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Electrochemical Degradation of C.I. Vat Brown

1 Dye on Carbon Electrode

Article · March 2013

DOI: 10.1166/acl.2013.1002

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 Copyright © 2013 by American Scientific Publishers Advanced Chemistry Letters
All rights reserved. Vol. 1, pp. 32–39, 2013
Printed in the United States of America (www.aspbs.com/acl)

Electrochemical Degradation of C.I. Vat Brown

1 Dye on Carbon Electrode
Prakash Kariyajjanavar1, ∗ , J. Narayana1 , and Y. Arthoba Nayaka2
1
Department of P.G. Studies and Research in Environmental Science, Kuvempu University, Jnana Sahyadri,
Shankaraghatta, 577451 Karnataka, India
2
Department of P.G. Studies and Research in Chemistry, Kuvempu University, Jnana Sahyadri,
Shankaraghatta, 577451 Karnataka, India

The electrochemical degradation of industrial wastewater has become an attractive method in recent years.
In this work simulated dye wastewater containing vat dye C.I. Vat Brown 1 is degraded from electrochemical
method using graphite carbon electrodes. The experimental results indicated that initial pH, current density
and supporting electrolytes were played an important role in the degradation of dye. Electrochemical behavior
of dye has been studied with cyclic voltammetry in basic medium using glassy carbon as working electrode.
The potential range selected for the dye was +0.6 to −1.0 V. The UV-Vis and chemical oxygen demand
(COD) studies were selected to evaluate the degradation efficiency. The maximum colour removal efficiency of
ARTICLE

94.55% and chemical oxygen demand (COD) removal of 82.49% could be achieved for dye at 25 g L−1 of NaCl
concentration. The LC-MS and FTIR studies revealed the degradation of dye and confirmed that aromatic rings
were destroyed. The results revealed the suitability of the present process for the effective degradation of dye
C.I. Vat Brown 1.
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KEYWORDS: Carbon Electrodes, Cyclic Voltammetry,
Copyright Electrochemical
American Scientific Degradation,
Publishers FTIR, LC-MS, UV-Vis, Vat Dye.

1. INTRODUCTION The treatment of textile dye effluent is difficult and

Textile wastewater has a high content of pollutants, the
sources of which are the natural impurities extracted from
the cotton fiber, the processing chemicals and the dyes.
The discharge of this wastewater to the environment causes
aesthetic problems due to the color and also damages the
quality of the receiving water. The color impedes light
penetration and the dyes and their degradation deriva-
tives can prove toxic to aquatic life.1 Vat dyes account
for about 15% of total consumption of textile dyes.2
They exhibit good fastness to light, acid, alkali, and sol-
vents, and they mainly used in dyeing cotton fibres.3
Vat dyes cause environmental concerns when released in
industrial wastewaters due to their carcinogenic health
effects.4 Vat dyes are practically insoluble in water, but
can be reduced in the presence of an alkali and a reduc-
ing agent to form a soluble dye known as the leuco
dye,5 6 which have a certain affinity to cellulosic fibers. It
needs to be reduced to its water soluble leuco-form before
dying.
∗
Author to whom correspondence should be addressed.
Email: prakashsk2678@yahoo.co.in
Received: 23 March 2012
Accepted: 7 May 2012
ineffective with conventional biological processes and
several physico-chemical methods viz., adsorption, photo-
degradation, chemical oxidation, membrane processes,
coagulation, flocculation etc. because many synthetic
dyes are very stable to light, temperature and are non-
biodegradable nature of most dyes.7 8 In this context,
electrochemical technique is considered to be a power-
ful means for the treatment of dyeing wastewater. Indeed,
electrochemical method has been successfully tested9
and it has certain significant advantages such as simple
equipment, easy operation and lower operating cost.10–12
The process requires significantly less equipment than
conventional biological treatment processes.13 14 Graphite
electrodes were used as anode and cathode by many
researchers for the application in organic oxidation.15 16
Hence, there is an interest in electrochemical methods to
develop an efficient, cost-effective and eco-friendly alter-
native for the degradation of dyestuffs.17 In the past,
graphite was frequently used as an anode for the elec-
trochemical degradation of textile dye as it is relatively
cheaper and gives satisfactory results.18 The aim of this
work was to test the feasibility of electrochemical method
for the degradation of C.I. Vat Brown 1 using graphite
carbon electrodes.

