International Journal of Scientific & Engineering Research, Volume 6, Issue 1, January-2015 1508

ISSN 2229-5518

Micellization Behavior and Thermodynamic

Properties of N-Alkyl Trimethylammonium Bromide
Surfactants in aqueous media at different
temperatures
Md. Manwarul Islam, Mohammad Rezaur Rahman *, Md. Nazrul Islam

Abstract - Knowledge of Micellar behavior of a surfactant is essential for its wide range of applications. Studies have been done on the micellar
behavior of some of the cationic surfactants individually, by different methods, which is not sufficient to correlate the trend of change of properties of the
surfactants in a particular series. A comprehensive study of Critical Micelle Concentration (CMC) and thermodynamic behavior of Tetradecyl
Trimethylammonium Bromide (TTAB), Hexadecyl Trimethyl ammonium Bromide (CTAB) and Octadecyl Trimethylammonium Bromide (OTAB) has been
herein conducted by conductivity measurements to represent the trend of micellar and thermodynamic properties of N-Alkyl Trimethylammonium
Bromide Surfactants, at different temperatures. The CMC studies have been utilized to evaluate the empirical relation (Stauff- Klevens rule), i.e. log
CMC= A – Bn, for this homologous series. It was found that the value of B of this relation changes from 0.283 to 0.271 with increase of temperature.
Thermodynamic parameters (the free energy, entropy and enthalpy of micellization) for these surfactants were calculated over the temperature range of
293K-328K. It was found that the free energy of micellization values become more and more negative whereas the entropy values becomes more
positive with increase of chain length of the surfactants. From the thermodynamic calculations it was found that the micellization processes of these
surfactants are enthalpy and entropy controlled.

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Index Terms - Cationic Surfactants, Counter ion binding, Critical micelle formation, Krafft temperature, Thermodynamic Parameters, Specific
conductivity, Stauff- Klevens rule
- - - - - - - - - - - - - ♦- - - - - - - - - - - - - -

1. INTRODUCTION portions can be exposed at the surface [1]. Thus a

surfactant molecule dissolves in water by a balance
Surfactants are extensively used in the field of interaction of the polar head group with water and the
detergents, paints, cosmetics and pharmaceutical tendency for water molecules to expel the nonpolar
industry for their typical structure which consists of a group. [2]. After a certain concentration of the surfactant
polar head group and a hydrophobic hydrocarbon in the system, micellization appears which is a delicate
chain. The polar head groups of ionic surfactants want balance between the hydrophobic interactions with in
to interact with water molecules and at the the alkyl chains and the opposing repulsive interactions
same times their hydrocarbon chains want to separate between the ionic head groups of an ionic surfactant
the water molecules, which cause an increase in energy [3],[4],[5],[6]. The opposing repulsive interactions
of the system. So the surfactant molecules present in the between the ionic head groups are greatly influenced
system arrange themselves so that the hydrocarbon (minimized) by the associated counter ions of the
surfactants [4], [7], [8]. Temperature influences the
————————————————
degree of counter ion binding which play an important
• Md. Manwarul Islam is a professor of Department of Chemistry. role on micelle formation. Thus micellization is greatly
Bangladesh University of Engineering and Technology, BUET. influenced by temperature, dielectric constant of the
Dhaka. Bangladesh medium and hydrogen bonding ability of the solvent [9].
• Mohammad Rezaur Rahman* is currently pursuing Ph.D in In the present work, efforts have been made to study
Chemistry in Bangladesh University of Engineering and the effect of chain length on the CMC of aqueous
Technology, BUET. Dhaka. Bangladesh. E-mail: solutions of N-Alkyl Trimethylammonium Bromide
[email protected]. Tel: + 88-01712799025 surfactant series at wider temperature variations. To
• Md. Nazrul Islam is a professor of Department of Chemistry. represent the series, aqueous solutions of Tetradecyl
Bangladesh University of Engineering and Technology, BUET. Trimethylammonium Bromide (TTAB), Hexadecyl
Dhaka. Bangladesh Trimethylammonium Bromide (CTAB) and Octadecyl
Trimethylammonium Bromide (OTAB) have been
studied by conductance measurements.

