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Transcript of Fenton’s pre-treatment of mature landfill leachate
Chemosphere 54 (2004) 1005–1010
www.elsevier.com/locate/chemosphere
Short Communication
Fenton’s pre-treatment of mature landfill leachate
Antonio Lopez a,*, Michele Pagano a, Angela Volpe a,Appio Claudio Di Pinto b
a Consiglio Nazionale delle Ricerche, Istituto di Ricerca Sulle Acque, Reparto di Chimica e Tecnologia delle Acque,
Via Francesco De Blasio, 5, 70123 Bari, Italyb Via Reno, 1, 00198 Roma, Italy
Received 14 April 2003; received in revised form 18 July 2003; accepted 11 September 2003
Abstract
The aim of this study was to check the effectiveness of the Fenton’s reagent (Fe2þ +H2O2 +Hþ) for the pre-treatment
of a municipal landfill leachate with the objective of improving its overall biodegradability, evaluated in terms of BOD5/
COD ratio, up to a value compatible with biological treatment. The leachate came from a municipal sanitary landfill
located in southern Italy and the average values of its main parameters were: pH¼ 8.2; COD¼ 10 540 mg l�1;BOD5¼ 2300 mg l�1; TOC¼ 3900 mg l�1; NH4-N¼ 5210 mg l�1; conductivity¼ 45350 lS cm�1; alkalinity¼ 21 470mg l�1 CaCO3. The effect of initial pH value on the pre-treatment effectiveness was evaluated by titrating the amount of
acidic by-products formed. The extent of leachate oxidation was monitored and controlled by both pH and redox
potential measurements. The best operational conditions for achieving the desired goal (i.e., BOD5/CODP 0.5) re-
sulted: Fe2þ ¼ 275 mg l�1; H2O2¼ 3300 mg l�1; initial pH¼ 3; reaction time¼ 2 h. At the end of the Fenton’s pre-treatment, in order to permit a subsequent biological treatment, residual ferric ions were removed increasing the pH up
to 8.5 by adding 3 g l�1 of Ca(OH)2 and 3 mg l�1 of a cationic polyelectrolyte, the latter as an aid to coagulation. This
final step also resulted in a further modest removal of residual COD due to co-precipitation phenomena.
� 2003 Elsevier Ltd. All rights reserved.
Keywords: Fenton’s reagent; Landfill leachate; Biodegradability enhancement; Oxidation processes
1. Introduction
Although landfill leachates have been proved to be
toxic and recalcitrant, landfilling still remains one of the
main methods for municipal and industrial solid waste
disposal. There are many factors affecting the quality
and the quantity of such leachates, i.e., seasonal weather
variation, landfilling technique, piling and compaction
method, waste type and composition, structure of the
landfill, etc. In particular, the composition of landfill
leachates varies greatly depending on the age of the
*Corresponding author. Tel.: +39-080-582-0506; fax: +39-
080-531-3365.
E-mail address: [email protected] (A. Lopez).
0045-6535/$ - see front matter � 2003 Elsevier Ltd. All rights reserv
doi:10.1016/j.chemosphere.2003.09.015
landfill (Baig et al., 1999). Accordingly, several treat-
ment technologies are used in practice (Haapea et al.,
2002).
To remove the bulk of pollutants, biological treat-
ments are usually preferred over physico-chemical (Im
et al., 2001). However, good performances are obtained
with biological processes only treating ‘‘young’’ biode-
gradable leachates. In the case of ‘‘old’’ leachates,
instead, COD (chemical oxygen demand) maximum
allowable concentration (MAC) for direct or indirect
discharge cannot be met because of the occurrence
of pollutants that inhibit biomass activity and/or are
recalcitrant to biological treatments. In such instances,
MAC values are usually achieved by more expen-
sive physico-chemical treatments such as flocculation–
precipitation, adsorption on activated carbon,
ed.
1006 A. Lopez et al. / Chemosphere 54 (2004) 1005–1010
evaporation, chemical oxidation, incineration. Among
them, growing interest has been focused on advanced
oxidation processes, AOP, (Huang et al., 1993; Sch-
roder, 1996) which, exploiting the strong oxidation po-
tential of hydroxyl radicals (HO�), can achieve two
alternative goals: (i) the reduction of the COD content
of wastewater up to the desired MAC value through the
mineralization of recalcitrant pollutants (i.e., their
transformation into CO2); (ii) the enhancement of the
biodegradability of treated effluents with the aim of
making their subsequent biological treatment possible.
