Brazilian Journal

of Chemical ISSN 0104-6632

Engineering Printed in Brazil
www.abeq.org.br/bjche

Vol. 26, No. 01, pp. 127 - 136, January - March, 2009

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 The surface oxygen functional groups can be

easily introduced to the carbon by different
Activated carbons are carbonaceous materials that activation methods including dry and wet oxidizing
can be distinguished from elemental carbon by the agents. Dry oxidation methods involve the reaction
oxidation of the carbon atoms found on the outer and with hot oxidizing gas such as steam and CO2 at
inner surfaces (Mattson and Mark 1971). These temperatures above 700oC (Smisek and Cerney
materials are characterized by their extraordinary 1970). Wet oxidation methods involve the reaction
large specific surface areas, well-developed porosity between the carbon surface and solutions of
and tunable surface-containing functional groups oxidizing agents such as phosphoric acid H3PO4,
(Baker et al. 1992, Zongxuan et al., 2003). For these nitric acid HNO3, hydrogen peroxide H2O2, zinc
reasons, activated carbons are widely used as chloride ZnCl2, potassium permanganate KMnO4,
adsorbents for the removal of organic chemicals and ammonium persulphate (NH4)2S2O8, potassium
metal ions of environmental or economic concern hydroxide KOH, etc. From the above oxidizing
from air, gases, potable water and wastewater (El- agents, phosphoric acid and zinc chloride are usually
Hendawy 2003). used for the activation of lignocellulosic materials,
*To whom correspondence should be addressed
128 Z. Al-Qodah and R. Shawabkah

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

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 Production and Characterization of Granular Activated Carbon from Activated Sludge 129

Figure 1: Chemical Structure of triadimenol

Characterization of the Activated Carbon spectroscopy grade (Merk, Darmstadt, Germany), in

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

Brazilian Journal of Chemical Engineering Vol. 26, No. 01, pp. 127 - 136, January - March, 2009
130 Z. Al-Qodah and R. Shawabkah

mixing different concentrations of pesticide with 0.1 Where k1 and k m are the equilibrium constants for
g of the produced carbon and allowing to equilibrate the first and subsuent layers, respectively.
in an isothermal shaker (22±1oC) for 24 h. These models were applied to fit the experimental
After equilibration, the solution was separated from data and the corresponding parameters were
the solid by filtration. The final concentration was obtained.
then measured using αS2 Heλios UV-Vis
Spectrophotometer at 219 nm. Similar procedures
were used at different values of the solution pH and RESULTS AND DISCUSSION
others were performed for blank samples.
Characterization of the Produced Carbon

THEORETICAL The physical properties of the carbon produced

from activated sludge obtained using ASTM tests (D
The mathematical interpretation of the adsorption 2854-96, D 2866-94, D28867-95, and D 3838-80)
isotherms is studied using the three popular models; are presented in Table 1. These results were
Langmuir, Freundlich and Brunauer, Emmett and compared with those obtained from NORIT SA5.
Teller (BET) models. Langmuir model is valid for The produced carbon has higher ash content, bulk
single-layer adsorption, which assumes maximum density and moisture content while it has a lower pH
adsorption corresponding to a saturated monolayer of and a close value of iodine number than Norit’s.
pesticide molecules on the surface of the carbon The FT-IR spectroscopic study of the produced
where the energy of adsorption is considered to be carbon is shown in Figure 2. The sample showed
constant. The mathematical expression for the four major absorption bands at 2900-3500 cm-1,
Langmuir model in terms of pesticide concentration 1300-1750 cm-1, 1000-1250 cm-1 and 450-750 cm-1.
in solution, Ce(mg / L) in equilibrium with that on A wide band with two maximum peaks can be
noticed at 2930 and 3450 cm-1. The band at 3450 cm-
the solid surface, qe(mg / g) is given by:
1 is due to the absorption of water molecules as
result of an O-H stretching mode of hydroxyl groups
QbCe and adsorbed water, while the band at 2930 is
qe = (2)
1 + bCe attributed to C-H interaction with the surface of the
carbon. However, it must be indicated that the bands
where Q(mg / g) is the maximum amount of adsorbate in the range of 3200-3650 cm-1 have also been
attributed to the hydrogen-bonded OH group of
per unit mass of activated carbon required to form a alcohols and phenols (Yang and Lua 2003, Puziy et
complete monolayer, and b(L / mg) is the Langmuir al., 2003). In the region 1300-1750 cm-1, amides can
constant related to the affinity of binding sites. be distinguished on surface of the activated carbon
Freundlich model is used to incorporate the effect which has two peaks at 1640 and 1450 cm-1. These
of heterogeneous surface energy in which the energy functional groups were obtained during the
term, b, in the Langmuir model varies as a function activation process as a result of the presence of
of surface coverage due to heat of adsorption. The ammonia and primary amines that usually exist in
Freundlich equation takes the form the sludge. Moreover, the band at 1500 cm-1 may be
attributed to the aromatic carbon–carbon stretching
q e = K F C eβ (3) 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.,
where K F and β are constants. 2005) or C-O stretching in alcohol, ether or hydroxyl
On the other hand, BET model assumes that a groups (Park et al., 1997, Attia et al., 2006). The
number of layers of pesticide molecules form at the band at 1150 cm-1 can also be associated with ether
surface of adsorbent and that the Langmuir equation C-O symmetric and asymmetric stretching vibration
is applied to each layer of adsorption thus: (-C-O-C- ring) (Lapuente et al., 1998). This band
could also be attributed to the antisymmetrical Si-O-
Qk1Ce Si stretching mode as a result of existing alumina
qe = (4) and silica containing minerals within the sludge
(1 − k m Ce )[1 + (k1 − k m )Ce ]
samples (Calzaferri and Imhof 1996).

