DOI 10.
1515/polyeng-2012-0129      J Polym Eng 2013; 33(2): 141–148
Germán Ayala Valencia, Ana Cecilia Agudelo Henao* and Rubén Antonio Vargas Zapata
Effect of glycerol concentration and temperature
on the rheological properties of cassava starch
solutions
Abstract: Glycerol/starch (G/S) solutions were prepared at
different concentrations, with a weight ratio of G/S=0.0,
0.1, 0.2, 0.3, 0.4 and 0.5, and rheological properties were
analyzed at 30, 40, 50, 60 and 70°C. Power law dependency
of the apparent viscosity as a function of the shear rate is
the most appropriate model for describing the rheological
behavior of cassava starch solutions as a function of glyc-
erol concentrations. All solutions showed a pseudoplas-
tic behavior; the flow index (n) did not show significant
changes as a function of temperature and glycerol con-
centration. However, the apparent viscosity (μa) and the
consistency coefficient (K) did show strong variations with
temperature and glycerol content. The temperature varia-
tion of both μa and K were better fitted to an exponential
model type exp(Ea/RT), logμa(K) vs. 1000/T. The activa-
tion energy of the K data for the solution without glycerol
(G/S=0.0) was 13.64 KJ/mol, and it decreased with increas-
ing the content of glycerol in the solutions, becoming
6.14 KJ/mol for G/S=0.5. On the contrary, the activation
energy for the μa data increased when increasing the glyc-
erol concentration. The effect of glycerol concentration was
also modeled using polynomial and exponential fittings.
Keywords: cassava starch solutions; glycerol; rheological
properties; pseudoplastic; consistency coefficient.
*Corresponding author: Ana Cecilia Agudelo Henao, Facultad de
Ingeniería y Administración, Universidad Nacional de Colombia
sede Palmira, Colombia, AA 237, Palmira, Colombia,
e-mail: acagudeloh@unal.edu.co
Germán Ayala Valencia: Basic Sciences Department ZAB/FZEA,
University of São Paulo, Av. Duque de Caxias Norte 225, 13635-000,
Pirassununga, SP, Brazil
Rubén Antonio Vargas Zapata: Departamento de Física, Universidad
del Valle, AA 25360, Cali, Colombia
1 Introduction
Biopolymers as cellulose, starch, chitin, protein, peptide
and their derivatives are well known because of their wide
range of industrial applications. Starch is recognized as
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the biopolymer second-most abundant in nature, with
excellent physicochemical properties, in addition to being
biodegradable, non-toxic and produced at low cost, thus
allowing sustainable development in different industries
in which it is used as a raw material [1–3]. Native starch is
involved in different applications as adhesives, foams, fer-
mented products, pharmacology, papermaking, binders,
packaging and the textile industry. Fermented starch is
used mainly in the food industry [4–8].
Depending on the starch source, its granule has dif-
ferent sizes and shapes; it can be round, elliptical, oval
or lenticular. The starch granules are the result of the
interaction of amylose and amylopectin chains formed
by a single monomer (α-D-glucose). Amylose is the result
of successive binding of the α-D-glucose through α-1,4
links, and amylopectin has the same amylose binding
with ramifications caused by the binding of α-D-glucose
through α-1,6 links [9]. The starch solutions are obtained
by heating starch grains above its gelatinization tempera-
ture. Gelatinization is a thermal transition in which the
starch granules absorb water, generating an increase in
the solution’s viscosity [10]. The degree of gelatinization
depends on temperature and moisture content, and these
parameters in turn depend on the nature of the starch [11].
Rheological models, such as the Newton, Bingham,
power law and Herschel & Bulkley models, have been
proposed to explain the viscosity behavior in food fluids
and derivatives that involve biological systems [12–16].
The rheological properties of starch solutions are studied
in order to establish their use in engineering processes
and to establish quality standards of raw materials and
manufactured products, wherein the starch is used to
thicken liquid food, such as soup and sauces [17–21]. For
this, different studies have looked at the viscosity behav-
ior in starch solutions at different concentrations [22–24].
Also, the effect of plasticizers as sodium hydroxide, ethyl-
ene glycol, polyvinyl alcohol, carboxymethylcellulose and
other compounds has been studied with possible appli-
cations in the packaging industry [21, 25, 26]. Lovedeeep
Kaur et al. [27] studied the effect of glycerol monostearate
