Question 1 Explain viscosity and also its measurement.

Ans: Viscosity is the resistance to deformation and flow. It is the measure of the internal friction
of a fluid. This friction becomes apparent when a layer of fluid is made to move in relation to
another layer. Different fluids deform at different rates under the same shear stress. Fluid with a
high viscosity such as syrup, deforms more slowly than fluid with a low viscosity such as water.
The greater the friction, the greater the amount of force required to cause this movement, which
is called "shear. Shearing occurs whenever the fluid is physically moved or distributed, as in
pouring, spreading, spraying, mixing, etc. Highly viscous fluids, therefore, require more force to
move than less viscous materials
Isaac Newton defined viscosity by considering the model represented in the figure below.

Figure: Isaac Newtons model for viscosity

Two parallel planes of fluid of equal area "A" are separated by a distance "dx" and are moving in
the same direction at different velocities "V1" and "V2." Newton assumed that the force required
in maintaining this difference in speed was proportional to the difference in speed through the
liquid, or the velocity gradient. To express this, Newton wrote:
F/A = dv/dx
Where is a constant for a given material and is called its "viscosity'. The velocity gradient,
dv/dx, is a measure of the change in speed at which the intermediate layers move with respect to
each other. It describes the shearing the liquid experiences and is thus called "shear rate ()." Its
unit of measure is called the "reciprocal second"(s-1). The term F/A indicates the force per unit
area required to produce the shearing action. It is therefore referred to as "shear stress () its unit
of measurement is "dynes per square centimeter" (dynes/cm2).
Viscosity may be defined mathematically by the formula:
A viscometer (also called viscosimeter) is an instrument used to measure the viscosity and flow
parameters of a fluid. Since viscosity cannot be measured directly, viscometers are instead used
to measure an experimental parameter that is related to viscosity in a known manner. Based on
instrumentation, it is of two types:
1) One point" instruments-
It provide a single point on the rheogram. Extrapolation of a line through this point to the
origin will result in the complete rheogram.
It is used for Newtonian fluids.
Since the rate of shear is directly proportional to the shearing stress.
The capillary and falling sphere are for use only with Newtonian materials.

a. Ostwald or Capillary Viscometer:

