Food Hydrocolloids 33 (2013) 142e150

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Food Hydrocolloids
journal homepage: www.elsevier.com/locate/foodhyd

Rheological characterisation of selected food hydrocolloids by

traditional and simplified techniques
Chiara Cevoli a, *, Federica Balestra b, Luigi Ragni a, Angelo Fabbri a
a
Agricultural Economics and Engineering Department, University of Bologna, Piazza G. Goidanich 60, 47521 Cesena (FC), Italy
b
CIRI-Interdepartamental Centre of Agri-Food Industrial Research, University of Bologna, Piazza G. Goidanich 60, 47521 Cesena (FC), Italy

a r t i c l e i n f o a b s t r a c t

Article history: Empirical and fundamental rheological properties of six food hydrocolloids (carboxymethylcellulose, tara
Received 10 September 2012 gum, guar gum, locust bean gum, xanthan gum and sodium alginate), as influenced by concentration,
Accepted 28 February 2013 were evaluated and correlated. Furthermore, the possibility to estimate the empirical and fundamental
parameters by using data coming from a very simple and inexpensive rotational viscometer prototype,
Keywords: was investigated. The prototype was build in laboratory and its simplicity consist of the capability to
Rheological properties
directly measure a voltage, correlated with the absorbed current, instead of a derived torque and rotation
Prototype
speed measurements of the cylinder probe. Fundamental rheological measurements were performed by
Hydrocolloids
Viscosity
using a controlled stress-strain rheometer, while a back extrusion test was performed in order to eval-
uate the empirical properties.
The results reported that all the measured parameters are strongly correlated with the dispersion
concentration. The simple prototype was able to predict the empirical parameters with R2 value from
0.976 to 0.999 by means of exponential, linear, or power law functions and to assess the viscosity from
power law or linear functions with R2 close to 1 for shear rate higher than 50 s
1.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction
Hydrocolloids are a heterogeneous group of long chain poly-
mers (polysaccharides and proteins) characterised by the property
of forming viscous dispersions and/or gels when dispersed in water
(Saha & Bhattacharya, 2010). Food gums/hydrocolloids are often the
determinants of texture and/or viscosity, other quality attributes
and stability of food system even when naturally occurring and not
added as ingredients (BeMiller, 2006).
Their behaviour helps to modify the food sensory properties,
and hence, hydrocolloids are used as important food additives to
perform specific purposes (Saha & Bhattacharya, 2010). These
functional ingredients are widely used in dairy and bakery prod-
ucts, canned foods, salad dressings, beverages, sauces, soups and
other processed foodstuffs to improve textural characteristics,
flavour and shelf life (Sahin & Ozdemir, 2004).
Hydrocolloids have a wide array of functional properties in
foods. These include thickening, gelling, emulsifying, stabilisation
and controlling of the crystal growth of ice and sugar. Hydrocolloids
commonly used as thickening are: starch, xanthan, guar, locust
* Corresponding author. Fax: þ39 0547 382348.
E-mail address: chiara.cevoli3@unibo.it (C. Cevoli).
bean, karaya, tragacanth, Arabic gum and cellulose derivatives. The
gelling type hydrocolloids are: alginate, pectin, carrageenan, gela-
tine, gellan and agar. As thickening agents, they find uses in soups,
gravies, salad dressings, sauces and toppings while, as gelling
agents, they are extensively used in products like jam, jelly,
marmalade, restructured foods and low sugar/calorie gels (Saha &
Bhattacharya, 2010).
Characterisation of gels is an essential task in the study of
thickened dispersions and gels formed by various hydrocolloid
gelling agents. Characterisation may involve rheological, structural,
microscopic and molecular aspects. Among these, rheological
characterisation of sample is the most important and generally
performed practice since it correlates to the textural attributes of
the product, which, in turn, determines its sensory characteristics
and consumer acceptability (Saha & Bhattacharya, 2010). Industries
producing and using hydrocolloids generally need an estimate of
apparent viscosity of a product at specified concentrations and at
specified shear rates (Mathur, 2011).
Moreover it is also well recognized that rheological properties
play a role in process design, evaluation and modelling. In fact
rheological data are required as an indicator of product quality,
for calculation in any process involving fluid flow (e.g. pump sizing,
extraction, filtration, extrusion, purification) and for the analyses
of flow conditions in food processes such as pasteurization,