on the rheological behavior of corn and potato starches.
These studies have revealed that starch solutions have a
142      G.A. Valencia et al.: Effect of glycerol concentration and temperature on the rheological
non-Newtonian behavior in which the viscosity can be
represented by the power law [28]. The mixture of starch
with different additives can lead to improved physical
properties and in this way expand the possibilities of its
application in technology. Glycerol is an additive used
in the production of biodegradable packaging films and
it can generate other desirable properties in the hybrid
materials [29, 30]. Recently, we reported a new potential
application of cassava starch films plasticized with glyc-
erol as a polymeric solid electrolyte, opening new applica-
tion of great interest in electrochemistry in the solid state
[31, 32]. However, the effect of combining glycerol and
cassava starch solutions is unknown. The present study
is concerned with the effect of glycerol concentration and
temperature on the rheological properties of cassava starch
solutions, which are precursors of biodegradable films.
2 Materials and methods
2.1 Raw material
Cassava starch HMC-1 (with age at harvest of 10 months)
was provided by the International Center for Tropical
Agriculture (CIAT, Palmira, Colombia), and commercial
grade glycerol (99%) was purchased from TC Química
(Cali, Colombia). All raw materials were used as received.
2.2 Proximate analysis of cassava starch
Humidity, ash and crude fat were analyzed using the
AOAC methods [33–35], crude protein was examined using
the Kjeldahl method [36], and crude fiber was determined
by means of the Van Soest method [37]. Total carbohydrate
content was calculated by weight difference. These deter-
minations were performed at least twice.
2.3 Preparation of glycerol/starch solutions
Glycerol/starch solutions at various concentrations were
prepared using a solution casting method reported by
Famá et al. [7], Cholwasa et al. [38], and Kechichian et al.
[39], which was slightly modified. Three grams of cassava
starch were gelatinized in 100 ml of water at 70 ± 1°C for
15 min under a constant agitation of 250 rpm. At the
end of this time, a viscous and transparent solution was
obtained. Glycerol, which acts as a plasticizer, was added
in different proportions into identical starch solutions in
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beakers at 70 ± 1°C and treated at this temperature for an
additional 15 min under a constant agitation of 250 rpm.
Six glycerol/starch (G/S) concentrations, with weight
ratio, G/S = 0.0, 0.1, 0.2, 0.3, 0.4 and 0.5, were prepared.
2.4 Rheological characterization of glycerol/
starch solutions
The rheological properties of the six G/S solutions
were measured using a viscometer (DV-E Brookfield,
Middleboro, MA, USA), starting at 70°C, then they were
measured while cooling at four temperatures (30, 40, 50
and 60°C). A spindle type S-62 was rotated between 4 and
100 rpm. Six hundred milliliters of solution was loaded into
the cylindrical cup and cooled in a water bath at specific a
temperature. All analyses were performed at least three times
using the Brookfield viscometer between 20  and 80% full
torque scale. Data were analyzed using MS-Excel® software.
3 Results and discussion
3.1 Proximate analysis of cassava starch
The analysis for humidity, as well as for ash, crude
protein, crude fat, crude fiber and carbohydrate contents
in the starting cassava starch (HMC-1) gave the following
mean values with the corresponding standard deviation:
13.60 ± 0.35, 0.42 ± 0.10, 0.61 ± 0.10, 0.73 ± 0.36, 0.60 ± 0.15 and
97.64 ± 0.71, respectively. This raw material shows a similar
composition to that reported by Mali et al. [40], Alvis et al.
[41], and Nwokocha et  al. [42], for the starch studied by
them. In addition, the humidity value is similar to that
reported by Ahmad et al. [43], obtaining moisture content
at around 12% for starches at environmental conditions.
3.2 Rheological behavior
The temperature dependence of the rheological results of
different glycerol/starch solutions obtained from curves
of shear rate vs. shear stress is shown in Figure 1. They
show a monotonic increasing non-linear relation between
shear rate and shear stress. The curves were better fitted
to a power law model [11] based on least-square analysis
of the corresponding data, obtaining straight lines that fit
well to the expression:
In(μa) = (n-1)In(4πN)+In(K)-nIn(n), (1)
 G.A. Valencia et al.: Effect of glycerol concentration and temperature on the rheological       143

