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Article history: Adsorption of surfactants onto reservoir rock surface may result in the loss and reduction of their concen-
Received 15 May 2013 trations in surfactant flooding, which may render them less efficient or ineffective in practical applications
Received in revised form 5 July 2013 of enhanced oil recovery (EOR) techniques. Surfactant flooding for EOR received attraction due to its abil-
Accepted 7 July 2013
ity to increase the displacement efficiency by lowering the interfacial tension between oil and water and
Available online 16 July 2013
mobilizing the residual oil. This article highlights the adsorption of surfactants onto sand surface with
variation of different influencing factors. It has been experimentally found that adsorption of cationic
Keywords:
surfactant on sand surface is more and less for anionic surfactant, while non-ionic surfactant shows inter-
Surfactant
Adsorption isotherm
mediate behaviour. X-ray diffraction (XRD) study of clean sand particles has been made to determine the
Isotherm model main component present in the sand particles. The interaction between sand particles and surfactant has
Adsorption kinetics been studied by Fourier Transform Infrared (FTIR) Spectroscopy of the sand particles before and after
Thermodynamics of adsorption aging with surfactant. Salinity plays an important role in adsorption of anionic surfactant. Batch experi-
ments were also performed to understand the effects of pH and adsorbent dose on the sorption efficiency.
The sand particles exhibited high adsorption efficiency at low pH for anionic and nonionic surfactants.
But opposite trend was found for cationic surfactant. Adsorption data were analyzed by fitting with Lang-
muir, Freundlich, Redlich-Peterson, and Sips isotherm models. Results show that the Langmuir isotherm
and pseudo-second order kinetics models suit the equilibrium and kinetics of adsorption on sand surface.
Thermodynamics feasibility of the adsorption process was also studied to verify the spontaneity of the
process.
© 2013 Elsevier B.V. All rights reserved.
0169-4332/$ – see front matter © 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.apsusc.2013.07.029
88 A. Bera et al. / Applied Surface Science 284 (2013) 87–99
spontaneity of the process. Semi-quantitative analysis of clean sand water for several times followed by settling and decanting. After
particles has been done by X-ray diffraction (XRD) study. removing the dust particles the residual wet sand particles were
dried at 353 K for 18 h. The clean dried sand particles were used for
2. Experimental the experimental purposes.
Fig. 3. FTIR spectra of sand particles before and after surfactant treatment in brine (2 wt% NaCl): (a) pure sand; (b) treated with SDS; (c) treated with CTAB; (d) treated with
Tergitol 15-S-7.
function of concentration in Fig. 4. The concentration at the inflex- parameter, and it is represented by the following equation [51,52]:
ion point of the curve is critical micelle concentration. The lowest
surface tension value achieved by Tergitol 15-S-7 is 30 mN m−1 1
which is significantly lower than the surface tension value of water. RL = (3)
1 + KL C0
The CMCs of the surfactants are found to be 0.23 wt%, 0.0345 wt%,
and 0.0051 wt% for SDS, CTAB, and Tergitol 15-S-7 respectively. where, C0 (mg/L) expresses initial adsorbate concentration in aque-
ous solution. KL (L/mg) is the Langmuir constant. The RL parameter
gives important signs on the compatibility of adsorption for the
selected adsorbent–adsorbate pair. There are four possibilities for
3.3. Adsorption isotherms of surfactants on sand particles
the RL value:
The Langmuir adsorption isotherm and the Freundlich adsorp-
• In the case 0 < RL < 1, adsorption is favorable.
tion isotherm are two common isotherms used to describe the
• In the case RL > 1, adsorption is unfavorable.
equilibrium adsorption isotherm. Another two isotherms such as
• RL = 1 indicates linearity of adsorption.
Redlich-Peterson and Sips are considered here to describe the
• In the case RL = 0, adsorption is irreversible.
experimental data and find out the best fitted model for adsorption
of surfactant on sand surface.
