34 Ind. Eng. Chem. Res.

2006, 45, 34-38

Electrochemical Treatment Applied to Food-Processing Industrial Wastewater

Ä vila-Córdoba,† Thelma Pavón-Silva,† and
Carlos Barrera-Dı́az,*,† Gabriela Roa-Morales,† Liliana A
Bryan Bilyeu ‡

Facultad de Quı́mica, UniVersidad Autónoma del Estado de México, Paseo Colón intersección Paseo Tollocan
S/N, C.P. 50120, Toluca, Estado de México, México, and Department of Materials Science and Engineering,
UniVersity of North Texas, P.O. Box 305310, Denton, Texas 76203-5310

The removal of organic pollutants from food-industry wastewater by an aluminum electrocoagulation process
was evaluated using a pilot batch reactor coupled to a rotating electrode. Under optimal conditions of pH 4,
18.2 A m-2 current density, and 150 rpm electrode rotational velocity, the electrochemical method yields a
very effective reduction of all organic pollutants. Treatment reduced chemical oxygen demand (COD) by
88%, biochemical oxygen demand (BOD5) by 52%, total solids by 82%, and total coliforms by 93%. The
effect on the species formed of reducing the pH of the aqueous solution with sulfuric acid was determined.
The wastewater quality was monitored using UV-vis spectrometry and cyclic voltammetry in order to
characterize initial and final pollutant levels. Finally, the morphology and elemental composition of the resulting
sludge was characterized using scanning electron microscopy (SEM) and energy-dispersion spectroscopy
(EDS).

1. Introduction have previously reported that electro-Fenton oxidation induced

in situ resulted in a reduction of 78% chemical oxygen demand
Water is used extensively in the food industry in preparing
(COD), 86% color, and 99.9% fecal coliforms in industrial
raw materials, generating vapor, cleaning packing materials, and
wastewater.6
washing equipment and floors. One of the main characteristics
Electrochemical methods have been used for fundamental
of the wastewater discharge from the food industry is the high
studies on the treatment of synthetic tannery solutions, dye
load of organic materials, such as sugars, carbohydrates, and
solutions, and aqueous herbicide solutions, obtaining in all cases
fermented products. Organic compounds in wastewater from
encouraging pollutant removal results.7-10
the food industry cause problems in the factories, in the
wastewater treatment facilities, and in the environment. Fats The aim of the present work is to investigate the feasibility
and oils in food-processing wastewater tend to clump together of the electrochemical method for removing nonbiodegradable
and clog drain lines and grease traps. If present in excessive organic compounds present in effluent of the food industry. In
amounts, they interfere with microbiological processes at the first phase of the study, the pH of the solution, electrode
wastewater treatment plants and lead to decreased or even agitation, and current density were used as variables to find
complete failure of treatment effectiveness. When discharged optimal conditions to reduce the organic compounds in the raw
to the environment, they can cause the formation of surface effluent. In the second phase, the electrochemical treatment was
films and shoreline deposits and lead to environmental degrada- applied to wastewater while the biochemical oxygen demand
tion.1 The food industry produces wastewater with high (BOD5), chemical oxygen demand (COD), color, microorganism
concentrations of organic compounds and refractory organics content and solids were monitored to determine process ef-
that are not completely removed by physiochemical preliminary fectiveness.
treatments (i.e., coagulation/flocculation and sedimentation) or
biological processes (i.e., anaerobic and aerobic attack). These 2. Materials and Methods
waste materials originate as process residues or as the repro-
Wastewater Treatment Plant. The food-industry wastewater
cessed scrap. Thus, environmental discharge limits are not
treatment plant under study employs a biological system to
always reached.
remove organic pollutants. The system consists of screens, a
New treatment processes are required to comply with legal
homogenization tank, an anaerobic upflow reactor, an extended
environmental standards. Among them, the use of electrochemi-
aeration aerobic tank, secondary clarifiers, and finally a
cal methods could represent an interesting option as many
disinfection system. Treated water coming from this plant does
chemical reactions occur simultaneously when they are applied.
not comply with environmental discharge limits. The biological
Electrochemical methods have been used as chemical coagula-
treatment system cannot respond quickly to the large variation
tion processes to remove color and cloudiness from turbid
in quantity and physicochemical composition of the influent
industrial wastewaters. In this application, the electrochemical
throughout the year. Therefore, new ways to treat this waste-
process generated numerous flocculates, achieving high ef-
water are needed. Electrochemical techniques offer advantages
ficiency in clearing the wastewater.2,3 Electrochemical treatment
over biological systems, including adaptability.
techniques have attracted a great deal of attention because of
Wastewater Samples. Samples of wastewater were collected
their versatility and environmental compatibility, which makes
from the treatment plant at different points in the system influent,
the treatments of liquids, gases, and solids possible. In fact, the
homogenization tank, anaerobic reactor, and aerobic reactor
main reagent is the electron, which is a ‘‘clean reagent”.4,5 We
effluent. Samples were collected in plastic containers, cooled
to 4 °C, and then transported to the laboratory for analysis and
* To whom correspondence should be addressed. Tel.: + (52)-(722)-
2173890. Fax: + (52)-(722)-2175109. E-mail: cbarrera@uaemex.mx. electrochemical treatment.
†
Universidad Autónoma del Estado de México. Electrochemical Reactor. The reactor consisted of a cylin-
‡ drical vessel and a shaft supporting a series of aluminum disks.
University of North Texas.