400
A 450 B
350
400
300
350

Shear stress (Pa)

Shear stress (Pa)

250 300

200 250

150 30°C 200 30°C

40°C 40°C
100 150 50°C
50°C
60°C 100 60°C
50 70°C 70°C
50
0.0 0.4 0.8 1.2 1.6 0.0 0.4 0.8 1.2 1.6
Shear rate (rps) Shear rate (rps)

450 450
C D
400 400

350 350
Shear stress (Pa)

Shear stress (Pa)

300 300

250 250

200 30°C 200 30°C

40°C
150 150 40°C
50°C
50°C
60°C
100 100 60°C
70°C
70°C
50 50
0.0 0.4 0.8 1.2 1.6 0.0 0.4 0.8 1.2 1.6
Shear rate (rps) Shear rate (rps)

450 500
E F
400 450

350 400
Shear stress (Pa)

300 350
Shear stress (Pa)

250 300

200 30°C 250 30°C

40°C
40°C
150 50°C 200
50°C
60°C
100 70°C 150 60°C
70°C
50 100
0.0 0.4 0.8 1.2 1.6 0.0 0.4 0.8 1.2
Shear rate (rps) Shear rate (rps)

Figure 1 Shear rate vs. shear stress for: (A) G/S = 0.0, (A) G/S = 0.1, (C) G/S = 0.2, (D) G/S = 0.3, (E) G/S = 0.4 and (F) G/S = 0.5 solutions,
at different temperatures.

where μa (Pa s) is the apparent viscosity of the solutions, N (Figure 1) indicates a pseudoplastic behavior in their
is the spindle frequency in cycles per second (rps), K is the rheological properties, as has been previously reported
consistency coefficient (Pa sn), and n is the flow behavior in the literature for other starch solutions [11, 20, 22, 24].
index (dimensionless). For each solution, the flow behav- This behavior has been attributed to the breakdown of
ior index and the consistency coefficient were determined structural units caused by hydrodynamic forces gener-
from the slope and the intercept of the linear regression to ated during cutting [11, 20, 44–46]. Conversely, Grigelmo
the above expression. Table 1 shows the fitting parameters et al. [12] claim that the degree of pseudoplasticity could
with a good coefficient of determination (R2 = 0.99). be related to the value of the flow behavior index, n, such
The observed power law functional variation of the that pseudoplastic systems are characterized by having a
above rheological results for glycerol/starch solutions flow behavior index < 1.0 (n < 1.0), which should be lower

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144      G.A. Valencia et al.: Effect of glycerol concentration and temperature on the rheological

