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Advances in rheological measurements of food

products
Jasim Ahmed

The measurement of food rheology has improved significantly
with time and the advent of instrumentation. Flow behavior, its
prediction, and industrial applications are today more realistic.
Evolution of tribology synchronized the measurement of food
texture with the dynamic of oral processing and opened a new
area of rheological study. Importance of small and large
amplitude oscillatory shear measurements for food products
have been highlighted in this review.
Address
Food and Nutrition Program, Environment & Life Sciences Research
Center, Kuwait Institute for Scientific Research, P.O. Box 24885, Safat,
13109, Kuwait
Corresponding author: Ahmed, Jasim (jaahmed@kisr.edu.kw)
Current Opinion in Food Science 2018, 23:127–132
This review comes from a themed issue on Food engineering &
processing
Edited by Hosahalli Ramaswamy
For a complete overview see the Issue and the Editorial
Available online 11th October 2018
https://doi.org/10.1016/j.cofs.2018.10.007
2214-7993/ã 2018 Elsevier Ltd. All rights reserved.
are elucidated. The development in flow rheology was
not substantial as compared to oscillatory measurement,
and therefore, the flow rheology is excluded in this
review.
Small amplitude oscillatory shear
measurement (SAOS)
To understand the dynamic response of a food material
over a time scale, small-amplitude oscillatory shear
(SAOS) measurements are considered as the best tech-
nique. SAOS analyses the linear viscoelastic characteris-
tics of complex fluid foods and also generate information
on material functions in terms of the elastic and viscous
modulus (G0 and G00 ), complex viscosity (h*), and yield
stress. SAOS can measure the change in the microstruc-
ture and entanglement of biomaterials during heating/
cooling or shearing in-situ without damaging the structure
of the test specimens. The measurement is capable of
tracing the possible phase changes occurring in the food
materials (e.g. protein denaturation or starch gelatiniza-
tion) during processing, and even elucidate the mecha-
nism/kinetics of the process. SAOS measurement has the
edge over the conventional DSC measurement [2]. The
theoretical backing of SAOS measurements is very strong
that allows the development of rheological models for
testing molecular and mechanistic hypotheses for a wide
range of frequencies.

Various geometries (e.g. parallel plate, cone-plate, and

Introduction
concentric cylinder/Couette cell) are employed in rota-
Rheology is the study of flow and its deformation. Rheo-
tional rheometers for SAOS experiments, which depends
logical measurements are important for food products, in
upon the nature of the sample. Parallel plate (PP) fixtures
particular, quality control, process equipment design, and
can be used for a wide range of materials with decent
transportation. The scope and application of rheology
sample size, and have the privilege of varying the gap
have broadened exceptionally. With the advancement
sizes. For example, the dough is the best sample for a
of science, the rheological measurement is not confined
parallel plate for its rheological characterization. A small
to flow measurement but also enable to capture the
size sample is adequate for a cone and plate (CP) geome-
microstructure of the fluid during shearing or heat treat-
try for its rheological characterization. CP fixtures can be
ment. The thixotropic loop can provide the structural
employed to determine the first normal force difference
breakdown of a time-dependent food product. A trans-
as shear stress, and shear rate are constant through the
formation of rheological measurement from age-old rota-
gap. The selection of cone angle is tricky, the smaller the
tional viscometry to the large amplitude oscillatory shear
cone angle, the greater the error is likely to be in gap
measurement or optimal Fourier Transformation rheo-
setting. By selecting a relatively large angle (4 or more),
metry imparted the accuracy and sophistication of rheo-
it becomes easier to get reproducibility of gap setting.
logical measurement [1

]. Recently, tribology a contrib-
The Couette cell with a large sample volume generates a
uting discipline similar to rheological studies for
homogeneous strain field and is capable of performing
understanding, as well as texture and mouthfeel has
more sensitive measurements than either parallel plate or
emerged for the characterization the oral processing of
cone-plate configurations because of the increased sur-
food. In this short review, a transition of rheological
face area-to-volume ratio of the annular setup.
measurements and their applications in food products

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128 Food engineering & processing

