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Enhanced electrokinetic remediation of polluted kaolinite with an azo dye

M. Pazos, M.T. Ricart, M.A. Sanromán, C. Cameselle ∗
Department of Chemical Engineering, University of Vigo, Building Fundicion, 36310 Vigo, Spain
Received 18 October 2005; received in revised form 16 March 2006; accepted 24 April 2006

Abstract
In this work, the feasibility of the combination of electrokinetic remediation and electrochemical oxidation for the remediation of polluted soil
with organic compounds had been development and evaluated in kaolinite spiked with Reactive Black 5 (RB5) an azo dye. The process consists
in the use of two combined phenomena to achieve a full remediation of RB5 spiked kaolinite and the degradation of the organic pollutant. Those
phenomena were soil electrokinetic treatment combined to liquid electrochemical oxidation. Reactive Black 5 (0.39 g dye kg−1 ) could be effectively
removed from the kaolinite matrix by electrokinetics, however the removal results largely depended on the operating conditions. Complete removal
of RB5 was achieved using K2 SO4 as processing fluid (which enhanced the desorption of RB5 from the kaolinite matrix) and operating with pH
control at 7 on the anode. This favoured the alkalinization of the system and, at high pH values, RB5 was ionized and migrated towards the anode
chamber where it was collected and could be oxidized electrochemically. Also, it must be pointed out that in these optimized conditions the electric
power consumption (56 kW/mg of removed dye) was ten times lower compared to the unenhanced electrokinetic process (with no pH-control in
the electrode solutions). Separate electrochemical decolourization tests of RB5 showed the effectiveness of K2 SO4 in the efficiency of the process.
A linear relationship between K2 SO4 concentration and the decolourization rate was found. Thus, nearly complete decolourization was achieved
after 2 and 3 h of electrochemical treatment when the electrolyte concentration was 0.1 and 0.01 M of K2 SO4 , respectively.
© 2006 Elsevier Ltd. All rights reserved.

Keywords: Electrokinetic; Decolourization; Electrochemical treatment; Reactive Black 5; Soil remediation

1. Introduction physical and chemical processes to remove organic pollutants

Around 106 tonnes are produced annually world wide and
used extensively in textile dyeing/finishing and also in food,
paper and cosmetic industries. It is estimated that about 15%
of total world production of wastewater are lost in industrial
effluents [1]. The discharge of these highly coloured wastewaters
into the ecosystem involves environmental problems. There are
more than 10,000 of chemically different synthetic dyes and
pigments. Among them, azo dyes are a major class of synthetic,
coloured organic compounds and account for about half of the
textile dyestuffs used today [2].
Several methods are using to decolourize wastewater (e.g.,
membrane technologies, coagulation and flocculation technolo-
gies) with different colour removal capabilities, costs and might
produce large amounts of solid wastes, which become pollu-
tants on its own creating disposal problems [3–10]. Biological,
∗ Corresponding author. Tel.: +34 986 812318; fax: +34 986 812380.
E-mail address: claudio@uvigo.es (C. Cameselle).
have been considered for remediation of contaminated soils [11].
However, few reports about dye removal from contaminated
soils were found in the literature. Hence, there is a great interest
for developing a soil remediation technology cost-effective and
ecofriendly to this kind of organic pollutants.
The application of electrokinetic remediation for the decon-
tamination of soil polluted with heavy metals has been very
promising, and recently this technique has been employed for
remediation of soil polluted with organic compounds [12,13].
The electrokinetic remediation is primarily a separation and
removal technique for extracting contaminants from soils. It
can be applied in situ, which allows soil to be treated with-
out being excavated and transported, resulting in potentially
significant cost savings and in a less destruction of the soil
matrix.
The principle of electrokinetic remediation is based on
the application of a low-intensity direct current through the
soil, between two electrodes (anode and cathode). Pollutants
are transported towards the electrodes by electromigration
(positively and negatively charged organic compounds are