0268-005X/$ e see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.foodhyd.2013.02.022
 C. Cevoli et al. / Food Hydrocolloids 33 (2013) 142e150 143

evaporation, drying and aseptic processing. The concentration and then were put at 5  C for 24 h before performing the analyses.
the temperature have an important influence on the flow behav- Hydrocolloids dispersions of varying concentrations were prepared
iour of hydrocolloid solutions (Marcotte, Taherian Hoshahili, & in duplicate. The characteristics of the dispersion preparation were
Ramaswamy, 2001). reported in Table 1.
Considering their role in the adjustment of viscosity and texture
of food formulations, the rheological behaviour of food products 2.2. Empirical properties evaluated by texture analyser
involving different hydrocolloids, either singly or in combination,
has been studied extensively using fundamental rheological mea- Textural characteristics were evaluated by using a Texture
surements (Casas, Mohedano, & Garcia-Ochoa, 2000; Doublier & Analyser (TA.HDi 500, Stable Micro Systems, Vienna Court, U.K.)
Cuvelier, 2006; Dunstan et al., 2001; Rodriguez-Hernandez & equipped with a 5 kgf load cell.
Tecante, 1999; Saha & Bhattacharya, 2010). The effect of concen- Back extrusion test was performed in order to evaluate the
tration and temperature were widely investigated by using a viscoelastic properties of the dispersions. Tests were carried out in
rotational viscometer (Gómez-Díaz & Navaza, 2003; Marcotte et al., a purpose-built back extrusion measuring system made up with an
2001; Mothe & Rao, 1999; Pilizota, Subarie, & Lovrie, 1996; Sopade extrusion disc (33 mm diameter) that was positioned centrally over
& Kiaka, 2001). the sample container (37 mm diameter). During the test, the disc
However, during processing, manufacture and consumption of proceeds into the sample (30 ml) to penetrate to a depth of 40% at
foods, these systems are subjected to large deformations. Hence, 1 mm/s test speed. At this point (most likely to be the maximum
rheological measurement of thickened dispersion/gel has been force), the probe returns to its original position. The ‘peak’ or
broadly categorized into small deformation and large deformation maximum force is taken as a measurement of firmness (N). The area
testing (Saha & Bhattacharya, 2010). To our knowledge information under the curve up to this point is taken as an indication of con-
regarding relationship between dynamic (rheometry) and static sistency (Ns). The negative region of the graph, drawn on probe
(texture) measurements on thickening and gelling agents is scanty return, is the result of the weight of sample which is lifted primarily
(Angioloni & Collar, 2009). on the upper surface of the disc on return, i.e. due to back extrusion
In this work empirical and fundamental rheological properties and hence gives an indication of the viscosity (Ns) (resistance to
of selected food hydrocolloids, as influenced by concentration, were flow off the disc). The maximum negative force is taken as an
evaluated and correlated. These measurements were carried out by indication of the cohesiveness (N) of the sample (Ciron, Gee, Kelly,
using a texture analyser (empirical properties) and a rheometer & Auty, 2010). An example of back extrusion curve was reported in
(fundamental properties). The main purpose of this research was Fig. 1. The measurements were carried out at room temperature
however to assess the possibility to estimate the empirical and
fundamental parameters by using data coming from a very simple Table 1
rotational viscometer prototype, build up in our laboratory. From an Characteristics of the hydrocolloidal water dispersion preparation.
industrial point of view the rheological models so obtained could Hydrocolloid Concentration Temperature Time
be useful to determine fundamental and empirical rheological (%, m/v) ( C) (min)
properties that usually need complex, expensive and time Sodium alginate 1 25 75
consuming instrumentation that is difficult to maintain in an in- 1.5 25 90
dustrial environment and that requires high levels of technical 2 25 165
skills to be performed. 2.5 25 180
Carboxymethylcellulose 2 25 75
2.5 25 130
2. Materials and methods 3 25 130
3.5 25 210
2.1. Sample preparation Guar gum 0.5 25 120
1 25 120
1.5 25 300
Six different hydrocolloids purchased from a local confectionary 2 25 300
company were analysed. In particular, five hydrocolloids commonly Locust bean gum 0.5 25 70
used as thickening, such as carboxymethylcellulose (CMC), tara 86e89 10
gum (TG), guar gum (GG), locust bean gum (LBG), xanthan gum 1 25 80
86e89 10
(XG) and one gelling hydrocolloid, the sodium alginate (AS), were 1.5 25 90
used. 86e89 10
Hydrocolloids were dispersed in 300 ml of distilled water and 2 25 100
mixed by a magnetic stirrer (ARE heating magnetic stirrer, VELP 86e89 10
Tara gum 0.5 25 60
Scientifica, Italy) following a combination of temperature and time
80 30
specific for each hydrocolloids. The concentrations (Dressler, 1 25 60
Fischer, & Windhab, 2003; Marcotte et al., 2001; Mathur, 2011; 80 30
Muller & Davidson, 1994; Ramsden, 2004; Sabra & Deckwer, 2005; 1.5 25 60
