Journal of American Science 2010;6(10)

Comparative Study of Oxidation of Some Azo Dyes by Different

Advanced Oxidation Processes: Fenton, Fenton-Like, Photo-Fenton
and Photo-Fenton-Like
S.A.Abo-Farha

Chemistry Department, Faculty of Science, Al-Azhar University (Girls), Nasr City, Cairo, Egypt
E-mail: [email protected]

Abstract: This study makes a comparison between Fenton, Fenton-like, photo-Fenton and photo-Fenton-like
treatment methods to investigate the removal of two acid dyes. The two selected acid dyes are C.I. Acid Orange 8
(AO8) and C.I. Acid Red 17 (AR17). These were chosen as model organic contaminants. The effect of operating
parameters, such as amount of Fenton’s reagent (H2O2 and Fe2+) and Fenton’s-like reagent (H2O2 and Fe3+),
hydrogen peroxide concentration, the two azo dyes concentration and the solution pH have been studied. Results
indicated that simultaneous utilization of UV irradiation with Fenton’s and Fenton’s-like reagent increase the
degradation degree (DD%) of (AO8) and (AR17). The dyes quickly lose their color, indicating that the dissolved
organics have been oxidized. The dye degradation is dependent upon, concentrations of Fenton’s and Fenton’s-like
reagents, H2O2 concentration, dyes concentration and the solution pH. Decolorization efficiency observed in the
order of photo-Fenton>photo-Fenton-like>Fenton>Fenton-like for the two azo dyes. The color removal was found
also to depend on the dye structure. Mono sulphonic azo dye (AO8) was degraded faster than disulphonic azo dye
(AR17). The results indicated that the treatment of the two azo dyes with four advanced oxidation processes (AOPs)
were efficient at optimum conditions. [Journal of American Science. 2010, 6(10):128-142]. (ISSN: 1545-1003).

Keywords : Advanced oxidation processes (AOPs); Azo dyes; Dye degradation; Fenton’s reagent; Fenton’s-like
reagent

1. Introduction during the dyeing process needs more effort to be

Synthetic dyes are present in many spheres studied and investigated [10,11].
of our everyday life and their application are Conventional treatment methods in the
continuously growing, e.g., in various branches of the textile dyeing industry for color removal include
textile industry, of the leather tanning industry, in coagulation/flocculation, and activated carbon
paper production, in food technology, in agricultural adsorption[12,13]. Both coagulation and adsorption
research, in light –harvesting arrays, in photo- generate large amounts of sludge and waste which
electrochemical cells, and in hair colorings. Moreover need further treatment for disposal. Biotreatment is
synthetic dyes have been employed for the control of still considered as an appropriate method for meeting
the efficacy of sewage and wastewater treatment, discharge standard but it still remains a color
etc.[1-5]. Dyes make our world beautiful, but they problem. Also, ozonation[14] effectively decolorizes
bring pollution. Wastewaters originating from dyes dyes but does not remove COD well and may
production and application industries pose a major produce exhausted ozone in the water and thereby,
threat to surrounding ecosystems, because of their increase the cost of treatment.
toxicity and potentially carcinogenic nature [6-8]. A The limitations of conventional wastewater
part from the aesthetic problems relating to colored treatment methods can be overcome by the
effluent, dyes also strongly absorb sunlight, thus application of the so-called advanced oxidation
impeding the photosynthetic activity of aquatic plants processes (AOPs)[15] defined by Glaze et al. [16],
and seriously threatening the whole ecosystem[9]. So which present a potential alternative to decolorize and
there is a clear need to treat dye wastewater prior to to reduce recalcitrant colored wastewater loads[15].
discharge into the effluent. Most of pollutants, except AOPs are based on the generation of very reactive
color, can be reduced by chemical, physical or species such as [17] hydroxyl radicals ( OH ), which
biological methods. Therefore, the color problem of have a very strong oxidative potential [E=+2.80v),
some textile wastewater caused by the residual dyes second only to fluorine. Hydroxyl radicals rapidly
and nonselectively oxidize a broad range of organic

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 Journal of American Science 2010;6(10)

pollutants[18]. Common AOPs involve Fenton, reagent is more effective than Fenton-like reagent
Fenton-like, photo-Fenton processes, ozonation, [32]. The above sequence of reactions begins very
photo chemical and electrochemical oxidation, quickly if there is an abundant supply of H2O2 and
photolysis with H2O2 and O3, high voltage electrical dye. In cases, though, where reactants are in small
discharge (corona) process, TiO2 photocatalysis, concentrations (<10 – 25 mg/L H2O2), the use of Fe2+
radiolysis, wet oxidation, water solutions treatment is more effective [33].
by electronic beams or -beams and various
combinations of these methods [19-23]. This reaction scheme is very attractive
Fenton’s oxidation, one of the ‘oldest’ because Fe2+ or Fe3+ ions reagents are inexpensive,
AOPs, is relatively cheap, easily operated and while H2O2 is also relatively inexpensive and is
maintained[9,24-27]. It has the advantages of both environmentally safe. Two disadvantages of the
coagulation and catalytic oxidation, as well as being method are: the highly to moderately acidic
able to generate oxygen in water. Fenton and photo- environment (pH 2-5) which has to be used, and the
Fenton type processes have proven to yield very good need to recover the Fe2+ or Fe3+ ions at the end of the
results either for complete mineralization of azo dyes treatment. Major potential applications of this method
results in the cleavage of the nitrogen double bond or are in the treatment of effluents from the textile
for their transformation into less complex structures industry, as well as from the cosmetic, pesticide and
that are more easily biodegradable[28-30]. detergent producing industries [33].