32 Adv. Chem. Lett. 2013, Vol. 1, No. 1 2326-747X/2013/1/032/008 doi:10.1166/acl.2013.1002

Kariyajjanavar et al. Electrochemical Degradation of C.I. Vat Brown 1 Dye on Carbon Electrode

2.0

V A 1. DC power supply 1.5

1.5 1.0 Ipc

+ –

Current 10–5 (A)

2. Electrode pair
0.5

Current 10–5 (A)

(1) (2) 1.0 Ipc
3. Electrolytic cell 0.0

–0.5
0.5
4. Magnetic stirrer 0.8 0.6 0.4 0.2 0.0 –0.2 –0.4 –0.6 –0.8 –1.0 –1.2
Potential (V)

(3) 0.0
Dye
Blank

–0.5

(4) 0.8 0.6 0.4 0.2 0.0 –0.2 –0.4 –0.6 –0.8 –1.0 –1.2
Potential (V)

Fig. 3. Cyclic voltammograms of dye C.I. Vat Brown 1 on glassy car-

Fig. 1. Schematic diagram of the experimental setup for the electro- bon. Scan rate: 100 V s−1 ; pH: 9; concentration of dye: 50 ppm (w/v).
chemical degradation. Inset plot: multiple scan (segments: 10).
2. EXPERIMENTAL PART
Austin, USA) controlled by electrochemical software.
2.1. Materials
A three electrodes system was used for the cyclic voltam-

ARTICLE
The commercial vat dye, Indanthren Brown BR Coll. (C.I. metric experiments. The working electrode was highly pol-
Vat Brown 1, CAS No. 2475–33–4) and was obtained ished, glassy carbon disc with an effective surface area
from textile industry Himatsingka Linens, Hassan, India. of 0.06 cm2 . A platinum wire and saturated calomel were
All other chemicals used for the experiments used as counter and reference electrodes, respectively.
were of Technology
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analytical grade reagents and obtained from s d fine
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chem-limited, Mumbai, India. Cylindrical carbon
Copyright elec- Scientific
American Publishers
2.2.2. Electrochemical Degradation Studies
trodes (Chemical composition: graphite carbon + coke:
85% and ash 15%) were obtained from Power Cell Bat- Figure 1 shows the experimental setup for the electro-
tery India Limited. A digital DC power supply (AD 302S: chemical degradation studies. Graphite carbon electrodes
30V, 2A) was used as an electrical source. Double distilled of 4.5 cm length and 0.8 cm diameter were used as anode
water was used to prepare the desired concentration of dye and cathode. The effective electrode area was 11.82 cm2 .
solutions and the reagents. The supporting electrolytes such as NaCl and Na2 SO4
were added to the electrolytic solution, which increases the
2.2. Instrumentation conductivity of the solution and reduces the electrolysis

2.2.1. Electrochemical Measurements

2.0 1.1 r 2 =0.9933
The electrochemical measurements were carried out using 1.0 Ipc
CHI660D electrochemical workstation (CH Instruments
Current 10 (A)

0.9
1.5
–5

0.8
Current 10–5 (A)

0.7

1.0 0.6

0.5

0.4
O O 0.5 0.15 0.20 0.25 0.30 0.35 0.40
–1
Square root of the scan rate (V )

0.150 Vs –1
0.0 0.125 Vs –1
NH NH O 0.100 Vs –1
O
0.075 Vs –1
–0.5 0.050 Vs –1
0.025 Vs –1

0.8 0.6 0.4 0.2 0.0 –0.2 –0.4 –0.6 –0.8 –1.0 –1.2
Potential (V)
O Fig. 4. Cyclic voltammograms of dye C.I. Vat Brown 1 on glassy car-
O
bon at different scan rate. pH: 9; concentration of dye: 50 ppm (w/v).
Fig. 2. Molecular structures of the vat dye, C.I. Vat Brown 1. Inset plots: linear relationship between the current and  1/2 .

