Desalination 278 (2011) 84–90

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Desalination
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / d e s a l

Removal of rhodamine B by ozone-based advanced oxidation process

Bai Cuiping a, c, Xiong Xianfeng b, Gong Wenqi a,⁎, Feng Dexin c,⁎, Xian Mo c, Ge Zhongxue b, Xu Nian a
a
School of Resources and Environmental Engineering, Wuhan University of Technology, Wuhan 430070, PR China
b
Xi'an Modern Chemistry Research Institute, Xi'an 710065, PR China
c
Key Lab of Biofuels, Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences, Qingdao 266101, PR China

a r t i c l e i n f o a b s t r a c t

Article history: The oxidation of rhodamine B in aqueous solution by conventional ozone process and the advanced ozone-
Received 18 January 2011 based oxidation processes was investigated. The reaction conditions such as ozone dosage, initial
Received in revised form 22 April 2011 concentration of the dye and pH in ozone process were optimized. The decolorization rate of rhodamine B
Accepted 3 May 2011
increased with the ozone dosage but decreased with the initial concentration of rhodamine B. Three oxidative
Available online 6 June 2011
processes including UV/ozone, US/ozone and ozone systems were assessed to select the most appropriate
Keywords:
oxidative process in terms of rhodamine B aqueous solution treatment and special emphasis was laid on the
Rhodamine B effect of reaction pH in the three methods. It was found that in all the three methods, the acid condition can
Ozonation promote the oxidation process. The UV/ozone process was the best ozone-based oxidization process, with the
Catalytic ozonation decolorization efficiency of 99.78% and COD removal rate of 47.43% after 15 min treatment. The pseudo-first
order kinetics was found to fit all the ozone-based processes, with regard to the decoloration and degradation
reactions.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction
In textile industry, more and more dyes and pigments are used to
color the products. In recent years, it is estimated that more than
100,000 dyes are available commercially [1] and their global
production exceeds 800,000 tons per year [2]. Dye-containing
wastewater as an important source of environmental contamination
has aroused more attention because most of the dyes molecules have
complicated structures and they are photolytically stable, which
render them resistant toward conventional biochemical decomposi-
tion [3,4]. To protect environment from being damaged by the dye
wastewater, the applications of some physical and chemical methods
have been reported.
Tradition physical and chemical techniques have been used in dye
wastewater treatment such as absorption by active carbon, coagula-
tion by chemical agents, and oxidation by Fenton and hypochlorite
methods [5]. However, these methods have high operational costs,
need long reaction time and contain the secondary pollution, since
solid wastes would be produced in these processes, which can bring
another environmental problem of sludge treatment and disposal [6].
Therefore, an affordable and easy-operated control technology
without the formation of sludge is needed [7].
Ozone and hydroxyl radicals generated in the dye aqueous
solution are able to quickly break the carbon–carbon bond in the
aromatic rings. Moreover, ozone is not only effective in decolorizing
⁎ Corresponding authors. Tel.: + 86 27 87372102; fax: + 86 27 87882128.
E-mail addresses: gongwenqi@yahoo.com.cn (G. Wenqi), fengdx@qibebt.ac.cn
(F. Dexin).
the dye effluent, but also it can convert biorefractory dyes in
wastewater into biodegradable organism [8]. It has been successfully
used in the degradation of dye wastewater such as reactive X-3B dye
[9] and reactive black 5 dye aqueous solution [10]. In addition, many
catalysts are used in combination with ozone to enhance the
oxidation process. As valid catalysts, ultraviolet and ultrasonic have
been used to produce more hydroxyl radical, which can improve the
degradation effect of organism pollution [11–13]. On the other hand,
the combination of ozone and ultraviolet or ultrasonic cannot cause
secondary pollution such as chemical sludge and the reaction process
is easy to control. They are efficient and eco-friendly advanced
oxidation method in wastewater treatment.
Rhodamine B is an important dye, which is widely used in textile
industry for dyeing silk, wool, jute leather and cotton. It may cause
carcinogenic and teratogenic effects on public health [14]. Few
methods were studied to remove it from wastewater; Libanori et al.
[15] used TiO2-coated activated carbon catalyst; Wang et al. [16]
reported its degradation by using swirling jet-induced cavitations
combined with H2O2; Chang et al. [17] also reported its removal by fly
ash adsorption with Fenton pre-oxidation. However, problems
correspondent with these methods exist such as secondary pollution,
high operational costs and long reaction time. Until now, there is no
literature that reports about the removal of rhodamine B by ozone and
the comparison with UV/ozone and US/ozone.
The purpose of this study was to obtain the appropriate
degradation parameters of rhodamine B by ozone system, such as
ozone dosage, pH and initial concentration of dye solution. A
comparative study was carried out with the aim of investigating the
effect of UV/ozone, US/ozone and ozone processes on the