Wielinga, 2009), time and temperature (García-Ochoa, Santos, 80 30
2 25 60
Casas, & Gómez, 2000; Marcotte et al., 2001; Sittikijyothin, 80 30
Sampaio, Gonçalves, 2007, 2010; Sittikijyothin, Torres, & Xanthan gum 1 25 60
Gonçalves, 2005) of different dispersions were chosen on the ba- 80 8
sis of the literature and on the basis of previous trials performed in 2 25 60
80 8
our laboratory. Since LBG, TG and XG are partially soluble in cool
3 25 60
water, were treated, for a long time, at room temperature (25  C) 80 8
and then were heated at 80e89  C, for a short time, to make easy 4 25 60
the total dispersion. 80 8
Dispersions were centrifuged (PK 110, ALC International s.r.l, Note: mass of added hydrocolloid, preparation temperature and time necessary to
Italy) for 10 min at 3800 rpm to remove entrapped air bubbles and obtain the dispersion were reported in the same line.
144
1.5
Firmness
Consistency index
0.5
Force (N)
0 5 10
-0.5
Viscosity index
-1.5 Cohesiveness
Fig. 1. Typical back extrusion curve.
(25  C). The analyses were performed in triplicate for each
dispersion prepared, six replicates in all.
2.3. Fundamental properties evaluated by rheometer
Fundamental rheological measurements were performed by
using a controlled stress-strain rheometer (MCR 300, manufactured
by Physica/Anton Paar; Ostfildern, Germany) in a system of coaxial
cylinders (CC27). The instrument measures the shear stress (Pa)
and the apparent viscosity (Pa s) at the vary of the shear rate (s
1).
Twenty ml of sample were loaded into the sample cup and
allowed to equilibrate for 3 min in order to achieve temperature
equilibrium (25  C) and stress relaxation.
The sample were subjected to a programmed shear rate loga-
rithmically increasing from 0 to 300 s
1 in 3 min. A flow curve is a
graphical representation of the behaviour of flowing materials
whereby a sample is subjected to ascending or descending shear
rates, with the corresponding shear stress and viscosity calculated
from instrument parameters. The analyses were performed in
triplicate for each dispersion realized, six replicates in all.
2.4. Measurements by a viscometer prototype
In rotational viscometers the torque required to turn an object in
a fluid is a function of the viscosity of that fluid. These instruments
Fig. 2. Prototype components: 1- DC motor connected to a shaft that terminates with a cylinder, 2- electric circuit, 3-multimeter and 4-power supply.
C. Cevoli et al. / Food Hydrocolloids 33 (2013) 142e150
measure the torque required to rotate a disc or bob of a certain
dimensions in a fluid at a known speed.
The rotational viscometers can be roughly grouped in the
following versions (Doebelin, 2010; McKenna & Lyng, 2003; Steffe,
1996): concentric cylinders; plate-and-plate, cone-and-plate.
Depending on which element rotates and which remains station-
ary, the cylinder viscometers can be grouped into two classes,
named Couette and Searle. In the first kind the outer cylinder ro-
tates and the inner cylinder is stationary, and vice versa in the
15 20
second one (our device falls into the latter). In the Couette
Time (s) viscometer the inner cylinder is suspended thought a radial arm by
a torsion wire or a spring and the torque is measured as angular
deflection by a linear variable differential transformer (LVDT) or by
an optical device. In the Searle type the torque is derived from a
current measurement of the motor that (where this last) is equip-
ped with air bearings to reduce the friction. Encoders are often used
to measure the rotational speed, that can be maintained constant at
a prefixed value. A control system of the fluid under test temper-
ature completes the viscometer.
The prototype (Fig. 2) built in our laboratory is made up of:
1 a miniature DC motor connected to a shaft that terminates with
a cylinder made of aluminium with diameter of 15 mm and
height of 11 mm;
2 an electric circuit able to measure the variation of the electrical
current that crosses the motor. This variation depend on the
torque generated by the friction between the sample material
and the rotational cylinder. The electrical current measured as
voltage is determined at the extremity of resistance connected
in series with the motors. This voltage is conveniently ampli-
fied by an operational amplifier. The higher the viscosity of the
sample, the higher the current absorbed by the motor and,
consequently, the voltage at the amplifier output (an essential
schematic of the electrical circuit is shown in Fig. 3);
3 a commercial multimeter which allows to visualize the voltage
(V) at the output of the electric circuit;
4 a power supply (from 3 to 12 V) that allows to modify the probe
rotation velocity inside the sample (in the present experience a
voltage of 5 V was selected).
The probe rotates inside 30 ml of sample in a commercial Becker
made of glass with diameter of 40 mm and height of 60 mm, and
after 20 s the voltage was evaluated. The analyses were performed
in triplicate for each dispersion realized, for a total of six replicates
and at room temperature (25  C). The peculiarity of this prototype
 C. Cevoli et al. / Food Hydrocolloids 33 (2013) 142e150 145

