Powder Technology 148 (2004) 32 – 37

www.elsevier.com/locate/powtec

Nonionic surfactants adsorption onto activated carbon.

Influence of the polar chain length
C.M. González-Garcı́aa, M.L. González-Martı́nb,*, J.F. Gonzáleza,
E. Sabioa, A. Ramiroa, J. Gañána
a
Department of Chemical and Energy Engineering, University of Extremadura, 06071-Badajoz, Spain
b
Department of Physics, University of Extremadura, 06071-Badajoz, Spain

Available online 12 October 2004

Abstract

The adsorption of a nonionic surfactants series characterized by a different length of the hydrophilic tail on an activated carbon has been
studied over a wide concentration range. Adsorption isotherms show two steps limited by the critical micelle concentration (c.m.c.) of the
surfactants. The adsorption extension depends on the oxyethylenic chain length, in such way that the amount adsorbed decreases with
increasing the chain length, although the effect is much lower for the longest polar chains. In the concentration range below the c.m.c. of the
surfactants, the molecules are adsorbed by direct interactions with the activated carbon surface, but with different configuration of the
polyoxyethylene chain (POE) directed to the aqueous phase. For concentrations above the c.m.c., the adsorption takes place by the
interactions between the adsorbed surfactants molecules and differences related to the length of the hydrophilic chain are also found.
D 2004 Elsevier B.V. All rights reserved.