Adv. Chem. Lett., 1, 32–39, 2013 33

 Electrochemical Degradation of C.I. Vat Brown 1 Dye on Carbon Electrode Kariyajjanavar et al.
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Fig. 5. Effect of supporting electrolytes (a) NaCl and (b) Na2 SO4 on decolourisation efficiency of the dye C.I. Vat Brown 1. Electrolysis condition:
concentration of the dye solution: 50 ppm (w/v); electrodes: graphite carbon; pH: 9; current density: 170 A m−2 ; time: 240 min.

time. The solution was kept under agitation using magnetic
stirrer.
2.2.3. UV-Visible Studies
A UV-Vis Spectrophotometer (Systronics-119) was
employed to measure the absorbance of dye solution
(max = 480) before and after electrolysis. The decolouri-
sation efficiency was calculated using the relation:
%E = Ai − Af /Ai  × 100
where, Ai and Af are absorbance values of dyes solu-
tions before and after treatment with respect to their max ,
respectively or Ai and Af are initial and final COD values
of the dyes solutions, respectively.
2.2.4. pH and Conductivity Measurement
A water analyzer (Systronics, Model-371) was used to
measure the pH and conductivity of the dye solution
before and after electrolysis under different electrolysis
conditions.
2.2.5. Liquid Chromatography-Mass Spectrometry
Studies (LC-MS)
(1)
The extent of degradation of dye samples were analyzed
by LC-MS studies (LCMS-2010A, Shimadzu, Japan). The
LC-MS was fitted with column C18. The mobile phase was
methanol: water (90:10). The flow rate was 0.2 mL min−1
and the injection volume of dye was 5 L. The dye

34 Adv. Chem. Lett., 1, 32–39, 2013

Kariyajjanavar et al. Electrochemical Degradation of C.I. Vat Brown 1 Dye on Carbon Electrode

6.0 Fourier Transform Infrared Spectrometry (FTIR) spec-

5.5 (a) trometer (model 3010 JASCO, JAPAN). The scan range of
the wave number was set from 400 to 4600 cm−1 . The dye
Voltage (V)

5.0
4.5 samples (freeze dried) were kept in the sample holder and
4.0
scanned to obtain the FTIR spectra.
3.5 NaCl
Na2SO4
3.0 3. RESULTS AND DISCUSSION
100
Decolourisation (%)

80 The structure of C.I. Vat Brown 1 is shows in Figure 2.

60
The dye shade is determined by the number and position of
the carbazole systems and by additional substituents, espe-
40
cially acylamino or alkoxyl groups. Anthraquinone car-
20 (b) bazoles make it possible to dye cellulose fibers in level,
0 very fast brown shades.19
5 10 15 20 25 30 35
Electrolyte concentration (g L–1)
3.1. Voltammetry
Fig. 6. Effect of supporting electrolytes on (a) voltage variation
The cyclic voltammagrams of C.I. Vat Brown 1 (50 ppm,
(b) decolourisation efficiency. Electrolysis condition: concentration of the
w/v) was recorded in pH 9 using glassy carbon as work-
dye solution: 50 ppm (w/v); electrodes: graphite carbon; current density:
170 A m−2 ; time: 240 min. ing electrode. The potential range selected was +0.6 to
−1.0 V. The voltammetric curve of C.I. Vat Brown 1
shows a cathodic peak at −0.61 V Ipc , and there was

ARTICLE
solutions were injected into LC column before and after
no anodic peak found, indicating the irreversible nature of
electrolysis. Analyses using ESI (electron spray ionization)
the dye (Fig. 3). The cathodic peak currents observed for
interface were done under the same chromatographic con-
C.I. Vat Brown 1 attributed to the reduction of ketones to
ditions as described for the APCI (atmospheric pressure
alcohols. These data are very much important to assess the
chemical ionization) analysis, except the guard
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which was not used in the ESI analysis. tion of the
Copyright American Scientific dye C.I. Vat Brown 1.
Publishers
Figure 4 shows the effect of scan rate on the cyclic
2.2.6. FTIR Studies voltammograms of C.I. Vat Brown 1. The reduction peak
current (Ipc ) increased linearly with square root of the
To study the structural changes of dye before and after scan rate ( 1/2 ) over the range 0.025 to 0.150 V s−1 . Inset
electrolysis the dye samples were characterized by using plots show a linear relationship (Fig. 4 inset) between  1/2

