameters.
measured values torque, deflection angle and speed The same is true for the shear rate, which correlates
using conversion factors (see Table 1). All further with the speed. If ketchup is measured in two different
parameters, such as viscosity, are not measured but measuring systems, one with a large shear gap and
calculated. one with a narrow shear gap, the same rotational
speed results in different flow velocities (or shear
Conversion rates). As with the calculation of the shear stress, for
Measurement Rheological
values factor parameter
the calculation of the rheological parameter shear
rate, the influence of the measuring system is
Torque M [mNm] CSS factor Shear stress τ [Pa] considered using a conversion factor.
Deflection angle φ
CSD factor Deformation γ [%] Viscosity values are calculated from the rheological
[μrad]
parameters which are independent of the instrument.
Speed n [min-1] CSR factor Shear rate γ̇ [s-1]
Table 1: Measuring values and rheological parameters with the
conversion factors

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 Figure 1: Setup of a modern air-bearing rotational and oscillatory rheometer with the most important components
However, every instrument has its limits (see the Tips
and Tricks from Joe Flow on the subject of measuring
range limits). To still be able to cover as large a
viscosity range as possible, there are a number of
measuring systems available which all have their own
conversion factor. That makes it possible to measure
almost all samples with one rheometer - from low
viscosity liquids to stiff solids.
These conversion factors are saved together with the
inertia, the expansion coefficients, the serial number
and the exact dimensions of the measuring system for
each system on the transponder chip in the measuring
system axis. Using ToolmasterTM which provides fully
automatic detection of the measuring system and
measuring cell, all relevant data are read out when the
measuring system is connected to the coupling of the
rheometer. This ensures that the software always
uses the correct conversion factors for the used
measuring system for the calculation of the
rheological parameters.
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What is measured in oscillatory tests?
If jello is in the shear gap, the aim of the test is usually
to investigate the viscoelastic behavior and the
characterization of the undestroyed structure at rest.
In this case it is not very useful to carry out a
rotational test. Instead, oscillatory tests with set
sinusoidal oscillation of the measuring system and the
sample are carried out. Also here, the rheometer
determines the deflection of the measuring bob and
the required torque. However, because jello has
viscoelastic properties, the response wave is time-
delayed compared to the set oscillation. This time
delay is called the phase shift δ.
The values measured by the rheometer (deflection
angle, torque and phase shift) together with the
conversion factors for the measuring system now give
all necessary data to calculate the required
rheological parameters such as the storage modulus
G’ or loss modulus G’’.
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What else does a rheometer measure?
The measuring temperature, which is an extremely
important parameter, is measured in the measuring
cells as well. Exact temperature control is very
important because all rheological parameters are
greatly affected by the temperature.
Modern rheometers simultaneously detect the axial
normal force FN. An MCR series rheometer does this
using a normal force sensor integrated in the air
bearing. The normal force is also used to
automatically determine the zero position of a cone-
plate or parallel-plate measuring system. In the past,
the zero position and measuring position had to be set
by hand. Today, this is done for you automatically by
the rheometer.
If you carry out temperature tests or curing, e.g. with a
parallel-plate system, the gap becomes bigger or
smaller due to thermal expansion or shrinkage of the
measuring system and sample. In this case, it is
recommended to set a constant normal force of, e.g.
FN = 0 N so that the measuring head compensates for
the expansion or contraction using an intelligently
controlled procedure. This ensures that the measuring
gap is always filled, even if the sample shrinks and
that no large normal forces occur if the sample
expands. In both cases the measuring gap changes.
However, because the MCR rheometer continuously
detects the measuring gap, the actual gap size at
every measuring point is used for further calculations.
Besides the benefits of easier handling, this opens up
completely new measuring possibilities, such as:
• dynamic-mechanical thermal analysis (DMTA) on
solids (torsion bars),
• tack and penetration measurements (see the Tips
and Tricks from Joe Flow on this subject),
• breaking tests (or fracture tests), as carried out by
texture analyzers,
• tribological measurements (wear measurements
between two media),
• determination of the amount of shrinkage (e.g. in
percent of the initial value).
In the past, individual instruments were used for each
of the mentioned test methods. Now, due to the
constant development of instrument types, it is
possible to cover a number of measuring tasks with
one instrument. As you see: modern rheometers
