Journal of Water and Environment Technology, Vol. 11, No.

4, 2013

Heavy Metal Removal and Phosphorus Retention Using

the Fenton Process for Sustainable Recycling of
Anaerobically Digested Sewage Sludge

Ayumi ITO*, Kenta TAKAHASHI**, Jyunya SUZUKI***, Teruyuki UMITA***

*Department of Frontier Materials and Function Engineering, Iwate University, Ueda 4-3-5,
Morioka, Iwate 020-8551, Japan
** Shimizu Corporation, Kyobashi 2-16-1, Chuo-ku, Tokyo 104-8370, Japan
***Department of Civil and Environmental Engineering, Iwate University, Ueda 4-3-5, Morioka,
Iwate 020-8551, Japan

ABSTRACT
Heavy metal removal from anaerobically digested sewage sludge and phosphorus (P) retention
in the sludge were investigated through batch experiments using H2O2 and Fe2(SO4)3 as the
agents for oxidizing insoluble metallic compounds under acidic condition at pH 2.5. The
addition of H2O2 to the sludge eluted Cd, Cu and Zn from the sludge more effectively than that
of acid only. The initial concentrations of H2O2 required for the maximum elution efficiency
were 1 g/L for Cd and Zn and 5 g/L for Cu. The addition of ferric ion (Fe(III)) also improved the
elution efficiency of Cu. Ferric iron addition under the initial H2O2 concentration of 0.2 g/L gave
rise to a more effective elution of Cu from the sludge than that in the absence of H2O2 or Fe(III).
The addition of acid only or both acid and H2O2 caused the elution of P together with heavy
metals. However, the addition of Fe(III) (1 g/L Fe) could retain P in the sludge, most of which
was present as a slow-acting P fertilizer.

Keywords: anaerobically digested sewage sludge, Fenton process, heavy metal removal,
phosphorus retention

INTRODUCTION
Wastewater treatment works bring about sound living and water environments, whereas
their expansion and process advancement have been increasing the production of
residual sludge. The sludge is frequently incinerated to decrease its volume and
especially in Japan where landfill sites are more limited, about 70% of sewage sludge is
being incinerated. This process requires an additional energy source such as fossil fuels
for combustion in some cases and involves emission of greenhouse gasses including
CO2 and N2O and their precursors such as CO, NO and NO2 (Murakami et al., 2009).
Sewage sludge is also partly used as an energy source and a raw material for fertilizers
or soil conditioners because it contains organic matter and nutrients such as nitrogen
and phosphorus (P). From the viewpoint of global warming prevention and appropriate
material cycle, the latter utilization will be the most reasonable option for sustainable
sludge recycling. However, hazardous substances such as heavy metals, endocrine
disrupting chemicals and pharmaceuticals can be transferred or accumulated into the
sludge through wastewater treatment processes and subsequent sludge treatment
processes (Giger et al., 1984; Chipasa, 2003; Radjenovic et al., 2009). Therefore, it is
necessary to reduce hazardous substance contents of the sludge applied to green and
agricultural lands.

In general, a portion of insoluble heavy metals in sewage sludge is eluted from the

Address correspondence to Ayumi Ito, Department of Frontier Materials and Function Engineering, Iwate
University, Email: aitou@iwate-u.ac.jp
Received November 8, 2012, Accepted February 26, 2013.
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sludge by acidification (Oliver and Carey, 1976). Biological acidification of the sludge
is a cost-effective process for the elution of heavy metals (Blais et al., 1992; Kitada et
al., 2001). Under acidic conditions, utilization of iron-oxidizing bacteria or oxidizing
agents such as ferric sulfate (Fe2(SO4)3) or hydrogen peroxide (H2O2) improved the
elution efficiency of heavy metals (Ito et al., 1998; Ito et al., 2000; Yoshizaki and
Tomida, 2000). Nowadays, it has been reported that heavy metal elution from the sludge
or soil was promoted by the Fenton process using H2O2 and ferrous sulfate (FeSO4)
(Dewil et al., 2007; Villa et al., 2008). Ito et al. (2008) showed that the addition of both
H2O2 (1g/L) and ferric ion (Fe(III)) (1g/L) enhanced the elution of Cu without P loss
from the anaerobically digested sewage sludge, whereas that of both H2O2 and ferrous
ion (Fe(II)) at the same concentrations resulted unexpectedly in low elution efficiency
of Cu. However, the mechanism of enhanced metal elution from the sludge by H2O2 and
Fe(III) addition is not fully understood and the quantitative influence of Fe(III) addition
as an operating parameter on both enhanced heavy metal elution and simultaneous P
retention remains unclear.

