Applied Catalysis B: Environmental 63 (2006) 215–221

www.elsevier.com/locate/apcatb

The kinetics of phenol decomposition under UV irradiation with and

without H2O2 on TiO2, Fe–TiO2 and Fe–C–TiO2 photocatalysts
Beata Tryba a,b, Antoni W. Morawski a, Michio Inagaki c, Masahiro Toyoda b,*
a
Technical University of Szczecin, ul. Pulaskiego 10, 70-322 Szczecin, Poland
b
Oita University, 700-Dannoharu, Oita 870-1192, Japan
c
Aichi Institute of Technology, Yakusa, Toyota 470-0392, Japan
Received 31 May 2005; received in revised form 5 August 2005; accepted 18 September 2005
Available online 14 November 2005

Abstract
H2O2 used in the photo-Fenton reaction with iron catalyst can accelerate the oxidation of Fe2+ to Fe3+ under UV irradiation and in the dark (in
the so called dark Fenton process). It was proved that conversion of phenol under UV irradiation in the presence of H2O2 predominantly produces
highly hydrophilic products and catechol, which can accelerate the rate of phenol decomposition. However, while H2O2 under UV irradiation could
decompose phenol to highly hydrophilic products and dihydroxybenzenes in a very short time, complete mineralization proceeded rather slowly.
When H2O2 is used for phenol decomposition in the presence of TiO2 and Fe–TiO2, decrease of OH
radicals formed on the surface of TiO2 and Fe–
TiO2 has been observed and photodecomposition of phenol is slowed down. In case of phenol decomposition under UV irradiation on Fe–C–TiO2
photocatalyst in the presence of H2O2, marked acceleration of the decomposition rate is observed due to the photo-Fenton reactions: Fe2+ is likely
oxidized to Fe3+, which is then efficiently recycled to Fe2+ by the intermediate products formed during phenol decomposition, such as
hydroquinone (HQ) and catechol.
# 2005 Elsevier B.V. All rights reserved.

