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LANDFILL LEACHATE TREATMENT USING ADVANCED OXIDATION

PROCESSES

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 Oxidation Communications 39, No 1-II, 493–502 (2016)

Petrochemical interactions

LANDFILL LEACHATE TREATMENT USING ADVANCED

OXIDATION PROCESSES

R. POBLETEa, N. K. SALIHOGLUb, G. SALIHOGLUb*

a
Escuela de Prevención de Riesgos y Medioambiente, Facultad de Ciencias del
Mar, Universidad Católica del Norte, Coquimbo, Chile
b
Environmental Engineering Department, Engineering Faculty, Uludag University,
Bursa, Turkey
E-mail: gurays@uludag.edu.tr

ABSTRACT
This study aimed to establish the efficiency of ozone-based oxidation processes in
the treatment of landfill leachate. Two reactors, one equipped with a UVC lamp, the
other subjected to natural sunlight, were set up for experimental purposes. TiO2 was
used as a catalyst in some of the experiments. Four groups of treatment routes, namely
UVSUN + O3, UVC + O3, UVSUN + O3 + TiO2 and UVC + O3 + TiO2, were applied to
treat the leachate by using the two reactors. After the application of each treatment
route, chemical oxygen demand (COD), oxide reduction potential (ORP), pH, ozone
levels and temperatures were measured. Highest COD removal efficiency of 61%
was obtained with the treatment route of UVsun + O3 + TiO2 followed by UVsun + O3
(32% COD removal), UVC + O3 + TiO2 (21% COD removal) and UVC + O3 (19%
COD removal). A positive correlation was found between the ORP levels and COD
removal efficiency. Use of TiO2 as a catalyst, increased the COD removal efficiencies,
however, did not affect the ORP levels.
Keywords: ozone, titanium dioxide, solar reactor, COD, ORP.

AIMS AND BACKGROUND

Municipal solid waste (MSW) management constitutes today a major environmen-
tal, economic and social challenge worldwide, mainly because the waste volume is
growing faster than the world population1. In most countries, sanitary landfilling is
the most common way to eliminate municipal solid wastes. The leachate generated
from MSW disposal sites is considered as one of the highly contaminated resources
from physical, chemical, and biological point of view. It may pose a severe pollution

*
For correspondence.

493
threat to ground water supplies. Year after year, the recognition of landfill leachate
impact on environment has forced authorities to fix more and more stringent require-
ments for pollution control.
Leachates are defined as the aqueous effluent generated as a consequence of
rainwater percolation through wastes, biochemical processes in waste cells and the
inherent water content of wastes themselves1,2. MSW leachate, a high strength waste-
water always with complex and changeable composition, is characteristically rich in
organic matters, ammonia, heavy metals, and other inorganic compounds, posing a
significant threat to the surrounding environment and human health1,3.
The removal of organic material based on chemical oxygen demand (COD), bio-
logical oxygen demand (BOD) and ammonium from leachate is the usual prerequisite
before discharging the leachates into natural waters. Due to the pollution potential to
the surrounding environment such as local surface water and groundwater, landfill
leachate must be treated to meet the local standard for discharge into the receiving
water4.
Among the physicochemical methods, advanced oxidation processes (AOPs) have
recently been revealed as effective technologies in improving the biodegradability of
wastewater5–7 and landfill leachate8. AOPs are regarded as ‘environmental-friendly’
processes as they do not transfer pollutants from one phase to another and do not pro-
duce hazardous sludge 9. AOPs generate the short-lived ·OH, called hydroxyl radical,
a non-selective, strong oxidant which alters organic compounds via H-abstraction or
OH-substitution at near-diffusion-limited rates of reaction. Fe/H2O2, TiO2/UV, UV/
H2O2, ozone (O3), and O3/H2O2 are the most frequently applied processes to generate
•
OH in secondary or tertiary wastewater effluents. Vilar et al.10 reported promising
results applying Fe+2/H2O2/UVsun, called solar photo-Fenton oxidation, in leachate
treatment. O3-based AOPs are frequently tested on laboratory bench scale for COD
and BOD oxidation in landfill leachate11. Among various AOPs, O3 and UV are the
two viable processes that chemicals are not used and therefore sludge is not formed.
Although O3 has the potential to completely oxidise most of the organic content in
leachate, its utility as a complete treatment method is limited due to the high doses
required and the necessary reaction time that increases the energy consumption12. High
energy demand and high capital cost of most AOPs necessitate development of more
energy efficient and cost effective methods13. Therefore, there is a growing interest
in developing AOP applications using solar energy, along with low-cost catalysts14,15.
Use of TiO2 as a catalyst with UV light is reported to give promising results for the
degradation of persistent organic pollutants16.
This study is aimed at establishing the efficiency of O3 based oxidation processes
in the treatment of landfill leachate. Artificial and natural UV sources and TiO2 were
also used.