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The cmc values of these surfactants are compared to 4.0 x 10-3 M CTAB and 2.5 x 10-3 M OTAB solutions were
study the empirical relation, log CMC = A- Bn [3], which prepared in pure water. These solutions are cooled in a
will give important information for the trend of change refrigerator for 24 h at about 3oC to get precipitate of the
of solution behavior and other properties of the cationic hydrated surfactants. The conductivity of this solution is
surfactants in the homologous series. In addition, the measured with gradual increase of the temperature at a
thermodynamic parameters, ∆G m o, ∆S m o and ∆H m o have rate of about 1oC/ 10 min with constant stirring. For each
also been estimated and analyzed for these surfactants in temperature the conductivity of the solution was
aqueous media. Although the typical (amphipathic) checked for about 3 min until it reached a steady value.
structure of surfactants cause significant changes on a The T K value was obtained at the sharp break point of
large number of physical properties of the solutions such the conductivity vs. temperature plot.
as conductivity, viscosity, molecular fluorescence,
surface tension etc. which is the basis of applications of
the surfactants in many purposes but these applications 3. RESULTS AND DISCUSSIONS
for a surfactant becomes insignificant below a certain The experimental conductivities (κ) for CTAB in pure
temperature. Because below a certain temperature water at different temperatures are shown in fig.1. It is
solubility of the ionic surfactant becomes very limited observed that the κ shows a linear increase with gradual
and the surfactant loses its activities such as dispersing, increase of concentration of the surfactant which is due
emulsifying and micelle forming properties. [10], [11]. to the increase of surfactant monomers. The break in the
This certain temperature for a specific (ionic) surfactant plot (which represents micelle formation) is due to the
is known as the Krafft temperature (T K ) which is binding of some counter ions of the ionic surfactant.

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generally considered to be the melting temperature for
hydrated solid surfactant [12],[13],[14]. The present
study reveals that the Krafft temperature (T K ) of TTAB,
CTAB and OTAB is 12.7 oC, 24.7 oC and 36.5 oC
respectively which is consistent with the reference
values [3]. So in the present experiment, the temperature
160
298 K
range selected for CTAB is 298 K – 328 K and OTAB is 140
303 K
Specific conductance (µ Scm-1)

313 K- 328 K. 120

308 K
313 K
100 318 K
2. METHODOLOSY 323 K
80 328 K

2.1 Materials. The surfactant Tetradecyl trimethyl 60

ammonium bromide (TTAB), Hexadecyl 40

Trimethylammonium Bromide (CTAB) and Octadecyl 20
Trimethylammonium Bromide (OTAB) with purity 99%
0
were purchased from Sigma –Aldrich and were used as
received. For all solution preparation purposes double -20 0 20 40 60 80 100 120 140 160

distilled water was used. [CTAB] x 10-5 M

2.2 Methods. Conductivity was measured with a

Eutech–Cyber Scan–Con–510 conductivity meter
equipped with a temperature compensated cell (the cell
constant provided by the manufacturer is 1.0 cm-1).
Temperature of the solution was controlled by using a Fig.1.Specific conductance (κ) vs. Concentration of
circulating water bath (Haake B 3, Germany) with a CTAB at different temperatures.
precision of ± 0.1 K. The conductivity cell was calibrated
with KCl solutions of appropriate concentration range.
For Krafft temperature measurements 7.5 x 10-3 M TTAB,
In solution, the counter ions stabilize ionic surfactant groups [15].The degree of ionization, α was determined
micelles by binding to the micelle surface and screening by the ratio, S 2 /S 1 of the slopes above and below the
the electrostatic repulsions between the ionic head break point (i.e. post and pre micellization) [16],[17].
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The fraction of counter ion binding (β) was obtained CMC values are in agreement with the reported values
from the relation β= (1 - S 2 /S 1 ). Table 1 shows CMC and [3]. Both the CMC 1 and CMC 2 values for OTAB were
the fraction of Counter ion Binding (β) for TTAB, CTAB found to increase with increase of temperature.
and OTAB at Different Temperature. For TTAB and At each temperature The CMC values were found to
CTAB it was found that the CMC, in pure water, decrease with gradual increase of alkyl chain length of
gradually increases with increase of temperature up to a the N-Alkyl Trimethylammonium Bromide surfactants
certain range and then the CMC values slightly decrease which is due to the increased hydrophobicity.
with further increase of temperature. The initial increase The β values were found, from table 1, to decrease
in CMC for increased temperature is due to the thermal gradually with increase of temperature. This gradual
solubility of the surfactant monomers and a slight decrease of β with increase of temperature indicates that
decrease of the CMC with further increase of the degree of dissociation of the micelle increase with
temperature is due to dehydration of the head group, increase of temperature which is caused by the decrease
resulting an increase in the hydrophobic character, of aggregation number [19]. After a certain range (i.e.
which dominates over the solubility effect [18]. OTAB above 308 K), further increase of temperature causes a
was found to produce two CMCs; the first has low much greater
aggregation, while the second one is higher. The second