Keywords: Phenol decomposition; Phenol conversion; Photo-Fenton reaction; H2O2

1. Introduction The photo-Fenton process has been studied by many

Carbon-coated TiO2 photocatalysts were recently developed
and studied [1–6]. It was proved that those photocatalysts could
adsorb a large amount of methylene blue (MB) from the
aqueous solution due to the porous carbon thin layer and had
higher photoactivity for MB decomposition than the pristine
TiO2 under UV irradiation [1–3,6]. Some advantages of carbon
coating were found, such as suppression of phase transforma-
tion from anatase to rutile during heat treatment at high
temperature, increase of the adsorptivity of the photocatalyst
surface, and prevention of the binder photodecomposition
under UV irradiation, when TiO2 is fixed to the reactor using an
organic binder [1–6]. Higher photodecomposition efficiency
was reported. It was also reported that carbon-coated TiO2
modified with Fe could work as photocatalyst for phenol
decomposition via the photo-Fenton process [7].
* Corresponding author.
E-mail address: toyoda22@cc.oita-u.ac.jp (M. Toyoda).
0926-3373/$ – see front matter # 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.apcatb.2005.09.011
researchers, because it can accelerate the degradation of many
organic compounds in water via hydroxyl radicals, which are
formed during photo-Fenton reactions [8–17].
The photo-Fenton process can be applied for the decom-
position of many organic compounds such as phenols, dyes,
pesticides, etc. It was reported that in the presence of Fe2+ and
H2O2, phenol decomposition was accelerated both in the dark
and under irradiation [8]. When iron is only in the form of Fe3+
in the catalyst, the Fenton reaction is limited by the reduction of
Fe3+ to Fe2+ in the presence of H2O2, which is considerably
slower than the oxidation of Fe2+. When starting from Fe3+, a
significant acceleration of the degradation is obtained after
buildup of Fe2+ [17].
In the mechanism of phenol decomposition via photo-
Fenton process, dihydroxybenzenes formed upon phenol
oxidation/hydroxylation are supposed to play an important
role. It was reported that the addition of hydroquinone or
catechol to the reaction solution could reduce Fe3+ to Fe2+,
accelerating in this way the decomposition of phenol. These
compounds are able to enhance the Fenton reaction also in the
216 B. Tryba et al. / Applied Catalysis B: Environmental 63 (2006) 215–221
dark. It was proposed that the active oxidizing agent was a
ternary HQ–Fe–H2O2 complex [17].
In the photo-Fenton process, a mechanism based on
hydroxyl radicals is the most popular to account for the
degradation of many organic compounds, but it was pointed out
that other reactive species could also be involved in the process.
In the case of decomposition of chlorophenol decomposition,
formation of an intermediate, highly-oxidized and unstable
form of Fe [Fe(IV)] was suggested [8].
The mechanism of the decomposition of formic acid on Fe/
TiO2 photocatalyst was also reported not to be a radical reaction
but to proceed via the formation of the [Fe–OOCH]2+ complex.
The [Fe–OOCH]2+ pathway was favored over the degradation
on TiO2 through hydrogen-carbonate formation [18].
Other authors reported that in the degradation of phenol via
the photo-Fenton process, iron complex(es) plays an
important role; phenol is more likely degraded through
oxidation by Fe complex(es) than by hydroxyl radical,
however they did not studied in details the complexes involved
in that process [19].
Phenol decomposition could follow different pathways,
giving different intermediates. For example, in the oxidation
of phenol on Cu catalyst, the main detected intermediates were
ring-retaining compounds (hydroquinone, catechol, benzo-
quinone), which then undergo ring opening to yield CO2 and
short chain acids, mainly maleic, formic, acetic and oxalic
acid, and also traces of malonic, succinic and fumaric acid. It
was reported that upon conversion of phenol to catechol,
higher rate of phenol mineralization was obtained than
through the conversion of phenol to hydroquinone. Oxidation
reactions of phenol and the cited intermediates were
investigated not only on the solid surface but also in the
liquid phase [20].
Ilisz et al. investigated the mechanism of phenol decom-
position in a TiO2 aqueous suspension under UV irradiation in
the presence of electron scavengers, such as O2, H2O2 and Ag+
[21]. They found that, in the presence of oxygen, phenol was
decomposed by the radical reaction with OH
to dihydrox-
ybenzenes (hydroquinone and catechol), which in turn
decomposed to trihydroxybenzenes. In the presence of H2O2,
phenol was decomposed by both radical oxidation with OH