494
EXPERIMENTAL
Two reactors were set up for experimental purposes. One of the reactors (UVC reactor)
was equipped with a UVC lamp; the other reactor was subjected to natural sunlight
(UVsun reactor or solar reactor). TiO2 was used as a catalyst in some of the experi-
ments. Four groups of treatment routes, namely UVsun + O3, UVC + O3, UVsun + O3 +
TiO2 and UVC + O3 + TiO2, were applied to treat the leachate, using the two reactors.
The treatment routes UVC + O3 and UVC + O3 + TiO2 were realised, using UVC
reactor, which is shown in Fig. 1a. The tank was filled with 10 l of leachate; the
leachate was recirculated with a flow rate of approximately 12 l/min throughout the
UVC reactor and returned back to the tank by using a centrifugal submerged pump
(36 W). The UVC lamp used was an Atman unit, with 254 nm wavelength and 36 W
of power, irradiating 477.7 W/m2, with a specific power of 0.028 W/ml of leachate.
Ozone gas was provided by an ozone generator CH-KTB3G, adding 3 g/h of ozone
to the solution. The concentration of TiO2 applied was 1 g/l. TiO2 was provided from
Degussa AG (Germany). It was a mixture composed of 20–30% rutile and 70–80%
anatase forms and had a surface area of 50 m2/g with primarily particle size of 30 nm.
The treatment routes UVsun + O3 and UVsun + O3 + TiO2 were conducted, using
UVsun reactor, which is shown in Fig. 1b. A cylindrical borosilicate glass tube of
1100 mm of length and 110 mm of diameter was filled with 8 l leachate, and placed
in the focus of a compound parabolic collector (parabolic mirror) to maximise the
solar irradiation. Parabolic mirror collects both direct and diffuse UVA, so the tube is
homogeneously illuminated even on cloudy days. The glass tube with the parabolic
mirrors was placed over a metallic structure, giving a slope of 30°, so as to receive the
sunlight. Ozone gas was provided by an ozone generator CH-KTB3G, adding 3 g/h
of ozone to the solution, as with the UVC Reactor. TiO2 concentration was again 1 g/l.
Leachate samples were obtained from the leachate collector of a municipal landfill.
The initial parameters of the leachate were measured as: COD – 6765 mg/l, pH – 8.84,
chloride – 50.00 mg/l, ammonia – 6400 mg/l, conductivity – 33.61 ms/cm, colour –
2010 PCU and total solids (TS) – 559.00 mg/l. The leachate samples were stored in
darkness at 4°C with minimum exposure to surrounding air till the experiments. The
experiments were conducted without any pretreatment, pH adjustment or filtration.
The pH was measured, using a pH meter (WTW 3150i unit). COD was deter-
mined according to EPA 410.4 method, using Colorimetric method. Ammonia was
determined using Nessler method (D1426-92). Free chlorine was measured using EPA
DPD method (330.5). Colour of water was determined using Colorimetric platinum
cobalt method, according to the standard methods. Oxide reduction potential (ORP)
and temperature were measured using a Wagtech multiparameter unit, and ozone
concentration was measured using DPD method. Solar UV radiation was measured by
a global UV radiometer (KIPP&ZONEN, Model CUV 5) on a platform tilted 30 (the
same latitude of Coquimbo, where the experiments were conducted), which provides
data in terms of incident irradiance (W/m2).

495
 For all the experiments the irradiation duration was 3 h, and the treated samples
were analysed for COD, ozone, temperature, ORP and pH, every 20 min.

Fig. 1. Experimental set up: a – UVC reactor and b – solar (UVsun) reactor

RESULTS AND DISCUSSION

Figure 2 shows the COD removal efficiencies obtained after the application of each
treatment combination. Highest COD removal efficiency of 61% was obtained with
the treatment route of UVsun + O3 + TiO2 followed by UVsun + O3 (32% COD removal),
UVC + O3 + TiO2 (21% COD removal) and UVC+O3 (19% COD removal). It can be
seen that there is an adverse relationship between COD and ORP levels. As the ORP
level increased during all of the treatment routes, COD level decreased. As can be
seen from Figs 2a, b, d, COD levels increased within the first 40 min of 3 treatment
applications, except for that of UVsun + O3 + TiO2 route. Possible formation of complex
by-products because of oxidation process might be a reason of this initial increase in
the COD level. However, the evolution of COD during the UVsun + O3 + TiO2 treatment

