Guidelines for rheology procedure and geometry selection

This document will help you to select the correct geometry for your sample and the correct procedure and test conditions
in order to answer your research question.

1. General information
The rheometer (Figure 1) consists of a frame on which a geometry is
attached. The lower part of the geometry is stationary and the upper
part is movable. It is moved up to load the sample and then moved
down again to set the measuring gap (i.e. the distance between the
upper and lower part of the geometry) determining the thickness of
the sample during the analysis. Once the sample is loaded the upper
part of the geometry (concentric cylinders, cone and plate, plate and
plate) applies a shear deformation by making a rotational movement
in the case of rotational testing as well as creep and relaxation
testing or the geometry makes an oscillation movement in the case Figure 1: rheometer
of oscillatory testing. An exception is the starch pasting cell where
the induced deformation cannot be specified as shear but is a more random, undefined deformation. All geometries are
temperature-controlled so exact time-temperature profiles and well-defined heating and cooling rates can be applied to
the sample during testing.

For stress controlled rheometers the stress (torque) is controlled and the deformation (rotational speed, deflection angle)
is measured. For strain controlled rheometers the deformation (rotational speed, deflection angle) is controlled and the
stress (torque) is measured. Consequently, the primary information obtained from an experiment are the stress and the
strain. All other parameters like viscosity, complex modulus,… can be calculated from those primary values using the
rheometer software or other software like excel.

2. Geometry selection
The choice of the geometry is very important for data quality. It depends both on sample characteristics as well as on the
type of rheological test that is intended.

The product parameters that should be considered when selecting the geometry:

— Highly viscous or elastic materials are difficult to load into the geometries
— Ensure that in case of flow measurements using plate/plate geometry, the volume between lower and upper
plate isn’t changing during measurements (draining of the sample is often seen at high shear rates).
— Low viscous materials have a too high risk of draining from plate/plate geometries so they should be measured
in a cup
— The presence and size of particles determines the minimum measuring gap and thus the geometry selection
— Destabilization mechanisms that can occur in the sample during the measurement:
▪ Sedimentation of particles
▪ Syneresis, i.e. the release of an aqueous phase due to contraction of the inner structure (e.g. yoghurt)
— Wall slip between the sample and the geometry can occur with e.g. fatty materials like butter. This can be avoided
by using sandblasted or profiled geometries
— Destruction of the material during sample loading
 — How much sample is available for the measurement?
— Is the material easy to clean?

The test parameters that should be considered when selecting the geometry:

— Heating and cooling rates

— High or low shear rates
— If high temperatures are used for some samples there is a risk on evaporation

Table 1 gives an overview of geometries that are most frequently used in food research. Figure 2 presents a tool to help
selecting the appropriate geometry.

Starch cell (no

Y oscillation or low
Low viscosity (oil, shear)
Particles?
sugar solutions…)
Concentric cylinders
N
Cylinders: lower
Y Plate-plate heating/ cooling
Medium viscosity rate
(ketchup, molten Particles?
chocolate…) Most geometries
N Cone-plate
are possible

Y Plate-plate Plate-plate
High viscosity
(bread dough, Particles?
custard…) Cone-plate or
N plate-plate

Figure 2: tool for selecting the geometry

After selection of the geometry, consider the following points of attention:

— In case of water-rich materials, drying out can compromise the rheological data: use cover (solvent trap)
— Risk on wall slip: use sandblasted/profiled surfaces
— Sample loading: take a homogeneous sample, use the correct amount of sample and standardize the sample
loading as this can affect the result
— Adapted sample loading protocols can be designed to limit sample destruction
— Temperature equilibration before the analysis to avoid temperature gradients in the sample
— For visco-elastic samples: sample relaxation occurs after loading so an initial resting/relaxation period should
be included in the test procedure
— Rheometer specifications:
o Make sure the proper geometry is selected in the software as the geometry inertia needs to be correctly
set to get valuable rheological data of your sample.
 Table 1: Overview of geometries frequently used in food research

Information Advantages Disadvantages

Concentric cylinders Inner cylinder (bob) + outer 1. Low-viscosity fluids cannot flow 1. Relatively large amount of
cylinder (cup) out of the geometry gap sample required
2. Good temperature control 2. Cleaning is difficult and can be
Narrow gap to correspond the 3. Gap remains filled, even for time-consuming
two-plates model: described by viscoelastic materials showing 3. For paste-like samples, air
standards ISO 3219 and DIN the Weissenberg effect bubbles can be introduced and
53019-1 4. Sandblasted or profiled to remain unnoticed
prevent wall slip (not available) 4. Low viscosity fluids: risk at flow
5. Cover to prevent evaporation instabilities and turbulent flow
at high rotation speeds