10.1021/ie050594k CCC: $33.50 © 2006 American Chemical Society

Published on Web 12/08/2005
 Ind. Eng. Chem. Res., Vol. 45, No. 1, 2006 35

This shaft was driven by a variable-speed motor. Five disks Table 1. COD Variation Monitored in Electrochemically Treated
were connected as cathodes and five as anodes. The anodes were Wastewatera
flat with a plain surface, whereas the cathodes had four paddle- % COD
current density electrode final COD removal
like projections to promote turbulence and enhance mass pH (A m-2) speed (rpm) (mg dm-3) efficiency
transfer. Each electrode disk had an area of 0.011 109 m2; thus,
4 9.1 0 11 555 44.97
the total electrode surface, Ae, was 0.111 09 m2. A bucket with 4 18.2 0 10 423 50.36
four baffles served as the supply reservoir for the reactor. The 4 9.1 150 10 197 51.44
4 18.2 150 9446 55.02
volume of liquid treated each time was 2 dm3. A dc source was 8 9.1 0 14 821 29.42
used to supply the system with 1 or 2 A at 9 V. Thus, the current 8 18.2 0 12 082 42.46
density corresponded to 9 or 18 A m-2. 8 9.1 150 17 620 16.09
8 18.2 150 10 391 50.51
Methods of Analysis. The effect of the electrochemical
a The electrolysis time was 15 min, and the initial COD value was 21 000
treatment was determined by analysis of the COD at different
mg dm-3.
time intervals. However, once the optimal conditions were
found, the raw and treated wastewater were analyzed using the
BOD5 and COD, as well as by the solids, chloride content, pH,
fecal coliforms, and turbidity, as indicated in the Standard
Methods procedures.11
Thermodynamic Study. The presence of Al(III) complexes
in aqueous solution has been reported.12,13 With this information,
the distribution diagrams of chemical species were calculated
using the MEDUSA program.14
Cyclic Voltammetric Measurements. Cyclic voltammetry
of crude and treated wastewater was performed using a standard
three-electrode cell. The waveforms were generated by a model
BAS-100W potentiostat, which was controlled by BAS software.
The carbon paste electrodes (CPEs) were circular and had a
surface area of about 3.5 mm2. The CPEs were prepared from
a 1:1 ratio mixture of 99.99% purity single-crystal graphite (Alfa
AESAR) and Nujol oil (Fluka). The paste was inserted into a Figure 1. COD variation as a function of electrolysis time (4) at pH 4, a
PVC tube and compacted to eliminate trapped air; then a copper current density of 18.2 A m-2, and an electrode speed of 150 rpm.
conductor was inserted before the paste set. The surface of the
electrode was renovated after each potential scan.15 The scan readily biodegradable. In general terms, the global efficiency
rate was 100 mV s-1. The reference electrode was Ag/AgCl of the wastewater treatment plant was around 60%.
saturated with KCl, and the counter electrode was a platinum Initial Conditions for the Electrochemical Treatment. The
wire. conditions that were applied in the electrochemical wastewater
UV-Vis Spectrometry. UV-vis spectra were obtained from treatment are presented in Table 1. The wastewater sample
samples of raw and treated wastewater using a double-beam treated was taken from the homogenization tank, the treatment
Perkin-Elmer 25 spectrophotometer. The scan rate was 960 nm time was 15 min, and the initial COD value was 21 000 mg
s-1 within the 900-200 nm wavelength range. The samples dm-3. The most significant parameter affecting COD removal
were scanned in quartz cells with a 1-cm optical path. was the pH of the aqueous solution, as verified by statistical
Sludge Characterization. The sludge produced by the analysis (not shown).
electrochemical process was analyzed by scanning electron In all cases, greater efficiencies were obtained at pH 4 than
microscopy (SEM) and X-ray microanalysis. The analysis was at an adjusted wastewater pH of 8. There was a small
performed on a Phillips XL-30 microscope to observe the contribution to the COD removal due to the effect of the current
composition and configuration of the structure. SEM provides density at pH 4. However, as indicated in Table 1, at pH 8, a