Table 1 Fitting parameters to Eq. (1), corresponding to the flow 3.3 The effect of temperature
behavior index (n), the consistency coefficient (K) and R2 (coefficient
of determination) for the various G/S solutions prepared in the
30–70°C temperature range. In liquids, the viscosity generally decreases with increas-
ing temperature because of breakdown in the polymer
G/S suspension Temp. (°C) K (Pa sn) n naverage R2 structure and weak interactions such as hydrogen bonds
[11, 12].
0.0 30 934.41 0.57 0.55 0.99
40 820.41 0.56 0.99 The apparent viscosity decreases exponentially as
50 834.43 0.61 0.99 μa = μ0exp(Ea/RT) with increasing temperature, where μ0,
60 667.88 0.52 0.99 is a constant parameter (Pa s), Ea, is the activation energy
70 464.88 0.50 0.99 (KJ/mol), R, is the universal gas constant (8.314 J/mol K)
0.1 30 1191.51 0.56 0.59 0.99
and T, the absolute temperature (K) [47]. For this fitting,
40 1108.22 0.59 0.99
the shear rate must be fixed for the analysis of the appar-
50 1014.35 0.59 0.99
60 963.65 0.60 0.99 ent viscosity as a function of temperature. Similarly, the
70 858.28 0.60 0.99 temperature dependence of the inverse consistency coef-
0.2 30 1137.37 0.56 0.57 0.99 ficient is generally fitted to the Arrhenius model, such
40 1079.90 0.59 0.99 that K = K0exp(Ea/RT). Figure 2 shows the effect of temper-
50 962.30 0.57 0.99
ature on the apparent viscosity of G/S solutions to a fixed
60 896.16 0.58 0.99
70 779.96 0.56 0.99 shear rate (0.5 rps); similarly, Figure 3 shows the effect
0.3 30 1313.29 0.57 0.59 0.99 of temperature on the consistency coefficient of G/S solu-
40 1259.84 0.59 0.99 tions. Table 2 gives the Arrhenius fitting parameters μ0,
50 1108.44 0.61 0.99 Ea, R2 (coefficient of determination) and K0, Ea, R2 for the
60 1057.31 0.60 0.99
temperature dependence of the apparent viscosity and
70 922.11 0.59 0.99
consistency coefficient, at various concentrations G/S
0.4 30 1446.86 0.57 0.57 0.99
40 1317.91 0.56 0.99 prepared.
50 1263.45 0.56 0.99 From Figure 2, it is clear that addition of glycerol
60 1141.30 0.59 0.99 increases the apparent viscosity. Moreover, the thermal
70 996.36 0.59 0.99 activation energy also increases with glycerol concen-
0.5 30 1636.15 0.56 0.57 0.99
tration (see Table 2), thus these results indicate that the
40 1545.20 0.57 0.99
50 1393.25 0.57 0.99 glycerol promotes interactions with the gelatinized starch
60 1324.45 0.58 0.99 increasing in this way the apparent viscosity. Conversely,
70 1238.64 0.59 0.99 it is apparent from Figure 3 that the consistency coeffi-
cient K also increases with the glycerol concentration, but,
contrary to the apparent viscosity, the thermal activation
(close to 0) for a higher pseudoplastic response [12]. Flow energy for K (see Table 2) decreases with glycerol content
behavior indices reported in Table 1 were lower than 1.0,
indicating a pseudoplastic behavior in these solution
mixtures with different glycerol concentrations. It is also
apparent from Table 1, by calculation of means and stand-
ard deviations, that the standard deviation of n as a func-
tion of temperature and G/S concentration is rather low,
giving a mean value n = 0.57 ± 0.02. However, the dispersion
of the data for the consistency coefficient, K, as a function
of both temperature and glycerol concentration was quite
significant.
It should be pointed out that most of the data plotted
in Figure 1, were recorded for a shear rate between 0.1
and 1.7 rps; however, for the suspension G/S = 0.3, shear
rate higher than 1.0 rps were not reported at lower tem-
peratures because of instability in the data recording. The
same behavior was observed for G/S = 0.5 suspension, in Figure 2 Effect of temperature on the apparent viscosity of G/S
which the segment of data points was < 1.7 rps. solutions at fixed shear rate (0.5 rps).

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 G.A. Valencia et al.: Effect of glycerol concentration and temperature on the rheological       145