Capillary viscometers measure viscosity by monitoring fluid flow through very narrow
glass tubes. In a capillary viscometer, a liquid is drained or forced through a finebore tube, and
the viscosity is determined from the measured flow rate, applied pressure, and tube dimensions.
For a given pressure drop, the time it takes for a fluid volume to flow a certain distance through a
tube is a function of the fluid's resistance to flow. A more viscous fluid will take a longer time to
travel that distance. When a liquid flows by gravity or by driving force, the time required for the
liquid to pass between two marks (shown in figure) through a vertical capillary tube is
determined to measure viscosity. Capillary viscometers are used to measure specific types of
fluids, such as opaque viscometers for darker fluids, or highviscosity viscometers for fluids with
particularly high viscosities.
b. Falling Sphere Viscometer:
Falling ball viscometers determine the viscosity of a Newtonian fluid by measuring the
velocity of a ball moving through the fluid. The fluid is placed in a container, such as a graduated
cylinder The sample and ball are placed in the inner glass tube cylinder and allowed to reach
temperature equilibrium with the water in the surrounding constant temperature jacket. The tube
and jacket are then inverted, which effectively places the ball at the top of the inner glass tube. A
lower fluid viscosity results in less resistance to flow, which corresponds to a faster velocity of
the moving object. The time for the ball to fall between two marks is accurately measured and
repeated several times The velocity of the moving object is then used to calculate the viscosity of
the fluid. Falling body viscometers are commonly used for lowviscosity substances in the
pharmaceutical, food, chemical and mineral oil industries.
2) Multi-point instruments
It is used with non-Newtonian systems.
They are rotational viscometers are made up of two parts: One that rotates, and another that
remains stationary
The instrumentation used must be able to operate at a variety of rates of shear.
Cup and Bob and Cone and Plate viscometers may be used with both types of flow system
(Newtonian and Non-Newtonian)
1. Cup and Bob Viscometer: The rotational viscometer consists of two basic parts separated by
the fluid being tested. The two parts may be: concentric cylinders (cup and bob), parallel plates, a
low angle cone and plate, or a spindle inside of a cylinder The sample is placed in the cup and
the bob is placed in the cup up-to an appropriate height. The sample is accommodated between
the gap of cup and bob. Rotation of the inner cylinder (cup or bob) generates shear on the fluid,
causing the fluid to flow within the viscometer. The torque required to produce a given angular
velocity, or the angular velocity resulting from a given torque, are measures of the viscosity of
the fluid.
2. Cone and Plate Viscometer:
The sample is placed at the center of the plate which is then raised into position under the cone.
The cone is driven by a variable speed motor & the sample is sheared in the narrow gap between the
stationary plate and the rotating cone. The rate of shear in rev./min. is increased & decreased by a selector
dial & the torque (shearing stress) produced on the cone is read on the indicator scale. A plot of rpm or
rate of shear versus scale reading (shearing stress) may be plotted.
Question 2: How are the New and Innovative rheological methods different from the
traditional rheological methods? Also enlist the various new and innovative techniques of
rheological measurements?
Ans:
Rheology is the study of the flow and deformation of matter. Rheological measurements
are used in the food industry for scale up and quality control as well as in the laboratory for
scientific research. Although there are many possible tests, analyses of interest in food rheology
may be grouped as either tensile, compressive, or shear testing. The validity and repeatability of
the measurements gathered from shear testing depend on both instrumentation and methodology.
For example, determination of rheological properties may be difficult when instrument
sensitivity is below that needed to determine the property, or if the methodology used requires
the sample to be altered (by mixing with a solvent, heating, cooling, shearing, etc.) or contains
assumptions that may not hold true for the sample. Additionally, certain foods such as foams,
foods with high lipid content, and foods containing hydrocolloids can be difficult to analyze, as
these foods can be extremely shear sensitive and exhibit phenomena such as slip or problems
associated with significant normal stress differences. Traditional rheological tests are inherently
disruptive to the sample, applying sufficient force to the sample to induce a deformation. This
force may damage sensitive structures, altering the rheological properties of the sample. It is
often necessary to develop protocol that is minimally disruptive to the sample. Depending on the