images of rough material with resolution at fractions of a higher the current density clearly resulted in a higher COD
micrometer, and energy-dispersion X-ray spectroscopy offers removal. The effect of electrode agitation was not significant.
in situ chemical analysis of the bulk. In fact, in the case of pH 8 and 9.1 A m-2 current density, a
higher final COD was reached without agitation of the elec-
3. Results and Discussion trodes. Thus, considering economic and practical aspects, the
use of rotating electrodes is not justified under these conditions.
Actual Performance of the Wastewater Treatment Plant. Pollutant Removal after Application of the Electrochemi-
The actual wastewater treatment plant consists of screens, a cal Wastewater Treatment. Figure 1 shows the relationship
homogenization tank, an anaerobic upflow reactor, an extended between COD and electrolysis time. The COD of the wastewater
aeration aerobic tank, secondary clarifiers, and finally a decreased as a function of elapsed time. After 30 min of the
disinfection system. Daily wastewater samples over an 8-month treatment, the COD value reached a minimum: an 88%
period were taken from the screening area, homogenization tank, reduction for a current density of 18.2 A m-2 on electrodes
anaerobic effluent, and aerobic effluent to measure the pollutant rotating at 150 rpm at pH 4.
removal efficiency in each unit operation. There was a large Once the optimal conditions of pH, rotational speed, and
variation in the concentration of the pollutants in the influent current density were found, a more detailed analysis of the
stream: the COD concentration ranged from 2500 to 23 000 wastewater was performed, as reported in Table 2. It is noted
mg dm-3. The concentration was very low in the first 3 months that the process reduced the COD by 88%, the BOD5 by 50%,
and extremely high in the last months, but the efficiency of the the fecal coliforms by 93%, and the total amount of solids by
anaerobic + aerobic treatment was consistent (low removal at 82%. In addition to the reductions in BOD5 and COD, the
low concentrations), indicating that the contaminant was not biodegradability index (BOD/COD) also showed marked im-
36 Ind. Eng. Chem. Res., Vol. 45, No. 1, 2006
Table 2. Selected Properties of Raw and Electrochemically Treated
Wastewatera
raw treated
parameter wastewater wastewater
COD (mg dm-3) 22956 2751
BOD5 (mg dm-3) 2688 1361
color (Pt-Co U) 150 12
turbidity (NTU) 120 25
chlorides (mg dm-3) 110 77
pH 4 5.5
fecal coliforms (MPN) 15000 1000
total solids (mg dm-3) 18773 3313
settable solids (mg dm-3) 20 1
dissolved solids (mg dm-3) 15760 1355
a The electrolysis was applied for 40 min at pH 4 with a current density
of 18.2 A m-2 using aluminum rotating electrodes.
provement, i.e., the ratio improved from 0.11 for the crude water
to 0.49 for the electrochemically treated water. Thus, electro-
chemically treated wastewater would be more suitable for
biological treatment than raw wastewater. From the data reported
in Table 2, it appears that all colloidal and suspended material
can be eliminated using the electrocoagulation technique. As
the solids are removed, color and turbidity decrease as well as
the BOD5 content of the treated water. The 23% reduction in
chloride content is due to a secondary reaction, as eq 1
indicates.3,16
2Cl- f Cl2(g) + 2e-
The chlorine produced is a strong oxidant that can degrade some
of the organic pollutants.17 The variation of the chloride
concentration in solution and its effect on the COD removal of
tannins has been studied; indeed, a high chloride concentration
of 6000 mg dm-3 improves the yields and lowers the energy
consumption.18 The role of chloride ions, present in the
wastewater, in the increased removal of COD has been observed.
Electrochemical oxidation of Cl- produces chlorine according
to reaction 1. Further oxidation and hydrolysis of chlorine yields
hypochlorous acid (HOCl) or the hypochloride ion (OCl-)
depending on the solution pH. Thus, at sufficiently high applied
potentials, Cl2 is the main chlorine species at pH < 3, HOCl in
the region 3 e pH e 7, and OCl- at pH > 7. Among these