models, and μ1, μ2, a, β are constant values [12, 47, 50, 51].
Both models were tested for the G/S solutions prepared,
however, the exponential model resulted in better coeffi-
cients of determination (R2). Table 3 shows the μ2, β and
R2 values obtained from the exponential model using a
fixed shear rate of 0.5 rps for different glycerol concentra-
tions and temperatures. Morgan et  al. [52] proposed, for
the first time, an exponential fits for correlating the con-
centration with the apparent viscosity in protein dough
during thermal processing, and laterly Dolan and Steffe
[53] applied this model in native corn starch solutions.
Other applications of exponential models for correlated
concentrations with apparent viscosity are reported for
pseudoplastic food-systems such as concentrated juices
Figure 3 Effect of temperature on the consistency coefficient of G/S and peach dietary fiber [12, 47, 51].
solutions. The shear rate was kept constant at 0.5 rps.
The effect of glycerol concentration on the consist-
ency coefficient was also examined by fitting the data to
in the solutions, indicating that on heating the starch functional expressions. Although the consistency coeffi-
become less viscous. Similar behavior of the apparent vis- cient increased monotonically with the glycerol concen-
cosity and consistence coefficient has been reported for tration, it was better fitted to a polynomial model of third
solutions of waxy maize, tapioca, potato, sweet potato and degree, as was the case for that reported by Li-ming Che
high amylose corn starch [22, 23, 48]. In contrast, Chien- et al. [20], who studied the rheological properties in dilute
Hsien Chen et al. [49] studied the rheological properties of aqueous solutions of cassava starch (see Table 4).
tapioca starch/decolorized hsian-tsao gum/glycerol solu-
tions and concluded that the glycerol concentration does
not have a strong impact on the viscosity, possibly because 3.5 The combined effect of temperature
glycerol is relatively a very small molecule in comparison and glycerol concentration
with tapioca starch and hsian-tsao gum.
Figure 4 shows the combined effect of temperature and
concentration on apparent viscosity to a fixed shear rate
3.4 The effect of glycerol concentration (0.5 rps). The observed behavior could be modeled by a
single equation that correlated both parameters, being
The effect of the glycerol concentration on apparent vis- better fitted to a polynomial model μa = β0+β1C-β2T+β3C2-
cosity can be explained by two mathematical models: the β4T2-β5CT, were T is the absolute temperature, C the glyc-
power law, μa = μ1Ca, or the exponential models: μa = μ2e  βC, erol concentration and β0, β1, β2, β3, β4 and β5 are constant
where C is the concentration of the suspension in both values. The β0 value is the mean of the apparent viscosity,
the others constant values are obtained from the effects
of each variable (glycerol concentration and tempera-
Table 2 Fitting parameters μ0, Ko, Ea and R2 (coefficient of determi-
nation) for the various G/S solutions prepared in the temperature ture) on the apparent viscosity. Therefore β1 and β2 are
range studied, from 30 to 70°C, using the models: μa = μ0exp(Ea/RT)
and K = K0exp(Ea/RT), respectively. The shear rate was kept constant
Table 3 Fitting parameters μ2, β and R2 (coefficient of determina-
at 0.5 rps.
tion) for the various G/S solutions prepared in the temperature
range studied, from 30 to 70°C, using the models: μa = μ2e  βC. The
G/S μa (Pa s) K (Pa sn) shear rate was kept constant at 0.5 rps.
μ0 (Pa s) Ea (KJ/mol) R2 Ko (Pa sn) Ea (KJ/mol) R2
Temperature (°C) μ2 β R2
0.0 884.19 3222.17 0.83 4.45 13.64 0.82
0.1 952.83 3728.91 0.95 78.98 6.86 0.98 30 425.03 1.19 0.95
0.2 923.58 3625.24 0.95 47.06 8.06 0.97 40 391.52 1.09 0.96
0.3 1127.90 4306.32 0.99 66.15 7.59 0.96 50 355.64 1.11 0.96
0.4 1345.00 5005.78 0.97 69.19 7.70 0.96 60 347.51 0.97 0.97
0.5 1392.50 5519.19 0.99 134.30 6.14 0.99 70 263.67 1.31 0.99

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146      G.A. Valencia et al.: Effect of glycerol concentration and temperature on the rheological

Table 4 Polynomial fitting of the effect of the glycerol concentration

on the consistency coefficient at different temperatures.
K=1279.61 + 1198.47C - 9.80T
Temperature (°C) R2
Mathematical model
1800 R2 = 0.92
30 K = 9421.9C3-6331.1C2+2194.8C+954.94 0.96 1600
40 K = 13300C3-9898C2+3050.3C+834.6 0.96
1400
50 K = 4313.3C3-2203.5C2+1128.8C+854.08 0.95
60 K = 12915C3-9610C2+2867.5C+688.19 0.95 1200

K (Pa sn)
70 K = 21802C3-16606C2+4375.7C+486.88 0.95 1000
800
600
70
calculated from the main effects of the concentration and 65
60

0.5
temperature, similarly β3 and β4 are obtained from the Te
m 5
pe 5 50 w)