Fuse Regression models between voltage value obtained by proto-

type (independent variable, x) and back extrusion parameters
(dependent variable, y) were evaluated. Moreover models between
voltage value or back extrusion parameters (independent variable,
Motor x) and viscosity at 50 s
1 (dependent variable, y) were explored.
Offset The shear rate of 50 s
1 was selected according to Morris (1983)
+ adjustement +
Power -
and Marcotte et al. (2001). The linear (eq (1)), power (eq (2)) and
supply - + exponential (eq (3)) models were explored. The viscosity was
defined by the following equation:
Signal
output s
m ¼ (4)
g_
Fig. 3. Schematic representation of the main electrical circuit. where s is the shear stress (Pa) andg_ is the shear rate (1/s).
For each concentration, the flow curves were evaluated using
is the ability to measure a voltage instead of torque and rotation the Ostwaldede Waele (eq (5)) and the Herschel-Bulkley (eq (6))
speed of the cylinder probe. rheological models (Steffe, 1996):
It has also to be pointed out that the fluid viscosity modifies the
rotational speed of the cylinder. For simplicity neither a kind of s ¼ kg_ n (5)
control to maintain the speed constant nor a speed measuring
system were provided for this apparatus. s ¼ s0 þ kg_ n (6)

2.5. Data analyses
For the back extrusion parameters a correlation matrix was
performed to detect a possible linear correlation.
The effect of hydrocolloid concentration (x) on the back extru-
sion parameters (y) and on voltage values obtained by prototype
(y), was examined using three models: linear model (eq (1)), power
model (eq (2)) and exponential model (eq (3)).
y ¼ a þ bx
where s0 is the yield stress, k the consistency coefficient (Pasn) and
n the flow behaviour index. The models with and without the
extrapolation of the yield stress from the experimental data were
calculated. The analysis was performed considering all the repli-
cates. For each hydrocolloid, the combined effect of the concen-
tration and shear rate on the shear stress was evaluated.
All the elaborations were performed with a confidence level
limit of 95%.
The data analyses were carried out by using Statistica 7.0
(1) (StatSoft Inc., Tulsa, USA).

y ¼ axb (2) 3. Results

3.1. Empirical properties evaluated by texture analyser

y ¼ aexpb (3)
Each model was evaluated for all hydrocolloids using the raw Using Pearson correlation analysis, a range of correlation co-
data of all six replicates and not the averaged ones. efficients (r) (from 0.98 to 1) was obtained for the relationships

Table 2
Mean and standard deviation values of the empirical parameters obtained by back extrusion and of the voltage by the prototype.