0011-9164/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2011.05.009
 B. Cuiping et al. / Desalination 278 (2011) 84–90
decolorization and COD removal of rhodamine B in aqueous solution.
The decolorization process was analyzed by UV-VIS spectra from the
absorbance variation in the 290–800 nm range. A simple pseudo-first-
order kinetic was proposed, which was in agreement with the
experimental data.
2. Materials and methods
2.1. Materials
Rhodamine B was supplied by Shanghai Chemical reagent Ltd. Co.
(Shanghai, China) and used without further purification. The solution
pH was adjusted by using 0.1 M HCl or NaOH aqueous solution. The
peroxide test was supplied by Merck KGaA. (Darmstadt, Germany)
and used to test the residual hydrogen peroxide in the solution.
Distilled water was used throughout. The molecular structure of the
dye is showing in Fig. 1.
2.2. Methods
2.2.1. Ozone
Ozone was generated from air by using an ozone generator with
input rate of 5 g/h. The applied ozone dosage was controlled by a
flowrator (Yinhuan Flowrator Ltd. Co., China) which had the
measuring range from 50 to 250 ml/min. The ozonation of 100 ml
dye solution was performed in a batch reactor, which was made of
Pyrex glass with the dimensions of 8.0 cm diameter and 13.5 cm tall. It
was used to facilitate the operation of all the ozone-based oxidation
processes. The reactor included input/output port for ozone gas
stream. Ozone was introduced through a porous fritted diffuser that
can produce fairly fine bubbles. The excess ozone at the outlet was
adsorbed by sequential 10% KI solution.
2.2.2. US/ozone
The equipment was identical with the ozone system. The
ultrasonic experiments were performed on a Kunshan KQ-300GVDV
ultrasonic cleaner (Kunshan Ultrasonic Ltd. Co., China) with frequen-
cies of 20 kHz, 45 kHz and 80 kHz. The above batch reactor was
located in the cleaning bath and the surface of reactants was slightly
lower than the level of water in the cleaning bath. The temperature of
the water bath was kept at 25 °C by the addition or removal of water.
2.2.3. UV/ozone
The equipment was identical with the ozone system. In the
ultraviolet light based process, a low pressure portable UV lamp (WD-
9403E) with an output frequency of 50 Hz was placed above the batch
reactor and the UV lamp power can be chosen as 8 W, 16 W and 32 W.
The distance between the UV lamp and the batch reactor was about
1 cm. The UV lamp housing was centered into the reactor. The
wavelength of the UV was 254 nm. A black box placed outside the
reactor was employed to minimize any penetration of UV light when a
UV-enhanced facility was operated.
Fig. 1. Molecular structure of Rhodamine B.
85
2.3. Analytical methods
The pH value of the solutions was measured by using a digital pH
meter (Sartorius, Germany). The UV-VIS spectra of rhodamine B
solution was recorded in the range from 290 nm to 800 nm using a
Cary 50 UV-VIS spectrophotometer (Varian, USA), showing that the
maximum absorbance wavelength of rhodamine B was 554 nm. Thus,
the concentration of rhodamine B versus time can be determined by
measuring the absorption intensity at 554 nm. A calibration curve was
obtained by using the standard rhodamine B solution with the known
concentrations before the measurement. COD determination was
conducted with the digestion system and COD determinator. (Lianhua
COD determinator Ltd. Co., China). The reaction products of
rhodamine B were detected by GC-MS. Electron impact mass spectra
were obtained with an Agilent Trace GC 5975C system coupled to a
quadrupole detector. The GC was equipped with an ion source
temperature of 220 °C and EI ionization at 70 eV.
3. Results and discussion
3.1. Effect of the rhodamine B initial concentration
The effect of the initial concentration of rhodamine B on the dye
decolorization by ozone was investigated in the range from 50 to
200 mg/l. The results are shown in Fig. 2. It is apparent that the
decolorization rate of rhodamine B decreased with the increase of the
initial concentration. After 10 min treatment, the decolorization rate
decreased from 97.67% to 72.8% when the initial concentration of
rhodamine B increased from 50 mg/l to 200 mg/l. At a certain
temperature, the ozone concentration in wastewater is constant, so
the amount of HO⋅ radicals in the system would be constant under the