desired measurement, it may also be necessary to couple rheological equipment with other
analytical tools such as microscopy or magnetic resonance equipment. In particular,
methodology that couples microscopy with traditional rheological techniques, or micro rheology,
has evolved significantly over the past decade. Although micro rheological measurements are not
directly relatable to Rheological Measurements. Traditional rheological measurements, micro
rheology is able to overcome several limitations of traditional shear rheology. Additionally,
methodology that can account for non-ideal behavior or behavior beyond the linear viscoelastic
region (LVR) may prove useful when measuring rheological properties of foods, given that foods
are ultimately subjected to stresses outside the linear elastic domain. The rheological
characteristics of a food product influence many aspects of the fluid performance during
processing (pumpability, droplet break-up in spray drying, emulsion formation, flow into molds,
foamability, etc.) and of the finished product quality (texture, flavour release, stability,
appearance). Knowledge of the rheological properties of materials during processing is important
for process design, process control and optimization, and the production of a consistent quality of
product. Traditional rheological measurements, from flow cups and Bostwick consistometers to
computer-controlled capillary and controlled-rate viscometers, have in many cases adequately
served the food industry for decades. What then, is the justification for moving away from these
tried and tested techniques?
The increasing competitiveness within the food industry has driven a conscious move from
traditional factory Quality Assurance laboratories to rapid, real-time response on quality and
process control which necessitates near-line or in-line measurement techniques. The
incorporation of a relevant in-line measurement into the production control procedures, be it in a
feed-forward or feed-back control loop, provides continuous monitoring of a key process
parameter with the option of an automated action. Correctly governed this can provide enhanced
process control, thus, consistent controlled product quality, thereby significantly reducing the
incidence of rework or waste at the finished product stage. Thus, real-time response and process
relevance are the primary Rheological Measurements.
Justifications for using in-line rheometers and viscometers in food production. The majority of
food materials, being primarily suspensions, emulsions, gels, foams, or frequently a combination
of these structures, display highly complex rheological behavior. This behavior encompasses
time-, shear-, temperature-, and pressure-dependence, each of which severely restricts the
validity of offline rheological measurements to provide information pertinent to the processing
conditions. An off-line analysis provides a retrospective snapshot of the sample rheology, which
may not reflect the sample behavior a minute before or after the sampling time. Meaningful
interpretation of off-line analysis in terms of the process, becomes considerably complicated
when dealing with complex food systems, for example:
A 50% total solids milk concentrate will flow readily into a sample container from the process
line, but frequently undergoes rapid gelation thereafter, even with controlled temperature, thus it
is not tested under relevant process conditions.
Chocolate displays marked dependence on shear history, requiring time consuming sample
preparation prior to measurement to eradicate the sampling and pre-shear conditions, thus the
measurement is not real-time.
 Sampling an emulsion system through a valve can result in high shear exposure for the
sample sometimes irreversibly altering its structure. Thus the sample properties measured off-
line may be a consequence of the sampling and are not representative of the sample under
processing conditions.
Although the process relevance of off-line measurements is often limited by the material
and the type of process information sought, plus the often fragile heterogeneous samples, modern
laboratory rheometry can provide access to a wide temperature and shear rate range, high
pressure, dynamic low strain measurements, normal stress measurement, creep experiments and
extensional rheology, therefore providing an in-depth characterization of a food system. For
research and finished product analysis modern laboratory rheometers offer an important source
of information. However, to obtain real-time knowledge of fluid performance during processing,
both in-line and on-line rheometry is extremely desirable.
The various new and innovative techniques which are used for the measurement of rheological
properties of food items are:
Large amplitude oscillatory shear
Rheology and Ultrasound
Rheology and Nuclear Magnetic Resonance
Rheology and Magnetic Resonance Imaging
Rheology and Confocal Scanning Laser Microscopy
Rheology and Atomic Force Microscopy
Rheology and Diffusing Wave Spectroscopy