Hydrocolloid Concentration Back extrusion Prototype

(%)
Firmness (N) Consistency (Ns) Viscosity index (Ns) Cohesiveness (N) Voltage (mV)
Sodium alginate 1 0.094 0.008 0.766 0.054 0.310 0.033 0.122 0.002 113.0 1.1
1.5 0.155 0.011 1.358 0.018 0.586 0.043 0.271 0.033 348.8 54.6
2 0.273 0.053 2.630 0.279 1.036 0.062 0.600 0.124 778.3 36.3
2.5 0.460 0.032 4.186 0.295 1.476 0.073 1.077 0.074 1127.2 14.8
Carboxymethylcellulose 2 0.126 0.008 0.960 0.077 0.406 0.038 0.183 0.024 226.3 12.7
2.5 0.178 0.011 1.494 0.081 0.624 0.017 0.311 0.020 433.2 69.7
3 0.253 0.022 2.237 0.141 0.879 0.041 0.501 0.047 638.0 50.0
3.5 0.346 0.003 3.126 0.035 1.147 0.010 0.729 0.021 924.7 46.8
Guar gum 0.5 0.091 0.005 0.788 0.110 0.199 0.001 0.101 0.005 32.8 2.8
1 0.261 0.022 2.511 0.009 0.704 0.003 0.344 0.034 146.2 21.6
1.5 0.755 0.151 8.464 0.585 1.761 0.126 1.126 0.254 472.3 81.7
2 1.147 0.047 13.487 0.105 2.717 0.056 1.848 0.154 704.5 26.1
Locust bean gum 0.5 0.085 0.003 0.793 0.001 0.278 0.023 0.118 0.000 63.7 9.4
1 0.224 0.020 2.050 0.280 0.762 0.082 0.374 0.038 313.3 49.7
1.5 0.685 0.106 7.215 0.957 1.937 0.161 1.295 0.182 799.8 50.8
2 1.482 0.197 16.790 0.765 3.930 0.175 2.839 0.415 1372.5 81.0
Tara gum 0.5 0.097 0.021 0.864 0.030 0.316 0.070 0.125 0.036 59.7 17.0
1 0.304 0.012 2.933 0.012 0.906 0.026 0.487 0.015 291.7 13.4
1.5 0.883 0.042 8.413 0.965 2.022 0.216 1.399 0.081 744.3 42.0
2 2.195 0.166 21.394 0.988 4.587 0.406 3.159 0.033 1285.8 73.3
Xanthan gum 1 0.281 0.029 2.683 0.447 0.601 0.110 0.289 0.045 136.7 12.1
2 0.611 0.008 6.009 0.504 1.187 0.098 0.651 0.002 301.9 21.0
3 1.159 0.023 11.625 0.979 2.297 0.016 1.298 0.012 541.7 19.4
4 1.816 0.180 18.567 1.041 3.338 0.230 1.849 0.087 798.3 39.2
146 C. Cevoli et al. / Food Hydrocolloids 33 (2013) 142e150

Table 3
Results of the correlations between concentration and back extrusion parameters.

Hydrocolloid Back extrusion

Function parameters Firmness Consistency Viscosity index Cohesiveness

Sodium alginate Power law a 0.07 0.64 0.30 0.10
b 1.99 2.04 1.73 2.57
R2 0.966 0.969 0.974 0.979
Carboxymethylcellulose Power law a 0.03 0.21 0.12 0.03
b 1.87 2.14 1.82 2.48
R2 0.974 0.971 0.977 0.982
Guar gum Power law a 0.03 3.32 0.75 0.44
b 7.86 2.05 1.76 2.06
R2 0.967 0.976 0.980 0.964
Locust bean gum Power law a 0.22 2.07 0.74 0.38
b 2.88 3.06 2.43 3.05
R2 0.982 0.984 0.978 0.988
Tara gum Exponential a 0.00 0.41 0.17 0.09
b 1.61 1.94 2.00 1.61
R2 0.977 0.993 0.992 0.977
Xanthan gum Power law a 0.22 2.03 0.48 0.26
b 1.55 1.59 1.40 1.44
R2 0.978 0.973 0.966 0.988

between the back extrusion parameters (firmness, consistency,
viscosity index and cohesiveness). The linear correlation between
these parameters is confirmed by the high values of r.
In Table 2 the means and standard deviations of the parameters
obtained on dispersions by back-extrusion for all the used hydro-
colloids are reported. The highest values were obtained for the tara
gum (2%) for all the considered parameters. The results of the re-
gression between the parameters of the back extrusion and the
dispersion concentration are reported in Table 3, in terms of deter-
mination coefficient and model parameters values (a and b). For all
the hydrocolloids, except for tara gum, power law functions well
describe the relationship between back extrusion parameters and
concentration. For the tara gum an exponential correlation was ob-
tained. The determination coefficients (R2) range from 0.966 to 0.993.
3.2. Fundamental properties evaluated by rheometer
The parameters obtained from the Ostwaldede Waele and the
Herschel-Bulkely models, are summarized in Table 4. The Herschel-
Bulkely model parameters were evaluated with and without the
extrapolation of the yield stress values from the experimental data.
For all hydrocolloids, an increase in the concentration causes an
increase in the pseudoplasticity showing a decrease in the flow
behaviour index (n). As expected, the consistency coefficient (k)
increased with the concentration (Gómez-Díaz & Navaza, 2003;
Marcotte et al., 2001; Wu, Cui, Eskin, & Goff, 2009).
The Ostwaldede Waele is the best model, in terms of R2, for all
the hydrocolloids, except for the XG that exhibits a Herschel-Bulkely
behaviour. The XG data were not elaborated by the Ostwaldede

Table 4
The Ostwald-de Waele and HerscheleBulkley parameters and the coefficient of determination of the models for the different hydrocolloid at different concentrations.