same conditions [2,18]. The high concentration of rhodamine B would
consume more HO· radical, so the effect would be reduced with the
increase of the initial rhodamine B concentration.
3.2. Effect of ozone dosage
The ozone dosage played an important role in the decolorization of
rhodamine B. A range of the ozone dosage from 10 ml/min to 40 ml/
min was studied and the results are presented in Fig. 3. It is clear that
the decolorization rate of rhodamine B was enhanced with the
increase of the ozone dosage. The increase of ozone dosage from
10 ml/min to 30 ml/min lead to an increase of the decolorization rate
from 72.6% to 92.15%. However, higher ozone dosage made the
decolorization rate increase very slightly. The reason for this
phenomenon is that ozone can transfer from gas phase to liquid
Fig. 2. Effect of the initial concentration of rhodamine B on the dye decolorization by
ozonation. PH = 3, applied ozone dosage = 30 ml/min.
86 B. Cuiping et al. / Desalination 278 (2011) 84–90
Fig. 3. Effect of zone dosage on the dye decolorization of rhodamine B. PH = 3, [RhB] =
100 mg/l.
phase and generate HO⋅ radicals [7,11,19]. Increasing the ozone
dosage can get more HO⋅ radicals and enhance the decolorization rate
of rhodamine B. When the ozone concentration in the liquid phase is
saturated, an excess ozone dosage cannot enhance the decolorization
of rhodamine B since the solubility of ozone is constant at a certain
temperature and a higher than optimum dose means that the
concentrations of hydroxyl free radicals and ozone in solution are
close to invariant [7].
3.3. Effect of initial pH
The effect of the initial pH on the decolorization of rhodamine is an
important parameter in ozone process. In general, ozone oxidation
pathways include direct oxidation by ozone and radical oxidation by
HO⋅ radical. Direct oxidation is more selective and predominates
under acidic conditions [20], while radical oxidation is less selective
and predominates under basic conditions [7]. A range of pH from 2 to
10 was investigated in the reaction. The results were shown in Fig. 4. It
was found that the removal of rhodamine B increased with the
decrease of pH. The pH value increased from 2 to 10, and the
decolorization rate of rhodamine B decreased from 85.64% to 77.73%
after 10 min. The reason that the decolorization rate in acid condition
is better than in alkali condition is that high pH in the solution leads to
the creation of more free radical scavengers (i.e. CO32−, HCO3−, etc.)
derived from mineralization of organic material, resulting in a
decrease in the concentration of HO⋅ radical [11,21].
Fig. 4. Effect of pH on the dye decolorization of rhodamine B. [RhB] = 100 mg/l, applied
ozone dosage = 30 ml/min.
3.4. Decolorization of rhodamine B by US/ozone
The ozonation reaction pathway strongly depends on the
characteristics of the wastewater, such as initial pH, initiators and
promoters in the reacting medium. Ultrasonic is an important assisted
method in the ozone process. The enhancement of organic compound
degradation via the coupling of ultrasound and ozone has been
investigated previously [13,22]. The different frequencies of ultrasonic
were studied to investigate its effect on the decolorization of
rhodamine B. Fig. 5 showed that the decolorization rate of rhodamine
B was improved with the increase of the frequencies of ultrasonic and
the decolorization rates were 89.02%, 94.05% and 95.24% after 10 min
respectively in frequency of 20 kHz, 45 kHz and 80 kHz. The results
showed that the high frequency of ultrasonic could improve the
decolorization rate. This trend was similar with many literatures
[11,22]. The reason is that the rate of formation of hydrogen peroxide
would be higher and more violent and quicker collapse of the cavities
at higher frequencies of ultrasonic [22]. However the improving
efficiency of ultrasonic will enhance very little, after the frequency up
to a specific value. The pH value ranged from 3 to 10 was researched to
investigate the US/ozone oxidation reaction pathways of rhodamine
B. The results are presented in Fig. 6, where it was shown that a higher
decolorization was presented in acid condition than in alkaline
condition and the decolorization rates of rhodamine B were 94.05%
and 84.2% respectively at pH = 3 and pH = 10 after 10 min. The trend
is similar with the single ozone effect that acid condition is more
