Granular Activated Crbon From Activated Sludge

ISSN 0104-6632
Printed in Brazil
www.abeq.org.br/bjche
Vol. 26, No. 01, pp. 127 - 136, January - March, 2009
*To whom correspondence should be addressed
Brazilian Journal
of Chemical
Engineering
PRODUCTION AND CHARACTERIZATION OF
GRANULAR ACTIVATED CARBON FROM
ACTIVATED SLUDGE
Z. Al-Qodah1*
and R. Shawabkah2,3
1
Department of Chemical Engineering, Al-Balqaa Applied University Jordan,
Amman, Marka, P. O. Box 340558, 11134, Jordan.
E-mail: z_Alqodah@hotmail.com
2
Present Address: Department of Chemical Engineering, King Fahd University of Petroleum & Minerals,
Dhahran, Kingdom of Saudi Arabia. E-mail: rshawabk@kfupm.edu.sa
3
Permanent Address: Department of Chemical Engineering, Mutah Univeristy, AL-Karak, Jordan.
E-mail: rshawabk@mutah.edu.jo
(Submitted: February 01, 2007 ; Accepted: February 01, 2008)
Abstract - In this study, activated sludge was used as a precursor to prepare activated carbon using sulfuric
acid as a chemical activation agent. The effect of preparation conditions on the produced activated carbon
characteristics as an adsorbent was investigated. The results indicate that the produced activated carbon has a
highly porous structure and a specific surface area of 580 m2
/g. The FT-IR analysis depicts the presence of a
variety of functional groups which explain its improved adsorption behavior against pesticides. The XRD
analysis reveals that the produced activated carbon has low content of inorganic constituents compared with
the precursor. The adsorption isotherm data were fitted to three adsorption isotherm models and found to
closely fit the BET model with R2
equal 0.948 at pH 3, indicating a multilayer of pesticide adsorption. The
maximum loading capacity of the produced activated carbon was 110 mg pesticides/g adsorbent and was
obtained at this pH value. This maximum loading was found experimentally to steeply decrease as the
solution pH increases. The obtained results show that activated sludge is a promising low cost precursor for
the production of activated carbon.
Keywords: Activated carbon; Activated biomass; Sulphuric acid activation; Carbon activation; Activated
carbon characterization; Spectroscopic analysis.
INTRODUCTION
Activated carbons are carbonaceous materials that
can be distinguished from elemental carbon by the
oxidation of the carbon atoms found on the outer and
inner surfaces (Mattson and Mark 1971). These
materials are characterized by their extraordinary
large specific surface areas, well-developed porosity
and tunable surface-containing functional groups
(Baker et al. 1992, Zongxuan et al., 2003). For these
reasons, activated carbons are widely used as
adsorbents for the removal of organic chemicals and
metal ions of environmental or economic concern
from air, gases, potable water and wastewater (El-
Hendawy 2003).
The surface oxygen functional groups can be
easily introduced to the carbon by different
activation methods including dry and wet oxidizing
agents. Dry oxidation methods involve the reaction
with hot oxidizing gas such as steam and CO2 at
temperatures above 700o
C (Smisek and Cerney
1970). Wet oxidation methods involve the reaction
between the carbon surface and solutions of
oxidizing agents such as phosphoric acid H3PO4,
nitric acid HNO3, hydrogen peroxide H2O2, zinc
chloride ZnCl2, potassium permanganate KMnO4,
ammonium persulphate (NH4)2S2O8, potassium
hydroxide KOH, etc. From the above oxidizing
agents, phosphoric acid and zinc chloride are usually
used for the activation of lignocellulosic materials,

128 Z. Al-Qodah and R. Shawabkah
Brazilian Journal of Chemical Engineering
which have not been carbonized before (Puziy et al.,
2002). On the other hand, potassium hydroxide is
usually used to activate coal or chars precursors. It
has been reported that zinc chloride produces
activated carbon with higher specific area than that
produced by using phosphoric acid (Okada et al.,
2003). However, phosphoric acid activation is
widely preferred over zinc chloride because ZnCl2
has bad environmental impact and the activated
carbon produced when using it can not be used in the
food and pharmaceutical industries (Srinivasakannan
and Abu Baker 2006).