The Fenton reagents involve the application Due to its slow dissociation rate in the dark,
of ferrous ions to react with hydrogen peroxide the generation of hydroxyl radicals was reduced. It is
producing hydroxyl radicals ( OH ) with powerful obvious that the most effective AOPs for treating dye
oxidizing ability to degrade organic pollutants [6]. solutions is a UV-enhanced H2O2/Fe2+ and H2O2/Fe3+
The Fenton reagent has been known for more than a solutions [15]. The high removal efficiencies of this
century and has proved to be a powerful oxidant. The method can be explained by the fact that oxidation
mechanism of the Fenton reaction is still under reaction are coupled to coagulation occurring due to
intense and controversial discussion. Generation of the presence of ferrous/ferric cations, thus these
OH radicals by the dark reaction of H2O2 with ferrous metallic ions play a double role as a catalyst and a
salt has been the subject of numerous studies during coagulant in the process.
the last decade [26].This method seems to decolorize
dyes with a variety of molecular structures. Moreover, in the Fenton process the
hydrogen peroxide reacting with ferrous ions forms a
The general mechanism using Fenton strong oxidizing agent (hydroxyl radical), whose
reagents, via which the hydroxyl radicals are oxidation potential is higher than that of ozone (2.8 V
produced, is a number of cyclic reactions, which compared to 2.07V).
utilize the Fe2+ or Fe3+ ions as a catalyst to
decompose the H2O2. These ions are regenerated in In Fenton-like reaction, ferric ions react with
their original state at the end of the cyclic reactions H2O2 to produce ferrous ions at very slow rate (k=
according to the following scheme of reactions [31]: 0.001 – 0.01 M–1s–1) few ferrous ions can be formed
and thus induce the Fenton reaction. Therefore, only
Fe2+ + H2O2 Fe3+ + OH– + OH (1) one process with Fe3+/ H2O2 reaction will
dominate[34].
Fe2+ + OH Fe3+ + OH– (2)
Fe3+ + H2O2 Fe-OOH2+ + H+ (3) The aim of this study is to examine in detail the
Fe-OOH2+ Fe2+ + OOH (4) effect of major system parameters on the
Fe2+ + OOH Fe3+ + ŌOH (5) decolorization kinetics and compare the
decolorization kinetics of the two dyes (C.I. Acid
Fe3+ + OOH Fe2+ + O2 + H+ (6) Orange 8 and C.I. Acid Red 17). The parameters,
H2O2 + O H H2O + OOH (7) which are examined separately, are the concentration
of Fe2+ (Fenton process), Fe3+ (Fenton-like process),
More than 25 reactions occur, several the concentration of H2O2, the initial dye
involving the dye molecule, but the above seven are concentration and the solution pH. In addition, for
the most significant involving ions and radicals. comparative reasons, the effect of the use of UV
When a Fenton-like reagent is used, the sequence of irradiated Fenton reagent (photo-Fenton process) and
reaction begins with reaction (3). There are many also UV irradiation Fenton-like reagent (photo-
bibliographic sources which report that Fenton

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 Journal of American Science 2010;6(10)

Fenton-like process) on the decolorization kinetics of meter, the Fe2+ or Fe3+ ions were quickly added
the two azo dyes are also examined. to the dye solution. At various intervals, samples
were quickly withdrawn for spectrometric
2. Experimental analysis in case of before and after UV
Samples of acid textile dyes C.I. Acid irradiation. The absorption spectra of the
Orange 8 (monosulphonic acid dye), were obtained prepared solutions were recorded using Perkin
from (ciba clayton limited, Manchester, England], Elmer-lambda spectrophotometer model 201
and C.I. Acid Red 17 (disulphonic acid dye) from (Germany). Irradiation used with microsol light
(ICI, Chemical Limited Imperial Industries). Their fastness tester equipped with a pre-stable timer
structures are depicted below. and water color jacket ( BS 1006 UK-TN ) filed
+
SO3Na

N +
CH3 SO3Na
N N O
+ H
NaO3S N O
H
C.I. Acid Orange 8
C.I.Acid Red 17
(Mol. wt. 364.360 g and max 490 nm) (Mol. wt. 502. 436 g and max 518 nm)

