Colloids and Surfaces A: Physicochem. Eng.

Aspects 259 (2005) 95–101

Effect of salt on the micelles of cetyl pyridinium chloride

D. Varade a,∗ , T. Joshi a , V.K. Aswal b , P.S. Goyal c ,
P.A. Hassan d , P. Bahadur a
aDepartment of Chemistry, South Gujarat University, Surat 395007, India
b
Solid State Physics Division, BARC, Trombay, Mumbai 400085, India
c IUC-DAEF, Mumbai Centre, BARC, Trombay, Mumbai 400085, India
d Novel Materials and Structural Chemistry Division, BARC, Trombay, Mumbai 400085, India

Received 12 June 2004; accepted 14 February 2005

Available online 16 March 2005

Abstract

Surface tension, conductance, viscosity, dynamic light scattering (DLS) and small angle neutron scattering (SANS) measurements were
carried out in order to investigate the effect of added salt NaCl and NaBr on micellization and structure of cetylpyridinium chloride (CPyCl)
micelles. Critical micelle concentration (CMC) of CPyCl decreases with increase in salts concentration, while CMC and counter ion dissociation
(β) increases with increase in temperature. At a given CPyCl concentration, the micelle size increases with increasing salt concentration above
a threshold value. Micellar growth in presence of salts is clearly reflected by an increase in viscosity, hydrodynamic diameter (d) from DLS
and aggregation number from SANS measurements. The effect of NaBr on CPyCl micelles was more pronounced in comparison to NaCl.
The difference in solution properties of Br− and Cl− is that Cl− counter ions being more hydrated are less effective to neutralize the charge
on the micellar surface.
© 2005 Elsevier B.V. All rights reserved.

Keywords: Micellization; SANS; DLS; Micellar growth

1. Introduction Cationic surfactants offer some additional advantages over

Micelles of ionic surfactants formed in aqueous media
are aggregates of surfactant molecules with different sizes
and shapes depending on given solution conditions. As for
the structure a micelle of ionic surfactants is composed of a
compressive core surrounded by a less compressive surface
structure [1,2]. In addition, counter ions are bound to mi-
celle surface. Looking at counter ion behavior, the binding
states are different depending on charge, size and polarity in
counter ions species themselves. The solution properties of
surfactant are all reflected from surfactant ions comprising
various combinations of hydrophobic tail with hydrophilic
head and from counter ion species.
∗ Corresponding author. Tel.: +91 261 2258384;
fax: +91 261 2256012/2227312.
E-mail address: dharmeshvarade2004@yahoo.com (D. Varade).
other class of surfactants [3–6]. These substances besides
their surface activity do show antibacterial properties and
are used as cationic softeners, lubricants, retarding agents,
antistatic agents and in some cases consumer use etc. Ionic
micelles of various cationic surfactants having chloride or
bromide as counter ion undergo the salt induced sphere-
to-rod transition, when NaCl or NaBr is added across a
certain threshold salt concentration. Experimentally, many
techniques have been used in order to investigate the sur-
factant concentration, added salt concentration and temper-
ature dependences of micellar solution properties [7–10].
Cetyltrimethylammonium bromide (CTABr) forms rodlike
micelles at concentration above 0.27 M in water at 28 ◦ C, on
the other hand, cetyltrimethylammonium chloride (CTACl)
do not show such a behavior, the aggregates remaining glob-
ular up to 0.7 M [11]. This point out the specific role played
by the counter ion and existence of spherical and nonspher-