and direct oxidation with holes, which proceeded parallel. With
the high concentration of H2O2 used, i.e. above ca. 0.05 mol/
dm3, the ring-opening products were dominant. Addition of
Ag+ as an electron scavenger changed the mechanism of phenol
decomposition, and only p-benzoquinone was observed as
decomposition product, which could be also a decomposition
product of hydroquinones; decomposition of phenol proceeded
mostly by direct oxidation [21].
In this study, three different photocatalysts based on TiO2,
TiO2 itself, Fe-loaded TiO2 (Fe–TiO2) and Fe-loaded carbon-
coated TiO2 (Fe–C–TiO2) were prepared, and the process of
phenol decomposition on these photocatalysts was studied
under UV irradiation with or without the addition of H2O2.
Some advantages by using the Fe–C–TiO2 photocatalyst in
phenol decomposition under UV, in the presence of H2O2 are
reported and discussed.
2. Experimental
2.1. Preparation
Phenol decomposition in aqueous solution was studied on
three different photocatalysts: TiO2, Fe–TiO2, and Fe–C–TiO2.
Anatase-type ST-01 was used as base TiO2 (Ishihara
Sangyo Co. Ltd., Japan). Fe–TiO2 was prepared by
mechanical mixing of TiO2 with FeC2O4 in the mass ratio
of 10:1, and by heating at 550 8C in air for 3 h. Fe–C–TiO2
photocatalyst was prepared from TiO2 and FeC2O4 by
mechanical mixing in the mass ratio of 10:1, and by heating
in Ar at 500 8C for 1 h. In this case small amounts of carbon
were present as residues.
2.2. Features of the photocatalysts
The photocatalysts thus prepared were characterized by
BET surface area, XRD, TG, content of iron and OH
radicals
formation under UV irradiation with or without H2O2.
BET surface area was determined from the adsorption
isotherm of N2 at 77 K. XRD analysis was performed using Cu
Ka radiation. Content of iron in the catalysts (Fe2+ and Fe3+)
was determined by extraction with 5 ml of 6 M HCl for 2 h
[22], followed by analysis with UV–vis spectrophotometry
using a colorimetric method. Iron detection was carried out
using the 2,4,6-Tris(2-pyridyl)-1,3,5-triazine reagent, which
has a very high sensitivity towards Fe2+.
Analysis of OH
radical formation on the surface of the
catalysts under UV irradiation and under UV/H2O2 was
performed by fluorescence technique using terephthalic acid,
which easily reacts with OH
to form the highly fluorescent
product 2-hydroxyterephtalic acid. The intensity of the peak
attributed to 2-hydroxyterephtalic acid was proportional to the
amount of OH
radicals formed [23].
2.3. Phenol decomposition
The photocatalysts at a loading of 0.2 g/L were suspended
in 500 mL of a 2.1  104 mol L1 phenol solution. The
suspensions were magnetically stirred for 3 h in the dark until
saturation with adsorption of phenol. After adsorption,
photodecomposition of phenol was carried out under UV
irradiation in a ‘‘batch mode’’ reactor equipped with three
black light blue fluorescent lamps of 20 W power. Those
lamps irradiate in the wavelength range 300–415 nm, with
maximum intensity at 352 nm. UV irradiation power inside
the reactor was 2.4 mW cm2 in the wavelength range 310–
400 nm and 1.9 mW cm2 in the range 360–470 nm. Experi-
ments were carried out with and without addition of 0.03 mol/
L H2O2 to the phenol solution. The time trend of phenol and
the generation of ring-retaining products such as benzoqui-
none, hydroquinone and catechol were measured by High
Performance Liquid Chromatography (HPLC). The concen-
trations of phenol and catechol were determined at the
wavelength l = 269 nm, BQ and HQ at 246 and 289 nm,
respectively.
 B. Tryba et al. / Applied Catalysis B: Environmental 63 (2006) 215–221 217

Table 1
Characteristics of TiO2, Fe–TiO2 and Fe–C–TiO2 photocatalysts
Sample code BET (m2/g) Carbon (mass%) Fe3+ (mass%) Fe2+ (mass%) Phases by XRD (A-anatase)
TiO2 300 – 0 0 A
Fe–TiO2 55 0.0 1.3 0.6 A, FeTiO3
Fe–C–TiO2 72 2.4 0.96 0.70 A, FeTiO3

