Basic Food Rheology 2016

BASIC FOOD RHEOLOGY
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INSTRUMENTAL ANALYSIS OF FOODS
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Prepared by: Dr Aishah INSTRUMENTAL ANALYSIS OF FOODS
LESSON OUTCOME
At the end of this lesson, you should be able to:
• Define the rheological terms

• Explain the importance of rheological measurement
• Describe factors that affects rheological properties of food material
• Understand the rheological models
• Describe the small and large deformation tests and their applications.
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LESSON OUTLINE
1.0 Introduction
- Terms and definition
- Deformation, stress, yield stress, strain, viscosity, storage
modulus, loss modulus, loss factor, phase angle
2.0 Importance of rheological measurement
3.0 Factors affecting rheological properties

- Chemical and physical factors
4.0 Difficulty in studying food rheology
5.0 Types of food materials and rheological models

- Hooke solid, Newtonian liquid
- Non-Newtonian fluids (Time-dependent and Time-independent)
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LESSON OUTLINE
6.0 Classification of Rheological Tests

- Fundamental, Empirical and Imitative Tests
7.0 Small Deformation Tests

- Capillary viscometer, Falling-ball viscometer
- Rheometer (cone and plate, parallel plate, concentric
cylinder), oscillation techniques – creep test, stress
relaxation
8.0 Large Deformation Tests

- Puncture, Bending, Tensile, Compression
- Texture Profile Analysis
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1.0 Introduction
• Rheology originated from Greek words
– ‘‘rheo’’ meaning flow and ‘‘logy’’ meaning science
• Definition of Rheology
“Science that is concerned with the flow and deformation

Rheology
characteristics in Daily
of material Life
under the influence of stress”
We normally take for granted a lot of things in life FST606

Term & Definition
a) Deformation
• Occur when an external force is applied to a food, it will either cause
movement and/or change in shape under a steady-state or dynamic
conditions.
• If the food material is solid – the applied force will result in
deformation such as change in shape, fracture or break.
• If the food material is liquid – the applied force will result in flow.
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Term & Definition
b) Stress
• Define as force per unit area of food material needed to cause
deformation. Unit: Pascals (Pa) or dynes/cm².
• Direction of force to the impacted surface area determine the type of
stress.
• Force applied perpendicular to the surface of a material - tensile stress.
• Force applied tangentially to the surface of material - shear stress.
• Or force can be applied at any other angle to the surface of the material.
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Term & Definition
c) Yield Stress
• Minimum amount of stress required to make a sample flow.
• In other words, shear stress necessary to initialise flow (semi-solid

food) or minimum force that has to be applied to a material before it
deforms (solid food).
Rheology
• Example of product having inaction
yield stress: honey, yogurt, chocolate syrup,
tomato ketchup, mayonnaise etc.
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Term & Definition
d) Strain
• The distance that the material travel/move before it break when
stress is applied (extension per unit length).
• Direction of applied stress with respect to material determine the
type of strain.
• Normal strain - when stress is normal to material surface. Food
materials show normal strain when compressed or pulled apart
(tensile stress) or shear strain.
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Term & Definition
Stress-Strain curve
1. Elastic limit
2. Yield point
3. Point of maximum stress
4. Point of fracture
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Term & Definition
e) Viscosity
• Resistance of a fluid to flow.
• Define as “Shearing force required to produce velocity of 1 cm/sec
between two parallel plane of liquid separated by 1 cm distance”.
• Some food materials have relatively constant viscosity (viscosity is
independent of applied force or intensity of mixing).
- eg. water, honey, cooking oil, glycerin etc.
• Most food products do not have constant viscosity value (viscosity
decreases/increases when external force is applied).
-exhibit both fluid-like (viscous) and solid-like (elastic) behavior.
-eg. chocolate brownie batter, peanut butter, cream.
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Term & Definition
f) Storage Modulus, G' (N/m2 or Pa)

