Applied Clay Science 99 (2014) 306–311

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Applied Clay Science

journal homepage: www.elsevier.com/locate/clay

Review article

Effect of polyethylene oxide (PEO) and shear rate on rheological

properties of bentonite clay
L. Hammadi ⁎, N. Boudjenane, M. Belhadri
Laboratory of Rheology, Transport and Treatment of the Complex Fluids, University of Science and Technology, Mohamed Boudiaf, P.O. Box 1505, El M'Naour, Oran 31000, Algeria

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

Article history: In this paper, the influence of polyethylene oxide (PEO) and shear rate on rheological properties of bentonite
Received 30 July 2013 suspensions is studied. The model of Herschel–Bulkley which is used to fit the flow curves of the mixture
Received in revised form 10 July 2014 which based on the bentonite-polyethylene oxide and the Generalized Kelvin–Voigt model has been successfully
Accepted 15 July 2014
applied to fit the creep and recovery data and to analyze the viscoelastic properties of mixture. The addition of
Available online 26 July 2014
polyethylene oxide (PEO) in a concentration range between 0 and 2% in 4% of bentonite induces not only an in-
Keywords:
crease of the yield stress and the consistency index of bentonite but also a decrease of the flow index of bentonite.
Bentonite clays It is also the addition of PEO between 0 and 2% to 4% that may cause an increase in the viscoelastic properties of
Polymer bentonite. For constant shear rate applied on the 4% bentonite at the 20 °C in which a thixotropic behavior was
Structural parameter observed and analyzed by using a modified model of Herschel–Bulkley a structural parameter λ is included in
Thixotropy order to account for time dependent effect.
Viscoelastic © 2014 Elsevier B.V. All rights reserved.

1. Introduction of bentonite clays on the flow properties of bentonite suspensions was

Bentonite clays are commonly used in many industrial applications,
especially in manufacturing ceramics, drug manufacturing, treating pol-
luted water, such as the adsorption of toxic organic compounds
(Alemdar et al., 2005; Gridi-Bennadj et al., 2011) and stabilization of
oil–water emulsions (Nciri et al., 2009). The bentonite is also used to
lubricate drill bit, to prevent fluid loss into the formations and to
apply hydrostatic pressure in the well bore (Mahto and Sharm, 2004).
The use of bentonite suspension as a drilling fluid causes a decrease in
density and viscosity. But during the operation of drilling fluids, several
requirements are imposed: the increase of density, the viscosity, the
gelation, and lubricity. The density can be increased by adding the barite
and even the viscosity can be also increased by adding some kinds of
polymers like cellulosics, guar gum, xanthan gum, polyacrylates, poly-
acrylamides, carboxymethyl cellulose (CMC) and polyethylene oxide
(PEO) are used for controlling the viscosity and the yield stress of
drilling fluids as well as reducing formation damage (Kelessidis et al.,
2011; Rossi et al., 2003). The rheology of bentonite–water systems
and bentonite-water-polymer has been widely studied and it was the
subject of many previous works (Benchabane and Bekkour, 2008;
Breen, 1999; M'bodj et al., 2004). The effect of sixteen different types
studied by Besq et al. (2003). It was observed that the rheological be-
havior of bentonite depends on the chemical compositions of each sam-
ple. Abu-Jdayil (2011) has shown that the addition of electrolytes such
as NaCl, Na2SO4, KCl, CaCl2, and BaCl2 in a concentration range of 0.02
to 0.2 M reduced the apparent viscosity of the bentonite suspensions
and changed its rheological behavior from shear thinning and thicken-
ing to Newtonian behavior. Benchabane and Bekkour (2006) showed
that when CMC and xanthan gum are added to Ca–montmorillonite
suspensions, the polymer coats the clay particles and prevents the
reorganization of the agglomerates by the usual mechanisms (face-to-
face connections),and the rheological behavior of the bentonite–CMC
suspensions depends on the structural state (flexible) of this polymer.
In the next paper, the effects of polymer and shear rate on the rheo-
logical properties of bentonite were studied, and a modified model of
Herschel–Bulkley was employed to describe the thixotropic behavior
of clays suspension.
2. Materials and methods
2.1. Materials

The used clay in this study is bentonite of Maghnia (West of Algeria)

⁎ Corresponding author. Tel.: +213 41 56 03 23. which is commercially by Bental Company. The chemical analysis of this
E-mail address: hammadi7280@yahoo.fr (L. Hammadi). bentonite is shown in Table 1.

http://dx.doi.org/10.1016/j.clay.2014.07.016
0169-1317/© 2014 Elsevier B.V. All rights reserved.
 L. Hammadi et al. / Applied Clay Science 99 (2014) 306–311 307

Table 1
Chemical analysis of bentonite samples in wt%.