Hydrocolloid Concentration (%) Ostwaldede Waele HerscheleBulkley

With extrapolated yield stress Without extrapolated yield stress

R2 k (Pasn) n s0 (Pa) R2 k (Pasn) n s0 (Pa) R2 k (Pasn) n

Sodium alginate 1 0.997 0.66 0.71 0.03 0.997 0.65 0.71
0.56 0.998 0.80 0.68
1.5 0.990 2.51 0.62 0.11 0.990 2.47 0.62
2.23 0.993 3.36 0.57
2 0.986 7.08 0.56 0.30 0.985 6.96 0.56
6.76 0.990 10.42 0.49
2.5 0.989 14.20 0.51 0.63 0.988 13.89 0.52
14.70 0.995 22.66 0.44
Carboxymethylcellulose 2 0.998 1.20 0.67 0.08 0.998 1.18 0.67
0.68 0.998 1.41 0.64
2.5 0.978 2.88 0.61 0.21 0.978 2.80 0.62
1.41 0.979 3.43 0.58
3 0.996 4.87 0.58 0.38 0.995 4.72 0.59
2.32 0.997 5.90 0.55
3.5 0.997 8.73 0.55 0.76 0.996 8.39 0.55
3.91 0.998 10.68 0.51
Guar gum 0.5 0.991 1.06 0.47 0.05 0.989 1.03 0.47
0.91 0.996 1.66 0.39
1 0.974 10.38 0.31 1.23 0.969 9.39 0.32
18.15 0.993 27.41 0.18
1.5 0.917 43.99 0.22 6.39 0.935 36.80 0.24
922.67 0.967 965.65 0.02
2 0.921 66.86 0.19 11.97 0.938 55.77 0.21
2171.00 0.988 2236.71 0.01
Locust bean gum 0.5 0.968 0.54 0.64 0.02 0.968 0.53 0.64
0.53 0.971 0.75 0.59
1 0.974 6.16 0.45 0.29 0.973 6.45 0.45
8.67 0.986 12.84 0.34
1.5 0.958 26.71 0.36 1.63 0.955 25.54 0.36
56.21 0.986 76.50 0.21
2 0.938 63.05 0.30 4.93 0.933 59.20 0.31
237.27 0.982 290.33 0.12
Tara gum 0.5 0.952 1.70 0.41 0.06 0.951 1.70 0.50
0.58 0.997 0.94 0.51
1 0.938 63.65 0.30 0.71 0.937 9.14 0.30
14.54 0.995 21.97 0.25
1.5 0.940 34.02 0.30 3.48 0.935 31.23 0.31
103.21 0.974 132.87 0.13
2 0.911 74.06 0.25 9.21 0.904 66.17 0.27
728.10 0.966 797.89 0.04
Xanthan gum 1 6.73 0.979 2.83 0.32 6.90 0.979 2.68 0.33
2 14.47 0.973 6.04 0.31 12.67 0.973 7.66 0.27
3 19.83 0.912 16.16 0.23
8.65 0.925 44.36 0.11
4 24.65 0.916 29.81 0.21
151.19 0.946 205.53 0.05
 C. Cevoli et al. / Food Hydrocolloids 33 (2013) 142e150 147

Waele because of a too high yield stress. This is in agreement with
Marcotte et al. (2001) and Szczesniak (1985) who indicated that the
presence of a yield stress followed by a shear-thinning is a typical
behaviour of XG. This phenomenon could be due to the intermo-
lecular association of the acetate residue.
The determination coefficients of the rheological models ob-
tained without the extrapolation of the yield stress are higher
compared to the extrapolated ones. The R2 value range from 0.912
to 0.998. The lowest determination coefficients were obtained for
XG at high concentrations.
3.3. Measurements by viscometer prototype
The mean values and standard deviation of the voltage obtained
(mV) for the different hydrocolloids and concentrations are re-
ported in Table 2. The sample LGB (2%) showed the highest value of
voltage (1372.5 mV), while GG (0.5%) had the lowest one
(32.8 mV).
Considering the same concentration range (0.5e2%: GG, LBG, TG
and 1e2.5%: SA, XG), the sodium alginate and the locust bean gum
showed the highest value of voltage.