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transported towards the cathode and anode, respectively) and
electroosmosis (the movement of a liquid containing ions
relative to a stationary charged surface) [14,15]. Moreover, the
oxidation/reduction of water at the anode/cathode generates H+
and OH− that move towards the cathode/anode creating an acid
and basic front in the soil, respectively [16].
During the electrokinetic treatment of a contaminated soil,
charged dye is transported towards one of the electrode chambers
where it will be concentrated. Removal of contaminants of this
concentrated solution may be accomplished by several means,
among which liquid electrochemical oxidation is a promising
technology. There are few reports that used the electrochemical
technology to degrade wastewater with high dye concentration.
Among them, Ciorba et al. [17], Gutierrez et al. [18], Donald-
son et al. [19], Kim et al. [20], Sanroman et al. [21,22] have
reported the enormous potential of the electrochemical technol-
ogy to decolourize wastewaters contaminated with several kinds
of dyes. They found that electrochemical oxidation is a versatile
alternative with a high potential to replace or improve existing
processes.
In this work, an environment-friendly in situ integral method
is presented. Hence, the method proposed in this paper consists
in two combined phenomena: soil electrokinetic treatment and
liquid electrochemical oxidation on the electrode (anode). This
coupling could permit the in situ total dye degradation. In order
to test the feasibility of the method purposed, the electrokinetic
remediation of kaolin polluted with a representative dye of the
azo group, Reactive Black 5 (RB5) and its degradation by elec-
trochemical oxidation have been studied.
2. Materials and methods
2.1. Electrokinetic treatment
2.1.1. Kaolinite sample preparation
Kaolinite samples were prepared mixing thoroughly 120 g of
kaolinite clay with 120 mL of a solution of RB5 (0.5 g L−1 ). A
slurry of 0.5 g dye kg−1 dry kaolinite clay was obtained. RB5
(Fig. 1) was purchased from Sigma. The mixture stood for 24 h
to allow the possible sorption of dye to the surface of kaolinite
particles. The pH of the mixture was 4. The resulting slurry was
compacted to a constant density and pressure in a consolidome-
ter unit [23], which creates homogeneous, near-saturated soil
Fig. 1. Chemical structure of Reactive Black 5.
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matrixes. During the consolidation process, a fraction of the
initial water and dye was eliminated from the slurry. RB5 con-
centration in the soil matrix after the consolidation process was
0.39 g dye kg−1 of dry matter, and its pH was 4.2. The moisture
content was around 32%, expressed as the weight of water per
unit weight of wet kaolinite. In this sample, RB5 was adsorbed
on the kaolinite particles since no dye was released in extraction
tests with deionised water.
Kaolinite was selected as model matrix since it shows much
lower buffering capacity, because of its lower cation exchange
capacity compared with other clay minerals. The kaolin used
has a particle size average of 3 ␮m and a specific surface of
13.5 m2 g−1 . The mineralogy analysis by X-ray diffraction indi-
cated the presence of kaolinite clay 85%, mica 14% and quartz
1%.
2.1.2. Electrokinetic cell
The experiments were performed in a cylindrical glass cell
depicted in Fig. 2. The sample, 80 g of RB5 spiked kaolinite
(dry weight) was introduced in the central tube whose dimen-
sions are 100 mm length and 32 mm inner diameter. The two
electrode chambers (with 300 mL working volume) are placed
at each end of the sample compartment isolated from this one by
a paper filter and porous stones. Graphite electrodes were used
for both anode and cathode (P1, P2 and P3). Three auxiliary
electrodes allow to measure the electric field distribution along
the sample. Electrode chambers were filled with K2 SO4 (0.1 M)
as processing fluid. Recirculation of liquid is applied by pumps
to avoid concentration gradients. In some experiments pH on
the anode or the cathode chambers was controlled using NaOH
0.1 M or H2 SO4 0.1 M, respectively.
A DC electric current with maximum values of 30 V or 10 mA
was applied in all experiments. Readings of the voltage drop,
current intensity and the pH in the electrode compartments were
taken periodically.
Analytical methods: upon completion of each experiment,
samples were taken from cathode and anode solutions and the
clay matrix for chemical analysis. The clay sample was divided
in five sections of approximately 16 cm3 each, named S1–S5
from anode to cathode. They were analysed for moisture content,
pH and RB5 concentration. The pH in the kaolinite sections after
the experiment was measured adding KCl 1 M to dry kaolinite in
a ratio 2.5 mL g−1 . After 1 h of contact time, pH was measured
with a pH-meter Sentron model 1001. The RB5 was extracted
from kaolinite sections with a solution of K2 SO4 0.1 M in a ratio
1 g of dry kaolinite: 8 mL. The extraction procedure was done
five times to assure a complete recovery of the dye. RB5 con-
centration was determined from the absorbance at the maximum
wavelength in the visible spectrum (597 nm) using a calibration
curve.
2.2. Liquid dye decolourization
2.2.1. Electrochemical cell
Experiments were carried out in an electrochemical cell with
a working volume of 300 mL. Electrodes were made of graphite,
with an effective area of 38 cm2 and the electrode gap was 8 cm.
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Fig. 2. Schematic diagram of experimental set-up: (1) soil sample, (2) porous stones, (3) electrodes, (4) electrode chambers, (5) auxiliary electrodes, (6) gas valves,
(7) recirculation pumps and (8) power supply.