favorable for the decolorization of rhodamine B. However, higher
decolorization efficiencies were discovered in US/ozone system than
in single ozone, which indicated that the ultrasonic can enhance the
decolorization rate at both pH. The reason for this phenomenon is due
to the generation of hydroxyl radical from ozone coupling with
ultrasonic and the color removal could be simply achieved via both
reaction pathways of ozone. Ozone coupling with ultrasonic can lead
to a variety of radical formation reaction as shown in Eqs. (1)–(6) [22].
Þ
ÞÞ
H2 O· → HO2 · + O· + HO· ð1Þ
HO2 ⋅ þ H⋅→H2 O2 ð2Þ
2HO⋅→H2 O2 ð3Þ
H2 O2 þ O3 →HO2 ⋅ þ HO⋅ þ O2 ð4Þ
Fig. 5. Effect of different frequencies of ultrasonic on the dye decolorization of
rhodamine B. [RhB] = 100 mg/l, pH = 3, applied ozone dosage = 30 ml/min.
 B. Cuiping et al. / Desalination 278 (2011) 84–90
Fig. 6. Effect of pH on the dye decolorization of rhodamine B in US/ozone. [RhB] =
100 mg/l, applied ozone dosage = 30 ml/min, applied ultrasonic frequency = 45 kHz.
HO2 ⋅ þ O3 →HO⋅ þ 2O2 ð5Þ
HO⋅ þ O3 →HO2 ⋅ þ O2 ð6Þ
3.5. Decolorization of rhodamine B by UV/ozone
UV light is an initiator which can promote the transfer of ozone to
more hydroxyl radicals and enhance the degradation of the pollutants.
This result has been proved in many literatures [3,23,24]. The power
of UV lamp in 8 W, 16 W and 32 W was researched to investigate its
effect on the decolorizaton of rhodamine B. Fig. 7 showed that the
decolorization rate of rhodamine B was very similar in the three
power and the decolorization rates were 97.45%, 97.76% and 97.76%
respectively in power of 8 W, 16 W and 32 W after 10 min. It proved
that the power of UV lamp has less effect on the decolorization of
rhodamine B in UV/ozone process. To illustrate the effect of pH in the
UV/ozone treatment and the reaction pathway of the system, the pH
was adjusted to 3, 7 and 10, respectively. The results were presented
in Fig. 8. It is apparent that the decolorization rate of rhodamine B
decreased with the increase of the initial pH. About 97.76% and 88.35%
decolorization at 10 min were observed at pH = 3 and pH = 10,
Fig. 7. Effect of different power of ultraviolet on the dye decolorization of rhodamine B
in US/ozone. [RhB] = 100 mg/l, pH = 3, applied ozone dosage = 30 ml/min.
87
Fig. 8. Effect of pH on the dye decolorization of rhodamine B in UV/ozone. [RhB] =
100 mg/l, applied ozone dosage = 30 ml/min, applied ultraviolet power = 16 W.
respectively. It had the same results with single ozone and US/ozone
processes that acid condition was optimized. However, higher
decolorization efficiencies were discovered in UV/ozone process. At
pH = 3, the decolorization rates of rhodamine B were 86.86%, 94.05%
and 97.76% respectively in ozone process, US/ozone process and UV/
ozone process during 10 min. UV/ozone process was the most
favorable for the decolorization of rhodamine B among three methods
and the decolorization can reach 99.78% after 15 min. The reason for
this phenomenon is that the ozone coupling with the UV light can
produce more hydroxyl radicals than in the case of only indirect
ozonation and also color removal was via both reaction pathways of
ozone [25]. According to the reaction pathway, one molecule ozone
produce two hydroxyl radicals in the UV/ozone process, which is two
times than that in US/ozone.
1
O3 þ hν→Oð DÞ þ O2 ð7Þ
1
Oð DÞ þ H2 O→H2 O2 ðhotÞ ð8Þ
H2 O2 ðhotÞ→2⋅OH ð9Þ
H2 O2 ðhotÞ→H2 O2 ð10Þ
H2 O2 þ hν→2⋅OH ð11Þ
3.6. The UV-visible absorption spectra analysis
In order to investigate the change in the molecule of rhodamine B
with the reaction time in the three methods, UV-VIS spectra changes
in the dye solution were observed and the corresponding spectra are
shown in Fig. 9. It is showed that the characteristic absorption peak of
rhodamine B in solution had two bands; the main band was in the
visible region, with its maximum absorption at 554 nm, and the other
band in the ultraviolet region located at 350 nm. The characteristic
absorption peak is attributed to the dye chromophore structure. In the
three systems, there were the same phenomena that the absorption
intensity of rhodamine B in solution became weaker along with the
reaction time. It can be explained that the aromatic ring structures of
88 B. Cuiping et al. / Desalination 278 (2011) 84–90