While comparing various geometries for rheological mea-
surements, higher normal stress and viscosity were
observed for PP than for CP at same shear rates [3,4].
However, some recent studies confirmed that consistency
of linear viscoelastic data obtained from both PP and CP
geometries. SAOS data obtained by using both geome-
tries coincide with each other for various complex fluids
[5]. However, results showed discordance between CP
and PP measurements in the nonlinear regime.
Large-amplitude oscillatory shear (LAOS)
The material stress response deviates from the propor-
tionality between the amplitude of the stress and the
amplitude of the deformation in the non-linear regime.
Typical stress response of aqueous carboxymethyl hydro-
xypropyl guar gum in SAOS and LAOS is illustrated in
Figure 1 [6]. In the non-linear region, the stress response
does not follow a sinusoidal wave form, and the G0 and the
G00 become functions of the strain amplitude, g 0 . LAOS
measurement could be extended for fundamental rheo-
logical measurements of food products in the nonlinear
region. Compared to SAOS, the analysis of test results
obtained by LAOS is more complex, and can be accom-
plished by different calculation techniques. The LAOS
data are analyzed by Fourier-transform rheology, Lissa-
jous plots, and Chebychev polynomial expansion,
however, the interpretation of the measurements is still
an active and challenging area of research.
Fourier Transform Rheology (FTR) is considered one of
the powerful tools to detect and quantify nonlinearities
(e.g. LAOS data). FTR is useful because it transforms the
measured stress data in the time domain into a frequency-
dependent spectrum, which can detect even very weak
nonlinearities in the stress response [7]. Furthermore,
both the intensities and phases of the higher harmonics
in the power spectrum provide valuable information
about the sample being evaluated. The interfacial tension
and droplet size of dilute monodisperse emulsions are
calculated by FTR [8]. FTR can quantify very weak
signals of the generated higher harmonics. However, this
method suffers from a rather complex interpretation due
to multiple higher harmonics.
LAOS tests were employed on hard wheat flour dough
samples (at the different time of mixing) and wheat
protein fractions (gliadin and glutenin) at strains ranging
from 0.01 to 200% and selected frequencies (20, 10, 1, and
0.1 rad/sec) [9
,10]. The Lissajous-Bodwitch curves for
the elastic component of stress in the form of normalized
stress and normalized elastic stress versus normalized
strain at selected frequencies and the selected phases

Figure 1

SAOS LAOS
102
G’, G” [Pa]

101

ω = 10 rad·s-1
G’
G”
100
10-1 100 101 102 103 104
γ [%]
40 80 100
1000
20 40 50
σ12 [Pa]

σ12 [Pa]

γ [%]
γ [%]

0 0 0 0
-20 -40 -50
-40 -80 -1000
-100
2000 2500 3000 3500 4000 2000 2500 3000 3500 4000

t [ms] t [ms]
Current Opinion in Food Science

Representation of SAOS and LAOS for an aqueous carboxymethyl hydroxypropyl guar gum (CMHPG) solution (1.25 wt%) at 10 rad s1.
Source: Reference [6]

Current Opinion in Food Science 2018, 23:127–132 www.sciencedirect.com

 Advances in food rheology Ahmed 129

of dough mixing showed the strain curves were super-
imposed and a comparison was made between the 1st and
4th phases of mixing (Figure 2). In the non-linear strains,
the Lissajous curves display perfect ellipses up to signifi-
cantly higher strains because of the reorientation of the
starch structure without actually dismantling the protein
network that maintains elasticity and intracycle linearity.
With increasing strain, intracycle strain stiffening is
observed because of the stiffening of the gluten network
[9
]. At the maximum frequency, the intracycle strain
stiffening happened rapidly. The Lissajous curves show
narrower elliptical trajectories as the mixing proceeds
[Figure 2a (1st phase) and Figure 2b (4th phase)], which
results in the development of the viscoelastic network of
gluten. The Lissajous curves for glutenin showed more
elastically dominated non-linear viscoelastic behavior
than gliadin, and the decay in elasticity with increasing
strain and frequency for glutenin was much slower than
gliadin [10]. The stress versus the strain rate for the
viscous Lissajous curves showed the elliptic shape as
strain and frequency increased (Figure 3). Additionally,
the larger contribution to the stress wave comes from the
elastic component. Nonlinearities were distinct in the
elastic component than the viscous component.
The small amplitude relaxation spectrum has been suc-
cessfully employed to calculate the LAOS predictions of
various large deformation models for blended dough
(wheat flour/rocket leaves powder) [11]. The LAOS the-
oretical calculations using the Phan-Thien model showed
a good agreement with the first harmonic stress data and
only qualitative agreement with the third and the fifth
harmonic stress values. Authors proposed an improved
damage function, where the time effect on network
damage was taken into consideration and fits Lissajous
stress-strain curves adequately.
LAOS has been tested to understand structural changes
of tomato paste at different deformations and time scales.
Tomato paste showed an irreversible structural change in
LAOS as shown by strain softening (in the mid-oscillatory
region) followed by strain hardening (in the large oscil-
latory region).
Tribology
Tribology is a field of study in friction between two
interacting surfaces, relating to wearing, tearing and
lubrication [12
]. Recently, the technique has been
employed for oral processing of foods, where the tongue
and upper-palate act two interacting surfaces in relative
motion. While food is being chewed, it passed through a
series of stages in the mouth starting from mastication to
chewing, mixing with the saliva and finally transformed
into a bolus ready to be swallowed. The whole process
requires a thorough understanding of the physical mech-
anisms governing dynamic oral processes and how they