The Langmuir equation relates the amount of solid adsorbate The values of RL obtained in this study were between 0.0445
adsorbed, , to the equilibrium liquid concentration at a fixed tem- to 0.3507, indicating that the adsorption of surfactant onto sand
perature. The equation was developed by Irving Langmuir [50] in surface is favourable.
1916 and is expressed in this nonlinear form as follows: The Freundlich isotherm assumes that if the concentration of the
solute in the solution at equilibrium, Ce , is raised to the power 1/n,
1/n
C
max KL Ce the amount of the solute adsorbed being , the e is constant
= (2) at given temperature and the nonlinear form of the equation is
1 + KL Ce
expressed as:
where, is the amount of adsorbate adsorbed (mg/g); max is the 1/n
= KF Ce (4)
maximum amount adsorbed (mg/g); KL is the Langmuir equilib-
rium constant (L/mg); Ce is the equilibrium aqueous concentration where, KF (mg/g) and n are the Freundlich adsorption constants
(mg/L). It is well-known that the Langmuir isotherm is applicable related to sorption capacity and sorption intensity, respectively.
for monolayer adsorption because of the homogeneous surface of Freundlich isotherm has been derived by assuming an exponen-
a finite number of identical sites. Another important parameter of tially decaying sorption site energy distribution. The Freundlich
the Langmuir isotherm model is the term “RL ” which is a nondi- isotherm assumes that the surfactant adsorption occurs on a het-
mensional constant and called as separation factor or equilibrium erogeneous surface by multilayer sorption.
92 A. Bera et al. / Applied Surface Science 284 (2013) 87–99
Fig. 4. Plot of surface tension vs. surfactant concentration for finding the CMCs of the surfactants: (a) SDS, (b) CTAB and (c) Tergitol 15-S-12.
The Freundlich constant (1/n) is related to the adsorption inten- where, max (mg/g) is the maximum monolayer surfactant adsorp-
sity of the adsorbent. When, 0.1 < 1/n < 0.5, adsorption is favourable; tion capacity on sandstone. KS [(L/mg)m s ] is the Sips isotherm
0.5 < 1/n ≤ 1, it is easy to adsorb; 1/n > 1, it is difficulty to adsorb [53]. constant representing the energy of adsorption. ms is the empir-
The Redlich-Peterson isotherm model is used as a compromise ical constant. The values of KS , max and m can be obtained by
between Langmuir and Freundlich isotherm models [54,55]. The
non-linearized form of Redlich-Peterson isotherm model can be
Table 1
given as follows:
Adsorption isotherm parameters of the surfactants.
KR Ce
= 
(5) Isotherm models Parameters Surfactants
1 + ˛RCe SDS CTAB Tergitol 15-S-7
Fig. 8. Adsorption isotherms of SDS at different NaCl salt concentrations at 303 K: (a) Langmuir equation fitting; (b) Freundlich equation fitting.
Table 2
Adsorption isotherm parameters of SDS at different salinities.
dt
= k1 (e − t ) (7)
dt
On integration of this equation for the boundary condition t = 0
Fig. 10. The effect pH on the adsorption process of the surfactants.
to t = t and e = 0 to e = t , gives:
ln(e − t ) = ln e − k1 t (8)
increases the adsorption sites also increase and the adsorption
process takes place easily with increase in order. After a certain where, e (mg/g) and t (mg/g) are the amount of surfac-
adsorbent dose there is no further adsorption because of gathering tants adsorbed on sand particles at equilibrium and at time t (min)
of huge adsorption sites and produced particle interaction among respectively. k1 (min−1 ) is the rate constant of the pseudo-first-
the sand particles in the system. Particle-particle interaction takes order adsorption. The values of k1 can be calculated experimentally
place from high adsorbent concentration which leads to a decrease from the slope of the linear plot of ln( e − t ) versus t.
in total surface area of the adsorbent and an increase in diffused In Fig. 11(a), adsorption kinetics of SDS surfactant on sand par-
path length [59]. ticle at different concentration at 303 K has been depicted. The
parameters are calculated from the model have been summarized
in Table 3.