0927-7757/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.colsurfa.2005.02.018
96 D. Varade et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 259 (2005) 95–101
ical aggregates can be understood in terms of more or less
efficient repulsions between the polar groups at the micellar
surface. It is well known that salts such as KBr and sodium
salicylate (NaSal) induce pronounced growth of CTABr mi-
celles due to charge neutralization at the micellar surface by
these salts [12,13]. The counter ion distribution or conden-
sation and size of the ionic micelles play an important role
to decide the effect of salt on the micellar systems [14]. We-
ican et al. [15] by means of laser light scattering, 1 H NMR
measurements and fluorescence probe reported that CTABr
forms rod-like micelles at 0.1 mol L−1 KBr and the worm
like micelles are formed at above 0.2 mol L−1 KBr.
In this paper we have reported systematic studies on influ-
ence of NaCl and NaBr salt on the micellization and struc-
ture of the micelles in cetylpyridinium chloride (CPyCl) so-
lution as studied by surface tension, conductance, viscos-
ity, dynamic light scattering (DLS) and small angle neutron
scattering (SANS) measurements. The results are interpreted
in terms of counter ion condensation on the ionic micelles,
which depends on the hydrated size of the counter ions.
2. Materials and methods
The cationic surfactant cetylpyridinium chloride (CPyCl),
salt NaCl and NaBr were highly pure samples purchased from
Fluka, Switzerland and were used as received. Triply distilled
water from an all Pyrex glass apparatus was always used for
the preparation of solutions for surface tension, conductance
and viscosity measurements. For DLS measurement Milli-Q
water having specific resistance 18.2 M cm was used. The
samples for SANS experiments were prepared in D2 O.
2.1. Conductance
Conductometric measurements were made with a digital
conductivity meter (Phillips, India) using a dip-type cell. All
measurements were done in a jacketed vessel, which was
maintained at the appropriate temperature (±0.1 ◦ C). The er-
rors in the conductance measurements were within ±0.5%.
The conductance was measured after thorough mixing and
temperature equilibrium at each dilution.
2.2. Surface tension
The surface tension of CPyCl solutions in absence and
presence of salts was measured by drop weight method using
a modified stalagmometer [16].
2.3. Viscosity
The viscosity measurements were carried out using an
Ubbelohde suspended level capillary viscometer. The vis-
cometer was always suspended vertically in a thermostat with
a temperature stability of ±0.1 ◦ C in the investigated region.
The viscometer was cleaned and dried every time before each
measurement. The flow time for constant volume of solution
through the capillary was measured with a calibrated stop-
watch.
2.4. Dynamic light scattering
DLS measurements were performed using a Malvern 4800
Autosizer employing 7132 digital correlator. The light source
was argon ion laser operated at 514.5 nm with a maximum
output power of 2 W. The average decay rate (Γ ) of the elec-
tric field autocorrelation function, g1 (τ), was estimated us-
ing the method of cumulants. The apparent diffusion coef-
ficients (D) of the micelles were obtained from the relation
Γ = Dq2 (q is the magnitude of the scattering vector given
by q = [4πn sin(θ/2)]/λ, n being the refractive index of the
solvent, λ, the wavelength of laser light and θ is the scatter-
ing angle) and the corresponding hydrodynamic diameters
(d) were calculated using the Stokes–Einstein relationship.
For all the solutions, Γ varies linearly with ‘q2 ’ indicating
translational diffusion of the scatterers.
2.5. Small angle neutron scattering
For SANS measurements, the sample solutions were pre-
pared in D2 O. The use of D2 O as solvent instead of H2 O
provides better contrast in neutron scattering experiments.
In all the measurements, CPyCl concentration (0.25 M) and
temperature (30 ± 0.1) ◦ C were kept constant. The solutions
were held in a quartz cell of 0.5 cm thickness with tight-fitting
Teflon stoppers. The SANS experiments were performed us-
ing a SANS diffractometer at the Dhruva reactor, BARC,
Trombay [17]. The diffractometer uses a polycrystalline BeO
filter as a monochromator. The mean wavelength of the in-
cident neutron beam is 5.2 Å with a wavelength resolution
( λ/λ) of approximately 15%. The angular distribution of
the scattered neutron was recovered by a linear 1 m long He3
position sensitive detector (PSD). The data were recorded in
the Q range of 0.02–0.24 Å−1 . All the measured SANS distri-
butions were corrected for the background and solvent con-
tributions and the data were normalized to the cross-sectional
unit using standard procedures [17].
3. Results and discussion
Conductivity measurements were performed in water for
CPyCl at various temperatures (30–60 ◦ C at an interval of
10 ◦ C) in order to evaluate the CMC and the degree of counter
ion dissociation, β. The plots of conductance data are pre-
sented as specific conductance versus concentration in Fig. 1.
The values of CMC and β at various temperatures for CPyCl
solution are recorded in Table 1. The values of CMC and
β increase with temperature in the range investigated. The
effect of temperature on the CMC of surfactants in aqueous
solution is usually analyzed in terms of two opposing factors.
First, as the temperature increases the degree of hydration of
 D. Varade et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 259 (2005) 95–101 97