496
did not show such an increase. The solar reactor (Fig. 1b) might have allowed more
reaction time than the UVC reactor (Fig. 1a) and allowed a higher level of ozone to
react. Existence of TiO2 in the presence of sufficient O3 with sufficient reaction time
might have prevented such an increase in the COD level, as would be seen in Fig. 2c.

a b

c d

Fig. 2. Evolution of COD and ORP during the treatment of the leachate samples: a – UVsun + O3; b –
UVC + O3; c – UVsun + O3 + TiO2; d – UVC + O3 + TiO2

It is known that the use of O3 in the leachate alters the molecular structure of
the organic compounds and oxidises them into smaller, more biodegradable products
which can be removed in biological treatment systems; it ruptures the unsaturated
bonds or aromatic rings and produces alcohols, carbonyl, and carboxyl compounds17.
At high pH conditions (pH > 8), O3 produces hydroxyl radicals, which accelerate the
oxidation of organic matter from the complex wastewater matrix18. It is reported that
during ozonation target compounds are either oxidised directly by O3, or indirectly by
OH· (Ref. 19). In all of the treatment routes shown in Fig. 2, the COD levels showed
a considerable decrease mostly with the influence of ozone in the system.
Figure 3 shows the evolution of several parameters during the treatment of the
leachate samples with UVsun + O3, UVC + O3, UVsun + O3 + TiO2 and UVC + O3 + TiO2.
When the COD removal efficiencies of UVsun + O3 and UVC + O3 are compared, it
would be noticed that a higher efficiency was obtained when the solar reactor col-
lecting daylight was used. The average solar irradiation was measured as 28.7 W/m2
during the eperiments. Several reasons might have caused the better perfomance of
UVsun + O3 route in COD removal. The UVsun reactor receives 8 l leachate, while the

497
UVC reactor receives 10 l, which might have caused a higher ozone concentration
in the UVsun reactor. Figure 3d confirms the higher ozon levels in the UVsun reactor.
When the COD removal efficiencies of UVsun + O3 + TiO2 and UVC + O3 + TiO2 are
compared, higher COD removal efficiency obtained with UVsun reactor would be
noticed again. The solar irradiation ranged between 26.9 and 28.7 W/m2 during the
experiments with the UVsun reactor. Malato et al.14 reported that a UV intensity ranging
between 20–30 W/m2 would be adequate to degrade organic pollutants.
When the influence of TiO2 questioned, it will be seen that its contribution to
COD removal is more obvious in the experiments conducted by using UVsun reactor.
The COD removal efficiency of UVsun + O3, which was 32%, increased to 61% when
TiO2 was added (1 g/l). However, it was also found that TiO2 had no effect on ORP
increase, as seen in Fig. 3b. Kurniawan and Lo20 reported that during the photo-catalytic
treatment of a leachate by using TiO2, high amount of oxidant radicals formed in the
process and the ·OH radicals rapidly degraded the target compounds. When ozone
acts alone, it has a slow reaction rate; however, when a catalyst such as TiO2 is used,
a photocatalytic oxidation process occurs, hydroxyl radicals are effectively formed
and the reaction is accelerated21. The results obtained in this study agree with the
those reported by Yixin et al.22, that TiO2-catalysed ozonation of a contaminated water
yielded superior results than the non-catalysed ozone application. Titanium dioxide
is known to have a high oxidising power in solar driven processes since it is capable
to absorb UV radiation from the solar spectrum14. Higher surface areas provided by
TiO2 and increased absorption of UV light is also reported by Arafat et al.16
The ORP evolution patterns of UVC + O3 and UVC + O3 + TiO2 were found to be
similar, confirming that TiO2 did not influence the increase in the ORP levels during
the treatment. When the ORP evolutions of UVsun + O3 and UVC + O3 routes were com-
pared, a higher ORP variation was seen with UVsun reactor. The ORP levels measured
at UVsun reactor varied between –75.5 and 100.7 mV, while varied between –76.7 and
–15.4 mV at UVC reactor. Similarly, UVsun + O3 + TiO2 reactor showed an ORP level
ranging between –73.4 and 100.1 mV, while that of UVC + O3 + TiO2 reactor ranged
between –78.1 and –17 mV.
The increase in temperature was also found to be higher in the experiments con-
ducted with UVsun reactor compared to those conducted with UVC reactor. Maximum
temerature obtained with UVC reactor was measured as 25oC, while UVsun reactor
reached a temperaure of 44oC (Fig. 3c).
Ozone levels measured at UVsun reactor were higher than the levels measured at
UVC reactor, and the TiO2 did not influence the ozone levels (Fig. 3d). The ozone levels
increased in all treatment routes during the treatment duration. A strong significant
correaltion was found between the ozone and ORP levels. The Pearson correlation
coefficient between ozone and ORP was found as R = 0.93 for the UVsun + O3 route.
R values were 0.72, 0.88, 0.76 for UVC + O3, UVsun + O3 + TiO2, UVC + O3 + TiO2
routes, respectively. The increase in the ozone concentration explains the increase in