3. Results and discussion

The features of the photocatalysts prepared are presented in

Table 1.
Original TiO2 (ST-01) has quite highr BET surface area than
the modified ones and consists of 7 nm diameter particles with
single anatase phase. After modification of TiO2, BET surface
area decreased in both Fe–TiO2 and Fe–C–TiO2 samples. Fe–
TiO2 and Fe–C–TiO2 photocatalysts showed two phases on
XRD patterns, anatase and FeTiO3, i.e. ilmenite structure. The
XRD pattern of the Fe–C–TiO2 photocatalyst is shown in Fig. 1.
The content of iron in the Fe–TiO2 photocatalyst was around
2 mass%. The higher content of Fe3+ than Fe2+ was reasonably
caused by the oxidation of iron in air atmosphere and by the
solid phase reaction between TiO2 and FeC2O4 during
preparation. The Fe–C–TiO2 photocatalyst had a little higher
BET surface area than Fe–TiO2 and an higher amount of Fe2+, Fig. 2. Decomposition of phenol under UV irradiation.
due to its different conditions of preparation. Content of Fe2+ in
a photocatalyst is important parameter in the Fenton reaction
with H2O2. absence of H2O2 has been observed on Fe–TiO2
The relative phenol concentration c/c0 in aqueous solution in (k = 0.127 h1). Fe–C–TiO2 showed lower photoactivity for
natural logarithm scale is plotted in Fig. 2 against UV phenol decomposition than pristine TiO2.
irradiation time on TiO2, Fe–TiO2, and Fe–C–TiO2. The Phenol decomposition was also performed on these
relationship between ln (c/c0) and time in Fig. 2 is photocatalysts under UV irradiation in the presence of H2O2,
approximately linear, and so the rate constant k for phenol which is used to initiate a photo-Fenton process. Decomposi-
photodecomposition could be calculated for each catalyst from tion of phenol in the presence of H2O2 without any
the line slope, according to the equation photocatalyst under UV irradiation was carried out for
comparison. The results are presented in Fig. 3. Rate constants
ln ðc=c0 Þ ¼ kt
k for phenol decomposition on those photocatalysts under UV
where c0 and c are the initial concentration of phenol and the irradiation with addition of H2O2 reported in Table 2.
concentration at irradiation time t (h), respectively. The rate constant of phenol decomposition on Fe–C–TiO2
The values of the calculated rate constant k are listed in was accelerated by addition of H2O2 (k = 0.258 h1). On the
Table 2. The highest rate of phenol decomposition in the other hand, on TiO2 and Fe–TiO2, phenol decomposition was
slightly slower in the presence of H2O2, though it was still faster
on Fe–TiO2 than on TiO2. Phenol was quickly decomposed by
H2O2 without any photocatalyst employed (k = 0.228 h1),
because under UV irradiation H2O2 is easily going upon
photolysis yielding in OH
radicals. It could be explained by the

Table 2
Calculated rate constant k for phenol decomposition on TiO2, Fe–TiO2, and Fe–
C–TiO2 photocatalysts under UV irradiation with and without addition of H2O2
Sample code Rate constant k (h1)
Without H2O2 With H2O2
TiO2 0.101 0.093
Fe–TiO2 0.127 0.106
Fe–C–TiO2 0.078 0.258
H2O2 – 0.228
Fig. 1. XRD pattern of Fe–C–TiO2 photocatalyst.
218 B. Tryba et al. / Applied Catalysis B: Environmental 63 (2006) 215–221

Fig. 3. Decomposition of phenol with time of UV irradiation with the addition

of H2O2.

pathway of phenol conversion, which was different on those

photocatalysts. The kinetic studies on phenol decomposition
were performed by HPLC. Fig. 4 shows phenol decomposition
under UV irradiation as studied by HPLC using Fe–C–TiO2
photocatalyst with H2O2.
Phenol and some ring-retaining products formed upon
phenol degradation could be identified by the different retention
time (phenol at 3.37 min, hydroquinone (HQ) at 1.89 min,
benzoquinone (BQ) at 2.25 min, catechol at 2.45 min), and
ring-opening products around 1.5 min, see Fig. 4. The ring-
opening products could not be identified by HPLC. However
the high intensity unknown peak of byproducts on the HPLC at
the retention time of 1.5 min was also observed by Ilisz et al.
[21]. The ring-opening products are supposed to be short chain
acids, such as acetic acid, maleic acid, oxalic acid, etc.,
however they were not identified by using the other analytical
methods.
Formation of the ring-retaining products upon phenol
decomposition under UV irradiation on TiO2 and Fe–TiO2 is
presented in Fig. 5. On Fe–C–TiO2, on the contrary, no
decomposition products of phenol were observed in solution
during 5 h of UV irradiation.
Phenol is converted to BQ and HQ on pristine TiO2, however
phenol is decomposed to HQ only using Fe–TiO2. There is no
peak at the retention time of 1.5 min in case of all those
photocatalysts under UV without H2O2. Formation of the
Fig. 5. Phenol decomposition and formation of the ring products of phenol
decomposition under UV on (a) TiO2, (b) Fe–TiO2, and (c) Fe–C–TiO2
photocatalysts.