Question 3: Describe the technique of ultrasound in determining the rheology of the food
materials?
Ans:
Ultrasound is defined as mechanical wavelengths ranging from 0.001 to 1.0 mm in
length. The methodology for using ultrasound to measure the rheological properties of materials
was developed in the late 1990s and has become widely used for characterizing rheological
properties of foods during the past decade. Ultrasound has been used to characterize many
different foods, including carrageenan gels, protein gels, dairy products, chocolate, cake batter,
flour doughs, honey, tomato concentrate, and tofu. Ultrasound may be used to measure the
rheological properties of either stationary samples or fluids flowing in a pipe. Both
methodologies use frequencies ranging from 1 to 100 Hz. The methodology of ultrasonic
measurements in a stationary sample involves two transducers placed on either side of a sample
chamber containing the material to be measured (Figure).
One transducer (T1) converts an input electrical impulse into a sonic pulse at a preset frequency
and directs the pulse at the sample. The sound waves travel through the sample and are detected
by the second transducer. The second transducer (T2) converts the waves back to an electrical
impulse and sends the electrical pulse to a computer for comparison to the input pulse for signal
loss due to attenuation and time delay. Various properties of the material, such as storage and loss
modulus, and size of suspended particles, can then be calculated from the velocity and time data.
A second method using ultrasound to calculate shear properties of materials was developed. This
method uses an ultrasonic shear transducer with a delay line. The transducer fires an ultrasonic
pulse along the delay line at the sample interface, which reflects the pulse, and the same
transducer detects the reflected pulse. The phase and magnitude as a function of frequency are
then analyzed by Fourier transform. Complex shear modulus, phase angle, and dynamic viscosity
may be calculated from the Fourier transform of the data. Ting et al. (2009) used a similar
method to examine changes in viscoelasticity of tofu during gelation. Although static
measurements of materials using ultrasound yield valuable rheological information, there are
several disadvantages to this method. Measurement rate is slow and generally provides data at a
single shear rate. It is also difficult to properly replicate process conditions in a laboratory, so the
properties or the velocity profiles of the material measured in the lab may not be the same as
those of the material in the process. In addition, calculating rheological properties from available
process information (temperature, pressure, etc.) is extremely difficult. Therefore, it is necessary
to measure rheological properties of the material during processing using an in-line technique.
Many studies have been done over the past decade to develop such techniques that utilize
ultrasound. Techniques using ultrasound to measure properties of fluids flowing in a pipe take
advantage of the Doppler Effect. A transducer is mounted at a set angle of inclination in a flow
adapter cell in the pipe in which measurements will be taken (Figure 3a). The transducer fires
short pulses of ultrasonic waves into the fluid as it flows through the pipe. The pulses are
separated by a set time period. The waves are reflected by the fluid and received either by the
same transmitter, which is switched into receiving mode when not transmitting ultrasonic pulses,
or a second transducer in receiving mode. The returned pulses are shifted slightly in frequency
owing to the Doppler Effect. A Fourier transform of the received waves may be used to calculate
the Doppler shift frequency spectrum at each radial position in the pipe. Frequency shift and time
interval between transmitted and received pulses are then used to calculate the velocity profile of
the fluid developed algorithms using fast Fourier transforms to improve the signal-to-noise ratio
for estimating velocity profiles. A second method of measuring properties of flowing fluids using
ultrasound involves two pairs of transducers (Figure 3b), one pair (T1 and T2) set perpendicular
to the pipe wall and a second pair (T3 and T4) set at an angle () to the pipe wall. The first pair
of transducers is used to measure the velocity of the fluid from time-of-flight measurements. The
second pair of transducers is used to determine the velocity profile of the fluid. This setup allows
simultaneous measurement of acoustic properties of the fluid and the flow profile of the fluid.
Velocity profile measurements derived from the ultrasonic measurements are often combined
with measurements of pressure drop in the fluid, resulting in a technique known as ultrasonic
pulsed echo Doppler-pressure difference (UVP-PD). UVP-PD may be used to measure flow
profiles, viscosity over a range of shear rates, wall slip behavior, yield stress behavior,
volumetric flow rate, and physical changes in process material. Ultrasound may be used to
measure various properties of foods such as gelling behavior, fat content, particle size, molecular
relaxation, shear properties, and viscosity. Ultrasound has also been used for quality control.
Advantages of ultrasound include nondestructive measurement of samples, precise and rapid
measurements, propagation of waves through opaque materials and pipe walls, relatively low
cost compared to other imaging techniques, and ability to characterize volumetric viscosity.
However, the sensitivity and accuracy of ultrasound measurements depend upon the penetration
depth of the sound waves. Too small a penetration depth decreases the signal-to-noise ratio of the
measurements, decreasing measurement accuracy. Penetration depth depends on the food and is
highly frequency dependent. In addition, air bubbles in the sample can increase attenuation at
low frequencies. Measurement sensitivity of in-line Doppler measurements is dependent on the
spatial resolution of the ultrasound measurements, which is impacted by pulse width, beam
width, and demodulation filter bandwidth. Finally, velocity measurements are very temperature
sensitive, requiring temperature control to 0.1C for accurate measurement.
Advantages of this method:
Nondestructive sample measurement.
 Precise measurements.
May be used with opaque materials.
Able to characterize volume viscosity.
Allows measurement of rheological properties under process conditions.
Low cost imaging technique.
Disadvantages of this method:
Velocity measurements are highly temperature dependent.
Slow measurement rate.
Provides data at a single shear rate.
Measurement sensitivity depends on.
Wave penetration depth (varies with food and frequency used).
Inline measurements dependent on spatial resolution.
Inline measurements require additional pressure drop measurements to calculate rheological
properties.
Applications of this method:
Homogenous liquids and semisolid foods that are able to flow under measurement conditions.