Keywords: Nonionic surfactants; Activated carbon; Adsorption; Langmuir equation

1. Introduction layer attains a high degree of structure and interactions

It is generally accepted that surfactant adsorption at solid/
liquid interfaces may involve hydrophobic interactions
between the adsorbed molecules similar to those in bulk
micelle formation, if their concentration exceeds the limit
given by the critical micellar concentration (c.m.c.) [1–4].
In general, surfactant adsorption isotherms from aqueous
solutions onto solids show several steps when equilibrium
concentration increases [3,5–7]. At the first retention stage,
well below the surfactant c.m.c., adsorbed molecules tend to
lie flat on the surface and interactions between them are
negligible. When adsorption increases, a progressive reor-
ientation of molecules to a more tilted position on the
adsorbent surface is then possible. The next stage of
adsorption, around the c.m.c. region, is dominated by
cooperative interactions (adsorbate–adsorbate); the adsorbed
* Corresponding author. Tel.: +34 924289532; fax: +34 924289651.
E-mail address: mlglez@unex.es (M.L. González-Martı́n).
0032-5910/$ - see front matter D 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2004.09.017
among adsorbed molecules are similar to those in the
micellar state. Equilibrium concentrations higher enough
than c.m.c. correspond in some cases to the appearance of a
plateau.
Several authors have already described this model of
adsorption for nonionic as well as for ionic surfactants [4,8].
However, an equation to express the adsorption equilibrium
relationship is often needed. This is usually done by fitting
experimental data to an isotherm model. Nevertheless, the
different kind of interactions that progressively dominates
the surfactants adsorption process suggests very unlikely
that a single adsorption equation—which comes at the end
from an assumed adsorption model dictated by a single kind
of interactions—could fit the whole range covered in the
isotherm.
The aim of our work is to describe the adsorption of a
nonionic surfactants series characterized by a different
length of the hydrophilic tail on an activated carbon by a
suitable equation that represents the adsorption systems.
This study has been extended to the equilibrium concen-
 C.M. González-Garcı́a et al. / Powder Technology 148 (2004) 32–37
tration range above the c.m.c. to elucidate interactions at the
solid–liquid interface between adsorbed surfactants mole-
cules. In order to analyze the extension at which each of the
mechanisms of nonionic surfactant adsorption can be the
main driven force of the process, and its relative weight
depending on the length of the surfactant hydrophilic tail,
we have modeled the adsorption process as a combination of
two simple contributions each of them characterized by a
simple Langmuir equation, by testing the whole set of
experimental results against a bi-Langmuir equation, which
allows to get a single monolayer coverage and a single
adsorption free energy for each of the assumed processes.
The proposed method was successfully applied to the
adsorption characterization of a given ionic or nonionic
surfactant on carbon blacks and activated carbons [9–13],
showing how topographical differences on samples affected
the adsorption process. It is expected that the application of
the bi-Langmuir equation to our systems can lead to a better
understanding of the role of the hydrophilic chain length in
adsorption for the analyzed surfactants.
2. Materials and experimental methods
Nonionic surfactants of the Triton X series (TX),
polyoxyethylenic octylphenol surfactants type, with an
average number of ethylene oxide units of 9.5 for Triton
X-100 (TX-100), 30 for Triton X-305 (TX-305) and 40 for
Triton X-405 (TX-405) have been used [14]. The surfactants
were used as supplied by Fluka (TX-100, purityN99%) and
Union Carbide (TX-305 and TX-405). Aqueous solutions of
surfactants were prepared with ultrapure water [Milli-Q Plus
(Millipore)]. Its critical micelle concentration in water at 20
8C [15] is given in Table 1. The molecular dimensions of the
surfactant molecules have been evaluated from the surface
area of each group of the surfactants [16,17]; that is,
hydrocarbon chain (HC), phenyl group (P) and polyoxy-
ethylene chain (POE) (Table 1).
The activated carbon Darco (D, Aldrich) was used as
adsorbent for this study. Some of the surface characteristics
of the carbon had been evaluated in a previous work [18]:
the nitrogen adsorption isotherms at 77 K were used to
calculate the BET-specific surface area accessible to N2
(S N2=611 m2 g
1), the micropore (V mi=0.25 cm3 g
1) and
mesopore (V me=0.41 cm3 g
1) volumes and mercury
porosimetry data were used to determine the macropore
Table 1
Characteristics of the surfactants
Surfactant
TX-100 TX-305
c.m.c.a (mol l
1) 3.010
4 1.010
3
Contactable surface 1.4829 3.4817
area (nm2 molecule
1)
a
Taken from Ref. [15].
33
(V ma=0.28 cm3 g
1) volume. Just prior to use as adsorbent,
the carbon was dried in an oven at 110 8C for 24 h.
The adsorption isotherms were established by the change
of the surfactant concentration before and after the contact
with the solid in an end-over-end stirrer, at 11 rpm, in an air
bath at 20.0F0.1 8C for 72 h. Approximately, 0.02 g of
activated carbon is added to 10 ml of the surfactant solution
of a given initial concentration. The supernatant was
separated from the solid by centrifugation at 4000 rpm for
10 min (Centrifuge Digicen-R). Determination of the
concentration was carried out by UV absorption at 278 nm.
3. Results and discussion
The adsorption isotherms of TX-100, TX-305 and TX-
405 surfactants from aqueous solutions onto the activated
carbon Darco are shown in Fig. 1, expressed as the amount
of surfactant adsorbed per gram of adsorbent (X) vs. the
logarithm of the equilibrium concentration (C). Isotherm
shapes display two clear sections limited around the c.m.c.
of the surfactants (logC c.m.c. equal to
3.5 for TX-100,
3
for TX-305 and
2.9 for TX-405), which indicate the
presence of at least two different adsorption mechanisms
involved in the whole adsorption process. As we have
previously indicated, we will analyze the adsorption
behavior with the help of a bi-Langmuir equation, but, as
a first step, we have studied the most diluted concentration
range (below the c.m.c. of the surfactants), where it could be
expected that the adsorption mechanism should be domi-
nated near exclusively by one kind of interaction, adsor-
bate–adsorbent.
The first section of the adsorption isotherms can be
analyzed with the help of a Langmuir equation, assuming
that in the low concentration range, there is not interaction
among adsorbed molecules and there is a constant average
adsorption free energy value. Langmuir equation [19]:
Xm Cb
X ¼ ð1Þ
1 þ Cb
provides an estimate of the maximum adsorption capacity,
assumed as a complete monolayer coverage, X m, and
through the parameter b a measure of the adsorbate–
adsorbent interaction free energy, DG ads:
DGads ¼
RT lnðbxÞ ð2Þ
where x refers to the water concentration in solution (55.55
mol l
1 at 20 8C).
Langmuir equation matches the experimental results very
accurately up to a concentration value around 1.810
4 mol
l
1 (TX-100), 8.210
4 mol l
1 (TX-305) and 8.410
4
TX-405 mol l
1 (TX-405), below but near the c.m.c. of the
1.210
3 surfactants, after which it gets worse. Nevertheless, the
4.4567 curves obtained from this adjustment have been extrapolated
for the entire range of C studied (Fig. 1), showing clearly
that contributions due to adsorption mechanisms different
34 C.M. González-Garcı́a et al. / Powder Technology 148 (2004) 32–37