In general, AOP are defined as oxidation processes
which generate hydroxyl radicals in sufficient quantity to
affect water and wastewater treatment (Huang et al.,
1993). The hydroxyl radical is one of the most reactive
free radicals and one of the strongest oxidants (HO� +
Hþ + e� )H2O; E0¼ 2.33 mV). Many systems can be
classified as AOP and most of them use a combination
of: two oxidants (e.g., O3 plus H2O2); catalyst plus
oxidant (e.g., Fe2þ +H2O2); oxidant plus irradiation
(e.g., H2O2 plus UV); oxidant plus photo-catalyst (e.g.,
H2O2 plus TiO2 plus hm); oxidant plus ultrasounds (e.g.,H2O2 plus ultrasounds). One common feature of such
systems is the high demand of electrical energy for de-
vices such as ozonizers, UV lamps, ultrasounds, and this
results in rather high treatment costs. The only excep-
tion is the Fenton’s process. In such a process, in fact,
under acidic condition, a Fe2þ/H2O2 mixture produces
OH� radicals in a very cost-effective way. The major
advantages of the Fenton’s reagent (Fe2þ +H2O2 +Hþ)
are: (i) both iron and hydrogen peroxide are cheap and
non-toxic; (ii) there is no mass transfer limitation due to
its homogeneous catalytic nature; (iii) there is no form of
energy involved as catalyst; (iiii) the process is techno-
logically simple.
Because of these features, Fenton’s process has been
applied in many areas (Prousek, 1995) including that of
recalcitrant wastewater and/or landfill leachates treat-
ment (Koyama and Nakamura, 1994; Gau and Chang,
1996; Tang and Huang, 1996; Bae et al., 1997; Kim
et al., 1997; Steensen, 1997; Kwong et al., 1999; Rivas
et al., 2001; Zhu et al., 2001). However, at least in the
case of landfill leachates, Fenton’s process has been used
mainly as a post-treatment to achieve desired COD
MAC values rather than as a pre-treatment in order to
permit a subsequent economical biological treatment
(Chamarro et al., 2001).
On the basis of the above considerations, the inves-
tigation described in the present work was carried out
specifically to check the effectiveness of the Fenton’s
process for pre-treating a municipal landfill leachate
with the aim of improving its overall biodegradability up
to a value compatible with subsequent aerobic biological
treatment. Measuring biodegradability as the ratio be-
tween the biochemical oxygen demand measured after 5
days (BOD5) and COD, such a value must beP 0.5.
2. Experimental
2.1. Fenton’s treatment procedure
Fenton’s treatment of landfill leachate was carried
out at ambient temperature according to the following
sequential steps. (1) Leachate sample was put in a beaker
and magnetically stirred; its pH was adjusted to fixed
values by H2SO4 95–97% (w/w). (2) The scheduled Fe2þ
dosage was achieved by adding the necessary amount of
solid FeSO4 Æ 7H2O. (3) A known volume of 35% (w/w)H2O2 solution was added in a single step. (4) After fixed
reaction time (2 h), before carrying out BOD tests, 3
g l�1 of calcium hydroxide and 3 mg l�1 of a cationic
polyelectrolyte (Dryfloc 652) were added to treated
leachate samples to precipitate residual ferric ions and to
better coagulate the resulting sludge. (5) At the end of
Fenton’s treatment, stirring was turned off and the
sludge was allowed to sediment. In every case, all the
analyses of treated leachate were carried out on filtered
samples.
2.2. Analyses and chemicals
Total organic carbon (TOC) analyses were per-
formed by a TOC 5050 analyzer from Shimadzu,
Japan. H2O2 concentration was determined by iodo-
metric method (Kolthoff et al., 1974). Metals were
analysed by inductively coupled plasma emission spec-
troscopy with an Optima 3000 ICP-OES system from
Perkin Elmer, Norwalk-CT/USA. Redox potential and
pH were measured by a Mettler DL 40 RC system
equipped with DG 111-SC and platinum DM 140
combined electrodes from Mettler-Toledo, Milano, It-
aly. BOD5, COD, TS, TSS, PO4-P, NH4-N, alkalinity
and chlorides were measured according to standard
methods (APHA, 1995). In Fenton treated leachate
samples, COD content was calculated as difference be-
tween the measured total COD and the COD due to
residual H2O2 (Kang et al., 1999). All the used chemicals
were analytical grade from Baker, Germany. Cationic
polyelectrolyte Dryfloc 652 was from Nymco-Acque,
Cormano, Italy.
3. Results and discussion
The composition of the investigated leachate is re-
ported in Table 1. Taking into account the low con-
centration of heavy metals, the pH value (8.2), the low
value of the BOD5/COD ratio [(2300/10540)¼ 0.2] andthe high contents of NH4-N (5210 mg l
�1) and alkalinity
(21 470 mg l�1), the leachate was classified as ‘‘old’’ and
non-biodegradable (Baig et al., 1999).