Activated carbon usually increases the cost of the
treatment process. Its economical drawback has
stimulated the interest to utilize cheaper raw
materials for the production of activated carbon
(Rengaraj et al., 2002). Consequently, a wide variety
of agricultural by-products and wastes has been
investigated as cellulosic precursors for the
production of activated carbon in addition to hard
wood and bituminous coal. These precursors include:
coconut shell and wood (Laine et al., 1989), Olive
stones (Rodrigues-Reinoso et al., 2001, Lafi 2001,
Elsheikh et al., 2003), sugarcane bagasse (Ahmedna
et al., 2000), pecan shells (Shawabkeh et al., 1998),
palm seed (Rengaraj et al., 2002), apple pulp (Garcia
et al., 2003), rubber seeds (Rengarag et al., 1996)
and molasses (Legrouri et al., 2005). Furthermore,
more interest has been devoted to utilize some
wastes of carbonaceous materials such as paper mill
sludge (Khalili et al., 2000), old newspaper (Okada
et al., 2003) and waste tires (Rozada et al., 2005).
Recently, activated sludge has been produced as a
result of wastewater treatment activities and has
emerged as an interesting option for the production
of activated carbon (Jeyaseelan and Lu 1996, Tay et
al., 2001). The results reported in these studies
indicate that chemical activation of the sewage
sludge with ZnCl2 and H2SO4 produced activated
carbon of high adsorption capacity comparable with
that of commercial activated carbon. In addition, the
choice of a cheap precursor for the production of
activated carbon means both considerable savings in
the production cost and a way of making use of a
waste material, thus reducing its disposal problem
(Rozada et al., 2003).
The sewage sludge used in the previous
investigations is characterized by its carbonaceous
nature and its high content of volatile compound.
However, this sludge seems to contain appreciable
quantities of inorganic impurities as it comes from
urban treatment plants. Therefore, H2SO4 seems to
be suitable as a chemical activation agent because it
is able to dissolve the majority of inorganic
impurities found in the sludge. For these reasons, this
investigation is directed to the use H2SO4 as a
chemical activation agent for the production of
activated carbon. A relatively pure biomass that is
obtained from a wastewater treatment unit of a dairy
factory was used as the precursor for the activated
carbon prepared in this study. It was reported that the
ash content of this biomass is less than 15% (Al-
Qodah 2006). The product properties were
characterized using some spectroscopic techniques.
Furthermore, the adsorption performance of the
produced activated carbon was tested with some
organic pesticides usually found in industrial
wastewater.
MATERIALS AND METHODS
Materials
Samples of activated sludge were collected from
a local dairy wastewater treatment unit, separated
from water, dried in an oven at 105o
C for 24 h,
grinded to pass 45 µm screens and stored in a closed
vessel for further usage. Sulfuric and nitric acids, and
sodium hydroxide of analytical grade were brought
from Scharlau chemical company, Spain. Pesticide
containing 25 wt% Triadimenol (Vydan) was kindly
donated by Veterinary & Agricultural Products
Manufacturing Company (VAPCO), Jordan. Its
structure is shown in Figure 1.
Deionized water was prepared using Milli Q
system (Millipore, France). All Chemicals were
analytical grade reagent and the glassware were
Pyrex washed with soap, rinsed with nitric acid and
then washed with deionized water.
Activation
The activation procedure was carried out in a 2 L
beaker where a sample of 200 g of dried sludge was
mixed thoroughly with 200 mL of concentrated
sulfuric acid. The mixture was heated to 200°C with
continuous agitation for 1h. During activation water
was evaporated and the mixture became slurry and
started to solidify. At this moment agitation was
stopped while heating continued until the produced
material became a carbon-like material. Trace
amount of distilled water was injected into the
carbonized material using 10 mL syringe to promote
activation. Then, the resulting carbon was allowed
to cool to room temperature; washed with distilled
water; soaked in dilute sodium hydroxide solution
for 30 min; washed a second time with distilled
water; dried; and stored in a closed container for
characterization.

