Research Article

Received: 18 February 2010 Revised: 2 September 2010 Accepted: 19 September 2010 Published online in Wiley Online Library:

(wileyonlinelibrary.com) DOI 10.1002/jctb.2524

Activated carbons prepared from biogas

residue: characterization and methylene blue
adsorption capacity
Xianzheng Yuan,a∗ Xiaoshuang Shi,a Shujuan Zenga,c and Yueli Weia,b

Abstract
BACKGROUND: In China, some biogas residue, which cannot be utilized by microbes in the anaerobic process, has been used
as fertilizer. More has been deposited in biogas plants or on land around the plants. This has an effect on the environmental
protection of the biogas plant, especially if the high lignin content in the biogas residue is not handled properly.

RESULTS: In this study biogas residue has been used for the preparation of activated carbons by phosphoric acid activation.
Textural characterization and feasibility of employing the prepared activated carbon to remove methylene blue (MB) from
aqueous solution were investigated. The results show that the activated carbons have high surface area (1950 m2 g−1 ) and pore
volume (1.232 cm3 g−1 ). Equilibrium data were best described by the Langmuir isotherm model, with a maximum monolayer
adsorption capacity of 344.83 mg g−1 at 25 ◦ C. Among the kinetic models studied, the pseudo-first-order model was found to
be the most applicable to describe the adsorption of MB.

CONCLUSIONS: The adsorption performance of activated carbons prepared from biogas residues (BR-AC) was comparable with
that of commercial material and other adsorbents reported in earlier studies and presents a high value added application for
biogas residues.

c 2010 Society of Chemical Industry

Keywords: biogas residue; activated carbons; methylene blue adsorption; adsorption isotherm; adsorption kinetics

INTRODUCTION Activated carbons are well-known adsorbents used extensively

Anaerobic digestion is receiving increased attention all over the
world owing to its potential for renewable energy production
and environmental protection. Many studies have shown that the
capture and energy recovery from biogas plants may contribute
considerably to a reduction in greenhouse gas emissions,
particularly if used as a biofuel.1 According to national plans,
by the end of 2010, 40 million household biogas digesters and
4000 large biogas plants will be built in China.2 The number of
biogas plants will be increased rapidly in the next few years in
China along with other countries, such as Germany,3 which will
result in the increased generation of residues from biogas plants.
Biogas residues are the final remnant of the original waste placed in
digesters, and which cannot be used by microbes in the anaerobic
process. This residue is used as a fertilizer instead of conventional
slurry to close the nutrient cycle in agricultural ecosystems.4
However in China, only a little biogas residue has been used as
fertilizer. Occasionally the local population would rather use the
slurry in the bottom of the residue tank as a fertilizer than the
cellulosic materials on the top. This is because the amount of lignin
in anaerobically digested residue is higher than in conventional
slurry, especially for anaerobic digestion of agricultural by-
products, such as dairy manure, straw and energy crops.5 More
of the biogas residue was deposited in biogas plants or on arable
land around the plants. In this case, it will have an effect on the
environmental protection of the biogas plant, especially if the high
lignin content of the biogas residue is not handled properly.
for purification and separation in many industrial processes and in
effluent treatment. The world consumption of activated carbons
is steadily increasing as applications concerning environmental
pollution emerge. However, for many countries commercially
available activated carbons are still considered expensive materials
due to the use of non-renewable and relatively expensive materials
such as coal, which can be a drawback to their use.6,7 Therefore,
in recent years, there has been a growing research interest in
the production of activated carbons from renewable and cheaper
precursors, mainly agricultural by-products.8 However, to our
knowledge the use of biogas residue as a precursor for activated
carbons has not previously been investigated. Conversion of
biogas residue to activated carbons will serve a double purpose.
First, unwanted biogas residue will be converted to a useful
∗ Correspondence to: Xianzheng Yuan, Key Laboratory of Biofuels, Qingdao
Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences,
Qingdao, Shandong Province 266101, P. R. China. E-mail: yuanxz@qibebt.ac.cn
a Key Laboratory of Biofuels, Qingdao Institute of Bioenergy and Bioprocess
Technology, Chinese Academy of Sciences, Qingdao, Shandong Province
266101, P. R. China
b College of Environment and Safety Engineering, Qingdao University of Science
and Technology, Qingdao, Shandong Province 266042, P. R. China
c Graduate University of Chinese Academy of Sciences, Beijing 100049, P. R. China