SiO2 Al2O3 Fe2O3 MgO CaO Na2O K2O TiO2 SO3 Rb2O

58.455 17.143 4.589 4.364 1.078 7.532 5.512 0.314 0.221 0.107

The polymer used in this work is polyethylene oxide (PEO), non-

ionic polymer chain flax [CH2 − CH2 − O]n with a molecular weight
of 106 g/mol ware obtained from Sigma-Aldrich Company and it is
often used in the formulation of drilling fluids.

2.2. Sample preparation

For each mixture, the base bentonite suspension has the same
mass concentration (4%). Given that the way of preparation has a
great influence on the final state of the suspensions and thus on
the rheological behavior, an identical experimental procedure was
Fig. 1. Shear stress as a function of shear rate at different mass concentrations of PEO add
used for the preparation of all suspensions. All tests were carefully
(0, 0.5, 1, 1.5 and 2%). The solid lines correspond to the curve fitting to Eq. (1).
carried out under equal conditions to allow a comparison in the re-
sults. The bentonite powder was dispersed in the required amount
of distilled water without any chemical addition. The homogeniza- 3. Results and discussion
tion was performed under continuous magnetic agitation for 24 h.
The additives under different concentrations (0.5, 1, 1.5 and 2%) 3.1. Effect of the PEO on bentonite rheological behavior
are then added to the base suspension. An average pH ranging be-
tween 9.6 and 11.5 was measured at ambient temperature. 3.1.1. Typical flow curve of the mixture
The variation of the shear stress τ as a function of the shear rate γ ˙ at
different mass concentrations of PEO (0 to 2%) adding in base bentonite
2.3. Experimental setup suspension (4%) is shown in Fig. 1. It shows clearly Non-Newtonian
behavior after a yield stress. Therefore experimental data were fitted
The rheological measurements were performed by using a torque to the classical model of Herschel–Bulkley:
controlled rheometer (RS600 from Thermo-Fischer), equipped with
a cone-plate geometry (diameter: 60 mm; angle: 2°; gap: 105 μm). It
n
has a Peltier temperature control system that allows having a very τ ¼ τ 0 þ Kγ̇ ð1Þ
quick response to any change in temperature. In order to prevent
changes in composition during measurements due to water evapo- where τ0 is the yield stress in Pa, K the consistency index in Pa.sn and n is
ration, a solvent trap was placed around the measuring device. the flow index.
Fig. 2 shows that the evolution of yield stress of mixture bentonite-
PEO as a function of mass concentration in PEO adds to the bentonite.
2.4. Experimental methods
We observe on the figure a rapid increase in the yield stress with dose
of PEO, this increase of yield stress related to the adsorption of PEO by
2.4.1. Flow curves of mixtures bentonite-PEO
bentonite. This adsorption makes the specific surface highly rigid
In order to avoid any memory effect, the sample was pre-sheared at
bentonite and causes an increase of interaction between the bentonite's
a frequency of 500 s−1 for 60 s in the measuring device. Then the sample
particles.
has kept at rest for 600 s prior to measurements in order to permit the
material recovering its initial structure partially at least. The imposed
shear rate range depends on the mass concentration of bentointe. The
following experiments give consequently a continuous ramp of shear
rate which is ranging from 0.5 to 500 s− 1 and has been applied on
each sample during 600 s.

2.4.2. Creep and recovery of mixtures bentonite-PEO

Creep and recovery tests are carried out as follows:
At time t = 0, a constant shear stress τ = 1 Pa was applied to the
mixtures and the compliance (J) was recorded as a function of creep
time; at t = 120 s the stress τ was set to zero and the recoverable part
of J was measured as a function of the recovery time equal to 120 s.

2.4.3. Effect of shear rate on apparent viscosity of bentonite

After a rest time of 600 s, the samples were sheared for 120 s at
different constant shear rates (100 s − 1 ,200 s − 1 ,300 s − 1 ,500 s − 1
and 600 s− 1) and at a constant temperature of 20 °C. In order to pre-
vent any irreversible evolution of the bentonite, a new fresh sample Fig. 2. Evolution of yield stress of mixture bentointe-PEO as a function of mass concentra-
was used for each applied shear rate. tion in PEO adds.
308 L. Hammadi et al. / Applied Clay Science 99 (2014) 306–311

increasing the additive concentration and the time necessary to reach

a constant deformation during recovery, after removal of the shear
stress, decreases. This is characteristic of systems with weak links in
the inner structure (base bentonite suspension), as compared to stron-
ger links when the PEO concentrations increase. This is in agreement
with the steady-state experiment results (see Fig. 1). The elastic proper-
ties were defined by correlating the results with the well-known visco-
elastic models of Burger model or Generalized Kelvin–Voigt model
(Dolz et al., 2008), comprising the association in series of the Maxwell
model and the Kelvin–Voigt.
The creep curves are described by:

X  

⌈ ⌉
N
t t
J F ¼ J0 þ þ J i 1− exp − ð2Þ
η0 i¼1 θi

Ji
Fig. 3. Evolution of consistency index and flow index of mixture bentointe-PEO as a func- θi ¼ : ð3Þ
ηi
tion of mass concentration in PEO adds.

Whereas the recovery strain is given by:

The evolutions of the consistency index and flow index of mixtures
     
of bentonite-PEO as a function of mass concentration in PEO adds to t 1 XN t t
the bentonite are presented in Fig. 3. In the figure we observe a decrease JR ¼ þ J i exp 1 −1 exp − ð4Þ
η0 i¼1 θi θi
of flow index and a significant increase in the consistency index of the
mixtures. The remarkable increase in the consistency index causes an where J0 is the purely elastic contribution (or the instantaneous elastic
increase in the friction and an increase in the viscosity of the mixture compliance), η0 is the purely viscous contribution, represented by the
due to the interaction between the solid particles and viscous effects. dashpot of the Maxwell model, i.e., the uncoupled or residual steady-
In this case, the interactions between the clay particles and polymer state viscosity obtained from the creep curve at long times when the
intensify lead to difficult movements in the dispersing medium. compliance curve is linear, Ji is the contribution to retarded elastic com-
pliance, θi is the retarded time, ηi is the retarded viscosity and t1 is the
time where the stress is applied for t ≤ t1 and removed at t = t1.
3.1.2. Creep recovery testing
The fittings in Fig. 4 were performed with just one Kelvin–Voigt solid
Creep and recovery testing are efficient tools for investigating the
(N = 1) and the fitting parameters are detailed in Table 2. The column
properties of dispersions under many conditions close to the at-rest
G0 ¼ J1 represents the instantaneous elastic modulus of the Maxwell
state, allowing investigating the clay–polymer interactions without 0

the destruction of the internal structure of the system. Fig. 4 shows unit at t = 0; that is, the instantaneous elastic response of the system
the values of compliance J ðt Þ ¼ γτ , as a function of time, for the creep and the column G1 ¼ J1 is the elastic modulus of Kelvin–Voigt. The latter
1

tests corresponding to the systems studied (mixtures bentonite-PEO), represents the contributions of the retarded elastic region to the total
in a time interval between 0 and 120 s. For the interval time 120 s compliance. The strong increase is observed in G0 and G1 when the con-
≤ 240 s, we have represented the corresponding recovery. We observe centration of PEO is changed between 0 and 2% cause the manifestation
on the figure a decrease of the elastic compliance with the increase in of the shift from viscous to elastic behavior and an increase of the visco-
polymer concentration adds in the base bentonite. i.e., increase of the elastic properties in that range of PEO.
elastic modulus ¼ 1J , indicating an increase of the viscoelastic properties Concerning η0 let us mention that it has the meaning of viscosity of
of mixtures. In other words, the creep deformation decreases with the system in the newtonian regime, whereas it shows a clearly increas-
ing trend as the concentration of PEO is increased. At high concentration
0,16 of PEO adds in the bentonite, the applied stress of 0.5 Pa is not sufficient
0 wt% PEO , 0.5 wt% PEO
1 wt% PEO , 1.5 wt% PEO to break weak particle-to-particle bonds, and the suspensions do not
0,14 2 wt% PEO , Model flow. For lower concentration values of PEO such resistance to flow is
not so large, and this explains the values of η0 and G1 in this case the re-
0,12
Creep tarded deformation, related to the breaking and reconstruction of weak
Recovery
links between the particles. The characteristic relaxation time associat-
Compliance (1/Pa)

0,10
ed with these breaking/reconstruction processes is θ1. Although this
0,08 time does not show a definite trend when estimated from creep data.
For higher polymer concentrations add in the clay, the system reaches
0,06 steady state rapidly due to a strong link between clay and polymer.

0,04
Table 2
0,02 Fitting parameters of the creep–recovery data in Fig. 4, with N = 1 in Eqs. (2) and (4).