Production and Characterization of Granular Activated Carbon from Activated Sludge 129
Brazilian Journal of Chemical Engineering Vol. 26, No. 01, pp. 127 - 136, January - March, 2009
Figure 1: Chemical Structure of triadimenol
Characterization of the Activated Carbon
a) Physical Properties
The apparent density of the material was obtained
by weighting five grams of the produced activated
carbon and transferring it into a 10 mL graduated
cylinder. The cylinder was tamping with a rubber
pad while activated carbon was being added until the
entire original sample was transferred to the cylinder.
Tamping was continued for 5 minutes until there was
no further settling produced. The volume was
recorded and the apparent density was calculated on
the dry basis:
weight of the sample (g)
Apparent density
volume of the sample (l)
= (1)
The iodine number is used to measure the
porosity of the activated carbon by adsorption of
iodine from solution. Each 1.0 mg of iodine adsorbed
is ideally considered to represent 1.0 m2
of activated
carbon internal surface area.
Ash content was measured by burning the produced
activated carbon in a muffle furnace at 973 K. One
gram of dry carbon was transferred into a crucible and
then placed in the furnace for four hours. The
difference between the original and final weight of the
carbon represents the ash content per gram.
Moisture content was also obtained by weighing
10 grams of the carbon and placed in an oven at
105o
C for 3 h. Then the carbon was cooled in the
absence of humidity and reweighed again. The
difference between the initial and final mass of the
carbon represents the water content in the sample.
b) Fourier Transform Infrared Spectroscopy
FTIR analysis was made using IPRrestige-21,
FTIR-84005, SHIMADZU Corporation (Kyoto,
Japan). Sample of 0.1 g was mixed with 1 g of KBr,
spectroscopy grade (Merk, Darmstadt, Germany), in
a mortar. Part of this mix was introduced in a cell
connected to a piston of a hydraulic pump giving a
compression pressure of 15 kPa / cm2
. The mix was
converted to a solid disc which was placed in an
oven at 105o
C for 4 hours to prevent any interference
with any existing water vapor or carbon dioxide
molecules. Then it was transferred to the FTIR
analyzer and a corresponding chromatogram was
obtained showing the wave lengths of the different
functional groups in the sample which were
identified by comparing these values with those in
the library.
c) X-Ray Diffraction Measurements
X-ray diffraction spectroscopy (XRD) analyses
were carried out with PANalytical X-ray, Philips
Analytical. A dried sample of the produced material
is grinded using an agate mortar and pestle and
tested at 40kV and 40mA. The spectra were analyzed
using PC-APD diffraction software.
d) Surface Morphology and Surface Area
Measurement
The surface morphology was studied using
electron scanning micrographs and then recorded
without sample coating by JOEL JSM-5600LV
Scanning electron microscope. The surface area was
estimated by agitating 1.5 g of the activated carbon
sample in 100 ml of diluted hydrochloric acid at a
pH = 3. Then a 30 g of sodium chloride was added
while stirring the suspension and then the volume
was made up to 150 ml with deionized water. The
solution was titrated with 0.10 N NaOH to raise the
pH from 4 to 9 and the volume V recorded.
Batch Asorption of Pesticide
Equilibrium isotherms for pesticide were
conducted in a set of 250-ml Erlenmeyer flasks by

mixing different concentrations of pesticide with 0.1
g of the produced carbon and allowing to equilibrate
in an isothermal shaker (22±1o
C) for 24 h.
After equilibration, the solution was separated from
the solid by filtration. The final concentration was
then measured using αS2 Heλios UV-Vis
Spectrophotometer at 219 nm. Similar procedures
were used at different values of the solution pH and
others were performed for blank samples.