Other reagents namely, hydrogen peroxide with 400 WMB7V lamp (Images H. Heal & Co. Ltd.
(30% w/v), FeSO4. 7H2O, FeCl3. 6H2O, HCl and Halifax England) high pressure Hg lamp, was used in
NaOH were of A.R. grade (from Merck). The effect order to stimulate day light, which is congenital for
of initial pH on treatment efficiency of the two azo such photooxidation studies. All the measurements
dyes were investigated, see Table (1). This was done were performed at room temperature. The color and
with the pH range of 2-6 when initial concentration decolorization ratios were measured with
of Fe2+ or Fe3+ and H2O2 were 1 x 10–5 M and 10 mM spectrophotometric technique and calculated
respectively, and at fixed dye concentration according to the literature [35]. This was done by
(1x10–5M). monitoring the absorbance change at max of
In an attempt to determine the effect of Fe2+, maximum peaks for each dye. The estimation of
3+
Fe and H2O2 concentrations on Fenton’s and decolorization degree (DD) was done according to
Fenton’s-like treatment, the amount of Fe2+ and Fe3+ the relation (8).
added was changed between 5 x 10–6 to 1 x 10–4M Ai  A t
when H2O2 concentration was kept constant at 10mM DD% = x 100 (8)
for Acid Orange 8 and 5,2 mM for Acid Red 17 in Ai
Fenton and Fenton-like process respectively. The Where, Ai is the initial intensity of color and At is the
amount of H2O2 added was changed between 2 and intensity of color at t time of the oxidation.
50 mM when Fe2+ or Fe3+ concentration was kept
constant at 1x10–5M for the two dyes. The effect of 3. Results and Discussion
initial dye concentration was also investigated 3.1. Fenton and photo-Fenton processes
between 1 x 10–5 to 1 x 10–4 M when H2O2 3.1.1. Effect of initial Fe2+ concentration
concentration and Fe2+ or Fe3+ ion concentrations and Dye degradation efficiency by Fenton process is
pH were fixed. The optimum dosages, which gave influenced by the concentration of Fe2+ ions which
better results in color removal, were selected based catalyze hydrogen peroxide decomposition resulting
on the results of the preliminary experiments, and as in OH radical production and consequently the
shown in (Table 1). degradation of organic molecule. According to the
Firstly, the H2O2 was added to the dye literature [6], increasing ferrous salt concentration,
solution and then the pH was adjusted to the desired degradation rate of organic compound also increases,
value by the addition of a few drops of either HCl or to certain level where further addition of iron
NaOH. Following the pH adjustment using a pH- becomes inefficient [16].

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 Journal of American Science 2010;6(10)

The effect of Fe2+ concentration on color reactive species than hydroxyl radicals and thus
removal was examined by changing the Fe2+ directly influence the efficiency of dye degradation.
concentration between 5x10–6 to 1x10–4M while During the determination of optimum H2O2 dose,
keeping the concentration of H2O2, pH and dyes studies were conducted at constant Fe2+ dosage as 1.0
concentration constant ([H2O2]=10mM for Acid x 10–5 M, at pH 3.0 and dye concentrations 1.0x10–5
Orange 8 and 5 mM for Acid Red 17, pH 3.0 and M for the two dyes. Varied dosages of H2O2 from
[dye]= 1x10–5M). Fig. 1a & b show that as Fe2+ doses 2mM to 50 mM were applied, see Table (1).
were increased from 5 x 10–6 to 5 x 10–5M, the Efficiencies of color removal of Acid Orange 8 in
removal % increased from 10% to 75% for Acid Fenton and photo-Fenton processes at varied dosages
Orange 8 and from 15% to 65% for Acid Red 17 at of H2O2 and constant concentration of Fe2+ are
30 minute. Hence, it can be said that higher ferrous illustrated in Fig. 2 as an example. The same results
doses lead to the generation of more OH radicals. It are obtained in case of Acid Red 17. The results
also shows that higher ferrous doses not only make showed that the color removal efficiencies for Fenton
the redox reaction complete but also cause is 10mM H2O2 and about 38% color removal at 45
coagulation resulting in improved removal. At higher minute while the better removal efficiencies were
doses, the efficiency decrease indicating that H2O2 reached with the photo-Fenton process to 100% at 27
becomes the limiting factor for further OH minute by using the same dosage of H2O2 (10mM).
generation [16]. The better removal efficiency for Acid Red 17 was
The existing results show that the system, 5mM for both Fenton and photo Fenton processes at
when operated with a source of UV light at the same the same conditions.
conditions for the two dyes, can be optimal for
complete textile wastewater decolorization and 3.1.3. Effect of initial dye concentration
mineralization. The best experimental results for the The effect of initial dyes concentration
photo-Fenton process proved the following: the (Acid Orange 8 and Acid Red 17) on the
removal of color was accomplished at two different decolorization degree at the optimum pH, Fenton
rates. A quick oxidation during the first 10 and 23 reagent concentration and H2O2 dosage, were studied
min (85%) for Acid Orange 8 ([Fe2+] = 2 x 10–5M and in both Fenton and photo-Fenton processes see
Acid Red 17 [Fe2+] =1x10–5M) respectively followed (Table 1). As an example, Dyes concentrations were
by a much slower reaction. At 47minute complete varied from 1x10–5 M, to 1 x 10–4M (Fig. 3) for Acid
removal occur for Acid Orange 8, while at 60 minute Orange 8. Fig. 3 shows that with the increase in dye
95% (decolorization degree) for Acid Red 17. It can concentration, the time required for degradation also
be hypothesised that in analogy to the oxidation with increases. At low concentration of dye, the
ozone, during the photo-Fenton process the percentage conversion is higher compared to that at
substances which are easy to oxidize are also higher concentration [16]. A quick oxidation during
removed readily. The reactions which occur in the the first 15 minute for Acid Orange 8 was followed
first step of the photo-Fenton process, a part from by a much slower reaction for the photo-Fenton
coagulation, are thus among those leading to process. At the optimum conditions for the two dyes,
modification of the structure of the dye, an the best dye concentration was equal to 1.0 x 10–5 M.
observation which can be confirmed by the rapid The color removal for Acid Orange 8 and Acid Red
decolorization of the solution at the outset of the 17 are 85.5% and 71% at 50 minute for Fenton
process [15]. processes while, the removal are 98.5% and 83% at
50 minute for photo-Fenton process for the two dyes
3.1.2. Effect of the H2O2 concentration respectively. Further decrease in the dye
Concentration of hydrogen peroxide is one decolorization in high concentrations of dye was
of the operating parameters that significantly probably due to the formation of dimmer
influence the final mineralization extent. With further molecules[37] through a sequence of reactions from
increasing hydrogen peroxide concentration, single dye molecules. Decolorization of the dimmer
degradation efficiency also increases with the molecule is more difficult, leading to the leveling off
achievement of certain optimal Fenton reagent ratio. color removal.
With further increasing of hydrogen peroxide
concentration, degradation efficiency is decreasing 3.1.4. Effect of initial pH
due to the scavenging nature of hydrogen peroxide Fenton oxidation is known as a highly pH
towards OH radicals eq.(7) when it is present in dependent process since pH plays an important role
higher concentration [36]. The result is the formation in the mechanism of OH production in the Fenton’s
of perhydroxyl radicals which are significantly less reaction [29]. At high pH (pH > 4), the generation of
OH gets slower because of the formation of the ferric