Table 1
The CMCs, degree of counter ion dissociation (β), standard molar Gibbs energies ( G◦ ), enthalpies ( H◦ ) and entropies ( S◦ ) of micellization for CPyCl in
water at different temperatures
Temperature (K) CMC (mM) β G◦ (kJ mol−1 ) H◦ (kJ mol−1 ) S◦ (kJ mol−1 )
303.2 0.98 0.41 −27.59 −10.17 0.057
313.2 1.11 0.43 −28.17 −10.85 0.055
323.2 1.30 0.45 −28.65 −11.55 0.053
333.2 1.45 0.46 −29.23 −12.28 0.050

the hydrophilic group decreases, which favors micellization; Fig. 2. The slope in the plot was taken as [(∂ln XCMC )/∂T].
however, an increase in temperature also causes the disrup- The standard molar entropy of micelle formation ( Sm◦ ) was

tion of the water structure surrounding the hydrophobic group
and this is unfavorable to micellization. It seems from the data
in Table 1 that this second effect is predominant in the tem-
perature range studied. On the other hand, β, also increases
regularly with temperature increase. This observed increase
in β is probably due to a decrease in the charge density at the
micellar surface caused by the decrease in the aggregation
number of the micelle.
The CMC values, as determined at various temperatures,
were further used for calculation of the thermodynamic pa-
rameters of micellization. In the charged pseudo-phase model
of micelle formation, the standard free energy of micelle for-
mation per mole of surfactant is given by
G◦m = (2 − β)RT ln XCMC
where R is the gas constant, T is the temperature in Kelvin
scale and XCMC stands for the CMC in the mole fraction unit.
The standard enthalpy of micelle formation ( Hm◦ ) can be
derived by the van’t Hoff equation

 
∂ ln XCMC
Hm◦ = −(2 − β)RT 2 (2)
∂T
The enthalpy of micellization can be obtained if the de-
pendence of the CMC on temperature is known. One can see
that the standard enthalpy of micelle formation is more neg-
ative or exothermic on higher temperature side. A linear plot
was observed of ln XCMC against T for CPyCl as shown in
calculated from


◦ Hm◦ − G◦m
Sm = (3)
T
The entropy change is positive in all cases. However, it
decreases with increasing temperature. The thermodynamic
parameters of micellization obtained by following the above
procedure are summarized in Table 1.
The surface tension (γ) of CPyCl solutions in absence and
presence of NaCl and NaBr was measured for a range of con-
centrations above and below the critical micelle concentration
(CMC). As shown in the Fig. 3 (for NaCl), a linear decrease
(1) in surface tension was observed with increase in surfactant
concentrations up to the CMC, beyond which no considerable
change was noticed. The electrical atmosphere in the aqueous
surfactant solution altered in presence of NaCl which neutral-
izes the effective head group charge resulting in reducing the
electrostatic repulsion between the polar head groups and the
micelles are formed at much lower concentration as compared
to that in pure water. The CMC of the surfactant decreased
in the presence of NaCl and NaBr, the decrease being de-
pendent upon the concentration of added salt. The effect was
more pronounced in case of NaBr. The area occupied by the
surfactant molecules in Å2 , at the air–water interface at satu-
ration monolayer was estimated using the surface tension (γ)

Fig. 1. Plots of specific conductivity vs. concentration of CPyCl in water at

different temperatures. Fig. 2. Plots of ln XCMC vs. temperature for CPyCl in water.
98 D. Varade et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 259 (2005) 95–101