The purposes of this study were to clarify the optimal condition of Fe(III) addition in
the presence of H2O2 for enhanced Cu elution and insoluble P retention in anaerobically
digested sewage sludge and to evaluate the potential bioavailability of P retained in the
sludge for reuse as a raw material for organic fertilizers or soil conditioners.

MATERIALS AND METHODS

The anaerobically digested sludge used in this study was taken from a sewage treatment
plant in Iwate Prefecture, Japan. In this plant, sewage is treated by a conventional
activated sludge process for carbonaceous removal, and the mixture of primary and
surplus activated sludges is mesophilically digested. Polyferric sulfate is introduced into
the sludge thickeners to control the emission of hydrogen sulfide. Total volatile solids
content of the sludge was 64% (w/w). Table 1 shows heavy metals and P contents of the
sludge. The concentrations of heavy metals and P were respectively measured with an
inductively coupled plasma mass spectrometer (HP-4500, Yokogawa Analytical
Systems, Tokyo, Japan) after digesting the sludge with aqua regia and with a
spectrophotometer (UV-1600, Shimadzu Corp., Kyoto, Japan) by the molybdenum blue
method after digesting the sludge with nitric acid and sulfuric acid (Japan Sewage
Works Association, 1997).

In the batch experiment, the sludge concentrated by centrifugation (M160-2A, Sakuma,

Tokyo, Japan) was distributed into 2 L shaking culture flasks (AGC Techno Glass Co.,
Ltd., Chiba, Japan). It is reported that the preferable pH value in the Fenton reaction
using Fe(II) for the degradation of organic pollutants is generally around 3 (Arnold et
al., 1995; Lin and Lo, 1997). However, ferric ion is precipitated as ferric hydroxide at
pH 3. In order to prevent Fe(III) added to the sludge from precipitating, the pH was kept
at 2.5 with dilute sulfuric acid during the experiment. Different amounts of 30% (w/v)
H2O2 solution were added to the acidified sludges to clarify the influence of H2O2
concentrations on heavy metal elution from the sludge under an acidic condition. The
initial concentrations of H2O2 were respectively 0.1, 0.5, 1, 5 and 10 g/L in the sludge,
and the control without H2O2 addition was examined as well (Table 2).

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Table 1 - Heavy metals and P contents of the sludge used in this study and their total
and dissolved concentrations in the batch experiments.
Elements Cd Cu Fe Mn Ni P Zn
Amount in sludge (mg/kg) 1.1 290 17,000 480 18 33,000 810
Total concentration (mg/L) 0.022 5.8 340 9.6 0.36 660 16.2
Dissolved concentration (mg/L) 0.004 0.014 – 0.002 0.017 24.5 0.001

Table 2 - Experimental conditions for metal elution from sludge.

Initial concentration of oxidizing agent added to sludge
H2O2 (g/L) Fe(III) (g/L)
0
0.1
0.5
0
1
5
10
0
0.1
0
0.5
1
0
0.1
0.2
0.5
1

Besides the condition described above, Fe2(SO4)3 solution was added to the sludge
before H2O2 addition. The initial concentrations of H2O2 and Fe(III) added were
respectively 0.2 g/L and 0, 0.1, 0.5 and 1 g/L in the sludge (Table 2). The controls
without H2O2 addition were tested as well.

In all conditions, the sludge concentration was adjusted to 20 g dry solid /L with ultra
pure water (Milli-Q, Millipore Corp., Tokyo, Japan). The flasks containing the sludge
were kept mixing with a shaker at 120 rpm and 25°C for 24 hours. The total
concentrations of heavy metals in the sludge slurry calculated based on the heavy metal
content of the sludge and the sludge concentration are shown in Table 1. The sludge pH
was measured with a pH meter (F-12 Horiba Ltd., Kyoto, Japan). The oxidation
reduction potential (ORP) was monitored with an ORP meter (HM-5S, TOA Corp.,
Kobe, Japan) in order to qualitatively compare the occurrence and elimination of
oxidizing agents during the process. About 80 mL of the sludge in the flasks was
collected in plastic tubes and was centrifuged at 10,000 rpm for 10 minutes. The
supernatant was filtrated through a membrane filter with a pore size of 1 μm (Advantec,
Tokyo, Japan) for dissolved heavy metals and P measurements as described previously.
The initial dissolved concentrations of heavy metals and P are shown in Table 1. Ferrous

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and ferric ions (Fe(II) and Fe(III)) in the filtrate were analyzed using a
spectrophotometer by the phenanthroline method (Japan Sewage Works Association,
1997). Before and after the experiment, phosphorus was extracted from the sludge with
pure water and 2% citric acid to evaluate the bioavailability as a slow-acting fertilizer of
P retained in the sludge (Adam et al., 2009). The sludge of 0.5 g and the pure water of
40 mL or 2% citric acid of 75 mL were mixed with a shaker for an hour.
Water-extractable P and 2% citric acid-extractable P were collected after centrifugation
of the mixtures (Yamane, 1988).