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 Journal of American Science 2010;6(10)

hydroxo complexes. The complexes would further 3.2.2. Effect of H2O2 concentration
form [Fe(OH)4] when the pH value is higher than 9.0 Concentration of H2O2 plays a more crucial
[38]. On the other hand, at very low pH values (<2.0) role in the overall efficiency of the degradation
hydrogen ions acts as OH radical-scavengers. The processes. Usually it has been observed that the
reaction is slowed down due to the formation of percentage degradation of the pollutant increases with
complex species [Fe (H2O)6]2+, which reacts more an increase in the dosage of H2O2 [24, 27, 28], but
slowly with peroxide compared to that of excess quantities are not recommended [40]. During
[Fe(OH)(H2O)5]2+. In addition, the peroxide gets the determination of optimum H2O2 dose, studies
solvated in the presence of high concentration of H+ were conducted at constant Fe3+ dose as 1.0 x 10–5 M,
ions to form stable oxonium ion [H3O2]+. An at pH 3.0 and dyes concentration 1.0 x 10–5 M.
oxonium ion makes peroxide electrophilic to enhance Varied dosage of H2O2 from 2mM to 50 mM were
its stability and presumably substantially reduces the applied. As demonstrated from the results, the better
reactivity with Fe2+ ion [32]. Therefore, the initial pH color removal efficiencies for Acid Orange 8 and
value has to be in the acidic range (2-4) to generate Acid Red 17 were obtained at concentration of 10mM
the maximum amount of OH to oxidize organic and 2mM H2O2 respectively see (Table 1). The colour
compounds [39]. In this study, optimum pH value removal for Fenton-like process reached 30% at 60
was determined for two acid dyes (Acid Orange 8 minute and was enhanced to reach 96% at 60 minute
and Acid Red 17). During this determination, pH was for Acid Orange 8 in photo-Fenton-like process. On
adjusted between 2 and 6 and efficiencies of color the other hand color removal in Acid Red 17, reached
removal (decolorization degree % (DD%)) were 35% at 60 minute and was enhanced to reach 85% at
observed. Maximum color removal efficiencies were the same time by photo-Fenton-like process.
obtained at pH 3.0, for the two dyes and in case of
Fenton and photo-Fenton processes. At pH 3.0 3.2.3. Effect of initial dye concentration
[dye] = 1 x 10–5 M, [Fe2+]=1x10–5M and [H2O2] = It has been found that with the increase in
10mM, the color removal gives the best results dye concentration, the time required for degradation
compared with the other pH’s. In Fenton processes also increases. At low concentration of dye, the
23% and 19% for AO 8 and AR 17 respectively were percentage conversion is higher compared to that at
observed at 27 minute. This result was enhanced to higher concentration [16]. The effect of the initial
100% and 83% at the same time for the two dyes concentration of dyes introduced in the reaction
respectively by using the photo-Fenton process under mixture on color removal for the two dyes was
the described experimental conditions. studied. This was conducted at pH 3.0, 10mM H2O2
for Acid Orange 8 and 2mM H2O2 for Acid Red 17
3.2. Fenton-like and photo-Fenton-like processes and 1 x 10–4 M Fe3+ for Acid Orange 8 and Acid Red
3.2.1. Effect of initial Fe3+ concentration 17.Dye concentrations were varied from 1 x 10–5 to
The effect of the initial concentration of Fe3+ 1x10–4 M see (Table 1). The optimum dye
introduced in the reaction mixture on color removal concentrations were 1 x 10–5 M for the two dyes. The
for the two dyes is presented in Fig. 4a,b . Such effect color removal in Fenton-like process reached 91% at
is measured at pH 3.0, 1.0 x 10–5 M dyes 30 minute and further reached 96% at 60 minute,
concentration and 10mM H2O2 for Acid Orange 8 while in photo-Fenton-like process the color removal
and 2mM H2O2 for Acid Red 17. The figure shows reached 90% at 10 minute and increased to 96% at 60
that a wide range of Fe3+ concentrations (5.0x10–6M minute for Acid Orange 8. In case of Acid Red 17
to1.0x10–4 M) can be used. The optimal Fe3+ efficiency of color removal reached 85% at 30
concentration for Acid Orange 8 was 1.0 x 10–4 M in minute, while in photo-Fenton-like process the color
both Fenton-like and photo-Fenton-like process. The removal reached 97.5% at 12 minute and increased to
color removal in Fenton-like process was fast where 99% at 55 minute.
(90%) was reached at the first 27 minute while 96%
was reached at 60 minute. In photo-Fenton-like
process the removal reached 91% at 15 minute and
reached 96.5% at 60 minute. The optimum Fe3+
concentration was 1x10–4 M for Acid Red 17 in both
Fenton-like and photo-Fenton-like processes and the
same behavior was observed. Photo-Fenton-like
process enhances only the color removal at first 12
minute (98% removal) and increases slightly to 99%
at 55 minute.