Magnetic stirring was used to avoid concentration gradients. A
constant potential difference (5 V) was applied with a power
supply (HP model 3662) and the process was monitored with
multimeter (Fluke 175). The electrochemical decolourization
of Reactive Black 5 (67 mg L−1 ) was studied using K2 SO4 as
electrolyte (10–100 mM).
2.2.2. Decolourization
Samples of reaction mixtures were taken from the electro-
chemical cell to be analysed for pH and dye concentration.
pH was measured with a Sentron pH meter (model 1001).
The dye concentration was measured from the absorbance at
the maximum wavelength in the visible spectrum (597 nm)
using a calibration curve. Dye decolourization was associated
with the decrease in the concentration and expressed in terms
of percentage. The assays were done in duplicate, and the
experimental error was less than 3%.
3. Results and discussion
3.1. Electrokinetic treatment of kaolinite polluted with RB5
A saturated kaolin clay sample polluted with RB5 was sub-
jected to the electrokinetic process. The objective of this experi-
ment (exp. 1) was to determine the feasibility of the remediation
of kaolin contaminated with RB5, using an electrokinetic tech-
nique to mobilize the dye and collect it in the chamber of one of
the electrodes.
In order to improve this electrokinetic process, it is necessary
to add an electrolyte that increases the electric conductivity and
favours the desorption of dye from the polluted clay sample.
Potassium sulphate was found to have been very effective in the
extraction of dye from the mineral matrix; in fact, potassium
sulphate was used in the extraction of the residual RB5 from
kaolinite in the analytical procedure. It is a strong electrolyte,
which is completely dissociated in solution. When a solution
of potassium sulphate is used as processing fluid in the elec-
trode chambers, K+ and SO4 2− ions are transported through the
kaolinite sample from one electrode chamber to the other by
the effect of the electric field. The presence of the potassium
sulphate increases the electric conductivity and favours the des-
orption of RB5 from the clay particles. Thus, the desorbed RB5
can be transported by electroosmosis and/or electromigration
towards the electrode chambers. For this reason, in this experi-
ment potassium sulphate was selected as processing fluid, filling
the anode and cathode chamber with 0.1 M potassium sulphate.
In this experiment, a pH jump between section S4 and S5
(Fig. 3) was developed due to the electrolysis of water upon
the electrodes [24]. The formation of this pH jump was the
responsible of the decreasing in the current intensity registered
from the second day of treatment and the large increase
observed in the electrical resistance.
As can be seen in Fig. 3, 14% of the initial RB5 was
removed from the soil and it is supposed to have reached the
electrode chambers by electromigration, electroosmosis and
diffusion. RB5 was almost complete removed from section
S5, its concentration was reduced by 94%. There was also an
important decrease in dye concentration after the treatment
in sections S1 (84%) and S2 (54%). However, RB5 was
accumulated in section S3 and especially in section S4, where
the final concentration was twice the initial one.
The electrokinetic treatment of the kaolinite sample polluted
with a coloured compound was followed visually. In the
beginning, the colour intensity was uniformly distributed along
the sample. The application of the electric field mobilized
the organic compound. The movement of RB5 results in the
appearance of white zones (or pale colour zones) on both sides
of the kaolinite sample. The thickness of those white zones
Fig. 3. Electrokinetic treatment of RB5 spiked kaolinite (exp. 1). Normalized
concentration (ⵦ) and pH ().