Referring to the Fenton process, it is well known that
higher hydrogen peroxide to substrate ratios result in
Table 1
Composition of the investigated landfill leachate
Parameter Unit Value
pH 8.2
Conductivity lS cm�1 45 350
Total COD mg l�1 10 540
TOC mg l�1 3900
BOD5 mg l�1 2300
Total solids (TS) mg l�1 20 255
Total suspended solids (TSS) mg l�1 1666
Alkalinity (CaCO3) mg l�1 21 470
NH4-N mg l�1 5210
PO4-P mg l�1 32
Cl� mg l�1 4900
Metal ions
Ca mg l�1 15.7
Mg mg l�1 24.1
Na mg l�1 3970
K mg l�1 3460
Fe mg l�1 2.7
Zn mg l�1 0.16
Ni mg l�1 0.31
Cr mg l�1 2.21
Mn mg l�1 0.04
Cd mg l�1 <0.02
Pb mg l�1 <0.03
01
23
45
67
0 250 500 750 1000
Fe2+ added (mg/l)
Res
idua
l H2O
2 (g
/l)
60
70
80
90
100
Rem
aini
ng C
OD
(%
)
50
60
70
80
90
100
Rem
aini
ng T
OC
(%
)
Fig. 1. Effect of Fe2þ dosage on selected parameters measured
in Fenton treated leachate’s samples. All the experiments were
carried out in batch at initial pH¼ 3.0, constant H2O2 dosage(6300 mg l�1), reaction time¼ 2 h.
A. Lopez et al. / Chemosphere 54 (2004) 1005–1010 1007
more extensive substrate degradation, while higher
concentrations of iron ions yield faster rates. However,
in order to maximise the effectiveness of the process,
it is preliminarily necessary to determine the optimal
operational H2O2/Fe2þ mass ratio. In fact, it must be
pointed out that Fenton’s reagent (Fe2þ +H2O2 +Hþ )
Fe3þ +H2O+HO�) is used to produce the hydroxyl
radicals necessary to oxidise organic substances (OM)
according to the following reaction (Edwards and Curci,
1992; Huang et al., 1993):
HO� þOM) Oxidation Products
ðk20 �C � 107–1010 M�1 s�1Þ ð1Þ
Particular attention must be paid to Fe2þ and H2O2dosages in order to avoid the following undesired HO�
radicals scavenging reactions occurring in the presence
of an excess of each of the two reagents (Tang and
Huang, 1997).
Fe2þ þHO� ) Fe3þ þOH� ðk20 �C ¼ 3� 108 M�1 s�1Þð2Þ
H2O2þHO� )H2Oþ �O2H ðk20 �C ¼ 2:7� 107 M�1 s�1Þð3Þ
Previous studies, in fact, have demonstrated that the
best oxidation efficiency is achieved by reaction (1) when
neither H2O2 nor Fe2þ is overdosed, so that the maxi-
mum amount of HO� radicals is available for the oxi-
dation of organic compounds (Tang and Huang, 1997).
In other words, an optimal ratio between H2O2 and Fe2þ
must be fixed in order to minimize scavenging effects. In
order to assess such a ratio, maintaining constant the
concentration of H2O2 as 6300 mg l�1, an arbitrary
value, a set of experiments was carried out progressively
increasing the dosage of Fe2þ. According to previous
studies, all the experiments were carried out fixing a
reaction time of 2 h and an initial pH of 3.0 (Prousek,
1995).
Fig. 1, that shows the results of such experiments,
demonstrates that in the treated leachate the remaining
COD values regularly decreased with increasing iron
dosages. However, when Fe2þ was overdosed (Fe2þ >
500 mg l�1) HO� radicals were scavenged through reac-
tion (2) and an opposite trend was recorded. Referring
to remaining TOC and residual H2O2 values, their
trends showed a clear decrease only up to a Fe2þ con-
centration of 250 mg l�1. The fact that, in the Fe2þ
concentration range 250–500 mg l�1, the decrease of
COD resulted much more sharp than that of TOC in-
dicates that, within this range, organic matter still con-
tinued to be oxidised but the extent of its transformation
into CO2 is lower than previously. Fig. 1 also shows that
1008 A. Lopez et al. / Chemosphere 54 (2004) 1005–1010
at Fe2þ concentrations higher than 500 mg l�1 residual
TOC values essentially remain constant although the
correspondent COD values regularly increase. This
means that the progressive organic matter mineraliza-
tion (i.e., its transformation into CO2), caused by in-
creasing Fe2þ concentration, just stops at a Fe2þ dosage
of 500 mg l�1. Any further addition of ferrous ions only
causes a progressive reduction of the oxidation degree of
the residual organic matter measured as TOC. In fact,
for a same amount of TOC, the lower its oxidation de-
gree the higher its correspondent COD. Once again,
such a trend can be explained taking into account that,
in the presence of an excess of Fe2þ, reaction (2) pre-
dominates over reaction (1). Therefore, the higher the
Fe2þ concentration, the lower the amount of OH� radi-
cals available to oxidise organic matter according to
reaction (1).