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Table 1. The characterizations of biogas residue
Proximate analysis Ultimate analysis Composition
(wt%) (wt%) (wt%)
Ash 2.15 nitrogen 1.95 cellulose 14.85
Fixed carbon 20.91 carbon 46.58 hemicellulose 19.72
Volatile 68.42 hydrogen 6.91 lignin 10.41
sulfur 0.44
oxygena 22.87
a Calculated from difference.
value-added adsorbent, and second, the use of activated carbons
represents a potential source of adsorbents to solve part of the
waste-water treatment problem in China.
Hence, in searching for high added-value applications of biogas
residue the feasibility of preparing activated carbons from biogas
residue was investigated. The focus of this research was to evaluate
the adsorption potential of biogas residue based activated carbons
(BR-AC) in removing methylene blue (MB) from aqueous solutions.
The equilibrium and kinetic data of the adsorption process
were then evaluated to study the adsorption mechanism of MB
molecules onto BR-AC.
EXPERIMENTAL
Materials
The biogas residue used in this study was obtained from the top of a
biogas residue tank in an 800 m3 size biogas plant (Jimo, Qingdao,
China) then air dried. The biogas plant was fed by dairy manure with
a 25 day retention time, operating at 32 ◦ C. The characterizations
of the biogas residue are shown in Table 1. This may be considered
a good precursor candidate for conversion to activated carbons
because of its relatively high carbon content and low ash.
Preparation of activated carbons
Before activation, the biogas residue (25 g) was impregnated with
30% v/v H3 PO4 (100 mL) for 24 h at room temperature and then
dried at 105 ◦ C overnight. The mixture was placed in a stainless-
steel reactor (550 mm length and 38 mm i.d.) and activated at
500 ◦ C for 2 h under a stream of N2 gas flowing at 30 mL min−1
at a heating rate of 5 ◦ C min−1 . After pyrolysis, the stainless-steel
reactor was cooled to room temperature in a N2 stream. Then, the
products were boiled under reflux with HCl solution to remove
impurities and reduce the ash content of the activated carbons.
After that, they were washed several times with hot distilled water,
and finally with cold distilled water until chloride ions were not
detected. The washed samples were finally dried at 105 ◦ C for 24 h
to produce the BR-AC. The average yield of BR-AC was 42.0%.
Textural and chemical characterization of BR-AC
The specific surface areas and porous texture of BR-AC were
measured using the adsorption of nitrogen at 77 K with a surface
area and porosimetry system (ASAP 2020, Micromerities, USA). This
experiment was carried out in duplicate, and the results expressed
as a mean. The surface characteristics of samples were analyzed
using scanning electron microscopy (JSM 5410, JEOL, Japan) and
elemental analysis was carried out in a CHNOS Analyzer (PE
2400, Perkin Elmer, USA). Prior to analysis, the samples were dried
overnight at 105 ◦ C and cooled in a desiccator. The oxygen content
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c 2010 Society of Chemical Industry
X Yuan et al.
was obtained by the difference between the total percentage and