Table-1 CMC and the fraction of Counter lon Binding (B) for TTAB, CTAB and OTAB at Different Temperature.
T/K TTAB CTAB OTAB
10 CMC/M
3 β 10 CMC/M
3 β 10 CMC 1 /M
5 β1

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(104CMC2 /M) (β 2 )
293 3.20 0.70 -- -- -- --
298 3.43 0.69 0.84 0.70 -- --
303 3.67 0.68 0.89 0.69 -- --
308 4.02 0.67 0.93 0.68 -- --
313 4.01 0.64 0.97 0.67 2.02 0.58
(2.96) (0.70)

318 3.99 0.62 0.96 0.66 2.22 0.57

(3.08) (0.69)

323 3.97 0.60 0.95 0.65 2.30 0.56

(3.19) (0.68)

328 3.95 0.58 0.94 0.60 2.41 0.55

(3.27) (0.67)

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International Journal of Scientific & Engineering Research, Volume 6, Issue 1, January-2015 1511
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decrease of β for TTAB compared to the other two
surfactants, which indicates that the surface charge -2.4

density of TTAB aggregates decreased with increasing

-2.6
temperature by the way of enhanced counter ion 313 K
318 K
dissociation.[20]. At every certain temperature, it was -2.8 323 K
328 K
found that the surfactant with larger alkyl chain length

log CMC
-3.0
has greater counter ion binding (β) value. For OTAB, the
counter ion binding (β) of second micelle was found to -3.2

be greater than the first, suggesting increased surface -3.4

charge density of the later.
Log CMC vs. n (number of carbon in the alkyl chain of -3.6

the surfactants) plots at 313 K- 328K temperatures are 14 15 16 17 18

shown in figure 2. Because of poor solubility of OTAB in Carbon number in chain (N)

pure water below 309.5 K and higher chance of solvent

evaporation above 328 K, This temperature range is Fig.2 Effect of chain length on CMC of alkyl
selected for the comparison study. Linear relationship trimethylammonium bromide surfactants ( CMC 2 of
between the log CMC vs. n were obtained which shows OTAB is used).
that the micellization of N- Alkyl trimethyl ammonium
bromide surfactants follow the Stauff-Klevens empirical These comparison studies, for our selected surfactants,
rule, log CMC= A – Bn. The values for A and B of these were not possible below 313 K temperature, since the

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plots are also in good agreement with few of the Krafft temperature of CTAB and OTAB were found to be
reference values [3]. It was observed that both A and B higher than this temperature. Experimental results show
values for this series decrease at increased temperature. that T K of TTAB, CTAB and OTAB are 12.4oC, 24.7 oC
This represents that, within this temperature range, and 36.5 oC respectively.
CMC of smaller chain surfactants decrease where as
CMC of larger chain surfactant increases with the
480
increase of temperature.
Table -2 Constants for the Relation of: Log CMC = A-BN 460

of N-Alkyl Trimthylammonum Bromides at Different 440

Specific conductance (µ S cm-1)

temperatures. 420

400
Temperature A B
380

313 1.55 0.283 360

340

318 1.48 0.278 320

2 4 6 8 10 12 14 16 18
323 1.41 0.274 Temperature (oC)

328 1.36 0.271

Fig.3 Krafft temperature (T K ) of TTAB

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3.1 Thermodynamics of micellization of the molecules at higher temperature [26],[27]. So less energy
surfactants: The free energy (∆G m o) and the entropy is required to break the ice berg structure around the
(∆S m o) changes of micellization have been calculated hydrophobic alkyl chain.
from the following expressions [6], [15]:
On the other hand, although temperature is raised the
∆G m o = (1 + β) RT ln X CMC ……………………………(2) ∆S m o of micelle formation is positive and its value
decreases with increase of temperature.
∆S m o = - { δ ∆G m o / δT } P ……………………………….(3)

Then the enthalpy (∆H m o) of micellization have been

calculated from the following expression: -40

-42
∆G m o = ∆H m o - T∆S m o …………………………………(4)
-44
313 K
318 K
Here Xcmc is the mole fraction of the surfactant at the 323 K
CMC. Table 3 shows thermodynamic parameters of -46

∆Gmo/KJmol-1
328 K
TTAB, CTAB and OTAB, in pure water. In the present -48
experiment the ∆G m o values for micellization of the
-50
surfactants in the given temperature range were found
to be negative which indicates the spontaneity of the -52
process.
-54
The ∆G m o values for TTAB, CTAB and OTAB (∆G m2 o for