Cone-and-plate Upper circular cone with 1. Uniform shear conditions 1. Maximum particle size is limited
angle<4° (1° recommended by because shear rate/deformation (dmax<a/5 with a the gap at the
ISO) is constant in the entire gap cone tip)
Lower plate diameter between 2 2. Small sample size 2. Not suitable for samples with a
and 20 cm 3. Easy cleaning 3D internal structure like gels,
4. Air bubbles are pressed out crystal networks, aggregates,…
Rotational tests: despite all during gap setting 3. During gap setting the force is
disadvantage it is the preferred concentrated at the cone tip
geometry because of the 4. Edge failure: flow out,
uniform shear conditions evaporation (use cover), flow
Oscillatory tests within the LVR: inhomogeneities,…
all geometries give results 5. Temperature is regulated at
independent of the strain so this bottom plate so a larger gradient
advantage does no longer count. exists when using larger plates
6. Sandblasted or profiled surfaces
are not possible
Plate-and-plate Upper circular plate and lower 1. Possibility to measure samples 1. Shear conditions are not
circular plate with relatively large particles constant: shear rate is zero in the
and with a 3D internal structure center and increases outwards.
2. Easy cleaning (not an issue for oscillatory tests
3. Sandblasted, serrated or profiled in the LVR)
surfaces are possible 2. Edge failure: flow out,
evaporation (use cover), flow
inhomogeneities,…
3. The larger the gap, the later the
temperature gradient
Starch pasting cell A removable cup with a rotating 1. A large gap allows structure 1. The impeller induces an ill-
impeller development without clogging defined flow
2. Very efficient and fast cooling
system
3. Easy cleaning
3. Rheological test
Figure 3 gives an overview of the rheological tests that are used frequently for food products. Rheology requires repeated
experiments to obtain a reliable value. A minimum of three repetitions is advised. After selection of a suitable test, the
repeatability of the procedure should be determined first. In case needed, optimize the rheological method to ensure a
good reproducibility. This includes the sample preparation, sample loading, the geometry as well as the rheological method
applied.

The following points of attention can help to decide about the type of test:

- Sample characterization? Comparison of samples?

- Simulating production process, storage conditions, consumption,…?
- Internal structure of the sample?
- In regard of yield stress determination, make sure you know which type you want to determine, namely true yield
stress (via stress sweep) or dynamic yield stress (via strain rate sweep).
- Frequency sweeps: data collection in frequency should be based on number of oscillations, rather than time
(standard measuring is done over 3 s periods; in case of a frequency of 0.01 s-1 one 1 oscillation takes 100 s, there
is no representative data collection).
- Rheometer specifications:
o Modern rheometers allow to define procedures under stress or strain control. The choice depends on
the type of sample, the variation among samples and exactness of results that are wanted.
o By setting up a method in the software of AR200(ex) rheometers, the software provides you the
potential maximum range by pointing to the white box.

Figure 3: overview of rheological tests frequently used for foods

4. Rheology @ the food structure & function research group
The information in this guideline is especially focused on the current availability of geometries and experimental set-ups
at the laboratory of Food Technology and Engineering (Ghent University). The following equipment is available:

Two TA instruments stress-controlled rheometers (AR2000ex and HR10) with temperature control: one water bath is
connected to both rheometers so controlling the temperature of both instruments. The temperature of the water bath is
ideally 10°C lower than measuring temperature. However, when using both reometers, the lowest measuring temperature
on one of either rheometers needs to be considered.

The following geometries are available:

- Concentric cylinders
- (corrugated) plate-plate
- Cone-plate
- Starch pasting cell

One Anton-Paar rheometer (MCR 302) with temperature control. The following geometries are available:

— Concentric cylinders (single & double gap)

— (Sandblasted) plate-plate
— Vane

5. Data processing
The data of a rheological experiment (AR2000/AR2000ex rheometers) can be analyzed using the Rheology Advantage
Data Analysis software. This software gives you a table of the raw data which you can export to a text file (File -> Export
To Text) and then use in another software (excel, sigmaplot, matlab,…) to analyze the data (e.g. fitting rheological models)
and make graphs. The Rheology Advantage Data Analysis software can also make graphs but to make the graphs uniform
in your scientific report it is advised to use the same software for all graphs (if possible).

Stress / frequency sweeps: blue data in a column in Data Analysis software indicated that the output data isn’t accurate as
for example the stress/deformation recorded is below or close the limit of detection.

6. Further information
There are other rheological techniques that are used in food research like interfacial rheology, rheomicroscopy, tribology,...

For more information you can refer to the following books which are available on request:

Mezger, T.G. (2014). The rheology handbook. European coatings tech files. 432p.

Mezger, T.G. (2014). Applied rheology: with Joe Flow on Rheology Road. Anton Paar GmbH. 192p.