3.6. Effect of pH on adsorption of surfactants
3.7.2. Pseudo-second-order kinetic equation
The pH of the aqueous solution is one of the important control- The pseudo-second-order kinetic model equation is expressed
ling parameters in the adsorption of surfactant on reservoir rocks. as follow:
Fig. 10 shows the effect of pH on the extent of adsorption of dif-
ferent surfactants (anionic, cationic and nonionic) on clean sand dt 2
= k2 (e − t ) (9)
surface. The sand particles exhibited high adsorption efficiency at dt
low pH for anionic and nonionic surfactants. As pH increases the and rearranging the Eq. (9) gives
adsorption decreases for anionic surfactant. The adsorption capac-
ity at alkaline solution is lower due to the decrease of positively dt
2
= k2 dt (10)
charged sites on adsorbent and the competition between OH− and (e − t )
anionic surfactant for the adsorption site. A number of research
where, k2 (g/mg/min) is the rate constant of the second-order
works has been reported regarding the effect of pH of solution
equation.
on adsorption of surfactants on rock surfaces [27,60–63]. At low
Now applying the boundary conditions t = 0 to t = t and e = 0 to
pH, SDS adsorption capacity of sand is high due to acidic nature
e = t , the integrated linear form of Eq. (10) can be rearranged to
of the solution which makes the sand surface more positive and
obtain Eq. (11).
that is why the interaction of sand surface with anionic surfactant
SDS is high and hence adsorption capacity is high. In case of Ter- t 1 t
gitol 15-S-7 (nonionic), adsorption decreases up to neutral pH and = + (11)
t k2 e2 e
remains almost constant at alkaline pH region. This can be demon-
strated that the presence of lone pair of electrons of the oxygen The plot of t/ t versus t has been shown in Fig. 11(b). The val-
atom of the ethylene oxide group of ethoxylated nonionic surfac- ues of equilibrium adsorption capacity e and rate constant k2 ,
tant which is broadly attracted by the positively charged surfaces calculated from the intercept and the slope of the linear plot of
of sand particles at pH values lower than 7. The lower adsorption of t/ t versus t, along with the value of regression coefficient R2 , MSE
the surfactant at alkaline region is due to hydrophobic interaction values are listed in Table 3.
only. As pH of the solution increases adsorption of CTAB surfactant
(cationic) also increases because positively charged head groups of 3.7.3. Intraparticle diffusion model
the cationic surfactant are strongly attracted at high pH with neg- The intraparticle mass transfer diffusion model was proposed
atively charged sand surfaces. So from this study the adsorption of by Weber and Morris [64]. For determination of rate constant and
the surfactants on rock surfaces can be reduced or alter by fixing reaction type, first-order and second-order kinetic models are gen-
the solution pH for nonionic and ionic surfactants which are very erally used. To understand the diffusion mechanism of adsorption
important issue regarding the economic feasibility for surfactant process it is very important to introduce intraparticle diffusion
flooding. model. In this model the fractional approach to the equilibrium
96 A. Bera et al. / Applied Surface Science 284 (2013) 87–99
Fig. 11. The kinetics models for adsorption of SDS surfactant on sand particle at different concentrations at 303 K: (a) Lagergren-first order kinetics; (b) pseudo second order
kinetics; (c) interparticle diffusion kinetics.
Table 3
Kinetics parameters for the adsorption of surfactant on sand particles at different surfactant concentrations.
Intraparticle diffusion kid (mg/g/min) 3.896 × 10−2 3.893 × 10−2 3.318 × 10−2
C 0.1313 0.2319 0.3197
R2 0.988 0.981 0.990
MSE 1.2678 1.1523 1.1235
A. Bera et al. / Applied Surface Science 284 (2013) 87–99 97
Fig. 13. Relationship between Langmuir constant and temperature for SDS adsorp-
Fig. 12. Langmuir equation fitting for adsorption isotherms of SDS at different tem- tion on sand surface.
peratures.
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