THEORETICAL
The mathematical interpretation of the adsorption
isotherms is studied using the three popular models;
Langmuir, Freundlich and Brunauer, Emmett and
Teller (BET) models. Langmuir model is valid for
single-layer adsorption, which assumes maximum
adsorption corresponding to a saturated monolayer of
pesticide molecules on the surface of the carbon
where the energy of adsorption is considered to be
constant. The mathematical expression for the
Langmuir model in terms of pesticide concentration
in solution, Ce(mg / L) in equilibrium with that on
the solid surface, qe(mg / g) is given by:
e
e
e
QbC
q
1 bC
=
+
(2)
where Q(mg / g) is the maximum amount of adsorbate
per unit mass of activated carbon required to form a
complete monolayer, and b(L / mg) is the Langmuir
constant related to the affinity of binding sites.
Freundlich model is used to incorporate the effect
of heterogeneous surface energy in which the energy
term, b, in the Langmuir model varies as a function
of surface coverage due to heat of adsorption. The
Freundlich equation takes the form
e F eq K C β
= (3)
where FK and β are constants.
On the other hand, BET model assumes that a
number of layers of pesticide molecules form at the
surface of adsorbent and that the Langmuir equation
is applied to each layer of adsorption thus:
1 e
e
m e 1 m e
Qk C
q
(1 k C )[1 (k k )C ]
=
− + −
(4)
Where 1k and mk are the equilibrium constants for
the first and subsuent layers, respectively.
These models were applied to fit the experimental
data and the corresponding parameters were
obtained.
RESULTS AND DISCUSSION
Characterization of the Produced Carbon
The physical properties of the carbon produced
from activated sludge obtained using ASTM tests (D
2854-96, D 2866-94, D28867-95, and D 3838-80)
are presented in Table 1. These results were
compared with those obtained from NORIT SA5.
The produced carbon has higher ash content, bulk
density and moisture content while it has a lower pH
and a close value of iodine number than Norit’s.
The FT-IR spectroscopic study of the produced
carbon is shown in Figure 2. The sample showed
four major absorption bands at 2900-3500 cm-1
,
1300-1750 cm-1
, 1000-1250 cm-1
and 450-750 cm-1
.
A wide band with two maximum peaks can be
noticed at 2930 and 3450 cm-1
. The band at 3450 cm-
1 is due to the absorption of water molecules as
result of an O-H stretching mode of hydroxyl groups
and adsorbed water, while the band at 2930 is
attributed to C-H interaction with the surface of the
carbon. However, it must be indicated that the bands
in the range of 3200-3650 cm-1
have also been
attributed to the hydrogen-bonded OH group of
alcohols and phenols (Yang and Lua 2003, Puziy et
al., 2003). In the region 1300-1750 cm-1, amides can
be distinguished on surface of the activated carbon
which has two peaks at 1640 and 1450 cm-1. These
functional groups were obtained during the
activation process as a result of the presence of
ammonia and primary amines that usually exist in
the sludge. Moreover, the band at 1500 cm-1
may be
attributed to the aromatic carbon–carbon stretching
vibration. The two peaks at 1125-1150 cm-1
yield the
fingerprint of this carbon. The sharp absorption band
at 1125 cm-1
is ascribed to either Si-O (Misra et al.,
2005) or C-O stretching in alcohol, ether or hydroxyl
groups (Park et al., 1997, Attia et al., 2006). The
band at 1150 cm-1
can also be associated with ether
C-O symmetric and asymmetric stretching vibration
(-C-O-C- ring) (Lapuente et al., 1998). This band
could also be attributed to the antisymmetrical Si-O-
Si stretching mode as a result of existing alumina
and silica containing minerals within the sludge
samples (Calzaferri and Imhof 1996).

Table 1: Physical properties of the produced activated carbon
compared with the commercial carbon obtained from Norit.
Material Produced AC Norit SA5 AC
Ash content wt% 12 6
Density (g/L) 1051 340
pH 5.5 Alkaline
Moisture wt% 10 10
Iodine number 660 650
Figure 2: FT-IR spectrum for activated carbon from sludge
The region 450-750 cm-1
show two bands in the
480 and 485 cm-1
which are associated with the in-
plane and out-of-plane aromatic ring deformation
vibrations (Socrates 1994). Peaks at 598 and 680 cm-
1
are assigned to the out-of-plane C-H bending mode.