decomposition products of phenol with UV irradiation in the

Fig. 4. HPLC chromatogram registered after 1 h of phenol decomposition
under UV and with H2O2 on Fe–C–TiO2 photocatalyst.
presence of H2O2 with and without photocatalyst such as TiO2,
Fe–TiO2 and Fe–C–TiO2 is presented in Fig. 6. When H2O2 was
added to phenol solution, the ring-opening products judged to
be formed by the appearance of the peak at the retention time
1.5 min appeared at the early stages of the decomposition
process, at the same time as HQ, BQ and catechol.
Conversion of phenol to catechol would have some benefits
in the photo-Fenton process. As it was shown in Fig. 3,
significant acceleration of phenol decomposition on Fe–C–
TiO2 photocatalyst was observed. A possible explanation is that
 B. Tryba et al. / Applied Catalysis B: Environmental 63 (2006) 215–221 219

Fig. 6. Phenol decomposition under UV with H2O2 on (a) TiO2, (b) Fe–TiO2, (c) Fe–C–TiO2, and (d) without photocatalyst.

catechol and hydroquinone might rapidly reduce Fe3+ to Fe2+ as

reported by Chen et al. [17].
Conversion of phenol to catechol is likely to be more
advantageous for the complete mineralization of phenol than
conversion to BQ or HQ, as reported by Santos et al. [20],
because catechol is decomposed to oxalic acid, and then to CO2
and water, whereas the pathways of mineralization of BQ and
HQ are much longer. When H2O2 was used for phenol
decomposition without the photocatalyst (Fig. 6d), the
conversion of phenol was quite rapid, and a high amount of
catechol formation was observed. The amount of OH
radicals
formed was however not sufficient to achieve complete
degradation of phenol and its ring-retaining intermediates
within 5 h of UV irradiation. Complete degradation was already
obtained after 3 h of UV irradiation only on Fe–C–TiO2
(Fig. 5c). In the case of Fe–TiO2, the addition of H2O2 did not
accelerate phenol decomposition, suggesting that the photo-
Fenton reaction of Fe2+ oxidation to Fe3+ and reduction to Fe2+
was not efficient.
Some measurements of OH
radicals formation on the
surface of TiO2, Fe–TiO2, and Fe–C–TiO2 were performed
under UV irradiation with or without addition of H2O2. These
results are presented in Fig. 7. From the OH
radicals
measurements it was observed a higher formation of OH

radicals on the surface of Fe–TiO2 under UV irradiation in
comparison with TiO2, but almost no OH
radicals were Fig. 7. OH
radicals formation on the photocatalysts, (a) under UV, and (b)
detected on Fe–C–TiO2. Increase in OH
radicals formation on under UV with H2O2.
220 B. Tryba et al. / Applied Catalysis B: Environmental 63 (2006) 215–221
Fe–TiO2 was probably due to the photo–Fenton reduction of
Fe3+ to Fe2+ under UV irradiation
Fe3þ þ OH þ hn ! Fe2þ þ OH