• Represents elastic storage of energy - measure how well structured
a sample is (eg. highly or weakly structured).
• G’ value will be large if sample is predominantly elastic or highly
structured.
• G' value will increase if structure being build and if structure is
being destroyed, G‘ value will decrease.
g) Loss Modulus, G" (N/m2 or Pa)
• Represents viscous dissipation or loss of energy.
• G” value will be large if sample is predominantly viscous.
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Viscoelastic response of a material
• If G’>G”: material behave more like a solid. However, if G”>G’: material

behave more like a liquid.
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Terms & Definition
h) Delta or loss factor/damping factor (δ)

• Shows the ratio of the viscous to the elastic portion of deformation
behavior
• δ will increase with increasing viscous behavior and decrease with
increasing elastic behaviour
i) Phase angle
• δ = 0o or tan δ = 0 corresponds to an elastic response, δ = 90o or tan
δ = ∞ is a viscous response
• If phase angle is within limits of 0 < δ < 90o material is viscoelastic
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2.0 Importance of Rheological Measurement
• Provide information about food structure - give insight into

structure of food products, eg. degree cross-linking indicate viscosity.
• Aid in design of food processing equipment – affect flow of product

during processing, eg. design of equipment such as pump, large/small
pipe line.
• Provide information related to shelf-life – indicate storage stability,

eg. separation of emulsion products such as mayonnaise & salad
dressing.
• Aid in product development - to correlate with consumer’s

acceptance (sensory), eg. texture, mouth feel.
• Production quality control – product specification and attribute limit

of acceptance.
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3.0 Factors Affecting Rheological Properties
A. Chemical Factors
i) Degree of polymerisation
- Food having longer polymer molecules may be susceptible to shear
depolymerisation, accompanied by decrease in viscosity.
- Eg. Starch, sodium alginate etc.
ii) Extent of Polymer hydration

- In hydrophilic polymer solution, molecules are completely
surrounded by immobilised water molecules forming solvent layer.
- Therefore, hydration of hydrophilic polymers cause increase in
viscosity.
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A. Chemical Factors…
iii) Presence of Impurities, Trace Ions and Electrolytes

- Chemical impurities are major factors in changing viscosity of
natural polymers.
- eg. Sodium alginate solution - viscosity will increase if traces of Ca
present due to formation of calcium alginate.
iv) Effect of pH
- Changes in pH greatly affect viscosity.
- Natural gums have relatively stable viscosity at pH 4 to 5, above
and below this pH range viscosity will decrease sharply.
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B. Physical Factors
i) Temperature
- Increase in temperature usually produces rapid decrease in
viscosity.
- Except of certain synthetic polymers such as methyl cellulose.
ii) Aeration
- Aerated products usually appear to be more viscous than non-
aerated, eg. egg white foam.
iii) Light
- Various hydrocolloids in aqueous solutions are reported to be
sensitive to light, eg. Sodium alginate and CMC.
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4.0 Difficulty in studying Food Rheology
• Food is heterogeneous, consists of enormous range of materials

(ingredients) – complex behaviour.
• Food behaves differently under different conditions.
- eg. ice-cream is in solid form at freezing temperature but in
liquid form at room temperature.
• To understand food texture and the relationship of stress-strain
and deformation – rheological model is used for comparative
purposes.
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5.0 Types of Food Materials and Rheological Models
Types of food materials:

a) Solid foods
eg: crackers, wafers
b) Fluid foods
eg: soft drink, fruit juice
c) Semisolid/structured fluid foods
eg: jelly, mayonnaise, jam
Rheological models:
a) Hooke solid – represent ideal solid
b) Newtonian liquid – represent ideal liquid
c) Bingham model – represent ideal plastic
d) Kelvin-Voight model – represent viscoelastic solid
e) Maxwell model – represent viscoelastic liquid
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i) Hooke Solid
- Ideal solid is perfectly elastic material or linear elastic.
- Obeys Hooke’s law: Stress = Strain x Modulus.
- Does not show flow behaviour (no viscous properties) and
independent of time.
- Not all solid materials are perfectly elastic or linear elastic.
- Can be elastoplastic (eg. butter, margarine, jellies) or may require
yield stress prior to deformation.
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ii) Newtonian Liquid
- Normally, Newtonian foods are homogenous mixture.
- Viscosity is not affected by changes in shear rate and remains
constant.
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iii) Non-Newtonian fluids
- Non-Newtonian foods are heterogeneous mixtures that exhibit
a change in viscosity as shear rate is increase/decrease.
- Different types of Non-Newtonian fluid depending on
behaviour of flow and effect of time.
- Time independent: pseudoplastic, dilatant, Bingham plastic
fluids.
- Time dependent: thixotropic and rheopectic fluids.
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Examples and characteristics of Non-Newtonian foods
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Time-Independent Non-Newtonian fluids
a) Pseudoplastic materials
- Exhibit shear-thinning behaviour (with/without yield stress).
- Viscosity decreases with time with irreversible change as shear
rate increases.
- Eg. some gum solutions and starch pastes.
b) Dilatant materials
- Exhibit shear-thickening behaviour (with/without yield stress).
- Viscosity increases irreversibly with time as shear rate increases.
- Eg. egg white or heavy cream.
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c) Bingham materials
- Materials which initially resist deformation, until certain yield
stress is reached.
- When the yield stress is exceeded, shear rate becomes
measurable and further stress leads to linear behaviour
(Newtonian) .
- Eg. Tomato paste, mayonnaise, margarine.
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Time-dependent Non-Newtonian fluids
a) Thixotropic fluids
- Viscosity decreases with increase time of shearing (time-
dependent shear-thinning).
- Change is reversible therefore if left undisturbed it will regains its
initial viscosity.
b) Rheopectic fluids
- Viscosity increases with increase time of shearing (time-
dependent shear-thickening).
- Change is reversible.
- Rarely observed in food materials.
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Relationship between shear stress and shear rate for Newtonian
and Non-Newtonian fluids
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6.0 Classification of Rheological Tests
• Classification of measurement technique:

a) Fundamental test
b) Empirical test
c) Imitative test
• Test for solid food materials – large deformation test (eg. puncture
test, bending test, compression test, tensile test etc.)
• Test for liquid food materials – small deformation test (eg.
viscosity, viscoelasticity - oscillation test, frequency sweep, creep
test etc.)
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1) Fundamental test
• Determine one or more physical constants to describe exactly the
properties of food in terms of well defined rheological parameters.
• Eg. shear modulus and loss modulus.
• Used mainly in research laboratories than in industrial QC.
• Assumptions made in conducting fundamental test:
– material is homogeneous, continuous and isotropic (exhibit
same physical properties in all direction)
– test piece of sample is uniform and regular shape
– use small strain (1-3% max).
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• Advantages:
- give measurement of well-defined mechanical or rheological
properties.
- able to express results in well-defined units - quantify effects of
sample on probe geometry, rate of deformation and other test
conditions.
• Disadvantages:
- give poor correlation with sensory methods.
- depend upon uniform and homogeneous samples
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2) Empirical tests
• Measure parameters that are poorly defined in rheological terms
but from practical experience are found to relate closely to the
property of interest (textural quality).
• Most widely used in the food industry, eg. study on puncture, shear
and extrusion.
• Advantages:
- easy, rapid and simple to perform
- suitable for routine QC
• Disadvantages:
- arbitrary procedure with no absolute standard available.
- test only effective with limited number of food commodity.
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3) Imitative tests
• Aims to reproduce the mechanical operations applied in human
evaluation.
• Measure various properties under conditions similar to those to
which food is subjected in practice – properties during handling
and consumption.
• Eg. dough testing equipment that imitate handling and working of
bread dough, butter cutting equipment, TPA tests imitates chewing
action.
• Advantages:
- closely duplicates mastication or other sensory method.
- good correlation with sensory methods.
• Disadvantages:
- may be considered as empirical test - tests are not fundamental.
- no fundamental understanding of the result.
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7.0 Small Deformation Tests
i) Capillary viscometer
- measure time taken for the test liquid to flow through a capillary
of a known diameter of a certain factor between two marked
points.
- Various design of glass capillary tubes – Ostwald, Cannon-Feske,
Ubbelohde.
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ii) Falling-Ball Viscometer
- Measure time taken for glass/steel ball to rolls down between two
marked points of glass tube containing test liquid.
- Rate at which the ball falls is an inverse function of viscosity of
sample.
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iii) Rheometer
• Have various geometries used for shear stress and shear rate
measurements
Measuring geometries:
(a) Concentric cylinder
(b) cone and plate
(c) parallel plate
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system is moved to the measuring po
will lead to large errors in the measure
a) Cone and Plate