the sum of percentages of nitrogen, carbon, hydrogen and sulfur.
Methylene blue adsorption
MB adsorption studies are widely used for the evaluation of
adsorbents because this dye can be viewed as a model for visible
pollution. A fixed carbon concentration (0.6 g L−1 ) was weighed
into 50 mL conical flasks containing 25 mL of different initial
concentrations of MB solution at pH 6.5. The flasks were agitated
mechanically for predetermined time intervals at 140 rpm using
a rotary orbital shaker, and maintained at 25 ◦ C for 48 h. The
suspensions were then filtered and the initial and equilibrium
concentrations were measured using a UV/visible spectrometer
(Cary 50, Varian, USA) at a wavelength of 665 nm. In addition,
a blank experiment was conducted to verify that there was
no adsorption on the walls. The amount of adsorbed MB at
equilibrium, qe (mg g−1 ) was calculated by:
qe = V(C0 − Ce )/w
where C0 and Ce (mg L−1 ) are the liquid-phase initial and
equilibrium concentrations of MB, respectively; V (L) is the volume
of MB solution, and w (g) is the mass of dry adsorbent used.
The equilibrium data were then fitted using four different
isotherm models, i.e. the Langmuir, Freundlich, Temkin and
Dubinin–Radushkevich models.9
Kinetic experiments were performed in glass beakers with an
activated carbon concentration of 0.6 g L−1 and MB concentrations
of 10, 20, 40 and 60 mg L−1 , respectively. The progress of the
adsorption process was determined on duplicate filtered 3 mL
samples by measuring the absorbance of the dye at different
time intervals. The methylene blue uptake by the adsorbent was
calculated using the following equation:
qt = V(C0 − Ct )/m
where qt (mg g−1 ) is the amount of MB adsorbed and Ct (mg L−1 )
the concentration of MB solution at time t. The kinetic data were
then fitted using the pseudo-first-order and intraparticle diffusion
models.10
RESULTS AND DISCUSSION
Characterizations of BR-AC
The BET surface area of BR-AC was 1950 m2 g−1 with a total
pore volume of 1.232 cm3 g−1 . The results indicated that BR-AC
contained relatively large surface area and total pore volume
compared with commercially available activated carbons, such as
BDH, F100 (Merck, UK) and BPL (Calgon, USA) with BET surface
areas of 1118, 957 and 972 m2 g−1 and total pore volumes of 0.618,
0.526 and 0.525 cm3 g−1 , respectively.11 Figs 1(a) and (b) show,
respectively, SEM images of the biogas residue and BR-AC and
show the drastic differences between these materials. The biogas
residue is a fibrous and compact material. On the other hand,
on the surface of BR-AC many pores in a honeycomb shape are
clearly found. This shows that H3 PO4 was effective in creating
well-developed pores on the surface of the biogas residue leading
to BR-AC with large surface area and porous structure.
Owing to the environmental benefits and several other
advantages such as ease of recovery, low energy cost and high yield
of activated carbon, phosphoric acid activation of lignocellulosic
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Activated carbons prepared from biogas residue www.soci.org