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was slowly widened during the first 5 days. However, no more
visual changes were observed during the rest of the experiment.
So, it suggests that the reported results in RB5 removal were
achieved in 5 days of treatment and the rest of the treatment do
not contribute significantly to the decontamination process.
The electric power consumption registered at the end of
the experiment was 60 kWh (907 kWh mg−1 of removed dye),
but considering that the treatment was not effective from the
fifth day on, the electric power consumption was only 37 kWh
(592 kWh mg−1 of removed dye).
In this experiment it is very clear that the pH jump limited
the current intensity and increased the electrical resistance of
the system. In other words, the transport of ions was limited
and therefore it affected the RB5 removal. On the other hand,
an important removal of RB5 was found on both sides of the
kaolinite sample, where the pH values were complete different.
On the anode side, the pH of the kaolinite was very acid (pH
2.4), and pH was alkaline on the cathode side (pH 9.7). So,
it is proposed to study the behaviour of the system under pH-
controlled conditions. It suppressed the pH jump and permitted
to study the removal of RB5 in alkaline or acid environment, with
the objective of revealing the optimum operating conditions for
RB5 removal.
3.2. Electrokinetic treatment with pH control on cathode
(exp. 2)
In this experiment, pH value was controlled at 6.8 ± 0.2 on
the cathode chamber with sulphuric acid 0.1 M. It avoided the
formation of an alkaline environment at the cathode side and
favoured the advance of the acid front. So, the kaolinite sample
was acidified reaching an almost flat pH profile (from 2.9 to 3.2)
as shown in Fig. 4. The pH control at the cathode avoided the
formation of the pH jump, and the electrical resistance of the
system was kept low compared to experiment 1.
The distribution of RB5 in the kaolinite was very different
compared to experiment 1 (Fig. 4). A very important decrease
in RB5 concentration was observed in section S4 (78%) and
especially in section S5 (92%). The final concentration of RB5
in section S3 (in the middle of the kaolinite sample) coincided
Fig. 4. Electrokinetic treatment of RB5 spiked kaolinite with pH control in the
cathode (exp. 2). Normalized concentration (ⵦ) and pH ().
Please cite this article in press as: M. Pazos et al., Electrochim. Acta (2006), doi:10.1016/j.electacta.2006.04.067
with the initial concentration, and a slightly accumulation in
sections S1 and S2 was observed. In these sections the final
concentration was 20% higher than the initial concentration.
These results show that RB5 migrated towards the anode. In
fact, during the experiment, the advance of the dye was followed
by the change in colour of the soil (from blue to white). The
white layer appeared in the soil close to the cathode on the
second day and it moved towards the anode at a constant rate
of 0.17 cm day−1 , until the day 15, when it reached a thickness
of 4 cm. It corresponds with sections S4 and S5, which shows
the highest removal.
The mass balance showed that 26% of RB5 was removed from
the kaolinite and was collected on the anode chamber, where it
was electrochemically decolourized. No RB5 was detected on
the anode and cathode solution at the end of the experiment. The
electric power consumption was 338 kWh mg−1 of removed dye.
3.3. Electrokinetic treatment with pH control on anode
(exp. 3)
The pH control on the anode depolarized the oxidation of
water avoiding the formation of H+ ions and the acid front.
NaOH 0.1 M was used in the pH control to keep the pH value at
7.2 ± 0.2 in the anode. In this condition, the basic front generated
at the cathode penetrated into the kaolinite sample, increasing
the pH of the interstitial fluid. At the end of the experiment, the
kaolinite sample reached a pH profile almost flat, from 9.7 to
9.9 (Fig. 5).
The electrical resistance of the system was slightly higher
than in experiment 2. It is probably due to the lower mobility
of the OH− ions (the predominant in experiment 3) than the H+
ions (the predominant in experiment 2).
At the end of the experiment, 94% of RB5 was removed from
the kaolinite sample demonstrating the high effectiveness of the
treatment. The removal degree in the different sections ranged
from 91% in S1 to 96% in S5 (Fig. 5).
During the experiment, it was observed that RB5 was trans-
ported towards the anode side. In the first day of treatment, a
white layer 1 cm width was detected on the cathode side. The
rest of the kaolinite sample was blue. Both zones were separated
Fig. 5. Electrokinetic treatment of RB5 spiked kaolinite with pH control in the
anode (exp. 3). Normalized concentration (ⵦ) and pH ().
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by a sharp line. The thickness of the white layer was increasing