Fig. 7. Absorption spectra for C.I. Vat Brown 1 dye solution before and after electrolysis at different pH. Electrolysis condition: concentration of the
dye solution: 50 ppm (w/v); electrodes: graphite carbon; NaCl: 25 g L−1 ; current density: 170 A m−2 ; time: 240 min.

Adv. Chem. Lett., 1, 32–39, 2013 35

 Electrochemical Degradation of C.I. Vat Brown 1 Dye on Carbon Electrode Kariyajjanavar et al.

100 the electrogenerated chlorine/hypochlorite, hydroxyl radi-

cals and the dye molecule. Figure 5(b) demonstrates the
95 effect of Na2 SO4 on the degradation of dye. The decolouri-
Removal of Colour & COD (%)

sation efficiency in presence of Na2 SO4 is attributed to the

90 generation of persulphate ions, which can oxidize organic
dyes.20
85
Moreover, the increased concentration of supporting
electrolytes results in a decrease in the operating voltage
80
at the given current density (Fig. 6(a)). An increase in
75 the concentration of NaCl up to 25 g L−1 accelerated the
Colour degradation rate, enabling the decolourisation efficiency of
COD
70 C.I. Vat Brown 1 of 94.55% (Fig. 6(b)).

65 3.2.2. Effect of Initial pH

85 170 255 340 425
Current density (A m–2)
Solution pH is one of the important factors that affect
the performance of electrochemical process. Hence exper-
Fig. 8. Effect of current densities on decolourisation and COD removal
iments were conducted to study the effect of pH on the
efficiencies of dye C.I. Vat Brown 1. Electrolysis condition: concentration
of the dye solution: 50 ppm (w/v); pH: 9; NaCl: 25 g L−1 ; current density
degradation efficiency of C.I. Vat Brown 1. A significant
170 A m−2 ; time: 240 min. difference in the extent of decolourisation was noted when
the concentration of NaCl was at 25 g L−1 . The initial pH
and current. The correlation co-efficient (r 2 ) of C.I. Vat of the solution (3–11) was adjusted using 1 M H2 SO4 or
ARTICLE

Brown 1 was found to be 0.9933 for cathodic peak cur- NaOH.21–22 The electrolysis was carried out at the current
rent (Ipc ) and indicated the diffusion controlled electrode density of 170 A m−2 for 240 min. with a dye concen-
process. tration of 50 ppm (w/v) at room temperature. From the
UV-Vis spectra, it was clear that, the absorbance in the
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on Dye On: Sat, visible
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3.2. Influence of Electrolysis Conditions 20 Aprregion is attributed to the presence of anthrquinone
2013 07:45:55
Degradation and carbonyl groups (C O). In basic pH, during elec-
Copyright American Scientific Publishers
trochemical degradation, the reduction of C O bonds
3.2.1. Effect of Supporting Electrolytes and cleavage of aromatic rings has taken place, which
results in the decrease in absorbance of the dye solution.
In UV-Vis spectra (Fig. 5(a)), it can be seen that, the addi- Also the absorption band has been shifted from visible
tion of NaCl to the dye solution increased the decolourisa- to UV region (Fig. 7), which indicated the degradation
tion efficiency. From this observation it could be concluded of larger dye molecules into smaller fragments.23 How-
that the introduction of NaCl can enhance the degradation ever, the hypochlorite can lead the partial mineralization
efficiency, which may be attributed to the reaction between of dyes.20 From Figure 7, it is clear that the decolouration
efficiency of C.I. Vat Brown 1 was higher in both neutral
85
(a) 90 and basic pH and slightly lower in acidic pH. After elec-
(b)
trolysis the final pH was found to be slightly increased to
80 basic.
80