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OTAB), in pure water at different temperatures, as a -56
14 15 16 17 18
function of carbon number in the alkyl chain of the
Carbon number in chain (N)
surfactants are shown in fig.4a. It is observed that the
negative ∆G m o values show a linear increase with
gradual increase of alkyl chain length of the surfactants,
which indicates that micellization becomes more Fig. 4 Effect of chain length on a. ∆G m o and b. ∆S m o of
spontaneous with increase of the alkyl chain length of
the cationic surfactants. This trend is attributed to
greater hydrophobic nature of the larger alkyl chain. For 80

OTAB, ∆G m o values of first micelle ware found to be

70
more negative than the second, suggesting the 313 K
spontaneity of first micellization -even at the lower 60 318 K
aggregation number. Micellization is associated with the 323 K
∆Smo/Jmol-1K-1

328 K
destruction of the higher degree of hydrogen bonding 50
around the alkyl chains which gives a positive enthalpy
40
change [6],[23],[24]. Despite the fact the ∆H m o is found to
be negative and becomes further negative with increase 30
of temperature. The negative ∆H m o is associated by the
way of (i) disruption of the hydrophobic hydration (or 20
melting of the “iceberg”) surrounding the hydrophobic
tails of the monomers, and (ii) increased degree of 10
14 15 16 17 18
freedom of the tails in the interior of the micelle [20]
Carbon number in chain (N)
where the London dispersion force is the major
attractive force and which is greater for a larger
hydrocarbon chain [16], [25]. In the present study the alkyltrimethyl ammonium bromide surfactants (∆G m2 o
∆H m o values are found to be increasing with increase of and ∆S m2 o of OTAB is used).
temperature which is attributed to the disruption of
greater number of hydrogen bonding between the water
This arises because the “structured water layer” around the hydrophobic moiety of a monomer surfactant

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International Journal of Scientific & Engineering Research, Volume 6, Issue 1, January-2015 1513
ISSN 2229-5518
becomes thinner as temperature increases or Greater entropy values are obtained for the surfactants
alternatively the degree of structure in the water layer with larger alkyl chain. This greater entropy of the
decrease. Therefore the extent of randomness increased system is obtained when the larger hydrocarbon chains
(producing a free energy gain) upon micelle formation are removed from aqueous medium to the interior of the
becomes less and less with increasing temperature [28]. micelle [3].

Table 3.Values of the free energy of micellization, ∆G m o , Enthalpy of micellization, ∆H m o and Entropy of micellization,
∆S m o for TTAB, CTAB and OTAB at various temperatures

T/K TTAB CTAB OTAB

∆G m o ∆S mo ∆H mo ∆G m o ∆S mo ∆H mo ∆G m1 o ∆S m1 o ∆H m o
(∆G m2 o) (∆S m2 o) (∆H m2 o)
293 -40.37 20.72 -34.30
298 -40.51 20.37 -34.44 -47.02 34.45 -36.75
303 -40.62 20.02 -34.55 -47.20 33.83 -36.95
308 -40.70 19.67 -34.65 -47.35 33.21 -37.12
313 -40.78 19.32 -34.73 -47.52 32.59 -37.32 -60.96 69.23 -39.29
(-53.72) (77.40) (-29.49)

318 -40.87 18.97 -34.84 -47.69 31.97 -37.52 -61.30 68.53 -39.51

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(-54.08) (77.00) (-29.60)

323 -40.98 18.62 -34.97 -47.84 31.35 -37.71 -61.65 67.83 -39.74
(-54.50) (76.60) (-29.76)

328 -41.09 18.27 -35.10 -48.00 30.73 -37.92 -61.98 67.13 -39.96
(-54.86) (76.20) (-29.87)

Energetic Parameters are expressed in KJ mol-1 for ∆Gm o and ∆H m o and J K-1 for mol-1 for ∆S m o .Subscript 1 and 2 to the
column title refer to micellization processes 1 and 2 respectively for OTAB.

The enthalpy – entropy compensation plots for bulk counterpart, the enthalpy term contributes more to keep
micellization (for CMC 1 ) of OTAB are shown in fig.5. the negative free energy nearly constant. In some of the
Linear relationships are obtained for micelle formation previous studies such behaviors were shown for
of each surfactant, which represents that when the aqueous solutions of ionic surfactants and smaller
entropy term contributes less to the free energy, its molecules [16], [29], [30], [31].

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-39.2
Here the authors would like to thank the members of the
-39.3
Board of Post- Graduate Studies (BPGS) of the
-39.4 Department of Chemistry, Bangladesh University of
-39.5
Engineering and Technology (BUET) for their helpful
discussion during preparation of the research project.
∆Hm / KJmol-1

-39.6 The financial assistance (CASR-232/52) approved by the

-39.7 committee for Advanced Studies and Research (CASR)
BUET for carrying out the present work is highly
appreciated.
-39.8

-39.9

-40.0
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