Fig. 3. Plots of surface tension vs. log CPyCl concentration in absence and Fig. 4. Relative viscosity vs. concentration of CPyCl in absence and presence
presence of varying amount of NaCl at 30 ◦ C. of NaCl concentration at 30 ◦ C.

data at temperature T and the Gibbs adsorption isotherm:

 
1 dγ
Γs − (4)
nRT d ln C
where Γ s is surface excess, R is the universal gas constant,
C is the concentration of the surface active compound and
n is taken as 2 because of the ionic nature of the surfactant.
Interfacial properties of CPyCl in water at 30 ◦ C are recorded
in Table 2.
The viscosity measurement for micellar solution of CPyCl
were made in absence and presence of NaCl and NaBr at
30 ◦ C in order to study the transition of micelle shape induced
by the change in ionic strength. The results obtained in NaCl
were quite interesting (Fig. 4). CPyCl shows a gradual in-
crease in viscosity with increase in concentration in absence Fig. 5. Variation of hydrodynamic diameter of 0.25 M CPyCl in varying salt
of NaCl. But the electrical atmosphere in the aqueous sur- concentration at 30 ◦ C.
factant solution is profoundly altered by the added NaCl and
this is turn influences the viscous flow of CPyCl. Initially, crease in viscosity at low salt concentration followed by a
the solution of CPyCl becomes less viscous with increase in dramatic increase at high salt concentration. CPyCl shows
the concentration in presence of lower NaCl concentration, an increase in viscosity (figure not shown) at much lower
but a dramatic increase in viscosity was observed in presence concentration of NaBr (0.2 M) as compared to NaCl (1.0 M).
of 1.0 M NaCl. This is evidently an indication of decrease The changes in the aggregation behavior of CPyCl mi-
in the electrostatic interaction between micelles which will celles in presence of NaCl and NaBr can be inferred from
be reflected as a decrease in the “effective volume fraction” DLS measurements. The apparent hydrodynamic diameter
in the presence of low NaCl concentration [19]. From the (d) of the micelles in presence of different amounts of NaCl
above results we can conclude that only above a certain salt and NaBr are depicted in Fig. 5. Considering the ionic nature
concentration there is a transition from globular to rodlike of the surfactant, in the absence of any salt, the measured
micelles. Almgren and coworkers [20] has also studied the diffusion coefficients will be modified due to the presence of
effect of varied NaCl concentration on the relative viscosity repulsive intermicellar interactions. Such repulsive interac-
of hexadecyltrimethylammonium bromide (CTABr, 25 mM) tions will lead to an increase in the diffusion coefficient and
solution, in which they have reported the similar initial de- hence a decrease in the apparent diameter of the micelles.