0.4
secondary effects of the same variables and β5 is attained ra (w/
ion

0.3
tu 45
re
40 nt rat

0.2
(°C
from the interaction effect between the glycerol concen- ) 35 co nce

0.1
30 ce rol
tration and temperature [54]. The mathematical model is Gly

0.0
shown in Figure 4, which gave a coefficient of determina-
tion of 0.93.
Figure 5 Combined effect of temperature and glycerol concentra-
Similarly, Figure 5 shows the combined effect of tion on the consistency coefficient.
temperature and concentration on the consistency coef-
ficient, K. Initially, the data were fitted to the model
In K = β0+β1(1/T)+β2C proposed by Velez and Barbosa [55], feature of both models is that the apparent viscosity and
however, the fit yielded a poor R2 correlation. Because of the consistency coefficient can be explained as a function
this adverse result, the best fitting was obtained by using of the two variables simultaneously.
a multiple linear regression model K = β0+β1T+β2C, which is
shown in Figure 5 (with R2 = 0.92). In comparison with the
apparent viscosity, the consistency coefficient is very well
fitted to a model that is characterized by only the β0 value
4 Conclusions
obtained as the mean of the consistency coefficients, and
The rheological testing performed on glycerol/starch solu-
the β1 and β2 values, calculated from the main effects for
tions as a function of glycerol concentration and tempera-
the temperature and glycerol concentration. The main
ture showed a pseudoplastic behavior for all concentra-
tions prepared in a range of temperatures between 30 and
70°C. The power law model (Eq. 1) is the most appropriate
μa=545.97+42183C - 2.91T + 701.43C2 -0.01T2 - 5.18CT model for describing the rheological behavior of cassava
starch solutions as a function of glycerol concentrations.
900 R2 = 0.93 There was no significant variation of the flow behavior
800 index n whose mean value remained at about 0.57 ± 0.02 at
700 different temperatures and glycerol concentrations, indi-
cating a strong pseudoplastic response in all solutions pre-
600
Viscosity (cP)

pared and in the tested temperature range. However, these

500
variables affected significantly the consistency coefficient
400
(K) and the apparent viscosity (μa). The results are consist-
300 ent with the interpretation that the addition of glycerol
70
65 increases the quantity of intermolecular forces among the
60
0.5

Te solutions, molecular groups, increasing in this way the

m 5
pe 5 50 w)
0.4

ra (w/
ion
0.3

tu 45 at
solution’s viscosity. The consistency coefficient decreases
re ntr
(°C 4 0
0.2

ce with increasing temperature, but it increases when

35 on
) ol c
0.1

30 er
lyc increasing the glycerol concentration in the solutions. The
0.0

G
effect of the increasing temperature on the decrease of the
Figure 4 Combined effect of temperature and glycerol concentra- apparent viscosity and consistency coefficient can be well
tion on the apparent viscosity at a fixed shear rate (0.5 rps). explained by an exponential model. Moreover, exponential

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 G.A. Valencia et al.: Effect of glycerol concentration and temperature on the rheological       147
and polynomial models are proposed to explain the effect
of glycerol concentration on μa and K, respectively. Finally,
two additional polynomial models were tested to describe
the combined effect of temperature and glycerol concen-
tration on μa and K (see Figures 4 and 5) at a fixed shear
rate (0.5 rps), also showing good correlation. Thus the
results show that the glycerol content and temperature of
the glycerol/starch solutions have a strong consequence
on their rheological properties, considering their poten-
tial use as precursors for biodegradable films or biopoly-
mer membranes for solid electrolyte applications [31, 32].
The results presented here provide a clear indication of a
strong coupling between glycerol and cassava molecular
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units, suggesting that those features could be correlated
and should be investigated further.
Acknowledgements: The authors gratefully acknowledge
financial support from “Universidad Nacional de Colom-
bia’’ “DIPAL’’ code number “QUIPU 2010100729 and
2020100626’’, and the “Laboratorio de Nutrición Animal,
Universidad Nacional de Colombia, Palmira’’ for the use
of installations. They are also grateful to Jefferson Paz for
his collaboration.
Received October 7, 2012; accepted January 3, 2013; previously
published online February 7, 2013
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