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 Journal of American Science 2010;6(10)

100 (a) 100 (b)

80 2+
2+ 80 [Fe ]M
[Fe ] M -6
-6 5 x 10
5 x 10 -5
-5 1 x 10
60 1 x 10 60 -5
2 x 10
DD%

-5

DD%
2 x 10 -5
5 x 10
-5 5 x 10
-4
40
1 x 10
-4
40
1 x 10

20
20

0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 0
0 10 20 30 40 50 60 70
Time(min)
Time (min)

Fig. (1): The degradation degree of (a) [AO8] and (b) [AR 17] = 1.0 x 10–5M with different initial
concentrations of Fe2+ in presence of [H2O2] =10mM for (AO 8) and 5mM for (AR 17) in Fenton (–)
and photo-Fenton (---) processes at pH3.0 .

100 100
[H2O2]mM
90
2
80 5 80 [dye] M
-5
10 70 1 x 10
-5
25 5 x 10
60 -5
60 50 7 x 10
DD%

-4
50 1 x 10
DD%

40
40
30
20
20 10
0
0 0 10 20 30 40 50 60 70
0 5 10 15 20 25 30 35 40 45 50 Time (min)
Time (min)

Fig. (2): The degradation degree of [AO 8] = 1.0 x Fig. (3): The degradation degree of different initial
10–5M with different initial concentrations concentrations of (AO8) in presence of
of H2O2 in presence of [Fe2+] =1.0 x 10–5M, [H2O2]=10mM, [Fe2+] = 2 x 10–5M, in
in Fenton (–) and photo-Fenton (---) Fenton (–) and photo-Fenton(----) processes
processes at pH 3.0. at pH 3.0 .

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 Journal of American Science 2010;6(10)

(a) (b)
100
100 3+
[Fe ] M
-6
3+
[Fe ] M 5 x 10
80 -5
-6 80 1 x 10
5 x 10 -5
-5 2 x 10
1 x 10 -5
-5 5 x 10
60 2 x 10 60 -4
1 x 10

DD%
DD%

-5
5 x 10
-4
1 x 10
40 40

20
20

0
0 0 10 20 30 40 50 60 70 80
0 10 20 30 40 50 60 70 80
Time (min)
Time (min)

Fig. (4): The degradation degree of (a) [AO8] and (b) [AR17] =1.0 x 10–5M with different initial concentrations of
Fe3+ in presence of [H2O2] =10 mM for AO8 and 2mM for AR17 in Fenton-like (––) and photo-Fenton-like
(----) processes at pH 3.0.

Table (1) Optimum parameter concentrations for C.I. Acid Orange 8 and C.I. Acid Red 17
in Fenton and Fenton-like Processes.

C.I. Acid Orange 8 C.I. Acid Red 17

Fenton's- parameter Fenton's-like parameter Fenton's- parameter Fenton's-like parameter
Range of
Conc. Conc. Conc. Conc.
Parameter parameter
pH [Fe2+] [H2O2] [Dye] pH [Fe3+] [H2O2] [Dye] pH [Fe2+] [H2O2] [Dye] pH [Fe3+] [H2O2] [Dye]
study
M mM M M mM M M mM M M mM M

pH 2–6 - 1x 10 1x - 1x 10 1x - 1x 10 1x - 1x 10 1x
10–5 10–5 10–5 10–5 10–5 10–5 10–5 10–5
H2O2 Conc. 2 – 50 mM 3 1x - 1x 3 1x - 1x 3 1x - 1x 3 1x - 1x
10–5 10–5 10–5 10–5 10–5 10–5 10–5 10–5
Fe2+ or Fe3+ 5 x 10–6 – 3 - 10 1x 3 - 10 1x 3 - 5 1x 3 - 2 1x
Conc. 1 x 10–4 M 10–5 10–5 10–5 10–5
Dye Conc. 1 x 10–5 – 3 5x 10 - 3 1x 10 - 3 5x 5 - 3 1x 2 -
1 x 10–4 M 10–5 10–4 10–5 10–4