498
the ORP levels and COD removal. This finding agrees with the literature that there
is a direct relationship between ORP and ozone concentration23.

b
a

d
c

Fig. 3. Evolution of several parameters during the treatment of leachate samples with UVsun + O3, UVC +
O3, UVsun + O3 + TiO2 and UVC + O3 + TiO2: a – evolution of COD; b – evolution of ORP; c – evolution
of temperatura; d – evolution of ozone level

Figure 4 shows the pH variations during the application of the treatment routes.
In all treatment routes, the pH of the leachate was always above 8. The pH generally
showed a decreasing trend till the end of first 60 min; it showed minimum levels
(around 8.02) within the second 60 min, then increased up to 8.68 as can be seen in
Fig. 4. It is reported that at these pH levels, the solution is favorable for the ozonated
system24. Radical reaction actively occurs when OH– concentration increases; the
direct reaction (oxidising agent: ozone) is dominant at pH < 4, while indirect reaction
(oxidising agent: hydroxyl radicals) is dominant at pH > 8 (Ref. 25). High pH levels
positively affect the photocatalytic ozonation reactions; the concentration of oxidising
species that favoured the ozone decomposition in water increases26,27. This increases
the ORP of the solution as the duration of ozone reactions prolongs. A close relation
is reported between the ORP levels and COD removal efficiencies when ozone is

499
applied as oxidant26,28, which agrees with the findings of this study. Thus, it can be
inferred that the ozone levels in the solution influences the ORP levels and affects the
treatment efficiency of the leachate.

Fig. 4. Variations of pH during the treatment of leachate samples

CONCLUSIONS
Several AOP combinations including the use of UV source (artificial or natural),
ozone, and catalyst TiO2 were tested to treat a municipal landfill leachate. Based on
the findings, following conclusions can be drawn:
1. Highest COD removal efficiency of 61% was obtained with the treatment route
of UVsun + O3 + TiO2 followed by UVsun + O3 (32% COD removal), UVC + O3 + TiO2
(21% COD removal) and UVC + O3 (19% COD removal). In all treatment routes,
the COD levels showed a considerable decrease mostly with the influence of ozone
in the system. Use of UVsun reactor always resulted better COD removal efficiencies
than the others.
2. As the ORP level increased during the application of the AOP treatment routes,
COD levels always decreased.
3. When TiO2 was used as a catalyst, higher COD removal efficiencies were
obtained. The COD removal efficiency of UVsun + O3, which was 32%, increased to
61% when TiO2 was added (1 g/l).
4. TiO2 had no visible effect on the increase in the ORP levels. The ORP evolu-
tion patterns of UVC + O3 and UVC + O3 + TiO2; UVsun + O3 and UVsun + O3 + TiO2
were found to be similar.
5. The increase in temperature was also found to be higher in the experiments
conducted with UVsun reactor compared to those conducted with UVC reactor.

500
 6. Ozone levels measured at UVsun reactor were higher than the levels measured
at UVC reactor, and the TiO2 did not influence the ozone levels. A strong significant
correlation was found between the ozone and ORP levels.
7. The results show the efficiency of using natural UV source, sun, in leachate
treatment and were found to be promising for leachate treatment, especially for the
geographical regions receiving moderate or high solar irradiation. Using natural
sunlight would be more economical than the other routes. However, it should also be
noted that higher ozone doses and configuration of plants that maximise contact time
between the leachate and ozone will be necessary for a full scale treatment. Use of
TiO2 as a catalyst would improve the COD removal efficiencies.

ACKNOWLEDGEMENTS
The author R. Poblete acknowledges the financial support by the Chilean Education
Ministry (MICINN), under the project FONDECYT (No 11140219) and the Central
Laboratory for Marine Aquaculture of the Marine Sciences Department at the Uni-
versidad Católica del Norte for equipment support. The authors G. Salihoglu and N.
K. Salihoglu acknowledge the financial support by Uludag University with Project
No OUAP(M)-2013/8.

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