RESULTS
Influence of initial H2O2 concentrations on heavy metal elution from sludge
The variation in elution efficiencies of (a) Cu and (b) Zn from the sludge with time at
different initial concentrations of H2O2 is shown in Fig. 1 as the examples of heavy
metal elution. The elution efficiency means a percentage of the amount of dissolved
heavy metals to the total amount of heavy metals in the samples shown in Table 1.
Elution efficiencies of Cu and Zn increased at certain elapsed time with an increase in
the initial H2O2 concentration and showed slower increases with time under lower H2O2
concentrations.

Figure 2 shows the maximum elution efficiencies of heavy metals from the sludge after
24 hours from the start of the experiment at different initial H2O2 concentrations. The
maximum efficiencies were 98% for Cd, 85% for Zn, 82% for Mn, 70% for Cu and
61% for Ni. Elution efficiency of Cu was positively correlated with H2O2 concentration
in the range of 0 to 1 g/L. In this study, the optimum H2O2 concentrations were 1 g/L for

Control 0.1 g/L 0.5 g/L 1 g/L 5 g/L 10 g/L

100 100
Elution efficiency (%)

Elution efficiency (%)

80 80

60 60

40 40

20 20

0 0
0 5 10 15 20 25 0 5 10 15 20 25
Elapsed time（h） Elapsed time（h）
(a) Cu (b) Zn
Fig. 1 - Variation in elution efficiencies of (a) Cu and (b) Zn from the sludge with
time at different initial H2O2 concentrations. Sampling at 0 h was conducted
before acidification and oxidizing agent addition.

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100
Cd

Elution efficiency (%)

80
Cu
60
Mn
40
Ni
20
Zn
0
0 2 4 6 8 10
H2O2 concentration (g/L)
Fig. 2 - Maximum elution efficiencies of heavy metals from the sludge after 24 hours
from the start of the experiment at different initial H2O2 concentrations.

Cd and Zn and 5 g/L for Cu. Yoshizaki and Tomida (2000) also reported that Cu was
effectively eluted from a filter cake by 20 g/L H2O2 addition in the presence of 8%
phosphoric acid, whereas elution of Cr and Ni were not improved, which corresponded
to the result of this study.

Figure 3 shows the variation in (a) Fe(II) concentration and (b) ORP value with time at
different initial H2O2 concentrations. The concentration of Fe(II) was increased to about
100 mg/L in the control with the addition of acid only, indicating that Fe(II) was eluted
from the sludge by acidification. In the case of H2O2 addition, Fe(II) concentrations
became low compared to the control. This was due to the oxidation of Fe(II) with H2O2
in the Fenton reaction shown in equation (1) (Neyens and Baeyens, 2003).
Fe2+ + H2O2 → Fe3+ + ･OH + OH－ (1)
However, the oxidation of Fe(II) was insufficient at an initial H2O2 concentration of 0.1
g/L. On the other hand, the addition of H2O2 resulted in high ORP values compared to
the control. The ORP values reached about 730 mV except for an initial H2O2
concentration of 0.1 g/L and then decreased to about 540 mV at initial H2O2
concentrations of 0.5 and 1 g/L, suggesting that H2O2 added to the sludge was almost
consumed after 24 hours. Improvement of Cu elution by H2O2 addition (Fig.1(a)) would
be owing to the oxidation of insoluble metallic compounds with oxidizing agents such
as H2O2, Fe(III) and/or hydroxyl radicals. In this case, however, Fe(III) and hydroxyl
radicals produced by the Fenton reaction probably played a minor role in enhanced Cu
elution because the amount of Fe(II) oxidized with H2O2 during the first six hours was
almost equal (about 65 mg/L) in the range of 0.5 to 10 g/L H2O2 concentrations
(Fig.3(a)). Therefore, in order to clarify how each oxidizing agent associated with the
Fenton process contributes to enhancement of heavy metal elution and to determine the
optimal condition for simultaneous P retention, the quantitative effect of Fe(III) addition
was investigated under lower H2O2 concentration (0.2 g/L) in consideration of the direct
H2O2 effect on metal elution as well as the economic aspect.