• Advantages:
Fig. 8 - 2 Measuring system filling
- system relatively easy to fill and to clean
- shear rate uniform across the plate. The volume required for concenctric c
- requires small sample volume the measuring system cup.
• Disadvantages:
- care required when setting gap
C22ib50-e
- sample can be expelled at very high shear rates

- not suitable for low viscosity fluids
- system susceptible to jamming by particulate samples
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b) Parallel Plate
• To overcome some of the problems associated with cone and plate
measuring systems
• Advantages:
- more suitable for highly viscous sample
- range of gap settings (up to max 5 mm) – able to use for samples
with particles
• Disadvantages:
- shear rate varies across diameter of plate (zero at middle plate to
max at rim) therefore calculation biased towards rim –
significant edge effect.
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c) Concentric Cylinders
• Advantages
- Useful for samples containing large particles.
- Not affected much by the gap setting and sample volume.
- Produce results with good repeatability but not always accurate.
(a) double gap

(b) cone and plate at the bottom
(c) hollow cavity bottom
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(a) Double gap
- most sensitive than other concentric cylinder.
- not suitable for particles > 10 μm.
- ideal for low viscosity samples
(b) Cone & plate at bottom (Mooney-Ewart cylinder)

- not as sensitive as double gap but better in term of accuracy
- not suitable for particles > 10 μm
(c) Hollow cavity (large recessed cylinder)

- suitable for large particles up to 100 μm.
- less sensitive than Mooney-Ewart cylinder.
- suitable for low shear measurements on dispersions.
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Techniques of measuring viscous material (Oscillation)
– A dynamic rheological test.

– Non-destructive test which measures simultaneously both the
viscous and elastic behaviour of a sample.
– Major limitation of an oscillatory rheometer is its torque range:
• For very viscous samples: rheometer must have enough torque to
displace the sample by an amount that can be measured
• For delicate samples: rheometer must be able to apply very small
torque so as not to destroy the structure
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3 types of dynamic tests can be conducted in oscillation technique:
a) Frequency sweep – studies in which G’ and G” are determined
as a function of frequency (ω) at fixed temp.
b) Temperature sweep – studies in which G’ and G” are
determined as a function of temp. at fixed frequency (ω)
c) Time sweep – studies in which G’ and G” are determined as a
function of time at fixed frequency (ω) and temp.
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Other small strain tests
i) Creep test
- Use to compare and predict material behavior
- Stress is applied to the material and strain is monitored
with time to establish an equilibrium yield stress
- point of abrupt change or sharp

fall in viscosity shows structure
breakdown
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Other small strain tests..
ii) Stress relaxation
- Stress is applied and then removed – a rapid drop in strain
will be obtained followed by a period of relaxation during
which the strain decreases a bit more before it become
constant.
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8.0 Large Deformation Tests
i) Puncture / Penetration Test