70
3.2.3. Effect of Current Density
COD removal (%)

COD removal (%)

75
60

70
The electrolysis of dye solution was carried out at differ-
50 ent current densities (85, 170, 255, 340 and 425 A m−2 )
65 40
at graphite carbon electrodes to investigate the influence
of current density on the degradation efficiency of C.I. Vat
30 Brown 1 keeping NaCl concentration at 25 g L−1 , dye
60
concentration at 50 ppm (w/v), pH at 9 and temperature
20
at 300 K. It can be found that, the decolourisation and
55
3 4 5 6 7 8 9 10 11 5 10 15 20 25 30 35 COD removal efficiencies increased (Fig. 8) with increas-
pH NaCl (g L–1) ing the applied current density.24 This is because of the
increased rate of generation of oxidants, such as chlo-
Fig. 9. Effect of pH and NaCl concentrations on COD removal efficien-
cies of the dye C.I. Vat Brown 1. Electrolysis condition: concentration rine/hypochlorite and hydroxyl radicals at higher current
of the dye solution: 50 ppm (w/v); electrodes: graphite carbon; current densities. Up to a current density of 170 A m−2 , the degra-
density: 170 A m−2 ; time: 240 min. dation efficiency of the dye was increased almost linearly.

36 Adv. Chem. Lett., 1, 32–39, 2013

Kariyajjanavar et al. Electrochemical Degradation of C.I. Vat Brown 1 Dye on Carbon Electrode

ARTICLE
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Fig. 10. Mass spectrum of C.I. Vat Brown 1: (a) before electrolysis, (b) dye residue (c) clear filtrate after complete electrolysis. Electrolysis condition:
concentration of the dye solution: 50 ppm (w/v); electrodes: graphite carbon; pH: 9; current density 170 A m−2 ; time: 240 min.

At higher current densities (>170 A m−2 ) the degradation
efficiency was attained almost constant. Also the energy
consumption was found to be more at higher current densi-
ties with a subsequent stripping of electrodes.25 Therefore,
the optimal current density for the successive electrochem-
ical degradation was fixed at 170 A m−2 .
3.3. Analysis of COD
The electrolysis was carried out at a current density of
170 A m−2 . At this current density, hypochlorite (HOCl− )
and • OH generated in the solution drives the oxidation pro-
cess at basic pH. The maximum COD removal efficiency
of 82.49% was observed at pH 9 (Fig. 9(a)). The percent

Adv. Chem. Lett., 1, 32–39, 2013 37

 Electrochemical Degradation of C.I. Vat Brown 1 Dye on Carbon Electrode Kariyajjanavar et al.
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Fig. 11. FT–IR spectrum of C.I. Vat Brown 1 (a) before electrolysis (b) intermediate dye molecule (c) after electrolysis, Electrolysis condition:
concentration of the dye solution: 50 ppm (w/v); electrodes: graphite carbon; pH: 9; current density: 170 A m−2 ; time: 240 min.

removal of COD increased with increase in the concentra-
tion of NaCl (Fig. 9(b)). This confirmed that the electro-
generated chlorine/hypochlorite will play an important role
in the electrochemical degradation process of the dyestuffs.
3.4. LC–MS Studies
LC–MS studies were employed to monitor the diminu-
tion in mass of the fragments of Vat Brown 1 dye before
and after electrolysis. MS spectrum of the dye C.I. Vat
Brown 1 recorded before electrolysis shows more num-
ber of peaks at higher m/z values due to the presence
of dye and other impurities (Fig. 10(a)). The MS spec-
trum of the dye residue (during electrolysis) shows newer
peaks (Fig. 10(b)) than the earlier peaks indicating par-
tially degradation of dye and formation of intermediates.
The MS spectrum of the filtrate solution after complete
electrolysis shows the absence of majority of the peaks
(Fig. 10(c)). This clearly indicated that almost all dye
was coagulated and removed in the form of sludge. The
remaining peaks at low m/z values in the mass spectra
may be due to the presence of substituted simple aromatic
compounds.