22]. Then, the minimum area occupied by each molecule

Fig. 1. Adsorption isotherms of TX surfactants onto the activated carbon
(., TX-100; E, TX-305; x, TX-405).
than direct adsobate–adsorbent interaction are gaining
importance as the concentration increases above c.m.c.
The X m values obtained (Table 2), show that the amount
of TX adsorbed decreases as the number of ethylene oxide
units in the TX molecules increases; according to the
general conclusion that the excluded area created by the
polyoxyethylene chain directed to the solution phase is the
principal parameter which limits the amount adsorbed [20–
will be dependent on the stereochemical requirements of the
oxyethylene chains protruding into the aqueous phase, since
the possible configurations of the flexible POE chain in
solution and at the solid–liquid interface are numerous
[8,23]. Conformations of the oxyethylene chain of adsorbed
surfactants depend on the degree of hydration of the chains
[8], its length and its interaction with the solid surface [23].
This conformation, especially for long POE chains, can
range from a flat to a coil configuration.
The X m sequence shown in Table 2, indicates that despite
the amount of TX adsorbed decreases with increasing the
length of the oxyethylenic chain, it does especially when the
change goes from 9.5 to 30 oxyethylene groups, but
remaining nearly constant when the number of these group
passes from 30 to 40. According to the results, the
adsorption extension does not depend on the length of the
hydrophilic moiety when the molecule is long enough,
which could indicate that the longest POE chains show a
random coil configuration which projects a similar excluded
area for the incoming molecules. Also, the very different
values of X m found between TX-100 surfactant (5.8310
4
mol g
1 ) and the other two ones (1.08 10
4 and
1.0510
4 mol g
1, for TX-305 and TX-405, respectively)
can indicate that the random coil conformation of the long
polar chains blocks the more internal positions of the
adsorbent and the retention would be prevented, because of
porosity and pore size distribution of the carbon. This fact
can also be confirmed from the area per adsorbed TX
molecule, A m, evaluated according to:
S
Am ¼ ð3Þ
Xm NA
where S is the accessible surface area of the carbon
determined by nitrogen adsorption at 77 K, S N2, and N A
is Avogadro’s number. The A m values obtained (Table 2)
can be compared with the contactable surface area of Triton
molecules evaluated from their molecular dimensions (Table
1). These values are lower than that of A m for all cases, in
accord with the non-accessibility to the whole S N2 for the
TX molecules. However, it is worth noting that whereas for
TX-100 surfactant the A m value is only slightly higher than
its molecular dimensions, for samples TX-305 and TX-405,
its values are much higher, with a difference of more than 6
nm2 molecule
1. This fact indicates the lesser contribution
from non-accessible surface in narrowest pores for TX-100
than for the other two surfactants.