measure considerably more than just viscosity values
and viscoelastic properties. They have become
universal test instruments.
The stiffness of a rheometer
For measurements on curing materials and on solids it
is important for the rheometer to be extremely stable,
both mechanically and thermally. However, each
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material has a certain compliance, which needs to be
known and compensated for. Therefore, even gap
change in the micrometer range must be detected and
corrected or actively adjusted, even when the normal
forces are large. Especially when using a cone-plate
geometry, it is very important to precisely control the
measuring gap (to keep the gap constant).
In torsion tests, the measuring systems and also the
rheometer are affected. For example, the measuring
system shaft may twist by a small amount when the
torque is applied because the sample in the
measuring gap resists deflection. The challenge for
the electronics is to detect the real deflection and
speed of the sample from the signals coming from the
encoder in the measuring head. There is also a
compensation value for this called torsional
compliance. The torsional compliance is known for
each measuring system and can therefore be
corrected.
Adjustment of parameters
At first, the rheometer does not know whether there is
a low viscosity, high-viscosity, ideally viscous or
viscoelastic sample or an elastic solid in the
measuring gap. It is therefore important to use
intelligent controllers which can adapt quickly to the
sample conditions. The TruRate™ motor controller of
the MCR series rheometers controls the sample
deformation, shear rate and shear stress exactly,
quickly and without overshoots so that all types of
samples can be investigated precisely.
When you set a shear rate, the rheometer controls the
speed appropriately. This is kept constant, unaffected
by the behavior of the sample in the measuring gap.
You should always remember this when interpreting
the data. If your sample leaves the gap due to
viscoelastic effects then the adaptive controller
adjusts to the set shear rate or speed. However, now
that there is less material in the gap, this results in a
lower required torque. In the flow curve, you can
usually see immediately that the shear stress function
suddenly becomes flatter or curves downwards. In the
fall of the viscosity curve, however, this effect is often
difficult to distinguish from shear-thinning behavior.
The real-time position control TruStrainTM was
developed for oscillatory measurements with set
deformation. It allows these tests to be carried out
without pretests and without subsequent adjustments
by the instrument control. The strain (deformation) is
adjusted in a real-time position control mode directly
on the (ideal) sine wave both within the linear
viscoelastic (LVE) range and also under LAOS
conditions (Large Amplitude Oscillatory Shear), i.e.
outside the LVE range. This makes oscillatory
measurements possible at the smallest torques and
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deformations, even on complex liquids such as Modern controllers adapt quickly to the behavior of
suspensions, emulsions, foams and surfactant your sample and allow precise measurements, even
solutions as well as gels. These oscillatory of samples with low structural strength, without
measurements are highly accurate and without drift. destroying them prematurely.
However, despite this highly developed rheometer
technology, you, as the user should always confirm
the measurements with a critical eye and check the
Ball bearing or air bearing? What do I need?
results, as a rheometer does not detect external
sources of error, for example, gap emptying.
There are rheometers with air bearing and rheometers
with ball bearing. What does that mean? As far as
instrument handling and sample handling are
concerned, there is no difference. However, the
instruments differ significantly in the internal friction of
the motor bearing and therefore in the smallest torque
which can be measured or usefully analyzed.
Fig. 2 clearly shows the different measuring range
limits for the viscosity when using an air-bearing
rheometer and a ball bearing rheometer with the same
cylinder system.
The type of rheometer bearing also has an effect on
the type of tests which can be carried out. Oscillatory
tests usually only provide useful results when carried
out on air-bearing rheometers.
The benefits of ball-bearing rheometers include their
lower purchasing costs and lower operating costs, as
no compressed air is needed. Many applications and
investigations require a higher resolution and
oscillatory measurements. This increasingly results in
users choosing air-bearing rheometers.

Figure 2: Theoretical viscosity range of rheometers with air-

bearing and ball-bearing when using a cylinder measuring
system, shown on double logarithmic scale

Summary

A rheometer measures the torque, deflection angle

and speed with very high accuracy. All required
rheological parameters are calculated using these
measured values together with the measuring-system-
dependent conversion factors. The temperature and
normal force are also determined.
As well as being very stiff, a rheometer should also Contact Anton Paar GmbH
have an exact gap control. www.anton-paar.com/contact

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