Creep Recovery
0,00
0 20 40 60 80 100 120 140 160 180 200 220 240 260 PEO (wt%) G0 (Pa) G1 (Pa) η0 (Pa.s) G1 (Pa) η0 (Pa.s) θ1 (s)

Time (s) 0 14.43 16.42 5330.44 116.69 13,544.02 28.88

0.5 33.07 16.39 7865.73 112.87 14,002.33 27.09
1 41.15 19.85 8905.52 116.69 18,375.70 24.29
Fig. 4. Compliance versus time in creep and recovery test at different mass concentration
1.5 76.39 45.66 18,929.96 241.54 28,985.50 14.45
of PEO add (0, 0.5, 1, 1.5 and 2%). The solid lines correspond to the curve fitting to Gener-
2 155.28 120.05 31,880.10 490.19 58,823.53 7.48
alized Kelvin–Voigt model.
 L. Hammadi et al. / Applied Clay Science 99 (2014) 306–311 309

0,10
-1 -1 -1
100 s 200 s 300 s
0,09 500 s
-1
600 s
-1
fitting to eq.12

0,08

0,07
Viscosity (Pa.s)

0,06

0,05

0,04

0,03

0,02

0,01
0 20 40 60 80 100 120
Time (s)

Fig. 5. Viscosity of based bentonite suspension as a function of time shears at 20 °C for

Fig. 6. Zero time shear stress τy0 as a function of shear rate for 4% of bentonite suspension
constant shear. The solid line corresponds to curve fitting to Eq. (12).
and comparison with the Herschel–Bulkley model (temperature 20 °C).

3.2. Effect of shear rate on apparent viscosity of bentonite

the apparent yield stress value obtained by extrapolation toγ̇¼ 0. The
Fig. 5 shows the apparent viscosity of based bentonite (4%) evolution resulting equation was:
as a function of time for different steady shear rates varying from 100 to
ð0:35Þ 2
500 s−1. For all values of shear rates, the viscosity decreases significantly τy0 ¼ 5:74 þ 0:84γ̇ ; R ¼ 0:994 ð7Þ
with time and tends to constant values.
In order to analyze the structural evaluation of the suspension, The structural parameters λ and λe are expressed in terms of the ap-
we applied the phenomenological model of Tiu and Boger (1974) parent viscosity η ¼ γ̇τ to find k2. Equating the Eq. (5) to the definition of
based on an approach initially suggested by Moore (1959) and re- the apparent viscosity which, in this case, is a function of both shear and
fined by Cheng and Evans (1965). This choice was motivated by time, it is found:
the simplicity (minimum number of parameters) and efficacy of
this model (Hammadi et al., 2013). Cheng and Evans (1965) argued ηγ̇
λ¼ ð8Þ
that the stress-strain equation depends on the fluid model and must be τy0 þ K 1γ̇ n1 :
completed with a kinetic equation of structural parameter λ changing
with time. This parameter describes the current state of agglomeration. Eq. (8) is valid for all values of λ including λe at ηe, the equilibrium of
As pointed out before, the flow curves of based bentonite suspension the apparent viscosity. Differentiating Eq. (8), with respect to time at a
were found to be well fitted by the model of Herschel–Bulkley, with sat- constant shear rate and combining the resulting equation with Eq. (4),
isfactory agreement (see Fig. 1). Following the model proposed by Tiu yields:
and Boger (1974), the Herschel–Bulkley model was modified to take
into account of state is assumed to be: dη  2
¼ −a1 η−ηe ð9Þ
  dt ;
n
τðt Þ ¼ λ τy0 þ þK 1γ̇ 1 : ð5Þ
where
The structural parameter ranges from an initial value of unity at zero
k2γ̇
shear time (agglomerated structure at rest). a1 ¼ ð10Þ
τ y0 þ K 1γ̇ n1 :
For their rate equation Tiu and Boger (1974) employed a second-
order kinetic equation:
Integrating Eq. (9) at constant shear rate from η = η0at t, = 0 at t, =
,
dλ 2 t yields:
¼ −k2 ðλ−λe Þ for λNλe ð6Þ
dt
1 1 0
¼ þ a1 t : ð11Þ
where k2 is rate constant that is a function of shear rate to determine ex- η−ηe η0 −ηe
perimentally and can be considered as a measure of the rate of structure
breakdown, i.e., the degree of thixoropy and the λe is the equilibrium The equilibrium viscosity ηe was found by fitting the time depen-
structural parameter. Then entire time-dependent behavior of our ben- dence of the viscosity (Fig. 5) by an exponential decay curve
tonite suspension might be completely described by Eqs. (5) and (6) (Hammadi et al., 2013) of the form:
with the parameters τy0, K1, n1and k2 evaluated from experimental 
data. The rheological constants τy0, K1 and n1 are determined with initial η ¼ ηe þ η0 −ηe expð−βt Þ ð12Þ
shearing conditions (λ = 1 and t = 0), and Eq. (6) reduces to the clas-
sical Herschel–Bulkley equation. In other words, they are determined where β is the rate constant in (s−1).
from the initial shear stress in the material, observed in the beginning Fig. 7 shows the variation of initial viscosity η0 and equilibrium
of a test, for each shear rate considered. Fig. 6 shows the zero shear viscosity ηe as a function of shear rate.
1
stress at a function of shear rate for mass concentration of bentonite Using Eq. (11), a plot of η−η versus t’, at constant shear rate, should
e
equal 4%. The curves were fitted to the model of Herschel–Bulkley and yield a straight line with a slope equal to a1. The same procedure is
310 L. Hammadi et al. / Applied Clay Science 99 (2014) 306–311