Table 2
Parameters found from the fitting of the experimental results of adsorption of TX surfactants onto the activated carbon by Langmuir equation in the
concentration range below the c.m.c. of the surfactants
Surfactant Xm b Am DG ads Dg ads
(10
4 mol g
1) (103 l mol
1) (nm2 molecule
1) (kJ mol
1) (10
20 J molecule
1)
TX-100 5.83 18.5 1.74
33.7
5.6
TX-305 1.08 5.7 9.37
30.8
5.1
TX-405 1.05 4.8 9.64
30.4
5.1
 C.M. González-Garcı́a et al. / Powder Technology 148 (2004) 32–37
Fig. 2. Fitting of the experimental results of TX-100 adsorption onto the
activated carbon by a double Langmuir scheme (curve 1) and each of the
summed curves (curves 2 and 3).
The accessibility of TX-100 to smaller pores than TX-
305 and TX-405 is also confirmed by the values of the
adsorption free energy obtained. The values of the free
energy of adsorption calculated from Eq. (2), DG ads, as well
as the values per molecule, Dg ads (Table 2), show the
stronger interaction for TX-100 molecules and also the same
sequence of variation as X m values is found, i.e., a higher
absolute value for TX-100 than for TX-305 and TX-405,
which have both the same value, and reflect that TX-100
adsorption occurs in pores small enough to allow the
adsorbed molecule experiences some enhanced potential,
due to simultaneous interactions of the adsorbed molecule
with both pore walls.
Fig. 3. Fitting of the experimental results of TX-305 adsorption onto the
activated carbon by a double Langmuir scheme (curve 1) and each of the
summed curves (curves 2 and 3).
35
When the equilibrium concentration increases, adsorp-
tion progresses on more open areas of the surface, and
around the c.m.c., lateral interactions at the adsorbed layer
could occur [1–4], which is usually displayed by a sharp
increase in adsorption isotherms [1]. Despite of differences
in the adsorption process at the lowest concentrations, the
presence in all the adsorption isotherms of an inflexion point
located at values of C around the c.m.c of each surfactant
(Fig. 1) suggests that the adsorption progress is similar in all
systems. Therefore, it would be reasonable to assume that
the rising part in the adsorption isotherms indicates that
adsorbate–adsorbate interactions at the solid–liquid interface
take place. Then, two adsorption mechanisms could be
adopted to explain the whole adsorption process of Triton
surfactants on the carbon surface.
As we have previously discussed, we will try to analyze
the adsorption behavior with the help of a double scheme of
Langmuir. For this purpose, the experimental results of the
surfactants adsorption onto the activated carbon for the
entire range of C studied were fitted to equation:
Xm2 Cb2 Xm3 Cb3
X ¼ þ ð4Þ
1 þ Cb2 1 þ Cb3
where the parameters have the habitual meaning of the
Langmuir equation. In Figs. 2–4, the different adsorption
isotherms, for the entire range of concentration studied,
Cc1.010
3 mol l
1, have been expressed as X vs. C. The
curves resulting from that fit, curve labeled as 1, have been
plotted in Figs. 2–4 together with each of the summed
curves (curves 2 and 3); hence, curve 1 is the sum of curve 2
and 3. It can be seen that curve 1 matches the experimental
dates very accurately and that each of the curves 2 and 3 has
a similar shape for all the adsorption systems. Curve 3 has a
nearly vertical branch at the lowest C but quickly reaches a
Fig. 4. Fitting of the experimental results of TX-405 adsorption onto the
activated carbon by a double Langmuir scheme (curve 1) and each of the
summed curves (curves 2 and 3).
36 C.M. González-Garcı́a et al. / Powder Technology 148 (2004) 32–37

Table 3
Parameters found from Eq. (4)
Surfactant X m2 X m3 X m3/X m3+X m2 b2 b3
(10
4 mol g
1) (10
4 mol g
1) (%) (102 l mol
1) (103 l mol
1)
TX-100 8.03 4.60 36 2.8 27.5
TX-305 2.88 0.51 15 2.4 7.8
TX-405 2.16 0.34 14 5.4 7.1

well-defined plateau. Curve 2 has a small slope at the lowest
C, but it changes smoothly with C in the whole range. Thus,
the behavior of curve 1 is controlled by curve 3 and 2 at the
lowest and the highest concentrations, respectively. This
mathematical behavior allows the analysis of the whole
Triton surfactants adsorption onto the activated carbon into
two steps: the surfactant adsorption by direct interaction
with the carbon surface, which can be assumed as
completed when concentration reaches values close to the
surfactant c.m.c. (curve 3); and a second process, mainly
above the c.m.c., for which the newly adsorbed molecules
are retained by interaction with those previously adsorbed
(curve 2), both of them described by a Langmuir equation.
The X m and b values found from both curves are reported
in Table 3, with the sub-index representing the curve from
which they were obtained. The value of area occupied per
molecule in each of the two proposed processes, A m3 and
A m2, and the adsorption free energy, DG ads3 and DG ads2, as
well as their values per molecule, Dg ads3 and Dg ads2, are
also given in Table 4.
As it was mentioned, at the lowest equilibrium concen-
trations, the adsorption process takes place by direct
adsorbate–adsorbent interactions, but with different config-
uration of the polar tail depending on its length. If a coil
conformation for the longest POE chains limits its adsorp-
tion in the low concentration range, this behavior must be
manifested in our treatment by the curve representative of
such process (curve 3).
For each sample X m3 is lower than X m2, although it can
be distinguished important differences related to its relative
contribution on curve 1 (Table 3). As can be seen, the
influence of curve 3 on curve 1 is much lower for TX-305
and TX-405 than that for TX-100, since for the last one the
contribution of both curves at the highest concentrations is
quite similar. Also, the values of Dg ads3 are similar to those
calculated from a simple Langmuir equation, Dg ads (Table
2), since both are related to the same type of interaction, and
they reflect the stronger adsorption of TX-100 surfactant. As
it can be seen from Tables 2 and 4, there is a very good
correlation in all systems between these two groups of
results, analysis of Langmuir equation at concentrations
below the c.m.c. and curve 3 from double Langmuir
scheme, which suggests that the treatment of the exper-
imental results with this scheme gives a good representation
of the adsorption systems.
The second adsorption mechanism that can be assumed
in our systems is that represented by curve 2 (Figs. 1–4) and
through A m2 and Dg ads2 values (Table 4). The A m2 values
are much lower that those corresponding to the process
represented by curve 3 (A m3). The lowest A m2 value
corresponds, as expected, to TX-100 surfactant. If these
last values are compared with the molecular dimensions of
surfactants (Table 1), it is obtained that both are similar for
TX-305 and TX-405, and lower for TX-100. Bearing in
mind that an important part of the BET-specific surface area
of the adsorbent is not accessible to the TX molecules, these
results reflect some arrangement of adsorbed molecules on
the carbon surface, as adsorption progresses probably by the
formation of surfactant aggregates in the adsorbed layer by
interactions of the newly adsorbed molecules with those
already fixed onto the solid surface.
This possibility of aggregate formation can be confirmed
by the adsorption free energy. Since micellization takes
place by the interactions of surfactants molecules through
water, a measure of the interaction free energy of surfactant
molecules in the aqueous phase can be obtained from their
micellization free energy, DG mi. In aqueous solutions where
the c.m.c. is lower than 10
1 mol l
1, DG mi can be
calculated according to [24]:
DGmi ¼ RT lnðc:m:c:=xÞ ð5Þ
Taking into account the c.m.c. of surfactants at 20 8C
(Table 1), the values per molecule, Dg mi, obtained are