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Control 0.1 g/L 0.5 g/L 1 g/L 5 g/L 10 g/L

100 800
Fe(II) concentration (mg/L)

80
700

ORP (mV)
60
600
40
500
20

0 400
0 5 10 15 20 25 0 5 10 15 20 25
Elapsed time（h） Elapsed time（h）
(a) Fe(II) (b) ORP
Fig. 3 - Variation in (a) Fe(II) concentration and (b) ORP value with time at different
initial H2O2 concentrations. Initial values of ORP at 0 h were measured
immediately after acidification and H2O2 addition

Effect of ferric sulfate addition on enhanced heavy metal elution by the Fenton
process and simultaneous phosphorus retention
Figure 4 shows the variation in (a) Cu elution efficiency, (b) P elution efficiency, (c)
Fe(II) concentration and (d) ORP value with time at different concentrations of Fe(III)
added. The elution efficiency of Cu with no addition of H2O2 was increased at certain
elapsed time with an increase in the concentration of Fe(III) added, indicating that
insoluble copper compound such as sulfide in the sludge would be oxidized by Fe(III)
(Ito et al., 2000). On the other hand, the addition of H2O2 accelerated the elution of Cu
from the sludge compared to no addition of H2O2, and its elution was significantly
enhanced at a Fe(III) concentration of 1 g/L. Although acidification of the sludge eluted
about 80% of P from the sludge, its elution efficiency was decreased with an increase in
the concentration of Fe(III) added and was less than 10% at a Fe(III) concentration of 1
g/L. This decrease was due to the formation of ferric phosphate or co-precipitation of
phosphate with ferric hydroxide. It was found that the Fe(III) concentration of 1 g/L was
required for sufficient P retention in the sludge solid phase under acidic condition.

In the absence of H2O2, the addition of Fe(III) elevated the concentrations of Fe(II)
compared to acidification only and their concentrations were increased at a certain
elapsed time with an increase in the concentration of Fe(III) added. These increases
indicate that a part of Fe(III) added to the sludge oxidized reducing substances such as
metal sulfide in the sludge and was reduced to Fe(II). The addition of H2O2 resulted in
low concentrations of Fe(II) compared to no addition of H2O2. The concentrations of
Fe(III) were less than 10 mg/L during the experiment under all conditions (data not
shown) due to precipitation with phosphate eluted from the sludge and possible
adsorption onto organic matters contained in the sludge.

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Acidification only Fe(III)(0.1g/L) Fe(III)(0.5g/L) Fe(III)(1g/L)

H2O2
H2O2 Fe(III)(0.1g/L) and H2O2
H2O2 Fe(III)(0.5g/L) and H
H2O2
2O2 Fe(III)(1g/L) and H
H2O2
2O 2

40 100
Elution efficiency (%)

Elution efficiency (%)

30 80

60
20
40
10
20

0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Elapsed time (h) Elapsed time (h)
(a) Cu (b) P

200 800
Fe(II) concentration (mg/L)

150 700
ORP (mV)

100 600

50 500

0 400
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Elapsed time (h) Elapsed time (h)

(c) Fe(II) (d) ORP

Fig. 4 - Variation in (a) Cu elution efficiency, (b) P elution efficiency, (c) Fe(II)
concentration and (d) ORP with time at different concentrations of Fe(III)
added.

In this study, the ignition loss of the sludge treated under the conditions described above
was analyzed to examine the reduction of organic substances in the sludge with H2O2
and/or hydroxyl radicals. However, no remarkable reduction of ignition loss was
observed in the sludge with the addition of H2O2 compared to those with no addition
(data not shown).

Extractability of phosphorus retained in sludge

Table 3 shows the extractability of P in the sludge before and after elution process using

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Table 3 - Extractability of P in the sludge before and after elution process (%).
Form of P Before elution process After elution process
Water-extractable 10 3
2% citric acid-extractable 78 84

both H2O2 and Fe(III) at a concentration of 1 g/L. Water-extractable P in the sludge was
decreased from 10% to 3%, whereas 2% citric acid-extractable P was increased from
78% to 84%, suggesting that most of the P retained in the sludge was immobilized as a
slow acting P fertilizer, although ferric phosphate is not generally used for fertilizing
purposes.

