`

Vol. 2(1), pp.10-17, November 2013

Available online at http://www.accessinterjournals.org/ajps
ISSN 2354-2438 Copyright 2013 Access International Journals





Full Length Research Paper

Micellization behaviour of cetyltrimethylammonium
bromide in methanol-water mixed solvent media in
absence and in the presence of a salt at (308.15, 318.15
and 323.15) K by conductometry

Sujit K. Shah, Sujeet K. Chatterjee and Ajaya Bhattarai

Department of Chemistry, M.M.A.M.C (Tribhuvan University), Biratnagar, Nepal.
Corresponding author. E-mail: bkajaya@yahoo.com

Accepted 11 November, 2013

Accurate measurements on the specific conductivity of solutions of cetyltrimethylammonium bromide
in absence and in the presence of potassium chloride in methanol-water mixed solvent media
containing 0.10, 0.20, 0.30 and 0.40 volume fractions of methanol at 308.15, 318.15 and 323.15 K are
reported. The concentrations of cetyltrimethylammonium bromide are varied from 4.010
-5
to 1.210
-2
mol.l
-1
.
.
The conductance of cetyltrimethylammonium bromide decreases with addition of methanol. It
has been observed that the conductance of cetyltrimethylammonium bromide increases with increase
in concentration as well as with addition of salt (KCl). The concentrations of KCl are taken 0.0001, 0.001
and 0.01 M during the experiments. The result shows that critical micelle concentration of
cetyltrimethylammonium bromide increases with addition of methanol and with rise of temperature.
Also, the critical micelle concentration of cetyltrimethylammonium bromide decreases with addition of
potassium chloride.

Key words: Cetyltrimethylammonium bromide, methanol-water mixed solvent media, potassium chloride,
critical micelle concentration, conductivity.


INTRODUCTION

Surfactants are class of compounds having applications
in different fields (Schramm et al., 2003). The quaternary
ammonium salts are known for their germicidal and
antifungal properties (Zhao and Sun, 2008; Chlebicki et
al., 2005); there is also a possibility of employing cationic
amphiphiles as vectors in gene delivery (Joestor et al.,



`




2003; Srinivas et al., 2009). The critical micelle
concentration (cmc) appears to be the most important
property in the study of micellization of surfactants and
the two models commonly employed in the theoretical
thermodynamic treatment of micelles, namely the mass
action model and the phase separation model both
required the knowledge of the critical micelle
concentration (cmc) which is often obtained from the
abrupt change in the physical property-concentration
curve (Tanford, 1980). Surfactants are used in the
presence of additives in order to improve their properties.
Among the very large number of additives revealed by a
literature survey, alcohols hold a special place, being by
far the most, frequently used. This has been especially so
in recent years because alcohols are the most common
cosurfuctants which are added to surfactant + oil systems
to generate microemulsions (Zana, 1995).
Comprehensive studies have been done on
physicochemical behaviour cetyltrimethylammonium
bromide (CTAB) in aqueous polyethylene glycol media
(Manna and Panda, 2011) and other alcohols (Li et al.,
2006; Akbas and Kartal, 2006). The gradual replacement
with water and other polar solvents allows one to explore
a wide bulk phase polarity range and its influence on
micellization. Addition of small amount of an organic
solvent has been known to produce marked changes, in
the critical micelle concentration (cmc) of ionic
surfactants due to tendency of added organic solvent
either to break or make the water structure through
solvation of the hydrophobic tail of the surfactant by the
hydrocarbon part of the organic solvent (Palepu et al.
1993; Ruiz, 1999). Akbas and Kartal (2006) carried out
an investigation on the effect of ethanol and ethylene
glycol on the critical micelle concentration (cmc) of CTAB.
They observed that cmc decreases upon the addition of
ethanol and ethylene glycol. In spite of these literatures,
the effect of methanol is not seen so far.
Interactions of foreign ions with the chromophoric
groups of amphiphilic compounds are of interest in
several areas of chemistry and biochemistry, where it has
been established that neutral salts can influence the
conformation of proteins and other macromolecules by
affecting the prevalent of hydrophobic or ionic
interactions. Such processes can usually be explained by
invoking the breaking up of the water structure around
the amphiphilic compounds due to lyophilic electrolytes
(Vijlder, 1985). Comprehensive studies on the effect of
electrolytes on ionic surfactants in n-Butanol, n-Pentanol
and n-Hexanol are found in literature (Singh et al., 1979).
Many techniques have been used in order to investigate
the effect of added salt on the micellization of ionic
surfactants solution (Aswal and Goyal, 2002; Simmonic
and Span, 1998).
Shah et al. 11



The effect of inorganic salt is explained in terms of the
shielding of the electrostatic repulsion by the counterions
(Miyagishi, 1974; Chung et al., 1991). The effect of KCl
and alcohol on the cmc of cetylpyridinium chloride (CPC)
was studied by Chung et al. (1991). They observed the
decrease in cmc with the addition of electrolyte and vice
versa. In this paper, we report a study of the aggregation
process of CTAB at three different temperatures in
absence and in the presence of KCl by conductivity
method in methanol water mixed solvent media.