the initiator of the ozonation and the degradation rates were better
than that in the single ozone degradation. On the other hand, the
efficiency of ultraviolet catalysis was better than that of ultrasonic.

3.7. Comparison of COD removal in ozone, US/ozone and UV/ozone

It is known that complete decolorization of rhodamine B does not

mean that it is completely mineralized. In order to know the
mineralization degree of rhodamine B by the three methods, COD
was investigated during the reaction. During the ozone oxidation
reaction, small value of H2O2 could be found, which probably had an
effect on the COD. The concentration of H2O2 was detected with
peroxide test after the oxidation reaction and the data were about
5 mg/l. On the other hand, the standard solution of H2O2 (5 mg/l) was
detected for COD as about 0 mg/l, which was the same as the distilled
water, so the effect of H2O2 on COD was ignored. The results of COD
are shown in Fig. 10 and Table 1. Fig. 10 showed that after 15 min
treatment, the COD removal effect was 35.72%, 42.97% and 47.43% in
ozone, US/ozone and UV/ozone process, respectively. It is apparently
found that rhodamine B was not mineralized completely in these
three processes. Ultrasonic and UV light can improve the COD removal
effect. This result proves that single ozone process can produce
hydroxyl radical, but the production efficiency of hydroxyl radical is
less than that of catalytic processes. It demonstrated that single ozone
treatment showed a limited mineralization of organic compound in
the dye solution [26,27]. However, promoted by ultrasonic and UV
light, ozone can generate more hydroxyl radical and get better
degradation effect, since the hydroxyl radical is a very powerful
oxidizing agent which can deal with organic compounds until
mineralized [27,28].
Table 1 showed the decolorization efficiency and the COD removal
efficiency of rhodamine B after 10 min treatment. It showed the same
trend between the decolorization efficiencies and the COD removal
efficiencies in the three processes. However, the decolorization
efficiency was much higher than the corresponding COD removal
efficiency. The COD removal efficiencies were only 21.43%, 32.14% and
39.72% in the three processes, while the corresponding decolorization
efficiencies were 86.86%, 94.05% and 97.76% after 10 min. The reason
is probably that the chromophore has been destructed completely,
but the organic pollutant has been oxidized to micromolecule
pollutants, which have not been oxidized to CO2 and H2O. By the
detection of GC-MS, the reaction products of rhodamine B were
mainly formic acid (M = 46), acetic acid (M = 60) and N, N-
diethylformamide (M = 101) in this ozonation process, which can
be biodegraded [8]. In ozone-based oxidation, the removal efficiency