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 Journal of American Science 2010;6(10)

3.2.4. Effect of initial pH HO2 + OH H2O + O2 (10)

The dependence of the decolorization degree OH + OH H2O2 (11)
on the solution pH is similar for the two dyes
examined in both Fenton-like and photo-Fenton-like It can be postulated that H2O2 should be
processes. In highly acidic solutions (pH 2.0) the added at an optimum concentration to achieve the
decolorization rates become significantly slower with best degradation. Hence 10mM of H2O2 appears as an
decreasing pH while a similar behavior is also found optimal dosage for Fenton and photo-Fenton
in highly alkaline solutions[38]. The optimal pH was processes in case of Acid Orange 8 as an example.
3.0 for both two dyes. In Fenton-like process the
decolorisation degree for Acid Orange 8 and Acid 3.3.3. Dye concentration
Red 17 reached 26% and 20% respectively at 50 For Fenton and photo-Fenton processes it
minute and was enhanced to 95% and 93% at the was observed that the rate constant of degradation of
same time for photo-Fenton-like process. In photo- Acid Orange 8 and Acid Red 17 decreased with
Fenton like process color removal reached 90% and increasing the initial dye concentrations. As an
84% at the first 27 minute for Acid Orange 8 and example Fig. 10 shows, that at low concentration of
Acid Red 17 respectively see Fig. 5. Acid Orange 8, the rate constant is higher compared
to that at higher concentration. The presumed reason
3.3. Degradation kinetics is that when the initial concentration of the dye
3.3.1. Fe2+ + Fe3+ concentration increased, the hydroxyl radical concentration
The kinetic model of Acid Red 17 and the remained constant for all dyes molecules and hence
degradation rates of Acid Orange 8 and Acid Red 17 the removal rate constant decreased [9,44].
distinctly increased with increasing the amount of
Fe2+ for Fenton and photo-Fenton processes see Figs. 3.3.4. pH.
6 and 7a,b. In Fenton process addition of Fe2+ from 5 The highest rate constant values were
x 10–6M to 5 x 10–5M increases rate constant of obtained for the two systems for Acid Orange 8 and
reaction for the two dyes. In photo-Fenton process Acid Red 17 when increasing the pH to 3.0. Fig. 11
the increase is to 2 x 10–5 M for Acid Orange 8 and 1 shows that, the results are in agreement with those
x 10–5 M for Acid Red 17. In case of Fenton like and reported in previous studies [41].
photo Fenton like for the two dyes the calculated rate
constants increase to concentration of 1 x 10–4M see 3.4. Comparison with Fenton, Fenton-like, photo-
Fig. 8a,b. The rate constant began to decrease above Fenton and photo-Fenton-like processes for Acid
these concentrations range. It is known that the Fe+2 Orange 8 and Acid Red 17.
and Fe3+ have a catalytic decomposition effect on Fig. 12 presents a comparison between the
H2O2 [33,41]. When Fe2+ and Fe3+ increased the Fenton, Fenton-like, photo-Fenton and photo-Fenton-
catalytic effect also increased. When the like processes for the two dyes. In these process, the
concentration of Fe2+ was higher, a great amount of Fe2+ and Fe3+ concentration is the same and equal to
Fe2+ exited easily in the form of Fe(OH)2 in acidic 1.0 x 10–5 M, in presence of 10mM H2O2 and pH 3.0.
environment [42] therefore, the decreases in the The concentration of the two dyes is the same in all
degradation rate occured. experiments (1.0 x 10–5 M). Fig. 12, shows that the
use of Fenton reagent is effective than the use of
3.3.2. H2O2 concentration Fenton-like reagent for both dyes. This is due to
The effect of H2O2 concentration on the reaction sequence (1) through (7). Use of a Fenton-
degradation rates of Acid Orange 8 is shown in Fig. like reagent necessitates additional steps, reactions
9. The degradation rates were increased by increasing (3) and (4), in order to produce Fe2+. This must then
the concentration of H2O2. This can be explained by react with H2O2 to produce hydroxyl radicals.
the effect of additionally produced hydroxyl radicals. Regarding decolorization efficiency after 30
With increasing H2O2 concentration from 2mM to minute reaction time, the Fenton and Fenton-like for
10mM for Fenton and photo-Fenton processes, the the two dyes achieve nearly identical decolorization
rate constant increased but above this range the efficiencies. When the time increased the
improvement was not obvious. This may be due to decolorization efficiencies increased rapidly the order
recombination of hydroxyl radicals and also hydroxyl of color removal for the two dyes in Fenton and
radicals reaction with H2O2 contributing to the OH Fenton-like processes.
scavenging capacity (Eqs. 9-11) [15, 43].