• Simplest method to obtain a stress-strain curve.
• Good and simple way to test food materials with heterogeneous
structure such as cereal bars and chocolates with various layers.
• Rule: a) sample size larger than the probe – no interfering effect of
sample geometry on to the puncture force, b)if base support is used,
sample must not be so flat – to avoid deformation curve to be of
compression rather than puncture, c) use support with a hole, diameter
1.5 to 3x of the probe diameter – to avoid it to be similar to bending test.
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ii) Compression Test
• Similar to puncture test, it measures either force needed to
produce a given deformation or deformation caused by a
given force.
• Rule of product dimension: “Sample being tested must have
surface area smaller than that of the probe being used”
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iii) Bending Test
• Mainly applied to solid food materials with more homogenous
shape or after cutting samples to constant size and shape.
• Material is subjected to tensile, shear and compression forces
• Important outcome: deflection point and Young/Elastic modulus (E).
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iv) Tensile and Extensibility Test
• Used to determine mechanical properties such as yield strength,
tensile strength and % elongation.
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TEXTURE PROFILE ANALYSIS (TPA)
- Texture profiling method involves compressing the test substance at

least twice and quantifying the mechanical parameters from the
recorded force-deformation curve.
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Texture Profile Attributes:
1. Fracturability (Brittleness)
• Force at which significant break occur in the curve (not always
present) or force at which material fractures.
2. Hardness (Firmness)
• Force required to attain a given deformation.
• Maximum force during the first compression cycle (“first bite”) .
3. Cohesiveness
• Ratio of the positive force area during the second compression to the
first compression (A2/A1).
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4. Adhesiveness
• Negative force area for the first bite.
• Representing work necessary to overcome attractive forces between
food surface and surface of probe.
5. Springiness / Elasticity
• Height that the food recovers during the time at the end of the first
bite and the start of the second bite.
• Representing the extent of which compressed food returns to its
original size.
6. Gumminess
• Hardness x Cohesiveness.
• Energy required to disintegrate a semi-solid food to a state ready for
swallowing.
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7. Chewiness
• Gumminess x Springiness
• Hardness x Cohesiveness x Springiness
• Energy required to masticate (chew) a solid food to a state of
swallowing.
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End of Lesson:
Basic Food Rheology
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Basic Food Rheology 2016

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BASIC FOOD RHEOLOGY

At the end of this lesson, you should be able to:

• Define the rheological terms

2.0 Importance of rheological measurement

3.0 Factors affecting rheological properties

4.0 Difficulty in studying food rheology

5.0 Types of food materials and rheological models

6.0 Classification of Rheological Tests

7.0 Small Deformation Tests

8.0 Large Deformation Tests

• Rheology originated from Greek words

– ‘‘rheo’’ meaning flow and ‘‘logy’’ meaning science

“Science that is concerned with the flow and deformation

We normally take for granted a lot of things in life FST606

• Minimum amount of stress required to make a sample flow.

• In other words, shear stress necessary to initialise flow (semi-solid

f) Storage Modulus, G' (N/m2 or Pa)

• If G’>G”: material behave more like a solid. However, if G”>G’: material

h) Delta or loss factor/damping factor (δ)

• Provide information about food structure - give insight into

• Aid in design of food processing equipment – affect flow of product

• Provide information related to shelf-life – indicate storage stability,

• Aid in product development - to correlate with consumer’s

• Production quality control – product specification and attribute limit

ii) Extent of Polymer hydration

iii) Presence of Impurities, Trace Ions and Electrolytes

• Food is heterogeneous, consists of enormous range of materials

Types of food materials:

• Classification of measurement technique:

a) Cone and Plate

- sample can be expelled at very high shear rates

(a) double gap

(b) Cone & plate at bottom (Mooney-Ewart cylinder)

(c) Hollow cavity (large recessed cylinder)

– A dynamic rheological test.

- point of abrupt change or sharp

i) Puncture / Penetration Test

- Texture profiling method involves compressing the test substance at

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