MATERIALS AND METHODS

Methanol (E. Merck, India, 99% pure) was distilled with
phosphorous pentoxide and then redistilled over calcium
hydride. The purified solvent had a density of 0.7772
g.cm
-3
and a co-efficient of viscosity of 0.4742 mPa.s at
308.15 K; these values are in good agreement with the
literature values (Apelblat, 2011).

Triply distilled water
with a specific conductance less than 10
-6
S.cm
-1
at
308.15 K was used for the preparation of the mixed
solvents. The physical properties of methanol-water
mixed solvents used in this study at 308.15, 318.15, and
323.15 K are reported in Table 1 have been taken from
the published papers(Bhattarai et al. 2006, 2011;
Chatterjee and Das, 2006). The relative permittivity of
methanol-water mixtures at the experimental
temperatures were obtained by regressing the relative
permittivity data as function of solvent composition from
the literatures (Albright and Gasting, 1946; Yilmaz and
Guler, 1998) and are included in Table 1.
Cetyltrimethylammonium bromide was purchased from
Loba Chemical Private Limited India and it was
recrystallised several times until no minimum in the
surface tension-concentration plot was observed and its
critical micellar concentration (cmc) agreed with the
literature value (Chakraborty et al., 2006).
Potassium chloride (KCl) was purchased from Loba
chemical, India and dried before use.
The conductivity values of CTAB in methanol-water in
absence and in presence of KCl were determined by
conductometric method using digital conductivity meter
from Systronics India Ltd with dip type conductivity cell
having cell constant 1.002 cm
-1
and having an uncertainty
of 0.01%. The cell was calibrated by the method of Lind
et al. (1959) using aqueous potassium chloride solution.
The measurements were made in a water bath
maintained within 0.01 K of the desired temperature.
Several independent solutions were prepared and runs
were performed to ensure the reproducibility of the
results.
The solutions were prepared by weight using analytical



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Adv. J. Phys. Sci. 12



Table 1. Properties of methanol-water mixtures containing 0.10, 0.20, 0.30 and 0.40 volume
fraction of methanol at (308.15, 318.15, and 323.15) K.

T/K
0
/g.cm
-3

0
/ mPa.s D
0.10 volume fraction of methanol
308.15 0.97973 0.8665 71.57
318.15 0.97604 0.7017 68.18
323.15 0.97438 0.6375 66.45

0.20 volume fraction of methanol
308.15 0.96632 1.0217 68.14
318.15 0.96162 0.8075 64.80
323.15 0.95875 0.7300 63.15

0.30 volume fraction of methanol
308.15 0.95160 1.1418 64.25
318.15 0.94626 0.8957 60.99
323.15 0.94331 0.8052 59.41

0.40 volume fraction of methanol
308.15 0.93364 1.2034 60.34
318.15 0.93140 0.9309 57.18
323.15 0.92800 0.8288 55.62



balance with the accuracy of 1 10
-4
g.