Question 4: Describe the technique of nuclear magnetic resonance in determining the

rheology of the food materials?
Answer: NMR, an analytical technique traditionally used to determine material components and
molecular structure, has been used in food science since the 1970s to study the structure and
dynamics of solid systems. Because NMR can differentiate between different structural
orientations and arrangements, it is commonly used as a fingerprinting method for various foods
and food components, such as carbohydrate, proteins, and lipids. Over the last decade, the use of
NMR in food science has begun to shift from a fingerprinting tool to a rheological tool. Several
advances in NMR technology have allowed rheological properties to be determined from NMR
output. In particular, NMR velocity profiling, Diffusometry, and relaxometry have been
particularly useful in determining rheological properties of foods. NMR velocity profiling
involves the use of MRI and will be discussed in the next section. NMR diffusometry examines
the translational motion of molecules and particles and has been widely used in the investigation
of colloidal and emulsion behavior. Pulsed field gradient (PFG) NMR (Figure) is the most
common type of NMR method used in this type of study, as it is most capable of quantitatively
measuring droplet size distribution. Knowing the droplet size distribution is critical to
understanding emulsion rheology and functionality. In PFG NMR, the sample is placed in a
chamber surrounded by a radio frequency (RF) coil. Two sweep coils are located on either side
of the sample. A transmitter fires two gradient pulses of the same magnitude and duration
through the RF coil into the sample. Because PFG NMR works on the basis of spin echo, a 180
pulse is fired into the sample between the two gradient pulses. The first gradient pulse dephases
proton precession frequency, whereas the second gradient pulse rephrases the frequencies.
Particle diffusion causes a phase shift in proton frequency, leading to signal loss in the second
pulse. The self-diffusion coefficient may be calculated from the phase shift and the gradient
pulse parameters. Droplet size distribution may also be calculated, as the phase shift is a
distribution rather than a single value. This technique has been used by many researchers to
study the behavior of various food and pharmaceutical colloids and emulsions, as well as gelatin.
NMR offers several advantages over other techniques used to study emulsions. Being
noninvasive, it may be used for opaque emulsions, emulsions contaminated with gas or
suspended solids, and highly concentrated emulsions (Gabriele et al. 2009, Johns 2009). NMR
also allows the identification and analysis of the behavior of each component in the sample from
a single measurement. However, the sensitivity of NMR in this application is limited by the
restricted molecular diffusion. A rule of thumb given by Johns (2009) for sufficient sensitivity is
that the mean molecular diffusion length should be approximately equivalent to the droplet
radius. Sensitivity is also limited by the instrument: Benchtop NMR instruments usually have
relatively low magnetic field homogeneity and strength. The lower-quality magnetic field results
in decreased measurement sensitivity reproducibility. However, recent technological advances
have been shown to improve measurement sensitivity. In addition, the sample must contain a
spin-active nucleus. Hydrogen (1H) is typically used when studying foods because it is the most
sensitive probe for water, which is generally present in large quantities in food products. NMR
relaxometry measures the spin-lattice and the spin-spin relaxation of particles in a material. Spin-
lattice relaxation refers to the interaction of a spin and the environment, whereas spin-spin
relaxation refers to the mobility of interacting spins. In relaxation, energy is exchanged between
a spin and the environment (spin-lattice) and among spins (spin-spin) to bring the material to an
equilibrium state. It is possible to relate the spin-lattice and the spin-spin relaxation of a particle
to the molecule containing the particle. In food systems, the most common spin-active molecule
used in this technique is 1H. By measuring the spin-lattice and spin-spin relaxation time of a
food component such as water, it is possible to determine the mobility of water in the food. It is
also possible to determine the mobility of components (polymers, etc.) in the water by examining
the chemical exchange of 1H between the water and the second component. This information
may be used to determine phase behavior, such as the transition from liquid to solid state. For
these reasons, NMR relaxometry has been used to examine gelling behavior of egg white protein,
fish proteins, gelatin, starches, various hydrocolloids, and pectin. Additionally, it has been used
to study the gelatinization behavior of starch, dough behavior, addition of starch to imitation
cheeses, fat content and crystallization, and melting behavior of sugar solutions with added
hydrocolloids. Many studies showed good correlation between traditional rheometry and NMR
data.
Advantages of this method:
Noninvasive technique.
May be used with opaque materials.
May be used with heterogeneous samples.
Allows identification of multiple components with one measurement.
Disadvantages of this method:
Measurement sensitivity limited by molecular diffusion.
Benchtop instruments have relatively low magnetic field strength and homogeneity.
Sample must contain a spin-active nucleus.
Applications of this method:
Gels and other foods with relatively few components.

Question 5: Describe the technique of magnetic resonance imaging in determining the