during the treatment and after 5 days all the dye was removed
from the kaolinite sample and was concentrated in the anodic
solution.
RB5 is a complex chemical compound that has four sulphonic
groups. In alkaline medium, those groups will be ionized form-
ing an anion with four negative charges. In the beginning, the
pH of the kaolinite sample is slightly acid (around 4) but, dur-
ing the electrokinetic treatment, the alkaline front increased the
pH of the kaolinite inducing the ionization of the dye molecule.
At the same time, potassium sulphate was transported by elec-
tromigration and electroosmosis from the electrode chambers
to the kaolinite sample. The presence of potassium sulphate
favoured the desorption of RB5 from kaolinite solid matrix. Both
phenomena desorbed and ionized the dye, which can migrate
towards the anode. The first 3 days, the registered migration
rate was 1 cm day−1 but the increase of pH and potassium sul- Fig. 6. Electrochemical decolourization of Reactive Black 5 with potassium
sulphate: 0.01 M (♦); 0.025 M (); 0.05 M (); 0.1 M ().
phate concentration into the kaolinite sample, accelerated the
migration reaching 3.5 cm day−1 on the fourth and fifth days.
On the fifth day the dye was colleted in the solution of the anode Sigma Plot curve fitter uses an iterative procedure, based on the
chamber, where it was electrochemically decolourized upon the Marquardt–Levenberg algorithm, which seeks the values of the
surface of the electrode. The electric power consumption was parameters that minimize the sum of the squared differences
only 56 kWh mg−1 of removed dye. between the observed and predicted values of the dependent
variable.
3.4. Electrochemical decolourization of RB5 dC
= −kC (1)
dt
In order to obtain the full remediation of polluted kaolin
it is necessary to study the electrochemical oxidation of RB5 where C is the concentration of RB5 (mg L−1 ), t the reaction
extracted from the soil by electrokinetic treatment and colleted time (min) and k is the pseudo-kinetic coefficient for the first
in the anode chamber. order reaction (min−1 ).
The electrochemical decolourization of RB5 in liquid phase As it can be seen in Fig. 7, the pseudo-kinetic coefficient
was studied in an electrochemical cell of 300 mL, with a solution depends linearly on the potassium sulphate concentration. So,
similar to that found in the anode chamber. The experiments were the previous kinetic expression can be rewritten as follows:
conducted at 25 ◦ C and at constant potential difference: 5 V. This
dC
value was selected since it was determined as the optimum value = −0.143 CPS C (2)
for treatment time and electric power consumption [21]. dt
The decolourization experiments were carried out in a where CPS is the concentration of potassium sulphate (M) and t
solution of RB5 with initial concentration of 67 mg L−1 is the reaction time (min).
and different concentrations of potassium sulphate. In the
electrochemical decolourization, potassium sulphate acted as
inert electrolyte [25]. In order to enhance the decolourization
process, the effect of the electrolyte concentration was studied
in the range from 0.01 to 0.1 M.
In Fig. 6, the influence of the concentration of potassium
sulphate in the RB5 decolourization is depicted. In general,
high electrolyte concentration increases the electric current
densities in the solution and, for this reason, high concentrations
of sulphate significantly increased the reaction rate, and the
total decolourization of the solution is reached in shorter
treatment time. Thus, 180 min are necessary to reach 90% of
decolourization with 0.01 M K2 SO4 . If the concentration of
sulphate is increased until 0.1 M, the treatment time necessary
to obtain the same decolourization was 110 min. This is an
important reduction in the treatment time.
The concentration profile along treatment time was fitted
Fig. 7. Relationship between the potassium sulphate concentration and
to a pseudo-first order kinetic equation (Eq. (1)), and the rate the pseudo-kinetic parameter obtained with Eq. (1) in the electrochemical
constant was calculated using the Sigma Plot 8.00 software. The decolourization of RB5.

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These results confirm the double utility of potassium sulphate
as processing fluid in electrokinetic treatment and as electrolyte,
which enhances the electrochemical decolourization of RB5.
Hence, its presence in the anode chamber favoured the electro-
chemical decolourization upon the surface of the electrode of the
dye that was transported from the soil to the electrode chamber.
Moreover, high concentration of potassium sulphate favoured
the electric conductivity and the desorption of RB5 in the soil,
and the dye decolourization in the processing fluid.
4. Conclusions
In view of the results obtained in the present paper, it can be
concluded that the combination of electrokinetic remediation
and electrochemical oxidation shows a great potential for the
remediation of polluted soils with anionic organic compounds.
The operating conditions, especially the pH value into the soil
sample, are decisive to achieve a full remediation. Moreover,
the effect of several electrolyte concentrations on liquid
electrochemical oxidation was assessed. It was found that high
concentration of potassium sulphate was able to electrocatalyze
efficiently the oxidation of dye shortening significantly the
treatment time of the processing fluid obtained from the
electrokinetic remediation.
The above results suggest the feasibility to apply the two
combined phenomena (soil electrokinetics combined to liquid
electrochemical oxidation) for remediation of soil environments
contaminated with organic pollutants. With the configuration
designed and employed in the present report, full remediation
of polluted kaolin at low cost without operational problems can
be achieved.
Acknowledgement
This research was funded by Xunta de Galicia (Project
PGIDIT04TAM314003PR).
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