RESULTS AND DISCUSSION

Conductivity technique has been found to be highly
useful for studying the association behaviour of various
systems (Fujiwara et al., 1997; Moulik et al., 1996;
Gonzalez-Perez et al., 2002, 2003). Specific
conductivities of surfactant solutions were measured as a
function of concentrations of CTAB in methanol-water
mixed solvent media containing 0.10, 0.20, 0.30 and 0.40
volume fractions of methanol in absence and in the
presence of KCl at (308.15, 318.15 and 323.15) K. The
cmcs were obtained from the inflections in the plots of
specific conductivity versus surfactant concentration. The
data points above and below the inflection were fitted to
two linear equations, and the cmcs were obtained from
the common intersection. This method is found to be
reliable and convenient for the present system because
of the significant variations of specific conductivity with
surfactant concentration in the pre- and postmicellar
regions which allowed us to draw two unambiguous
straight lines above and below the cmc. A typical plot of
specific conductivity () vs. concentration of CTAB in 0.1
volume fraction of methanol at 308.15 K is presented in
Figure 1.
The effect of water-alcohol mixed solvent media can be
found to play important roles in different research fields
(Prasad and Singh, 1990; Akbas and Kartal, 2006; Li et
al. 2005; Manna and Panda, 2011; Gutmann and Kertes,
1974; Zana et al., 1980). There has been less work done
particularly in methanol-water system. When methanol is
mixed with water, several physical properties such as
density, viscosity, surface tension, relative permittivity are
changed due to molecular interactions (Carr and Riddick,
1951; Mikhail and Kimel, 1961). The cmc values of CTAB
in methanol-water mixed solvent media containing 0.10,
0.20, 0.30 and 0.40 volume fractions of methanol in
absence and in the presence of KCl at 308.15, 318.15
and 323.15 K are listed in Table 2.
Figure 2 shows that increase in volume fraction of
methanol in water results in increase in cmc values. The
alcohol added to a micellar surfactant solution is
distributed between the micelles and the bulk solvent,
forming mixed micelles with the surfactant. When the
alcohol concentration increases the dielectric constant of
the mixture becomes lower and lower as a result of the
electrostatic interaction of the ionic head groups in
micelles. This is due to co-solvent effects on the



`
Shah et al. 13



0
100
200
300
400
500
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1.1 1.2
CONCENTRATION OF CTAB X10
-2
M
S
P
E
C
I
F
I
C

C
O
N
D
U
C
T
A
N
C
E

/

c
m
-
1


Figure 1. Plot of specific conductivity vs. concentraion of CTAB in 0.1 volume
fraction of methanol at 308.15 K.



1
3
5
7
9
0 0.1 0.2 0.3 0.4 0.5
323.15 K
318.15 K
308.15 K
Volume Fractions of Methanol-Water
C
M
C

(
m
M
)


Figure 2. Variation of cmc with different volume fractions of methanol-water
at (308.15, 318.15 and 323.15) K.



interactions and on the property of solvent. The addition
of cosolvent changes the dielectric constant of solvent
and the degree of structuring. The more cosolvent is
added, the lower is the dielectric constant of the mixtures
and the micelles expand. The cosolvent molecules at the
micelle/solution interface lower the repulsion between



`
Adv. J. Phys. Sci. 14



Table 2. The critical micellar concentration (cmc) values of cetyltrimethylammonium bromide in absence
and in the presence of KCl from conductometry in methanol-water mixed solvent media containing 0.10,
0.20, 0.30 and 0.40 volume fraction of methanol at (308.15, 318.15, and 323.15) K.

Methanol %
Concentration
KCl /M
Critical Micellar Concentration(cmc)/mM
308.15 K 318.15 K 323.15 K
0.10 volume fraction of methanol
0.0000 1.37 1.68 1.79
0.0001 1.32 1.54 1.70
0.0010 1.10 1.22 1.40
0.0100 0.89 0.94 1.18

0.20 volume fraction of methanol
0.0000 1.80 2.63 2.81
0.0001 1.75 2.53 2.68
0.0010 1.13 2.48 2.58
0.0100 1.07 1.98 2.03

0.30 volume fraction of methanol
0.0000 4.60 5.75 5.81
0.0001 4.50 5.47 5.61
0.0010 4.19 5.42 5.56
0.0100 3.14 5.04 5.23

0.40 volume fraction of methanol
0.0000 7.21 7.49 7.71
0.0001 6.42 7.18 7.20
0.0010 6.19 6.87 6.97
0.0100 4.73 6.78 6.87



CTA
+
head groups due to an increase in the ionic
strength of the bulk phase (Vijlder, 1985). Furthermore,
with the increase in cosolvent concentration, the
hydrophobic interaction between hydrophobic groups of
surfactants is gradually reduced (Ray, 1971), that is, the
micellization potential decreases.
An increase in the volume fraction methanol results in
increase in the viscosity of the medium which eventually
results in the increase in the hydrophobic hydration of the
CTAB; hence the surfactant monomer would prefer to
remain in the bulk than to form the micelle. Moreover, it is
illustrated that presence of methanol decreases the
number of hydrogen bonds between the water molecules
(Farhadian and Shariaty-Niassar, 2009) due to which the
hydrophobic repulsion decreases. Li et al. (2005) studied
the effect of ethanol-water mixed solvent media and
concluded that there is significant increase in the cmc of
CTAB with increase in volume fraction ethanol. Ghosh
and Baghel (2008) carried out investigation on the
micellar properties of benzyldimethyldodecylammonium
bromide in aquo-organic solvent media and discussed
that the addition of organic solvent to water decrease the
dielectric constant and increase the cmc value with
increase in volume fraction of methanol.
It is clear from the Table 2 and Figure 3 that on
increasing the temperature, cmc increases. The effect of
temperature on the micellization is usually discussed in
terms of two opposite factors. First, as the temperature
increases, the degree of hydration of the hydrophilic
group decreases, which favors micellization; however, an
increase in temperature also causes the disruption of the
water structure surrounding the hydrophobic group and
this is unfavorable to micellization. It seems from the data
in Table 2 that this second effect is predominant in the
temperature range studied (Varade et al., 2005). The
value of cmc increases with increase in temperature,
such behavior is also observed by Dubey (2008).
From the data of Table 2, the cmc of the surfactant
CTAB decreases with increasing salt concentration and
the decrease of the cmc with increasing salt
concentration follows the Shinoda equation (Shinoda,
1953) which represents the total counter ion binding to
the micelle at the cmc, that is:

log cmc = A B log(cmc + [KCl]) (1)

where A and B are constants. The plot of log cmc against
log (cmc +[KCl]) is shown in Figure 4. The results of plot



`
Shah et al. 15



3
6
9
305 310 315 320 325
0.4 volume fration of methanol
0.3 volume fraction of methanol
0.2 volume fraction of methanol
0.1 volume fraction of methanol
T / K
C
M
C

/

m
M


Figure 3. Variation of CMC with temperature at different volume fractions of
methanol water.



-3.3
-3.0
-2.7
-2.4
-2.1
-1.8
-3.0 -2.7 -2.4 -2.1 -1.8 -1.5
0.4 volume fraction of methanol
0.3 volume fraction of methanol
0.2 volume fraction of methanol
0.1 volume fraction of methanol
Log ( cmc + [KCl] )
L
o
g

c
m
c


Figure 4. Plot of log (CMC+[KCl]) vs log CMC in different volume fractions of methanol-
water at 308.15 K.


in Figure 4 are listed in Table 3. The correlation
coefficients of fits (as r
2
) are higher than 0.900 numerical
value. Hence, the fitting of the data looks good. It Is seen
that the cmc values of CTAB in 0.1, 0.2, 0.3 and 0.4
volume fractions of methanol solution decreases with
increase of KCl concentration. As the salt is added, the



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Adv. J. Phys. Sci. 16



Table 3. Linear Regression Analysis of the cmc: The correlation
coefficients of fits (as r
2
) and A and B are constants in methanol-
water mixed solvent media containing 0.10, 0.20, 0.30 and 0.40
volume fraction of methanol at 308.15 K.

Volume fraction of methanol A B r
2

0.1 -3.40 0.174 0.913
0.2 -3.25 0.269 0.993
0.3 -3.13 0.331 0.991
0.4 -3.01 0.375 1.000



electrostatic repulsive force between ionic head groups of
the surfactant molecules is reduced by shielding of
micelle charge, so that spherical micelles are more
closely packed by the surfactant ions (Aswal and Goyal,
2002; Shinoda, 1953), hence a decrease in the cmc
values after adding 0.0001, 0.001 and 0.01 M
concentrations of KCl.


CONCLUSIONS

The effects of concentration, temperature and solvent
composition on the conductance of CTAB in absence and
presence of KCl in methanol (1) + water (2) mixed solvent
media have been studied by measuring specific
conductance through conductometric method. The
following conclusions have been drawn from the results
and discussion. The specific conductivities are found to
increase with increase in concentration over the entire
concentration range investigated whereas the specific
conductivities of CTAB decrease with increase in volume
fraction of methanol. Also, the specific conductivities of
CTAB in presence of KCl are found more than in absence
of KCl in methanol-water mixed solvent media. The cmc
of CTAB increases with increase in temperature and with
increase in volume fractions of methanol and cmc
decreases with addition of KCl in methanol-water mixed
solvent media.


ACKNOWLEDGEMENTS

One of the authors (Sujit Kumar Shah) is thankful to
University Grants Commission for financial support in
order to pursue the Ph.D. work. The authors are thankful
to the faculties of Central Department of Chemistry,
Tribhuvan University, Kirtipur, Nepal for valuable
suggestions during the research works. The authors are
also thankful to Associate Professor Ghanashyam
Shrivastav, the Head of Department of Chemistry,
Mahendra Morang Adarsh Multiple Campus, Tribhuvan




University, Biratnagar, Nepal for providing us the
research facilities to conduct this research work.
Especially Sujit Kumar Shah is highly obliged of Honble
Geeta Didi and her learned team members, Brahma
Kumaris Meditation Centre, Biratnagar, Nepal, for
inspiration and guidance.


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