Sodium Alginate Carboxymethylcellulose

1400 1000
0.99
1.69 y = 221.88x
y = 112.45x 2
1200 R = 0.996
2
R = 0.997 800
1000
600

Voltage (mV)
Voltage (mV)

800

600 400
400
200
200

0 0
1.0 1.5 2.0 2.5 2.0 2.5 3.0 3.5
Concentration (%, m/v) Concentration (%, m/v)

Guar gum Locust bean gum

1000 2.28
1600
2.24
y = 32.62x y = 65.06x
2 1400 2
800 R = 0.993 R = 0.999
1200

600 1000
Voltage (mV)

Voltage (mV)

800
400 600
400
200
200
0 0
0.5 1.0 1.5 2.0 0.5 1.0 1.5 2.0
Concentration (%, m/v) Concentration (%, m/v)

Tara gum Xanthan gum

1600 1000
2.23 1.27
y = 60.82x y = 132.66x
1400 2 2
R = 0.999 800 R = 0.997
1200
1000 600
Voltage (mV)
Voltage (mV)

800
600 400

400
200
200
0 0
0.5 1.0 1.5 2.0 1.0 2.0 3.0 4.0
Concentration (%, m/v) Concentration (%, m/v)

Fig. 4. Correlation models between concentration and voltage values obtained by prototype.
148 C. Cevoli et al. / Food Hydrocolloids 33 (2013) 142e150

Table 5
Results of the regressions between back extrusion parameters (dependent variable) and voltage by the prototype (independent variable).

Hydrocolloid Back extrusion

Function parameters Firmness Consistency Viscosity index Cohesiveness

Sodium alginate Exponetial a 0.087 0.780 0.351 0.137
b 0.002 0.002 0.001 0.002
R2 0.998 0.994 0.978 0.994
Carboxymethylcellulose Linear a 0.001 0.003 0.001 0.001
b 0.047 0.203 0.167
0.011
R2 0.996 0.997 0.997 0.996
Guar gum Linear a 0.002 0.019 0.004 0.003
b 0.033
0.092 0.107
0.020
R2 0.999 0.997 0.997 0.995
Locust bean gum Linear a 0.001 0.012 0.003 0.002
b
0.062
1.182
0.055
0.186
R2 0.976 0.968 0.986 0.978
Tara gum Power law a 0.001 0.000 0.001 0.001
b 1.532 1.565 1.268 1.381
R2 0.995 0.994 0.985 0.997
Xanthan gum Linear a 0.002 0.024 0.004 0.002
b
0.068
0.981
0.012
0.043
R2 0.998 0.997 0.998 0.998

Carboxymethylcellulose
1.00 Sodium alginate 1.00

0.99
0.99
0.98

0.97 0.98
R2
2
R

0.96
0.97
0.95

0.96
0.94
0 50 100 150 200 250 300 0 50 100 150 200 250 300
shear rate (1/s) shear rate (1/s)

Guar gum Locust bean gum

1.00 1.00

0.97
0.97
0.94
0.94
0.91
R2

R2

0.91
0.88

0.85 0.88

0.82 0.85
0 50 100 150 200 250 300 0 50 100 150 200 250 300
shear rate (1/s) shear rate (1/s)

Tara gum 1.00 Xanthan gum

1.00

0.99
0.97

0.98
0.94
2
R2

0.91 0.97

0.88 0.96

0.85 0.95
0 50 100 150 200 250 300 0 50 100 150 200 250 300
shear rate (1/s) shear rate (1/s)

Linear Exponential Power law

Fig. 5. Trend of the determination coefficient for linear, exponential and power models between voltage obtained by the prototype and viscosity.
 C. Cevoli et al. / Food Hydrocolloids 33 (2013) 142e150 149

Table 6
Results of the regressions between viscosity at 50 s
1 (dependent variable) and back extrusion or prototype parameters (independent variable).

Hydrocolloid Back extrusion Prototype

Function Firmness Consistency Viscosity index Cohesiveness Function Voltage

parameters parameters
Sodium alginate Linear a 5323.51 566.31 1.67 2028.10 Power law a 1.89
b
254.01
211.81 367.32 4.23 b
64.66
R2 0.997 0.999 0.992 0.998 R2 0.985
Carboxymethylcellulose Linear a 4921.60 501.52 1466.01 1984.62 Linear a 1.58
b
288.38
157.55
297.19
32.70 b
57.35
R2 0.996 0.995 0.987 0.995 R2 0.996
Guar gum Linear a 2485.10 180.57 935.83 1320.10 Linear a 3.42
b
30.60 61.01
58.05 72.75 b 40.66
R2 0.998 0.995 0.999 0.994 R2 0.998
Locust bean gum Linear a 2864.21 247.27 1112.31 1466.52 Linear a 3.12
b 69.96 182.94
77.64 146.46 b
151.54
R2 0.992 0.986 0.997 0.993 R2 0.996
Tara gum Linear a 2198.72 268.42 845.78 1508.41 Power law a 3.89
b 0.95 0.93 1.12 0.92 b 0.96
R2 0.981 0.984 0.985 0.995 R2 0.998
Xanthan gum Power law a 0.91 127.37 485.53 863.24 Power law a 2.96
b 0.89 0.85 0.15 0.87 b 0.93
R2 0.994 0.994 0.988 0.985 R2 0.991