DISCUSSION
As shown in Fig 4 (c), when 1 g/L Fe(III) was added to the sludge with no addition of
H2O2, the concentration of Fe(II) reached about 125 mg/L (2.2 mM) after the first one
hour from the start of the experiment. On the other hand, when 0.2 g/L H2O2 (5.9 mM)
was added to the sludge, the molar ratio of H2O2 (5.9 mM) to Fe(II) (2.2 mM) would be
approximately 2.7 to 1. For instance, Jiang et al. (2010) investigated the effect of iron
concentration on the degradation of phenol in an aqueous solution by the Fenton process
at pH 3 and showed that more than 90% of phenol could be degraded even though the
molar ratio of H2O2 (1.0 mM) to Fe(II) (0.4 mM) was 2.5 which is lower than the ratio
of this study. Therefore, it is likely that in this process the Fenton reaction occurred
between H2O2 and Fe(II) which is both eluted from the sludge by acidification and
produced by oxidation of the sludge with Fe(III) added, and hydroxyl radicals were
produced as described previously. The difference of the Fe(II) concentration after one
hour of the experiment between H2O2 addition and no addition shows the amount of
Fe(II) oxidized with H2O2, which was increased with an increase in the concentration of
Fe(III) added. This suggests that the amount of hydroxyl radicals produced by the
Fenton reaction would be increased similarly. When H2O2 was added, the initial ORP
values were higher than 700 mV and was the highest in the addition of both H2O2 and
Fe(III) at a concentration of 1 g/L as shown in Fig. 4(d). Hence, it is likely that the
formation of more oxidant such as hydroxyl radicals by the addition of both H2O2 and
Fe(III) at a concentration of 1 g/L gave rise to a rapid elution of Cu present as metallic
sulfide (Ito et al., 2000) and organically bound compound (Yoshizaki and Tomida,
2000) in the sludge during the first one hour compared to the addition of either H2O2 or
Fe(III). Little information on the removal of heavy metals from sewage sludge by the
Fenton process is available. However, Dewil et al. (2007) reported that Fenton’s
peroxidation at pH 3 resulted in a significant reduction of Cd, Cu, Ni and Zn in the
sludge cake when the amounts of Fe(II) and H2O2 added to the sludge were respectively
0.55 g/kg dry sludge and in the range of 10 to 50 g/kg dry sludge. In addition, the effect
of hydroxyl radicals on the release of heavy metals from the sludge remained unclear
because no controls (i.e. without addition of Fe(II)) and no determination of Fe(II)
concentration were investigated.

In terms of the effect of Fe in the sludge on the soil environment, the Fe content of the
sludge after this process is estimated to be about 70 g/kg-dry sludge where the original
Fe content of the sludge is 20 g/kg-dry sludge and the amount of Fe(III) added was 50

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g/kg-dry sludge. It has been reported that the average Fe contents of the field and paddy
soils in Japan are around 40 g/kg dry solid and 50 g/kg dry solid, respectively (Uchida
et al., 2007a, b). Considering the essentiality of Fe to the plants and the dilution of the
sludge with the original soils, the sludge containing 70 g/kg of Fe could be used for
fertilizer and soil conditioner.

From these results, it was revealed that the Fenton process in the presence of H2O2 and
Fe(II) which was both eluted from the sludge and produced by the oxidation of reducing
substances in the sludge with Fe(III) added could enhance the Cu elution from
anaerobically digested sewage sludge and simultaneously retain P in the sludge for
fertilizing purposes.

CONCLUSIONS
In this study, heavy metal removal from anaerobically digested sewage sludge by the
Fenton process and simultaneous P retention in the sludge were investigated under
acidic condition at pH 2.5. The optimal H2O2 concentrations for heavy metal elution
from the sludge were 1 g/L for Cd and Zn and 5 g/L for Cu. Their maximum elution
efficiencies were 98% for Cd, 70% for Cu and 85% for Zn. When the concentrations of
H2O2 and Fe(III) added were respectively 0.2 g/L and 1 g/L, the elution of Cu was
enhanced by the Fenton process as compared to cases when neither H2O2 nor Fe(III)
was added. Phosphorus in the sludge was effectively retained as the slow-acting
fertilizer. This process will be a useful option for sludge detoxification and recycling.

ACKNOWLEDGEMENTS
This study was financially supported by the Grant-in-Aid for Scientific Research of the
Japanese Ministry of Education, Culture, Sports, Science and Technology, and the Iwate
Prefectural Sewage Public Corporation.

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