Figure 2

σ”/σo 20 rad/s σ”/σ o 10 rad/s σ’/σ o 1 rad/s σ’/σ o 0.1 rad/s

1 1 1 1
o

o
o

σ/σ

σ/σ
σ/σ

σ/σ

0 0 0 0

-1 -1 -1 -1
γ/γ γ/γ γ/γ γ/γ
o o o o
-1 0 1 -1 0 1 -1 0 1
-1 0 1
(a)

20 rad/s 10 rad/s 1 rad/s 0.1 rad/s

σ”/σo σ”/σo σ’/σ o σ’/σ o
1 1 1 1
o

o
o

o
σ/σ

σ/σ
σ/σ

σ/σ

0 0 0 0

-1 -1 -1 -1
γ/γ γ/γ γ/γ γ/γ
o o o o
-1 0 1 -1 0 1 -1 0 1 -1 0 1
(b)
Current Opinion in Food Science

Lissajous curves for the elastic component of wheat flour dough obtained from (a) the 1st and (b) the 4th phase of Farinograph mixing.
Source: Reference [9
]

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130 Food engineering & processing

Figure 3

σ”/σ 20 rad/s σ”/σ 10 rad/s σ”/σ 1 rad/s σ”/σ 0.1 rad/s

o o 1
o 1
o
1 1

o
o

o
o
σ/σ
σ/σ

σ/σ
σ/σ
0 0 0 0

-1 -1 -1 -1

γ/γ • •
o γ/γ • •
o γ/γ
• •
o
γ/γ
• •
o

-1 0 1 -1 0 1 -1 0 1 -1 0 1
(a)

σ”/σ o 20 rad/s σ”/σ o 10 rad/s σ”/σ o 1 rad/s σ”/σ 0.1 rad/s

1 1 1 1
o

o
o

σ/σ

σ/σ
σ/σ

σ/σ

0 0 0 0

-1 -1 -1 -1

γ/γ
• •
o γ/γ
• •
o γ/γ
• •
o γ/γ • •
o

-1 0 1 -1 0 1 -1 0 1 -1 0 1
(b)
Current Opinion in Food Science

Lissajous curves for the viscous component of wheat flour dough obtained from (a) the 1st and (b) the 4th phase of Farinograph mixing.
Source: Reference [9
]