However, reaction (1) did not work in the case of Fe–C–TiO2,
although this photocatalyst has around 1 mass% of Fe3+. It can
be explained by the fact, that Fe–C–TiO2 is covered by a thin
layer of carbon (the color of its catalyst is grayish), so adsorp-
tion of water molecules on the surface of this photocatalyst was
reduced due to the hydrophobic nature of carbon. Phenol
decomposition on Fe–C–TiO2 under UV irradiation is thus
likely to proceed by direct oxidation with the holes rather than
by radical reaction.
A quite different behavior of OH
radical formation was
observed on the photocatalysts in the presence of H2O2. A
higher amount of OH
radicals is formed in the presence of
H2O2 alone under UV irradiation than in the presence of H2O2
and TiO2 particles, possibly because a certain amount of H2O2
is reasonably consumed in the oxidation of the photocatalyst
surface. Increase in OH
radicals formation on Fe–C–TiO2 was
observed in the presence of H2O2 under UV irradiation due to
the photo-Fenton reaction of oxidation of Fe2+ to Fe3+
Fe2þ þ H2 O2 ! Fe3þ þ OH
þ OH
On Fe–TiO2 and TiO2 photocatalysts, OH
radical formation
was decreased upon addition of H2O2 to the solution.
OH
radicals are formed on the surface of TiO2 mostly by the
reaction of holes formed after excitation of semiconductor with
adsorbed hydroxyl ions on the surface of TiO2
TiO2 þ hn ! e þ hþ
hþ H2 OðadsÞ ! OH
ðadsÞ þ Hþ ðadsÞ
Decrease of OH
radicals formation could be caused by the
process of OH
scavenging by supplied H2O2
H2 O2 þ OH
! HO2
þ H2 O
Phenol is not only decomposed by radical reaction. The amount
of OH
radical formation on the surface of TiO2 and Fe–TiO2
under UV irradiation in the presence of H2O2 is comparable to
that formed on Fe–C–TiO2, but phenol is decomposed much
faster on Fe–C–TiO2. This could be explained by a different
mechanism of phenol decomposition occurring on Fe–C–TiO2,
TiO2 and Fe–TiO2. On TiO2 and Fe–TiO2 photocatalysts the
mechanism of phenol decomposition through the radical reaction
plays the most important role whereas on Fe–C–TiO2 photo-
catalyst some complex reactions with iron have to be involved.
4. Conclusions
Phenol photocatalytic decomposition on TiO2 and Fe–TiO2
is faster than on Fe–C–TiO2. Acceleration of phenol decom-
position could be obtained on Fe–TiO2 under UV irradiation in
the absence of H2O2 due to the photo-Fenton reaction of Fe3+
reduction to Fe2+, yielding OH
radicals. However, the highest
rate of phenol decomposition was observed on Fe–C–TiO2
(1) under UV upon addition of H2O2. It is proposed that the
dihydroxybenzenes formed upon phenol decomposition on Fe–
C–TiO2, catechol, and hydroquinone (HQ) could reduce Fe3+
rapidly by the formation of a ternary HQ–Fe–H2O2 complex.
On the other hand, the addition of H2O2 to the phenol solution
reduced the amount of OH
radicals formation on the surface of
TiO2 and Fe–TiO2, because of OH
scavenging by H2O2.
The photo-Fenton process is very efficient in the decom-
position of many organic compounds in water through the
formation of OH
radicals, which have a high potential of
oxidation. However, it was shown that phenol is more likely
oxidized by a Fe(IV) complex than by radical reaction.
Therefore some benefits of phenol oxidation under UV with
H2O2 on Fe–C–TiO2 photocatalyst were found, H2O2 could
change the pathway of phenol oxidation to catechol, which is
mineralized faster than BQ and HQ, and the formed
dihydroxybenzenes (1,2-HQ and 1,4-HQ) could reduce Fe3+
to Fe2+, which speeds up the process of phenol decomposition.
On Fe–TiO2 photocatalyst, however, dihydroxybenzenes
(1,2-HQ and 1,4-HQ) were also formed upon phenol
decomposition under UV with H2O2, though they were not
(2) present on the photocatalyst surface and did not take part in the
photo-Fenton process of Fe3+ reduction. The detailed discus-
sion on it will be carried out in further studies.
Acknowledgement
The present work was supported by the Research Project of
Environmental Technology Development Fund.
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