Fig. 7. Initial viscosity and equilibrium viscosity determined by Eq. (12) as a function of Fig. 9. Parameters a1 and k2 of Tiu and Boger model as a function of shear rate for 4% of
shear rate. bentonite suspension.

repeated at different shear rates. Fig. 8 shows the data for bentonite The value of the structural parameter λe was determined at each
suspension (4%). shear rate by using Eq. (15).
Fig. 9 shows the evolution of the parameters a1 and k2 as a function
of shear rate for 4% bentonite suspension. It was found that both a1 and ηe
λe ¼ : ð15Þ
k2 can be described by a power function of shear rate: η0

β1 Where η0 is the initial viscosity and ηe the equilibrium viscosity

a1 ¼ α 1γ̇ ð13Þ
determined by Eq. (12). Fig. 10 shows the evolution of equilibrium
structural parameter as a function of shear rate.
As the rate equation Eq. (6), cannot be integrated analytically for
β2 varying shear rate conditions, further progress is still necessary to pre-
k2 ¼ α 2γ̇ ð14Þ
dict shear stress at a given constant shear rate. In order to derive an
equation that would predict the structural parameter, λ for a constant
With shear rate after a given time, Eq. (8) was rearranged to yield

2 1
α 1 ¼ 0:00006; β1 ¼ 1:267; R ¼ 0:993 λ ¼ λe þ : ð16Þ
1
þ K2t
ð1−λe Þ

2
α 2 ¼ 0:00004; β2 ¼ 1:950; R ¼ 0:998: Fig. 11 shows the evolution of structural parameter as a function of
time for each value of shear rate. As shown, structural parameter

1
Fig. 8. Linear relationship between η−η and time for different shear rates (4% bentonite
e
suspension) at temperature 20 °C. The solid line corresponds to a fitting of data by linear Fig. 10. Equilibrium structural parameter versus shear rate at 20 °C (4% of bentonite
regression. suspension).
 L. Hammadi et al. / Applied Clay Science 99 (2014) 306–311 311

0,98
into account the structural evolution of the bentonite suspension, the
100 s
-1
model of Herschel–Bulkley was modified by the introduction of a
0,96 200 s
-1

-1
structural parameter which allows a good description of the thixotropic
300 s
0,94 400 s
-1 behavior of the bentonite suspension.
structural parameter λ (-)

-1
600 s

0,92 References

0,90
0,88
0,86
0,84
0,82
0 20 40 60 80 100 120
Time (s)
Fig. 11. Structural parameter as a function of time at 20° (4% of bentonite).
changes are most significant during the initial shear period, after which
they maintain a nearly constant value.
4. Conclusion
In this paper, first the effect of polyethylene oxide on the flow behav-
ior and viscoelastic properties of clay bentonite was investigated. The
addition of polyethylene oxide (PEO) in a concentration range between
0 and 2% in 4% of bentonite induced not only an increase in the yield
stress and the consistency index of bentonite but also a decrease of
the flow index of bentonite. This increase of yield stress and the consis-
tency index of bentonite related to the adsorption kinetics of PEO by
bentonite. Even this addition in bentonite causes a sharp increase in
the instantaneous elastic modulus of the Maxwell unit and elastic
modulus of Kelvin–Voigt unit. This increase in instantaneous elastic
modulus and retarded elastic modulus causes an increase in the
viscoelastic properties of bentonite.
Secondly, the effect of shear rate on break-down behavior of benton-
ite suspension was examined. The time dependent viscosity decreased
rapidly with shearing time and reached a steady state. In order to take
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