Fig. 9. UV-VIS spectra changes of rhodamine B with three methods after different
reaction time (A) UV/ozone, (B) US/ozone, (C) ozone.

rhodamine B molecules were destructed in the ozonation. However,

there were some differences in the reaction rate of rhodamine B. In
the UV/ozone process, the absorption peak quickly diminished and
disappeared in 20 min and the decolorization rate was the highest in
the three processes during the same reaction time. The second one
was the US/ozone process and the single ozonation was the last one.
The absorption peak of rhodamine B at 350 nm had the same trend
with the 554 nm. These results were in agreement with the above
outcomes and further proved that the ultraviolet and ultrasonic were Fig. 10. COD removal of rhodamine B during three ozonation processes.
 B. Cuiping et al. / Desalination 278 (2011) 84–90
Table 1
Comparison of decolorization and COD removal of rhodamine B (10 min treatment).
process Decolorization efficiency (%) COD removal efficiency (%)
Ozone 86.86 21.43
US/ozone 94.05 32.14
UV/ozone 97.76 39.72
of COD had been largely enhanced and the reaction time was much
shorter than that of the other methods reported before [15–17].
3.8. The reaction kinetic study on ozone-based processes
The degradation and decolorization kinetics of rhodamine B in
aqueous solution were investigated, using ozone-based processes
under various optimum conditions. The pseudo-first-order kinetic
Eq. (12) was employed to compare the effect of reaction in the three
ozonation processes.
lnðC0 = C Þ = kt
Where C0 is the initial concentration of rhodamine B and C is the
concentration of rhodamine B at time t, k is the degradation rate
constant, and t is the degradation time. The calculated kinetic
parameters of degradation and decolorization using different ozone
process are listed in Table 2.
From Table 2, it is shown that the decolorization and degradation
reaction obeyed the pseudo-first order kinetics. The calculated
Kdecolorization and Kdegradation of rhodamine B were the highest in UV/
ozone processes and the lowest in single ozone processes. It was
concluded that the UV/ozone process was the most efficient and the
ozone process was the least efficient. These results are consistent with
the discussion concerning the decolorization and degradation of
rhodamine B in the previous section.
4. Conclusions
The treatment of rhodamine B in aqueous solution has been
investigated by ozone-based processes. Under the optimum condi-
tions, the decolorization rate of rhodamine B increased with the ozone
dosage, but decreased with the initial concentration of rhodamine B in
the ozone process. The decolorization rate was more efficient in acid
medium in all ozone-based methods. Rhodamine B decolorization and
its COD removal efficiencies were in the decreasing order of UV/
ozone N US/ozone N ozone and UV/ozone was the best ozone-based
oxidization process. The decolorization of rhodamine B in ozone-
based processes was much higher than that in COD removal efficiency.
And GC-MS spectra showed that the reaction products were mainly
formic acid, acetic acid and N,N-diethylformamide. By analysis of the
UV-VIS spectra, the reaction rate in UV/ozone was faster than in the
other processes, and US/ozone was the second one. The catalyst in
ozonation reaction can enhance the efficiency of decolorization and
degradation of rhodamine B. The UV/ozone process was the optimum
candidate for dye degradation in wastewater treatment and this study
provided a new method for the effective degradation of dyes in
wastewater. The decolorization and degradation reaction obeyed the
pseudo-first order kinetics in all ozone-based processes. Finally,
Table 2
Pseudo-first order rate constants for decolorization and degradation of rhodamine B in
ozone-based processes.
Process Kdecolorization (min−1) R2 Kdegradation (min−1)
Ozone 0.5214 0.9955 0.0712
US/ozone 0.6789 0.9895 0.0847
UV/ozone 0.7487 0.9961 0.0943
89
ozone-based process is suitable for the treatment of dye wastewater.
It is environmentally friendly since no toxic reagents and secondary
pollution could be found. Among these methods, the UV/ozone
system is most effective and less expensive than convention
processes.
Acknowledgements
This research was financially supported by the National Natural
Science Foundation project (No. 20872075) and Hubei Key Laboratory
of Pollutant Analysis and Reuse Technology Open Fund Project (No.
KY2010G19).
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