These spectra were also suggested to be due to
alkaline groups of cyclic ketons and their derivatives
added during activation (Park et al., 1997, Guo and
Lua 1999).
X-ray diffractograms for both the activated
sludge and activated carbon are shown in Figures 3
and 4. The XRD spectra of the activated sludge
illustrated the presence of different alumino-silicate
minerals. Zeolite X-Y was observed at 2θ = 29.4o
with relative intensity of 158 cps, followed by
faujasite detection at 2θ = 26.5o
. Other peaks where
located at 2θ = 32.9, 35.9 and 39.4o
for mullite,
hematite and quartz, respectively. While the rest of
the peaks for sodalite, analcime and sodium silicates
were located at 2θ = 43.1, 47.5 and 48.5o
,
respectively. When this sludge is treated with acids
the majority of those peaks disappear due to leaching
out the corresponding minerals during activation and
washing with water. However, minor peaks were
observed at 2θ = 32 and 41.5 zeolite X and mullite,
respectively. These minerals might be formed after
washing and neutralizing the produced carbon with
sodium hydroxide which could react with the
remaining aluminosilicates in the yielding zeolite
according to the following equation (Shawabkeh et
al., 2004):
o
25 C
2 2 a 2 b 2 c
2 j 2 j 2 2
NaOH AlO ...SiO Na (AlO ) (SiO ) .
NaOH.H O Na (AlO ) (SiO ).2H O
+ →
→
(5)
The surface area of the produced carbon can be
precisely estimated using the physical adsorption
of nitrogen at 77K. However, Sears’ method was
applied to give a rapid and estimated value of the
surface area according to the equation (Sears,
1976):
S (m2/g) = 32 V – 25 (6)
where V is the volume of sodium hydroxide required
to raise the pH of the sample from 4 to 9. This
volume was measured in replicate and found 28.9 ml
and the corresponding surface area is 900 m2
/g.

Figure 3: X-ray diffractogram for sludge sample
Figure 4: X-ray diffractogram for activated carbon from sludge
Adsorption of Pesticide by Activated Carbon
a) Adsorption Isotherm
Adsorption isotherm for Triadimenol pesticide
using the produced activated carbon is illustrated in
Fig. 5. It is clear that an S-shaped curve appeared
which indicates the formation of a multilayer of
pesticides molecules on the surface of the carbon.
This behavior could be attributed to the deposition of
Triadimenol on the surface of the produced carbon.
The molecular structure of triadimenol has both ionic
and organic qualities. The ionic nature could play a
large role in retaining the species on the surface of
the carbon by electrostatic attraction in one hand. On
the other hand, the organic part of the triadimenol
has hydrophobic moieties. If these groups approach
closely to the surface oxygen atoms in carbon
surface, van der Waals interaction becomes very
strong and dominates the influence of the
hydrophobic binding sites of the carbon (Lagaly
2001).

0
50
100
150
200
250
300
350
400
450
500
Ce (mg/L)
0 10 20 30 40 50 60 70
qe(mg/g)
Langmuir
Freundlich
BET
0
50
100
150
200
250
300
350
400
450
500
0
50
100
150
200
250
300
350
400
450
500
Ce (mg/L)
0 10 20 30 40 50 60 700 10 20 30 40 50 60 70
qe(mg/g)
Langmuir
Freundlich
BET
Figure 5: Adsorption isotherm and models of triadimenol
Table 2: Adsorption isotherm model parameter at different pH values..