relate to mechanoreceptor stimulation [13
]. From food changes in the frictional properties of food materials
sensory perspective, tribology can be considered as the are described through ‘Stribeck curves’ (Figure 4), which
frictional and other related physical properties exhibited can be divided into three regimes: boundary (speed is
by food when squeezed and sheared between the two low), mixed (speed is increasing) and hydrodynamic
moving surfaces (i.e. the tongue and the palate) during (speed is very high) [12
].
oral processing [14]. The best implications of food tribol-
ogy are the study of smoothness sensation, an essential Rheology and soft tribology have been applied to gain
texture feature linked to the presence of fat or oil and insight into the physical origins of mouthfeel and the
creaminess perception. dynamics of oral lubrication, including the role of saliva
for some soft-food systems (e.g. custards, yogurt, and
A typical Tribo-Rheometry Accessory is illustrated in thickened creams) [13
]. Foods within a similar product
Figure 4a (mostly, the attachment is compatible with a series exhibit unique tribological properties, attributed to
standard rheometer), which facilitates the capability to the preferential entrainment of different phases and
make the coefficient of friction measurements between components at the narrow gap. Food–saliva interactions
two solid surfaces under dry or lubricated conditions. The play a crucial role in determining transient lubrication
basic equation for tribology is FR = m  FL, where FR properties, which may reflect dynamic oral processes. The
stands for the frictional force, m is the friction coefficient, lubrication property of low-fat pot-set yogurt under tri-
and FL is the surface load. The friction coefficient is the bological measurement was found to depend on the fat
most important parameter for measurement of tribology. content, the type and loading concentration of hydrocol-
It gives a quantitative description of the nature of surface loids [15]. A four-zone tribology model for yogurt using
interactions. The value of m depends on the surface ring-on-plate tribo-rheometry and Transpore Surgical
roughness and the geometric nature of surface asperities. Tape as the tongue model and each zone corresponds
If a lubricant is applied, then the m is an effective to different mechanisms of fluid entrained between the
indication of the lubricating status between the two two contact surfaces [15]. The tribological behavior of the
surfaces. In this case, m is no longer a constant but yogurt fluid, therefore, can be represented by the position
becomes a function of the surface properties, the surface of each transition point and the slope of each friction
load, the moving speed, as well as the lubricant charac- zone, which were aligned with the sensory scores from the
teristic. The speed-dependent film formation and trained panel.

Current Opinion in Food Science 2018, 23:127–132 www.sciencedirect.com


Figure 4
(a)
(b)
Tribology
dominated
Boundary
Regime
Friction coefficient (μ)
Mixed
Regime
Viscosity (ƞ) x Speed (V) / Load (PL)
Current Opinion in Food Science
(a). Tribo-rheometry accessory (Courtesy: TA Instruments) (b). A
Stribeck curve where the friction coefficient is plotted against the
combined parameters of the viscosity, entrainment speed and the
surface load.
Source: Reference [12
]
The tribological properties of suspensions of cooked
swollen starch granules are characterized by systems
based on maize starch and potato starch [16]. In a soft-
tribological contact, maize suspensions reduce friction
compared to the solvent (water), generate bell-shaped
tribological profiles characteristic of particle entrainment
and show marked concentration dependence, whereas
potato suspensions exhibit lubrication behavior similar
to water. Interplay between particle microstructure and
the resultant rheological and lubrication dynamics of
starch ghost suspensions contributes to an enhanced
mechanistic understanding of textural and other
www.sciencedirect.com
Advances in food rheology Ahmed 131
functional properties of cooked starches in food and other
applications.
Tribology was employed on the detection of melamine
from milk [17]. The frictional pairs consist of a nitrile-
butadiene rubber ball and a silicone rubber substrate.
The friction coefficients of both casein and melamine
solution increased sharply with increasing the sliding
speed from 0.2 to 2 mm/s, then remained almost constant
at the speed of 2–8 mm/s, and fluctuate in the higher
speed (8–20 mm/s). The m of the milk adulterated by
melamine was much larger than that of the original
solution, and the difference is two to three orders of
higher than the resolution of the measurement instru-
ment, which can be used to detect melamine from the
milk.
Conclusions
Rheological advances have revolutionized the concept of
food product development by including the sensory anal-
Rheology ysis components in the measurement. Knowledge of the
dominated dynamics of food systems at larger deformations (LAOS)
is vital about typical processing operations, and provides
Hydrodynamic
the real-time structure during processing.
Regime
Funding
This research did not receive any grant from funding
agencies in the public, commercial, or not-for-profit
agencies.
Conflict of interest statement
Nothing declared.
References and recommended reading
Papers of particular interest, published within the period of review,
have been highlighted as:

of special interest


of outstanding interest
1. Ahmed J, Ptaszek P, Basu S: Food rheology: scientific


development and importance to food industry. In Advances in
Food Rheology. Edited by Ahmed J, Ptaszek P, Basu S. Elsevier;
2016:1-4.
This book covers recent development in rheological measurements for
food products, in particular, SAOS, LAOS, FTRheology, extensional
rheology, Time-temperature-superposition principles. Experts from the
field contributed to their vast experiences, and it helps interested
researchers or professionals to understand and find the equipment/type
of measurement they are looking for their work.
2. Ahmed J, Al-Ruwaih N, Mulla M, Rahman MH: Effect of high
pressure treatment on functional, rheological and structural
properties of kidney bean protein isolate. LWT — Food Sci
Technol 2018. In press.
3. Keentok M, Tanner RI: Cone-plate and parallel plate rheometry
of some polymer solutions. J Rheol 1982, 26:301-311.
4. Djalili-Moghaddam M, Ebrahimzadeh R, Toll S: Study of
geometry effects in torsional rheometry of fibre suspensions.
Rheol Acta 2004, 44:29-37.
5. Song HY, Salehiyan R, Li X, Lee Seung Hak, Hyun Kyu: A
comparative study of the effects of cone-plate and parallel-
plate geometries on rheological properties under oscillatory
shear flow. Korea-Aust Rheol J 2017, 29:281-294.
Current Opinion in Food Science 2018, 23:127–132
132 Food engineering & processing
6. Daniel Szopinski, Luinstra Gerrit A: Viscoelastic properties of
aqueous guar gum derivative solutions under large amplitude
oscillatory shear (LAOS). Carbohyd Polym 2016, 153:312-319.
7. Hyun K, Kim W: A new non-linear parameter Q from FT-
Rheology under nonlinear dynamic oscillatory shear for
polymer melts system. Korea-Aust Rheol J 2011, 23:227-235.
8. Reinheimer K, Grosso M, Wilhelm M: Fourier Transform
Rheology as a universal non-linear mechanical
characterization of droplet size and interfacial tension of
dilute monodisperse emulsions. J Coll Interf Sci 2011, 360:818-
825.
9. Yazar G, Duvarci O, Tavman S, Kokini JL: Effect of mixing on

LAOS properties of hard wheat flour dough. J Food Eng 2016,
190:195-204.
This research paper is focused on LAOS of wheat flour dough. It provides
an insight of the dough structure during mixing and new insights into the
non-linear rheological behavior of wheat flour doughs such as the intra-
cycle behavior of dough in both linear and non-linear region.
10. Yazar G, Duvarci O, Tavman S, Kokini JL: LAOS behavior of the
two main gluten fractions: gliadin and glutenin. J Cereal Sci
2017, 77:201-210.
11. Almusallam AS, Ahmed J, Nahar S, Chacko S: Oscillatory
shearing behavior of rocket leaves powder incorporated
dough. Korea-Aust Rheo J 2016, 28:149-158.
12. Prakash S, Tan DDY, Chen J: Applications of tribology in

studying food oral processing and texture perception. Food
Res Int 2013, 54:1627-1635.
Current Opinion in Food Science 2018, 23:127–132
This review paper provides information on tribology and its relationship to
the oral processing of food. Additionally, it provides information on
selected tribological systems employed for various food systems. The
operation principles, advantages, and disadvantages of tribometers have
been discussed.
13. Selway N, Stokes JR: Insights into the dynamics of oral

lubrication and mouthfeel using soft tribology: Differentiating
semi-fluid foods with similar rheology. Food Res Int 2013,
54:423-431.
This research paper describes some commercial soft-food systems,
which were characterized by rheology and tribology to gain insight into
the physical origins of mouthfeel and the dynamics of oral lubrication.
Challenges associated with the application of tribology have been
elaborated.
14. Dresselhuis DM, Hoog EHAD, Stuart MAC, Aken GAV: Application
of oral tissue in tribological measurements in an emulsion
perception context. Food Hydrocoll 2008, 22:323-335.
15. Nguyen PTM, Bhandari B, Prakash S: Tribological method to
measure lubricating properties of dairy products. J Food Eng
2016, 168:27-34.
16. Zhang B, Selway N, Shelat KJ, Dhital S, Stokes JR, Gidley MJ:
Tribology of swollen starch granule suspensions from maize
and potato. Carbohyd Polym 2017, 155:128-135.
17. Liu Y, Hu J, Zhong M, Xu W: A novel, simple and rapid method
for the detection of melamine from milk based on tribology
measurements. Tribology Int 2018, 119:66-72.
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