In practice, Fig. 1 indicates that the optimal (H2O2/
Fe2þ) mass ratio should be about 12 [i.e. (6300/500)].
However, as proved by other authors, this value can
greatly fluctuate according to the class of pollutants and
to the matrix effect in complex wastewaters (Prousek,
1995; Tang and Huang, 1997).
Maintaining constant the H2O2/Fe2þ ratio, the steady
state concentration of hydroxyl radicals depends upon
the absolute amounts of H2O2 and Fe2þ. Therefore, in
order to assess the relationship between the percentage
of removed COD and such amounts, a set of experi-
ments was carried out fixing the H2O2/Fe2þ mass ratio
(i.e., 12) and treating the leachate with increasing
amounts of both reagents. In Fig. 2, in addition to the
results of such experiments, it is shown also the further
COD removal due to the final polishing step (i.e., the
0
10
20
30
40
50
60
70
80
90
100
0 5000 10000 15000H2O2 added (mg/l)
Rem
aini
ng C
OD
(%
)
Fig. 2. Effect of increasing dosages of H2O2 and Fe2þ, at con-
stant mass ratio (H2O2/Fe2þ ¼ 12), on COD removal. Residual
COD values were measured at the end of Fenton treatment
before () and after () adding 3 g l�1 of Ca(OH)2 and 3 mg l�1of a cationic polyelectrolyte (Dryfloc 652). Experimental con-
ditions: initial pH¼ 3.0, reaction time¼ 2 h.
addition of calcium hydroxide and cationic polyelec-
trolyte) necessary to permit successive biological treat-
ment. Fig. 2 demonstrates that the COD values of the
treated leachate regularly decreased with increasing
amounts of H2O2 and Fe2þ up to a H2O2 value of 10 000
mg l�1; afterwards, greater dosages did not modify re-
sidual COD value. Such a trend can be explained con-
sidering that the end by-products of oxidation reactions
are mainly made of short chain organic acids that are
difficult to be further oxidised (Rivas et al., 2001). Fig. 2
also demonstrates that the more oxidised was the
leachate (i.e., the lower is its COD), the greater was the
additional COD removal due to the polishing step. This
result is due to the fact that HO� radicals, in addition to
oxidation reactions, induce secondary effects, such as:
(i) the formation of colloidal particles from dissolved
organic matter through condensation and/or polymeri-
sation reactions that shift organic matter size distribu-
tion towards larger sizes; (ii) the improvement of ferric
ions complexation by oxidised organic matter resulting
in easier precipitation of the latter (Lee et al., 1996;
Kang and Chang, 1997; Kang and Hwang, 2000; Lau
et al., 2001).
Once assessed the optimal H2O2/Fe2þ mass ratio (i.e.,
12), the maximum achievable COD removal (i.e., 60%)
and the absolute amounts of H2O2 and Fe2þ necessary
to achieve this maximum removal (i.e., H2O2¼ 10 000mg l�1 and Fe2þ ¼ 830 mg l�1), experiments were carriedout to evaluate leachate’s biodegradability enhance-
ment, in terms of BOD5/COD ratio increase, achieved
during the Fenton’s treatment. The results of these ex-
periments are shown in Fig. 3 and indicate that, to
achieve an exploitable biodegradability improvement
(BOD5/COD >0.5), it is sufficient to treat the leachate
0.20
0.25
0.30
0.35
0.40
0.45
0.50
0.55
0.60
0 2500 5000 7500 10000
H2O2 added (mg/l)
BO
D5
/CO
D
Fig. 3. Effect of increasing dosages of H2O2 and Fe2þ, at con-
stant mass ratio (H2O2/Fe2þ ¼ 12), on BOD/COD ratio mea-
sured after adding 3 g l�1 of Ca(OH)2 and 3 mg l�1 of a cationic
polyelectrolyte (Dryfloc 652). Experimental conditions: initial
pH¼ 3.0, reaction time¼ 2 h.