(a) SEM image of raw biogas residue (b) SEM image of BR-AC

Figure 1. SEM image of: (a) raw biogas residue and (b) BR-AC.

Table 2. Isotherm parameters for MB on BR-AC at 25 ◦ C

Langmuir Freundlich

R2 Q0 (mg g−1 ) KL (L mg−1 ) R2 n KF (mg g−1 (L mg−1 )1/n )

0.9981 344.83 0.31 0.9563 2.63 84.21
Temkin Dubinin–Radushkevich

R2 B A (L mg−1 ) R2 qs (mg g−1 ) E (kJ mol−1 )

0.9777 54.11 6.70 0.6839 187.00 2357.02

where:
Q0 = maximum amount of MB per unit weight of BR-AC to form a complete monolayer on the surface;
KL = the affinity of the binding sites;
KF = the adsorption capacity of the adsorbent;
n = an indication of adsorption intensity;
B = related to the heat of adsorption;
A = equilibrium binding constant;
qs = theoretical monolayer saturation capacity;
E = mean adsorption energy.

materials has become, in recent years, a popular method for
the large-scale manufacture of activated carbons.12 According to
earlier studies, phosphoric acid acts in two major ways during the
conversion of precursors into highly porous activated carbons. On
the one hand, it acts as an acid catalyst to promote bond cleavage,
hydrolysis, dehydration and condensation, accompanied by cross-
linking reactions between phosphoric acid and biopolymers.13,14
These lead to further incorporation of phosphoric acid into the
interior of the botanical structure to form a composite consisting
of phosphoric acid, polyphosphoric acid and biopolymers. On
the other hand phosphoric acid may function as a template with
several studies indicating that the volume occupied by phosphoric
acid in the interior of the activated particles is coincident with the
micropore volume of the activated carbon obtained.14,15
Adsorption isotherm
MB is often used as a model compound for adsorption of organic
contaminants by mesoporous materials, and is accessible to pores
with diameters larger than 1.5 nm. Thus in this work, to evaluate
the liquid phase ability adsorption of BR-AC, adsorption isotherms
are performed using the molecule.
The isotherm parameters calculated from the models together
with the correlation coefficients are listed in Table 2. The data
show that, compared with the other three models, the Langmuir

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Table 3. Comparison of the maximum monolayer adsorption of MB on various agro-based activated carbons
Agro-based activated Surface area Pore volume Maximum monolayer adsorption
carbons (m2 g−1 ) (cm3 g−1 ) capacity (mg g−1 ) Reference

Biogas residue 1950 1.232 344.83 Present studies

Oil palm fibre 1354 0.778 277.78 18
Coconut husk 1940 1.143 434.78 9
Oil palm shell 596.20 0.34 243.90 19
Dehydrated wheat bran 9.5 – 122.0 20
Rattan sawdust 1083 0.644 294.12 21
Rosa canina sp. Seeds 799.52 – 47.2 22

(a) MB adsorption as a function of adsorption time and kinetic model (b) MB adsorption as a function of time for the initial 25 minutes
fitting at 25°C adsorption and kinetic model fitting at 25°C

Figure 2. Adsorption kinetics of MB onto BR-AC at 25 ◦ C (points, experimental data; dash curves, pseudo-first-order model fit; solid curves, intraparticle
diffusion model fit). (a) MB adsorption as a function of adsorption time and kinetic model fitting. (b) MB adsorption as a function of time for the initial
25 min adsorption and kinetic model fitting.

model yielded the best fit with R2 values of 0.9981. The maximum
Langmuir monolayer adsorption capacity (Q0 ) was 344.83 mg g−1 .
The different shapes of the adsorption isotherms are due
to the different porous structures of adsorbents and of the
adsorbate–adsorbent interactions. The agreement between
the experimental data and the Langmuir model suggested the
homogeneous nature of the prepared activated carbon surface,
i.e. each dye molecule/prepared activated carbon adsorption had
equal adsorption activation energy. The results also demonstrated
the formation of monolayer coverage of dye molecules on
the outer surface of BR-AC. In addition, this indicated that MB
adsorbed on BR-AC is associated with a very high adsorption
affinity and relatively strong adsorbent–adsorbate interactions.
Similar observations were reported for the adsorption of MB on
activated carbons prepared from jute fibre,16 olive-seed waste
residue11 and corncob.17
The maximum monolayer adsorption capacities of MB onto
various agro-based adsorbents are listed in Table 3. Compared
with other sorption capacities in the literature BR-AC had a
higher surface area (1950 m2 g−1 ) and relatively large adsorption
capacity of 344.83 mg g−1 . Previous research showed that
adsorption does not always increase with surface area.23 In
addition to the physical structure, the adsorption capacity of a
given carbon is strongly influenced by the chemical nature of the
surface and the acid and base character of a carbon influences
the nature of the dye isotherms. The adsorption also depends
on various adsorbate/adsorbent interactions e.g. electrostatic
and non-electrostatic interactions. In addition, variation in the
adsorption capacity compared with other agro-based activated
carbons might be due to the original nature of the precursors and
the processes applied to produce the adsorbent.
Adsorption kinetics
Figure 2 shows the adsorption capacity versus the adsorption time
for various initial MB concentrations. The sorption ratio decreased
with increase in initial MB concentration but the amount of MB
adsorbed per unit mass of BR-AC increased with increasing MB
concentration. The unit adsorption for MB thus increased from
17.30 to 78.19 mg g−1 as the MB concentration increased from 10
to 60 mg L−1 . Equilibrium was established in 180 min for all the
concentrations studied.
To study the adsorption of organic molecules on the activated
carbons from the liquid phase and to interpret the experimental
data obtained, pseudo-first-order and intraparticle diffusion
models have been used. To compare quantitatively the accuracy of
the model the correlation coefficient R2 and normalized standard
deviation
q (%) were calculated (Table 4). The normalized
standard deviation
q (%) was calculated as follows:



 [qt,exp − qt,cal )/qt,exp ]2


q(%) = 100 ×
n−1

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Activated carbons prepared from biogas residue
Table 4. Kinetic parameters for the adsorption of MB onto BR-AC at 25 ◦ C
Kinetic model Parameters 10 mg L−1
pseudo-first-order qe (mg g−1 ) 17.35
k1 (h−1 ) 0.057
R2 0.9709

qt (%) 0.2882
intraparticle diffusion kint (mg g−1 h−1/2 ) 1.47
C 2.72
R2 0.8166

qt (%) 0.7515
where:
qe = amount of MB adsorbed at equilibrium;
k1 = pseudo-first-order rate constant;
kint = intraparticle diffusion rate constant;
C = intercept.
where qt,exp and qt,cal refer to the experimental and calculated
values and n is the number of data points.
The correlation coefficients for pseudo-first-order kinetics were
between 0.8837 and 0.9709, which were higher than those for the
intraparticle diffusion equation (0.8166–0.9041). The pseudo-first-
order kinetic model also yielded the lowest
q values ranging
from 0.2420–0.8495%. Based on the highest R2 values which
approached unity and the lowest
q value, the pseudo-first-
order model was the most suitable equation to describe the
adsorption kinetics of MB on BR-AC. However, it seems clear that
the model only fits well the lower BR-AC loadings, and become
less well-behaved as the contact time increases. MB adsorption
as a function of time for the first 25 min and the fit of the kinetic
model is shown in Fig. 2(b). It shows that during the first 25 min,
the correlation coefficients for pseudo-first-order kinetics decrease
from 0.9154 to 0.7778 as the BR-AC concentration increases from 10
to 60 mg L−1 , while the correlation coefficients of the intraparticle
diffusion equation were 0.9737, 0.9821, 0.9824 and 0.9455 with
BR-AC concentrations of 10, 20, 40 and 60 mg L−1 . During the
adsorption process dye molecules first encounter the boundary
layer effect and then diffuse from the boundary layer film onto
the adsorbent surface; finally, they have to diffuse into the porous
structure of the adsorbent.16,24 Hence, initially MB adsorption on
BR-AC is dominated by intraparticle diffusion.
CONCLUSIONS
Biogas residue was used as raw material for the production of
activated carbons using H3 PO4 as activation agent. The physical
and chemical properties of BR-AC, as well as its characteristics for
liquid-phase adsorption were investigated. The results indicated
that BR-AC contained relatively large surface area (1950 m2 g−1 )
and total pore volume (1.232 cm3 g−1 ) comparable with some
commercially available activated carbons. Initially the sorption
of MB onto BR-AC was dominated by intraparticle diffusion. Of
the two kinetic equations used, the pseudo-first-order equation
is the best model to describe the adsorption of MB onto
BR-AC. Compared with the other three models the Langmuir
model is the most suitable model for describing adsorption
of MB on BR-AC (R2 > 0.99), with an adsorption capacity
of 344.83 mg g−1 . The adsorption performance of BR-AC was
comparable with commercial activated carbons and some other
adsorbents reported in earlier studies.
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20 mg L−1 40 mg L−1 60 mg L−1
28.67 53.88 70.31
0.063 0.066 0.081
0.9198 0.9179 0.8837
0.1562 2.5294 3.3302
2.39 4.51 5.62
5.62 10.90 18.56
0.9006 0.9041 0.8622
0.4878 1.0781 1.1212
ACKOWLEDGEMENTS
This work was supported by Key Projects in the National Science
& Technology Pillar Program in the Eleventh Five-year Plan Period
(grant no. 2008BADC4B18) and Key Science & Technology Project
of Shandong Province of China under Grant No. 2008GG20007003.
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