Table 2
Interfacial properties of CPyCl in water at 30 ◦ C
Surfactants CMC (mM) C␲ = 20 (mM) γ CMC (mN m−1 ) Area/molecule (Å2 )
Experimental Literature [reference]
CPyCl 0.95 1.00 [18] 0.5 42.0 42.0
 D. Varade et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 259 (2005) 95–101
Thus, the observed diameter of the micelles in the absence of
salts will be slightly underestimated as no account of inter-
particle interaction has been taken into consideration. This
is evident from the smaller diameter of micelles (2 nm) as
compared to that expected from the length of hydrocarbon
chain of the surfactant (3.2 nm). With addition of salts, an in-
crease in the apparent diameter of the micelles from ∼2 nm
to ∼8 nm is observed suggesting an increase in size of the
micelles. This observed change in apparent size arises from
both decrease of intermicellar interaction and growth of the
micelles. Considering large changes in the relative viscosity
of the solution with addition of salt, a prolate ellipsoidal or
rod-like growth of the micelles can be envisioned. The ob-
served micellar growth is significantly different for NaCl and
NaBr. In presence of NaCl, the apparent diameter reaches a
value of 8 nm at a salt concentration of 1.2 M while the same
effect could be observed for NaBr even at 0.2 M. This sug-
gests that the nature of the condensation of counter ions on
the micelle surface is different for Cl− and Br− .
In SANS experiments one measures the differential scat-
tering cross-section per unit volume (dΣ/dΩ) as a function of
scattering vector Q. For a system of monodisperse interacting
micelles (dΣ/dΩ) is given by [21]
dΣ
(Q) = n(ρm − ρs )2 V 2 [F (Q)2 
dΩ
+F (Q)2 (S(Q) − 1)] + B
where n denotes the number density of the micelles, ρm and ρs
are, respectively, the scattering length densities of the micelle
and the solvent and V is the volume of the micelle. F(Q) is the
single particle form factor and S(Q) is the interparticle struc-
ture factor. B is a constant term that represents the incoherent
scattering background, which is mainly due to hydrogen in
the sample.
The micelles formed at the CMC are spherical. If the so-
lution conditions (e.g., concentration, ionic strength, etc.) of
the micellar solutions are changed that favors the growth of
the micelles, they grow along one of the axial directions of
the micelles. The growths of the micelles along other two
axial directions are restricted by the length of the surfactant
molecule to avoid the energetically unfavorable any empty
space or water penetration inside the micelle [22,23]. The
prolate ellipsoidal shape (a = b = c) of the micelles is widely
used in the analysis of SANS data because it also represents
the other different possible shapes of the micelles such as
spherical (a = b) and rod-like (a b). For such an ellipsoidal
micelle
 1
F 2 (Q) = [F (Q, µ)2 dµ] (6)
0 the fractional charge have been determined from the anal-
 2
1
F (Q)2 = F (Q, µ) dµ
0 SANS data. The aggregation number is calculated by the
3(sin x − x cos x)
F (Q, µ) =
x3
99
1/2
x = Q[a2 µ2 + b2 (1 − µ2 )] (9)
where a and b are, respectively, the semimajor and semiminor
axes of the ellipsoidal micelle and µ is the cosine of the angle
between the directions of a and the wave vector transfer Q.
In general, micellar solutions of ionic surfactants show
a correlation peak in the SANS distribution [24]. The peak
arises because of the corresponding peak in the interparticle
structure factor S(Q) and indicates the presence of electro-
static interactions between the micelles. S(Q) specifies the
correlation between the centers of different micelles and it
is Fourier transform of the radial distribution function g(r)
for the mass centers of the micelle. Unlike the calculation of
P(Q), it is quite complicated to calculate S(Q) for any other
shape than spherical. This is because of S(Q) depends on the
shape and as well as on the orientation of the particles. To
simplify this, prolate ellipsoidal micelles are assumed to be
equivalent spherical. We have calculated S(Q) as derived by
Hayter and Penfold [25] from the Ornstein–Zernike equa-
tion and using the mean spherical approximation. The mi-
celle is assumed to be a rigid equivalent sphere of diameter
σ = 2(ab2 )1/3 interacting through a screened Coulomb poten-
tial, which is given by
exp[−κ(r − σ)]
u(r) = u0 σ , r > σ, (10)
r
(5) where κ is the Debye–Huckel inverse screening length and is
calculated by

1\2
8πNA e2 I
κ= (11)
103 εkB T
defined by the ionic strength I of the solution
I = CMC + 21 αC + Cs, (12)
where I is determined by the CMC, dissociated counter ions
from the micelles and the salt concentration. The fractional
charge α (=Z/N, where Z is the micellar charge) is the charge
per surfactant molecule in the micelle and is a measure of
the dissociation of the counter ions of the surfactant in the
micelle. C and Cs present the concentrations of the surfactant
and salt in the solution, respectively. The contact potential u0
is given by
Z 2 e2
u0 = (13)
πεε0 σ(2 + κσ)2
where ε is the dielectric constant of the solvent medium, ε0
is the permittivity of free space and e is the electronic charge.
The dimensions of the micelle, aggregation number and
ysis. The semimajor axis (a), semiminor axis (b = c) and
the fractional charge (α) are the parameters in analyzing the
(7)
relation N = 4πab2 /3v, where v is the volume of the sur-
factant monomer. Throughout the data analysis corrections
(8)
were made for instrumental smearing [26]. The parameters
100 D. Varade et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 259 (2005) 95–101