species, HOCl is the strongest oxidant and the predominant
species at pH 4. Under actual working conditions, HOCl is the
most important species generated by indirect electrochemical
oxidation of chlorine that contributes at COD removal.19,20
However, increasing the amount of chloride could also lead to
the formation of undesirable organic chloride compounds; thus,
in this work, sulfuric acid was used to adjust the pH instead of
hydrochloric acid.
Aluminum Concentration in Aqueous Solution. The Al
concentration in wastewater plays an important role. Concentra-
tion and pH define the different possible Al chemical species
present in aqueous solution. Using Faraday’s law to calculate
the maximum amount of Al produced in the electrochemical
process in eq 2, with the experimental conditions of 2 A of
current and 40 min of electrolysis along with the Faraday
constant (F ) 96 500 C mol-1) and the charge on the cation (z
) +3), it is possible to calculate the maximum amount of Al,
in this case 0.016 mol or 0.44 g.
it
n)
zF
Recent studies indicate that, at dilute Al concentrations (5 ×
10-3 M), the following chemical species can be found in
aqueous solution: Al3+, Al(OH)2+, Al(OH)3, Al13(OH)345+, and
Figure 2. Predominant aluminum species in aqueous solution when sulfate
is present. [Al(III)] ) 16.0 mM and [SO42-] ) 184 mM.
Al13(OH)327+. The distribution of the Al species depends on
the pH of the aqueous solution. In the present study, where the
working pH is 4, the predominant species are Al3+ and Al-
(OH)3, which are present in equal amounts. However, at pH
4.5, the predominant species is only Al(OH)3, which can be
soluble, insoluble, or colloidal.21,22
In this electrochemical treatment applied to wastewater, the
(1) pH is initially 4.0, but it rises to 4.5-5.0 by the end of the
treatment. This rise in pH is likely due to cathodic reactions.
The sludge is associated with the formation of insoluble Al-
(OH)3 species. The chloride concentration in the wastewater
was 110 mg dm-3 as indicated in Table 2. This concentration
was directly measured from the wastewater, as previously
indicated. The concentration of sulfate ions (15.5 mL per liter
of wastewater) was calculated from the volume of sulfuric acid
needed to adjust the aqueous solution to pH 4 and the density
(1.18 g mL-1) and molar mass.
The concentration of S042- affects the chemical equilibrium
conditions of the process, and new chemical species are formed.
In Figure 2, the distribution of the chemical species in the actual
solution with the sulfate ions as a function of pH is presented.
Note that, at pH 4, new insoluble species appear in the system,
namely, 85% AlOHSO4(s), 12% Al(SO4)2-, and 1.5% AlSO4+
and Al(OH)2+, which enhance the pollutant separation process.
Figure 6 below shows a confirmation of the presence of Al and
S in the sludge.
UV-Vis spectra. The UV-vis spectra of the raw and
electrochemically treated wastewater are shown in Figure 3. The
three main peaks at around 400, 475, and 625 nm in the spectra
correspond to components of the wastewater. It is interesting
that the intensity of these peaks decreases as the electrochemical
treatment time is increased. The peak around 475 decreases by
60% (initial absorbance value 0.8 decreases to 0.33 after
treatment). The peaks at 400 and 625 decrease by about 55%.
These results indicate that there is a significant color reduction
of the raw wastewater when the electrochemical treatment is
applied. Color removal is associated with both the electroco-
agulation and electro-oxidation processes that are taking place
when the electrochemical treatment is carried out.
Cyclic Voltammetry. To obtain further information on the
electrochemical processes occurring at the electrodes, a series
of cyclic voltammetric experiments were performed using a CPE
(2) as the working electrode. Cyclic voltammetry results indicate
that a chemically irreversible oxidation peak in the wastewater
is detectable at potentials lower than those corresponding to
oxygen evolution, as shown in Figure 4. This peak corresponds
to the direct electrochemical oxidation of pollutants present in