The ratio between the lowest to the highest concentration was
8.97, 3.07, 20.48, 20.54, 20.53 and 48.4 for the SA, CMC, GG, LGB, TG
and XG, respectively.
The behaviour of the samples characterized by the 0.5e2%
concentration range (GG, LBG and TG) was very similar, the voltage
raised of 4.75  0.21, 2.78  0.32 and 1.64  0.11 times, passing
from 0.5 to 1%, from 1 to 1.5% and from 1.5 to 2%, respectively. Even
for SA and XG (concentration from 1 to 2.5%) the voltage increase
was similar: 2.65  0.44, 2.01  0.22 and 1.46  0.2 times, passing
from 1 to 1.5%, from 1.5 to 2% and from 2 to 2.5%, respectively.
The correlation models between concentration and voltage are
reported in Fig. 4. For all the hydrocolloids, power law functions
well describe the relation between the voltage and the concen-
tration. The determination coefficient ranges from 0.993 to 0.999.
CMC and TG showed the highest R2 value.
3.4. Relationships between fundamental and empirical data
The regression model parameters (a and b) and the related
determination coefficients obtained from the regression between
the voltage values of the prototype (independent variable) and the
back extrusion parameters (dependent variable) are reported in
Table 5.
For all hydrocolloids, except for SA and TG, linear functions were
found. For SA and TG exponential and power law functions were
obtained, respectively. The determination coefficient ranges from
0.976 to 0.999.
For each hydrocolloid, all viscosity values obtained by the flow
curves were separately correlated with the voltage parameter in
order to determine at which shear-rate (from 0 to 300 s
1) there is
the best relation between the voltage and the viscosity. In Fig. 5 the
determination coefficient vs. the shear rate for linear, exponential
and power law regressions are shown. The worst trend of R2 is
related to exponential regression, while the determination co-
efficients of the linear and power law regression are similar and
high. Generally, after 50 s
1, the R2 values are constant and the
highest.
In Table 6 the results obtained from the regressions between the
voltage values of the prototype (independent variable) or the back
extrusion parameters (independent variable) and the viscosity
value at 50 s
1 (dependent variable) are reported. In particular the
regression model parameters (a and b) and the related determi-
nation coefficients are shown.
The hydrocolloids characterized by a linear correlation between
voltage value and back extrusion parameters (CMC, GG, LBG and
XG) showed the same regression model with the viscosity, for both
independent variables (voltage or back extrusion parameters).
Considering the back extrusion parameter as an independent var-
iable, a linear regression was observed, excepted for the XG (power
law). While for the voltage parameters, a linear regression was
reported for CMC, GG and LGB and a power law for the SA, TG and
XG. The determination coefficients are high and range from 0.986
to 0.999.
Therefore, it is possible to assess the rheological properties of a
sample using the developed prototype by means of the equations
reported in Table 6. These equations can be considered as the
calibration curve to determine the back extrusion parameters or
the viscosity using the voltage value obtained by prototype as a
starting points.
4. Conclusions
Both empirical and fundamental rheological properties of six
different hydrocolloidal water dispersions, at different concen-
tration, used in food preparation were evaluated. All the measured
parameters showed strong correlations with the dispersion con-
centration. Firmness, consistency, viscosity index and cohesive-
ness, measured by back extrusion, fit well with power or
exponential law showing an R2 ranging from 0.966 to 0.993. The
yield stress, the consistency coefficient and the n index from the
flow curves and the Ostwald-de-Waele and HerscheleBulkley
methods showed R2 model values from 0.911 to 0.998. The power
law model showed the highest determination coefficient for all
the hydrocolloids, except for the xanthan gum. The voltage data,
obtained by the rotational viscometer prototype, were highly
correlated with the concentration through a power law function
(R2 from 0.933 to 0.999). This simple prototype turned out to be
able to predict the empirical parameters with R2 value from 0.976
to 0.999 by means of exponential, linear, or power law functions,
depending on the hydrocolloid analysed. The prototype was also
able to assess the viscosity from power law or linear functions
with R2 often close to 1 for shear-rate >50 s
1 (from 0.985 to
0.998, at 50 s
1). Correlation between viscosity and empirical
parameters was characterized by R2 from 0.981 to 0.999. In
conclusion, the suggested prototype appeared an useful and
inexpensive tool to monitor concentration or texture attributes of
150 C. Cevoli et al. / Food Hydrocolloids 33 (2013) 142e150
food dispersions from direct measurement or through the pre-
diction of their rheological properties by means of calculated
equations.
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