Table 3
Micellar parameters from 0.25 M CPyCl in presence of varying NaCl and NaBr concentration at 30 ◦ C
Salt [Salt] (M) Aggregation number, N Fractional charge, α Semiminor axis, b = c (Å) Semimajor axis, a (Å) Axial ratio a/b
NaCl 0.0 104 0.2 18.1 44.3 2.4
0.1 113 0.2 18.7 45.3 2.4
0.5 131 0.2 19.5 48.4 2.5
1.0 229 0.2 18.4 94.4 5.1
NaBr 0.1 139 0.2 19.2 52.7 2.7
0.2 368 0.07 19.5 136.0 7.0

in the analysis were optimized by means of nonlinear least-
square fitting program and the errors of the parameters were
calculated by the standard methods used [27].
Figs. 6 and 7 show the SANS data from 0.25 M CPyCl
micellar solution with and without the addition of salt NaCl
and NaBr at temperature 30 ◦ C, respectively. The SANS dis-
tribution from a pure 0.25 M CPyCl shows a well defined
peak at the wave vector transfer Q ∼ 0.076 Å−1 . This cor-
Fig. 6. SANS data from 0.25 M CPyCl micellar solution with varying con-
centration of NaCl.
relation peak is an indication of strong repulsive interaction
between the positively charged CPyCl micelles. The peak
usually occurs at Qm ∼ 2π/d, where d is the average distance
between the micelles and Qm is the value of Q at the peak
position. As shown in the figure cross-section increases and
the peak position shift to lower Q values with the increase in
the salt concentration. This reflects the increase in the size of
the micelles in the presence of salt [7,14]. The broadening of
the correlation peak is due to screening of charge by the salt
between the micelles. The micellar parameters obtained for
these systems are given in Table 3.
It is seen that in case of NaCl the fractional charge on
the micelle remains nearly same but the aggregation num-
ber increases when the NaCl concentration in the micellar
solution is increased. This indicates that the counter ion has
equal affinity to stay in water as well as condense on the
micelles. For the same concentration of the salt NaCl and
NaBr, the charge neutralization on the ionic CPyCl micelles
is different for these salts, and this leads to the formation of
different micellar structures when NaCl and NaBr are added.
For example the aggregation number of CPyCl micellar so-
lution increases from 104 to 229 upon addition of 1 M NaCl;
while aggregation number increases upto 368 by the addi-
tion of only 0.2 M NaBr. These results are well supported by
viscosity and DLS measurements discussed earlier.
The charge neutralization at the surface of the micelle by
the increase in the counter ion condensation decreases the
effective head group area for the surfactant monomer to oc-
cupy in the micelle and hence the increase in the aggregation
number of the micelle. The difference in solution properties
of Br− and Cl− is that Cl− counter ions are more hydrated.
This suggests that the hydrated size of the counter ion similar
to the size of the micelle plays an important role to control
the properties of micellar solution. The comparison of the
micellar parameters in Table 3 suggests that counter ion con-
densation is more effective to neutralize the charge on the
micellar surface when the hydrated size is small. The solid
lines in Figs. 6 and 7 are fitted curves to the experimental
data using Eq. (5).

4. Conclusions

Fig. 7. SANS data from 0.25 M CPyCl micellar solution with varying con- We have studied the effect of added salt NaCl and NaBr
centration of NaBr. on micellization and structure of cetylpyridinium chloride
 D. Varade et al. / Colloids and Surfaces A: Physicochem. Eng. Aspects 259 (2005) 95–101
(CPyCl) micelles. It was found that the micelle size increases
with increasing salt concentration above a threshold value.
The observed micellar growth is significantly different for
NaCl and NaBr. The effect of NaBr on CPyCl micelles was
more pronounced in comparison to NaCl. The results are
interpreted based on the dependence of the counter ion con-
densation.
Acknowledgements
Financial assistance from IUC-DAEF Project No.
IUC/CRS-M-103/2001 and help from J. Mata for DLS mea-
surements is gratefully acknowledged.
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