Figure 3. UV-vis spectra of (O) the raw wastewater and treated water as
a function of time: (2) 0, (0) 30, and (b) 40 min.
Figure 4. Cyclic voltammograms recorded at the 3.5 mm2 CPE over the
potential window from -1.4 to 1.2 V of the raw (s) and the electrolytically
treated (- - -) wastewater at a scan rate of 0.1 V s1.
wastewater. It is important to note that, when cyclic voltammetry
is applied after the wastewater is electrochemically treated, the
peak does not appear in the voltammogram, indicating that
pollutants in the solution have been oxidized. On the other hand,
the voltammetric curves of reduction present similar behavior
before and after the electrochemical treatment. This is possibly
due to anions such as Cl- and SO42- in the wastewater. Thus,
these voltammograms clearly indicate that processes attributable
to the direct oxidation of pollutants are occurring and these
phenomena contribute to the destruction of organic matter
present in the solution.
Similar processes in the cathodic reactions in solutions
containing chlorides and sulfates, conceivably due to the chloride
evolution process, appear before the oxygen evolution reaction
when the solution contains NaCl. The same behavior is observed
in the presence of Na2SO4.8
The possible cathode loss reaction is given by
ClO- + H2O + 2e- f Cl- + 2OH-
The current efficiency (CE) for the anodic oxidation of the
organic compounds can be calculated from the values of the
COD using the relationship23
F∆cV
η)
8Q
Ind. Eng. Chem. Res., Vol. 45, No. 1, 2006 37
Figure 5. Micrograph of the sludge produced in the electrochemical
process. The photograph was recorded at 500× magnification, and the
marker is 50 µm.
where F is the Faraday constant (96 487 C mol-1), ∆c is the
decrease in COD the chemical oxygen demand (g of O2 dm-3),
V is the volume of the electrolyte (dm3), Q is the charge [i.e.,
current (A) times electrolysis time (s)], and 8 is the number of
milliequivalents for oxygen.
Using the values presented in Table 2, an efficiency of 101%
was calculated. The very high current efficiency obtained with
this electrode cannot be attributed to direct electrochemical
oxidation of the pollutants mentioned in the discussion of Figure
4, but is also due to the electrochemically assisted destabilization
of the colloidal mater (electrocoagulation) mentioned of Figure
2. Similar high current values have been reported previously.8
Cyclic voltammograms using an aluminum working electrode
(not shown) found results similar to those obtained with the
CPE electrode. The pollutant removal from wastewater is carried
out in three ways: aluminum-induced electrocoagulation,
indirect electrochemical process (chlorine), and direct oxidation
at the aluminum electrode.
Scanning Electron Microscopy Images. Previous studies
indicate that the morphology and elemental composition of the
sludge can be determined by SEM and energy-dispersion
spectroscopy (EDS). Voids in the sludge particle structure can
be seen in SEM images, whereas the EDS spectra identify the
elemental composition and the relative amounts of elements
present in the sludge.24,25 To characterize the structural features
of the sludge that was generated by the electrochemical
processes, a series of SEM images were recorded. The micro-
photograph in Figure 5 shows granular and spherical aggregates
with diameters of 5-25 µm. This technique also allows
elemental analysis of the sample, as shown in Figure 6. The
peaks indicate that carbon, oxygen, aluminum, calcium, and
sulfur are present in the sludge. This information confirms that,
once the colloidal matter is destabilized, it can be separated
from the wastewater and that the aluminum generated by the
electrolysis forms complexes with the sulfur in the sludge.
(3) Conclusions
The electrochemical method used in this study reduces the
concentration of organic pollutants in industrial wastewater.
Analysis of the predominant chemical species in aqueous
solution allowed the evaluation of increasing pollutant removal
from wastewater at pH 4. Optimal conditions for the pollutant
removal can be designed with this methodology. Cyclic volta-
(4)
mmetry and UV-vis spectroscopy confirm the improvement
38 Ind. Eng. Chem. Res., Vol. 45, No. 1, 2006
Figure 6. Energy-dispersion X-ray spectra of the sludge produced during
the electrochemical process. Note that aluminum and sulfur are present in
the sludge.
in the wastewater quality and removal of pollutants by the
electrochemical treatment. Finally, the morphology of the sludge
particles is revealed by scanning electron microscopy, and the
presence of carbon, oxygen, aluminum and sulfur in that sludge
is confirmed by elemental analysis.
Acknowledgment
The authors acknowledge the support given by the Univer-
sidad Autónoma del Estado de Mexico, specifically the Facultad
de Quı́mica (Project 2054/2005 UAEM) PROMEP/103.5/04/
2644. Acknowledgment is also given to Dr. Fernando Ureña-
Nuñez for the SEM analysis at the ININ. Support from
CONACYT and supporting research by SNI are greatly ap-
preciated.
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ReceiVed for reView May 19, 2005
ReVised manuscript receiVed October 31, 2005
Accepted November 4, 2005
IE050594K