H2O2 + OH H2O + HO2 (9)

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 Journal of American Science 2010;6(10)

100

80

pH 2.0
pH 3.0
60
pH 4.0
DD%

pH 5.0
pH 6.0
40

20

0 10 20 30 40 50 60 70
Time (min)

Fig. (5): The degradation degree of Acid Red 17 at different pH in presence of [dye] = 1 x10–5M
, [H2O2] = 10mM and [Fe3+]=1x10–5M in Fenton-like (–) and photo-Fenton like (---)
processes.

0.2
0.0
-0.2
2+
-0.4 [Fe ]M
-6
-0.6 5 x 10
-0.8 -5
1 x 10
-1.0 -5
2 x 10
-1.2 -5
-1.4 5 x 10
ln At/Ai

-4
-1.6 1 x 10
-1.8
-2.0
-2.2
-2.4
-2.6
-2.8
-3.0
-3.2

0 10 20 30 40 50 60 70
Time (min)

Fig. (6): Kinetic of photodegradation of [AR17] = 1.0 x 10-5 M at different initial

concentrations of Fe2+ in presence of [H2O2] = 5mM in Fenton (–) and photo-Fenton
(---) processes at pH 3.0.

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 Journal of American Science 2010;6(10)

(a) (b)
140 60
120 50

3
3

k(min ) x 10
100
k(min ) x 10

40
80 30

-1
-1

60
20
40
10
20
0
0 0 2 4 6 8 10 12
0 2 4 6 8 10 12
2+ 5
2+ 5
[Fe ] x 10 M
[Fe ] x 10 M

Fig. (7): Plot of k(min–1) vs. [Fe2+] in presence of [H2O2]=10mM for (AO8) and 5mM for (AR 17), (a) (AO8)
and (b) [AR 17] = 1.0 x 10–5M at pH3.0 in Fenton (–) and photo-Fenton (---) processes.

(a) (b)
90 60
80
50
70
3
3

K(min ) x 10
K(min ) x 10

60 40
50
30
-1
-1

40
30 20
20
10
10
0 0
0 2 4 6 8 10 12 0 2 4 6 8 10 12
3+ 5 3+ 5
[Fe ] x 10 M [Fe ] x 10 M

Fig. (8): Plot of k(min–1) vs. [Fe3+] in presence of [H2O2]= 10mM for (AO8) and 2mM for (AR17), (a) [AO8] and (b)
[AR17] = 1.0 x 10–5M at pH3.0 in Fenton-like (––) and photo-Fenton-like (---) processes

250

200
k(min -1) x 103

150

100

50

0
0 10 20 30 40 50 60
[H2O2] m M

Fig. (9): Plot of k(min–1) vs. [H2O2] in presence of [Fe2+]=1.0 x 10-5M, [AO8]=1.0 x 10-5M at pH 3.0 in
Fenton (–) and photo-Fenton (---) processes.

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 Journal of American Science 2010;6(10)

140
120
100

k(min-1) x 103
80
60
40
20
0
0 2 4 6 8 10 12
[Dye] M

Fig. (10): Plot of k(min–1) vs. [dye] in presence of [H2O2] =10mM, [Fe2+] = 2 x 10–5M at pH 3.0 in
Fenton (––) and photo-Fenton (---) processes.

60

50
k(min-1) x 103

40

30

20

10

0
0 1 2 3 4 5 6 7
pH

Fig. (11): Plot of k(min–1) vs. pH in presence of [H2O2]=10mM, [Fe3+]=1 x10–5M and [AR 17]=1 x
10–5M in Fenton like (––) and photo-Fenton like (---) processes.

100
F e n to n lik e R e d 1 7
P h o to -F e n to n - lik e R e d 1 7
F e n to n - lik e O r a n g e 8
80 P h o to -F e n to n - lik e O ra n g e 8
F e n to n O ra n g e 8
P h o to -F e n to n O r a n g e 8
F e n to n R e d 1 7
P h o to -F e n to n R e d 1 7
60
DD%

40

20

0
0 10 20 30 40 50 60 70
T im e (m in )

Fig. (12): The degradation degree of [AO 8] and [AR17]=1.0x10–5M in (–) Fenton, Fenton-like, (---)
photo Fenton and photo-Fenton-like processes [Fe2+] = [Fe3+] = [1.0 x 10-5M] in presence of
[H2O2]= 10mM and pH 3.0.