0
2
4
6
8
10
12
0 25 50 75 100 125 150
NaOH added (meq/l)
pH
pH0 =2pH0 =3
pH0=4
Fig. 5. Titration curves of leachate’s samples collected after
Fenton treatments carried out fixing different initial pH values
(pH0). Experimental conditions: H2O2¼ 6300 mg l�1, Fe2þ ¼500 mg l�1, reaction time¼ 2 h.
A. Lopez et al. / Chemosphere 54 (2004) 1005–1010 1009
with amounts of H2O2 and Fe2þ of 3300 and 275 mg l�1
respectively, avoiding the need to use greater amounts
only to reduce the COD (see Fig. 2).
Tests were also carried out to assess whether reaction
times greater than 2 h, i.e. the time fixed during the
whole investigation, would result beneficial to the extent
of leachate’s oxidation. The results shown in Fig. 4
confirmed that after two hours the oxidation was over
and, then, this is the value that has to be used during
reactor designing steps. Fig. 4 also demonstrates that the
progress of Fenton’s treatment can be monitored by
measuring pH or redox potential evolution during
leachate’s oxidation. This is particularly important from
the technological stand point as the possibility of mon-
itoring a process ‘‘on-line’’ is always desirable.
Finally, the effect of initial leachate’s pH on Fenton’s
oxidation effectiveness was evaluated in terms of acidic
by-products formation. In fact, as previously pointed
out, the end by-products of Fenton’s reactions are
mostly made by carboxylic acids. Therefore, the higher
the Fenton’s oxidation extent the greater the amount of
acid by-products formed. Fig. 5 shows the curves ob-
tained by titrating with 1 N NaOH Fenton treated
leachates whose initial pHs were different. This figure
clearly demonstrates that the highest amount of NaOH
necessary for neutralizing the treated leachate was re-
quired when the pH, before Fenton’s treatment, was
50
60
70
80
90
100
Rem
aini
ng C
OD
(%)
50
60
70
80
90
100
Rem
aini
ng T
OC
(%)
0
2000
4000
6000
8000
Res
idua
l H2O
2
(mg/
l)
400
450
500
550
600
650
0 100 200 300 400 500Time (min)
red
ox p
oten
tial
(m
V)
2.02.22.42.62.83.03.2
pH
Redox potential
pH
Fig. 4. Trends of selected parameters during leachate’s Fenton
treatment. Initial experimental conditions: pH¼ 3.0, H2O2¼6300 mg l�1, Fe2þ ¼ 500 mg l�1.
fixed at 3.0, thus confirming the appropriateness of the
value scheduled and fixed for carrying out the whole
investigation.
4. Conclusions
An investigation aimed at checking the effectiveness
of Fenton’s reagent (Fe2þ +H2O2 +Hþ) for the en-
hancement of the biodegradability of real old municipal
landfill leachate has been carried out at lab scale at
ambient temperature. The investigation has led to the
following results:
• Themaximum amount of COD that could be removed
by the Fenton’s pre-treatment was about 60% of the
initial value (i.e., 10 540 mg l�1). Such a maximum re-
moval was achieved using reagent dosages as high as
10 000 mg l�1 of H2O2 and 830 mg l�1 of Fe2þ.
• BOD5/COD ratio of the leachate could be increased
from 0.2, the initial value, up to 0.5, the minimum
value compatible with a subsequent biological post-
treatment, using the following optimum operational
conditions: initial pH¼ 3.0; Fe2þ ¼ 275mg l�1; H2O2¼3300 mg l�1; reaction time¼ 2 h.
• The progress of Fenton’s pre-treatment could be in-
strumentally monitored by measuring pH or redox
potential evolution during leachate oxidation, thus,
indicating the possibility of an on-line process moni-
toring.
• A simple acid–base titration of Fenton pre-treated
leachate proved that a relevant fraction of by-prod-
ucts formed during the treatment was made of acidic
compounds, thus demonstrating that the higher the
extent of Fenton’s oxidation the greater was the
amount of acids formed.
1010 A. Lopez et al. / Chemosphere 54 (2004) 1005–1010
• After the Fenton’s pre-treatment, in order to permit
subsequent biological treatment, residual ferric ions
were precipitated and coagulated with 3 g l�1 of
Ca(OH)2 and 3 mg l�1 of a cationic polyelectrolyte.
This final polishing step caused an additional modest
removal of residual COD.
In conclusion, the above results seem rather encour-
aging and worthwhile confirming on a larger scale as
they indicate a technologically simple and cost-effective
method for improving the biodegradability of recal-
citrant wastewater.
Acknowledgements
The authors thank Mr. Michele Cammarota and Mr.
Giuseppe Labellarte for their technical assistance during
the investigation.
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