38 Adv. Chem. Lett., 1, 32–39, 2013

Kariyajjanavar et al. Electrochemical Degradation of C.I. Vat Brown 1 Dye on Carbon Electrode

Table I. The electrical energy consumed during decolourisation and dye. Cyclic voltammograms of C.I. Vat Brown 1 shows
electrocoagulation of C.I. Vat Brown 1 dye solution (50 ppm, w/v): irreversible electrochemical natures. UV-Vis, MS spectral
Current Electrolysis Energy consumption
studies and FT-IR studies confirmed that the proposed
Current (A) density (A m−2 ) time (min.) (kWh m−3 ) electrochemical degradation process is an effective method
for the degradation of C.I Vat Brown 1 dye.
0.10 085 240 7060
0.20 170 240 1464
0.30 255 240 2976 Acknowledgments: The Authors are grateful to DBT,
0.40 340 240 4080 DST and UGC, New Delhi for the financial support
0.50 425 240 6300 extended. Also grateful to Kuvempu University, Power
Cell Battery India Limited, DyStar Textilfarben GmbH &
Co. Deutschland KG for their support to carry out
3.5. FT–IR this work.
The IR spectral study is employed to follow up the degra-
dation process. The results in Figure 11 revealed that the References and Notes
ring structures of C.I Vat Brown 1 was degraded because 1. D. Georgiou, C. Metallinou, A. Aivasidis, E. Voudrias, and
the peaks of the wave number between 670 and 750 cm−1 , K. Gimouhopoulos, Biochem. Eng. J. 19, 75 (2004).
which denote aromatic rings, gradually disappeared after 2. M. V. B. Zanoni, W. R. Sousa, J. P. de Lima, P. A. Carneiro, and
degradation. Moreover, the cleavage of anthraquinone A. G. Fogg, Dyes and Pigments 68, 19 (2006).
3. T. Zhang, X. Fei, S. Wang, and C. Zhou, Dyes and Pigments 45, 15
rings was also evidenced by the peak 1660 cm−1 , shifting (2000).
towards lower wavelength region, which is responsible for 4. D. S. L. Balan and R. T. R. Monteiro, J. Biotechnol. 89, 141 (2001).
the combination of stretching vibration of C O conju- 5. U. Nahr and W. Von Bistram, Textil Praxis Int. 46, 978 (1991).

gated with C C26 after degradation. In addition, the broad
peak around 3400 cm−1 , which assigns to N–H vibration,27
also became smaller after degradation (Fig. 11(b)).
Delivered by Publishing Technology
3.6. Electrical Energy Consumption IP: 14.139.133.2 On: Sat, 20 AprSzpyrkowicz,
Copyright American Scientific
The major operating cost is associated with the electrical
energy consumption during electrochemical degradation
process. The electrical energy consumption (E) is required
to decompose 50 ppm (w/v) C.I Vat Brown 1 dye solu-
tion at various current densities was calculated using the
relation:
E = VItE /Vs  × 10−3 (2) 14. F. Li, Z. Yanwei, Y. Weishen, C. Guohua, and Y. Fenglin, Dyes and
where, E is the electrical energy consumption (kWh m−3 ),
V is the applied voltage (V), I is the applied current (A),
tE is the electrolysis time (h) and Vs is the volume of dye
solution (m3 ). As per the results, the minimum electrical
energy consumption was 14.64 kWh m−3 at 170 A m−2
current density. At higher current densities, the energy
consumption was found to be increased and it may be
attributed to the increased hydrogen and oxygen evolution
reaction (Table I).
4. CONCLUSIONS
In the present work the electrochemical degradation of
C.I Vat Brown 1 was carried out using graphite carbon
as anode and cathode, in the optimal operating conditions
(current density 170 A m−2 , NaCl concentration 25 g L−1
and at room temperature). Increasing the initial pH will
lead to corresponding decrease in the degradation effi-
ciency of C.I Vat Brown 1 dye. The effect of the hypochlo-
rite at pH 9 can lead the degradation efficiency of the
ARTICLE
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Adv. Chem. Lett., 1, 32–39, 2013 39