MODEL
pH
LANGMUIR FREUNDLICH BET
3
Q = 111.8 mg/g
B = 24.16 L/mg
R2
= 0.795
KF = 2.284
β = 1.257
R2
= 0.861
Q = 110.0 mg/g
k1 = 0.138 L/mg
km = 0.0128 L/mg
R2
= 0.948
5
Q = 66.43 mg/g
b = 0.014 L/mg
R2
= 0.555
KF = 0.00288
β = 2.582
R2
= 0.875
Does not fit
9
Q = 48.85 mg/g
B = 0.031 L/mg
R2
= 0.610
KF = 3.517×10-5
β = 3.455
R2
= 0.726
Does not fit
The isotherm data were fitted to different sorption
isotherm models namely Langmuir, Freundlich and
BET. The corresponding parameters are shown in
Table 2. The monolayer capacity s ranging from
48.85 to 111.80 mg/g obtained by Langmuir model
which is developed to represent the physical
adsorption of adsorbates to cover monolayer on the
surface of adsorbent. However, this model did not
fit the data adequately especially when the solute
concentration exceeded 40 mg/L where the second
layer started to occur. Also Freundlich model has a
poor fit to the experimental data at such high level of
concentration. This isotherm does not predict any
saturation of the pesticide by the carbon surface.
Nevertheless, it gives an indication about the surface
heterogeneity where non-uniform surface may
display various levels of energetic heterogeneity.
Apart from the above models, BET shows a good
fit to the experimental data at pH 3 with R2
= 0.948
and 2
(error) 6710=∑ . The monolayer of adsorption is
predicted by this model with a value of 110.0 mg/g
which is in good agreement with the experimental
data and that obtained by Langmuir model (111.8
mg/g). Other isotherms obtained at different pH
values of 5 and 9 did not fit by BET model
adequately.
b) Effect of pH
Fig. 6 shows the effect of pH on adsorption of
pesticide onto the produced activated carbon. It is
evident from Fig. 6 that the adsorption capacity
increases significantly as pH decreases. The
monolayer adsorption capacity at pH 3 is ten times
more than that at pH 9. The increase in solution
acidity can affect the mobility of pesticide ions in the
surface and subsurface of the carbon. Moreover,
Triadimenol pesticide is a polar compound which
easily hydrolyzes at high pH values. The non-
hydrolyzed molecule is more easily adsorbed on the
surface of the activated carbon due to its higher
hydrophobicity than the hydrolyzed molecule (Yang
et al., 2005). Also, effect of pH might suggest a
possible mechanism of chemical reaction between
the reactive groups (–OH) of pesticide and the
surface of the activated carbon according:

(7)
Figure 6: Effect of pH on adsorption of triadimenol by activated carbon
Consequently, a covalent bond between the
pesticide and the surface of the carbon is formed.
Kiriakopoulos et al. indicated that this phenomenon
usually occur due to possible changes in the solid
surface charge and ionization of the molecule groups
or atoms, altering therefore the mechanisms and the
extent of adsorption (Kyriakopoulosa and
Anagnostopoulos 2005, Rosen 1989). At low pH the
pesticide molecule possesses charged sites which
could be attracted by the carbon surface. Moreover,
the ionization of nitrogen atoms and/or NH groups in
pesticide molecules is likely to occur, leading to the
adsorption of more pesticide molecules on the
surface of the carbon.
CONCLUSIONS
Activated carbon was produced from activated
sludge using sulphuric acid as a chemical activation
agent. The properties of the produced activated
carbon such as surface area, chemical functional groups
and chemical composition reveals that it had an
improved adsorption behavior comparable to those of
high performance adsorbents. The adsorption behavior
of the produced activated carbon was tested with
pesticides in aqueous solution. The adsorption isotherm
data obtained at pH 3 were closely fitted to the BET
adsorption model indicating multilayer pesticide
adsorption. The estimated maximum adsorption
capacity was 110 mg/g and this value was sharply
reduced by increasing the pH of the solution.
ACKNOWLEDGMENT
The authors acknowledge KFUPM and Mutah
University for supporting this research. The authors
acknowledge also Alaa Aloush, Noora abu Safia and
Shadia Sakarnah for performing some of the

experimental work and Eng. Reema Jaradat for the
analysis of the experiments.
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