4.910
20,
4.410
20 and
4.310
20 J molecule
1
for TX-100, TX-305 and TX-405, respectively. From
comparison between the values of Dg ads2 (Table 4) and
Dg mi, it can be seen that the values of Dg ads2 are lower in
absolute value than Dg mi. If we assume that the adsorption
process related to curve 2 takes place by lateral interactions
between TX molecules, the lower value of Dg ads2 indicates

Table 4
Free energy of adsorption, its value per molecule and area per molecule from curves 2 and 3
Surfactant DG ads2 DG ads3 Dg ads2 Dg ads3 A m2 A m3
(kJ mol
1) (kJ mol
1) (10
20 J molecule
1) (10
20 J molecule
1) (nm2 molecule
1) (nm2 molecule
1)
TX-100
23.5
34.7
3.9
5.8 1.23 2.20
TX-305
23.1
31.6
3.8
5.2 3.52 19.79
TX-405
25.1
31.4
4.2
5.2 4.68 29.29
 C.M. González-Garcı́a et al. / Powder Technology 148 (2004) 32–37
that the arrangement of TX molecules on the adsorbed layer
is worse than in micelles. However, the correlation between
both values is better as the length of the oxyethylenic chain
increases, reaching very similar values for TX-305 surfac-
tant and then suggesting that as the length of the POE chains
increases the two interaction mechanism are more similar. In
accordance with the proposal that above the c.m.c., the
adsorption mechanism of TX molecules takes place through
interactions with those previously adsorbed, it is expected
that the differences found in the first adsorption layer are
also reflected on the second adsorbed layer. The longest TX
molecules retained by direct interaction with the carbon
surface have a more tilted orientation to the surface than that
for the TX-100 surfactant, because of its weaker interaction
predicted by Dg ads and Dg ads3 (Tables 2 and 4), their
configuration allowing a interaction between surfactant
molecules more similar than that in micelles, in reference
to TX-100 surfactant, and then decreasing the differences
between Dg ads2 and Dg mi values.
4. Conclusions
Based on our results, it can be concluded that the use of a
double Langmuir scheme for the analysis of the studied
adsorption system provides a deeper information on the
evolution of the retention process and the differences in the
behavior of the surfactants selected. At the lowest equili-
brium concentrations, surfactants are adsorbed directly to
the carbon surface, allowing their polar tail in a more or less
coil configuration be directed to the liquid phase. This
arrangement in the first adsorption layer drives the
adsorption progress by surfactant–surfactant interactions
more similar to those taking place in micelle formation as
much the molecules adsorbed on the carbon surface have a
longer part directed to the liquid phase.
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