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 Journal of American Science 2010;6(10)

Fenton-like (Red 17) < Fenton-like (Orange From the previous experiments, it seems
8) <Fenton (Red 17) < Fenton (Orange 8) at 30 that, the best conditions for degradation of Acid
minute. Orange 8 in Fenton, Fenton-like, photo-Fenton and
photo-Fenton-like processes are as represented in Fig.
Fig. 12 shows also a comparison 14a. The degradation degree for Acid Orange 8
between the photo-Fenton and photo-Fenton-like enhances from 33% see (Fig. 12) to 90% see Fig. 14
at 55 minutes in Fenton process for Acid Orange 8.
process for both dyes (UV-irradiated-Fenton and
This is due to use of optimal Fe2+ concentration [5.0 x
Fenton-like reagent). Runs were made at the same
10–5 M] see (Table 2).
previous conditions. From Fig. 12, it can be
concluded that, the color removal appeared faster at
the first 25 minutes as follows, 78%, 82%, 86%, 95% In Fenton-like process the color removal
for photo-Fenton-like (Red 17), photo-Fenton (Red was 28% and enhanced to 93% at 55 minutes, due to
17), photo-Fenton-like (Orange 8) and photo-Fenton use of [Fe3+] = 1 x 10–4M ions as shown in Table (2).
(Orange 8), and increased to 88%, 91%, 96% and UV irradiation-Fenton and Fenton-like reagent for
99.5% respectively at 60 minutes. The order of color Acid Orange 8 showed remarkable enhancement at
removal of the two dyes in photo-Fenton-like and the first 10 minutes. The degradation degree was 49%
photo-Fenton is as follows: at the first 10 minutes and was enhanced to reach
83% when optimum condition was used of [Fe2+] = 2
x 10–5M. It then further increased to 99% at 55
Photo-Fenton-like [Red 17] < photo-Fenton
minutes for photo-Fenton process. Also, similar
(Red 17) < photo-Fenton-like (Orange 8) < photo-
behavior was observed in photo-Fenton-like process
Fenton (Orange 8) at 60 minute. The degradation
in presence of optimum condition [Fe3+] = 1 x 10–4M,
rates for the four advanced oxidation processes of
Acid Orange 8 and Acid Red 17 are presented in Fig. where the degradation started fast and reached 96% at
55 minutes. Similar behavior was observed with Acid
13.
Red 17 in presence of optimum condition as seen in
Fig. 14b and Table 3.

Table (2). Best conditions for degradation of Acid Orange 8 in Fenton, photo-Fenton,
Fenton-like and photo-Fenton-like processes.

Processes
Fenton Photo-Fenton Fenton-like Photo-Fenton like
Factors
H2O2 Conc. 10mM 10mM 10mM 10mM
Fe2+ or Fe3+ Conc. 5 x 10–5M 2 x 10–5M 1 x 10–4M 2 x 10–5M
Dye Conc. 1 x 10–5M 1 x 10–5M 1 x 10–5M 1 x 10–5M
pH 3 3 3 3

Table (3). Best conditions for degradation of Acid Red 17 in Fenton, photo-Fenton, Fenton-
like and photo-Fenton-like processes.

Processes
Fenton Photo-Fenton Fenton-like Photo-Fenton like
Factors
H2O2 Conc. 5mM 5mM 2mM 2mM
Fe2+ or Fe3+ Conc. 5 x 10–5 1 x 10–5 1 x 10–4 1 x 10–4
Dye Conc. 1 x 10–5 1 x 10–5 1 x 10–5 1 x 10–5
pH 3 3 3 3

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 Journal of American Science 2010;6(10)

100
90
80
70
60
k(min-1)
50
40
30
20
10
0
Fenton- Fenton- Fenton Fenton photo- photo- photo- photo
like Red like Orange 8 Red 17 Fenton Fenton Fenton Fenton
17 Orange 8 like Red Red 17 like Orange 8
17 Orange 8
Advanced Oxidation processes

Fig. (13): Plot of k(min-1) vs. four advanced oxidation processes of [AO8] and [AR17]= 1x 10–5M,
[Fe2+], [Fe3+] = 1 x 10–5M, [ H2O2] = 10mM and pH 3.0.

(a) (b)
100 10 0

80 80

Fenton-like
Fenton F enton like
60 60
photo-Fenton like F enton
DD%

DD%

photo-Fenton photo-Fenton lik e

40 40
photo Fenton

20 20

0 0
0 10 20 30 40 50 60 0 10 20 30 40 50 60 70
Time (min) T im e (m in)

Fig. (14): The degradation degree of (a) (AO 8) and (b) (AR17) at the best conditions in Fenton, Photo-Fenton,
Fenton-like and Photo-Fenton-like processes
(DD%) for Acid Orange 8 at optimum conditions in
4. Conclusion Fenton, Fenton-like, photo-Fenton and photo-Fenton-
Four advanced oxidation processes were like processes were 89%, 93%, 99.5% and 96% at 55
used, for degradation of the two azo dyes Acid minutes respectively. On the other hand the
Orange 8 and Acid Red 17. These were degradation degree for Acid Red 17 at optimum
comparatively examined. Based on the above results, conditions in the same previous processes were 78%,
it can be concluded that, the decolorization degree of 98%, 95% and 99% respectively at 55 minutes. From
the two azo dyes is strongly dependent on Fe2+ and these results, it can be concluded that the four
Fe3+ ion concentrations, the H2O2 concentration, the advanced oxidation processes were effective in color
initial dye concentration and the solution pH. removal for the two azo dyes when optimal
Optimal operating conditions for each conditions were used.
process were established. The degradation degree

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 Journal of American Science 2010;6(10)

Corresponding author phase. J. Hazard. Mater. 175(2010) 593-

S.A.Abo-Farha 599.
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