rheology of the food materials?
Answer:
MRI, an analytical technique that forms images from NMR data, is generally associated
with the medical field as a diagnostic tool, but it can be used for many other purposes. Recently,
it has been used to measure many different parameters in many branches of science, including
food science and rheology. An MRI apparatus generally consists of three parts: a magnet, an RF
coil, and gradient coils (Figure). The magnet creates a constant, homogenous magnetic field in
the sample, and the RF coil both sends out and detects pulses in the sample. The gradient coils
detect motion in the sample, allowing the motion to be resolved spatially. This spatial resolution
allows parameters such as proton density, spin-lattice relaxation, spin-spin relaxation, and
diffusion properties, as well as a general profile of the sample, to be mapped. A sequence of these
mapped parameters over time yields valuable information on material behavior, e.g., the
interaction of water with other compounds in the sample and the relative amounts of water and
lipid present. Studies examining foams, emulsions, oil migration in confectionary products, pasta
drying, structural changes in bread during baking, changes in foods during storage, and gelation
of meat systems have taken advantage of this ability, revealing new insights on these food
processes. MRI has advantages and disadvantages similar to NMR: It is a nondestructive
technique that can be used on opaque, but its sensitivity is limited by the strength and
homogeneity of the magnetic field. One novel application of MRI that is of particular interest in
rheology is MRI velocity profiling, also called rheo-NMR. This has been done in both a cup and
bob apparatus and in pipe flow. The principle for either experiment remains the same. The
velocity of the material in the apparatus is measured by using the time-of-flight, spin-tagging, or
phase-shift method, with time-of flight and phase-shift being the most common methods. The
time-of-flight method is the oldest method of velocity measurement and tracks the NMR
excitation of a predetermined part of the sample. The displacement of that part of the sample is
tracked over time, allowing calculation of the velocity. This technique is relatively simple to
perform and gives accurate results at steady- state flow but cannot be used for multidirectional
flow and is not sensitive enough to measure low velocities (less than 1 mm s1). The spin-
tagging method is similar to this method but looks at the magnetic pattern over the whole
sample, allowing flow in the entire sample to be mapped. The phase-shift method is more
accurate than time-of-flight and spin-tagging. This technique maps the NMR signal in the sample
and compares the measured phase of each pixel with the phase of that pixel in a flow-
compensated reference map. Determination of the velocity profile of the material allows the
calculation of flow properties such as viscosity, yield stress behavior during flow, thixotropic
behavior, and shear stress and shear. MRI velocity profiling can also be used to study complex
flow, shear banding phenomena, wall slip, and crystallization behavior. Because most foods are
complex, viscoelastic, non-Newtonian, or a combination thereof, this technique is highly useful
in studying flow behavior of foods, although few foods have been studied in this manner. Foods
studied in a Coutette-type apparatus using MRI velocity imaging include lipids and food
emulsions. MRI velocity profiling data had similar results to traditional rheometry data. MRI
velocity imaging of foods has also been studied in pipe flow of hydrocolloids, yogurt, and biscuit
dough. Advantages of MRI velocity imaging include the ability to measure opaque materials and
to measure velocity without the need for flow markers or optical access, as well as noninvasive
measurements. It also has the ability to measure materials during processing, yielding valuable
information on food behavior under processing conditions. Disadvantages include possible
image blurring at high velocities, the need for large sample sizes with time-off light methods to
improve signal strength, and the inability to use the Couette cell with certain materials such as
pastes. However, these disadvantages are mitigated by several recent advances, such as rapid
imaging techniques and the use of Fourier transforms.
Advantages of this method:
Noninvasive technique.

May be used with opaque materials.

May be used with heterogeneous samples.

Allows study of complex flow behavior.

Enables velocity measurements without flow markers or optical access.

Allows for measurement of rheological properties under process conditions.

Disadvantages of this method:

Benchtop instruments have relatively low magnetic field strength and homogeneity.

Sample must contain a spin-active nucleus.

Possible image blurring at high velocities.

Large sample sizes required with time-of-flight methods.

Certain materials may not be used in a Couette cell.

Applications of this method:
 Low-viscosity liquids, pumpable liquids, and semisolids.
Question 6. List the importance of rheological data in food industry?
Ans:
Rheological data are needed in numerous areas in the food industry:
a. Process engineering calculations involving a wide range of equipment such as pipelines,
pumps, extruders, mixers, coaters, heat exchangers, homogenizers, and on line viscometers;
b. Determining ingredient functionality in product development;
c. Intermediate or final product quality control;
d. Shelf life testing;
e. Characterizing ingredients and final products, as well as for predicting product performance
and consumer acceptance.
f. Evaluation of food texture by correlation to sensory data;
g. Analysis of rheological equations of state or constituent equations.
h. They are also a way to predict and control a host of product properties, end use performance
and material behaviour as well as sensory analysis and quality control of foods.