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 Production and Characterization of Granular Activated Carbon from Activated Sludge 131

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

Brazilian Journal of Chemical Engineering Vol. 26, No. 01, pp. 127 - 136, January - March, 2009
132 Z. Al-Qodah and R. Shawabkah

Figure 3: X-ray diffractogram for sludge sample

Figure 4: X-ray diffractogram for activated carbon from sludge

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

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 Production and Characterization of Granular Activated Carbon from Activated Sludge 133

500
450 Langmuir
Freundlich
400 BET
350

qe (mg/g)
300
250
200
150
100
50
0
0 10 20 30 40 50 60 70
Ce (mg/L)

Figure 5: Adsorption isotherm and models of triadimenol

Table 2: Adsorption isotherm model parameter at different pH values..
MODEL
LANGMUIR FREUNDLICH BET
pH
Q = 110.0 mg/g
Q = 111.8 mg/g KF = 2.284
k1 = 0.138 L/mg
3 B = 24.16 L/mg β = 1.257
km = 0.0128 L/mg
R2 = 0.795 R2 = 0.861
R2 = 0.948
Q = 66.43 mg/g KF = 0.00288
5 b = 0.014 L/mg β = 2.582 Does not fit
R2 = 0.555 R2 = 0.875
Q = 48.85 mg/g KF = 3.517×10-5
9 B = 0.031 L/mg β = 3.455 Does not fit
R2 = 0.610 R2 = 0.726

The isotherm data were fitted to different sorption mg/g). Other isotherms obtained at different pH
isotherm models namely Langmuir, Freundlich and values of 5 and 9 did not fit by BET model
BET. The corresponding parameters are shown in adequately.
Table 2. The monolayer capacity s ranging from
48.85 to 111.80 mg/g obtained by Langmuir model b) Effect of pH
which is developed to represent the physical
adsorption of adsorbates to cover monolayer on the Fig. 6 shows the effect of pH on adsorption of
surface of adsorbent. However, this model did not pesticide onto the produced activated carbon. It is
fit the data adequately especially when the solute evident from Fig. 6 that the adsorption capacity
concentration exceeded 40 mg/L where the second increases significantly as pH decreases. The
layer started to occur. Also Freundlich model has a monolayer adsorption capacity at pH 3 is ten times
poor fit to the experimental data at such high level of more than that at pH 9. The increase in solution
concentration. This isotherm does not predict any acidity can affect the mobility of pesticide ions in the
saturation of the pesticide by the carbon surface. surface and subsurface of the carbon. Moreover,
Nevertheless, it gives an indication about the surface Triadimenol pesticide is a polar compound which
heterogeneity where non-uniform surface may
easily hydrolyzes at high pH values. The non-
display various levels of energetic heterogeneity.
hydrolyzed molecule is more easily adsorbed on the
Apart from the above models, BET shows a good
surface of the activated carbon due to its higher
fit to the experimental data at pH 3 with R2 = 0.948
hydrophobicity than the hydrolyzed molecule (Yang
and ∑ (error)2 = 6710 . The monolayer of adsorption is et al., 2005). Also, effect of pH might suggest a
predicted by this model with a value of 110.0 mg/g possible mechanism of chemical reaction between
which is in good agreement with the experimental the reactive groups (–OH) of pesticide and the
data and that obtained by Langmuir model (111.8 surface of the activated carbon according:

Brazilian Journal of Chemical Engineering Vol. 26, No. 01, pp. 127 - 136, January - March, 2009
134 Z. Al-Qodah and R. Shawabkah

(7)

Figure 6: Effect of pH on adsorption of triadimenol by activated carbon

Consequently, a covalent bond between the agent. The properties of the produced activated
pesticide and the surface of the carbon is formed. carbon such as surface area, chemical functional groups
Kiriakopoulos et al. indicated that this phenomenon and chemical composition reveals that it had an
usually occur due to possible changes in the solid improved adsorption behavior comparable to those of
surface charge and ionization of the molecule groups high performance adsorbents. The adsorption behavior
or atoms, altering therefore the mechanisms and the of the produced activated carbon was tested with
extent of adsorption (Kyriakopoulosa and pesticides in aqueous solution. The adsorption isotherm
Anagnostopoulos 2005, Rosen 1989). At low pH the data obtained at pH 3 were closely fitted to the BET
pesticide molecule possesses charged sites which adsorption model indicating multilayer pesticide
could be attracted by the carbon surface. Moreover, adsorption. The estimated maximum adsorption
the ionization of nitrogen atoms and/or NH groups in capacity was 110 mg/g and this value was sharply
pesticide molecules is likely to occur, leading to the reduced by increasing the pH of the solution.
adsorption of more pesticide molecules on the
surface of the carbon.
ACKNOWLEDGMENT

CONCLUSIONS The authors acknowledge KFUPM and Mutah

University for supporting this research. The authors
Activated carbon was produced from activated acknowledge also Alaa Aloush, Noora abu Safia and
sludge using sulphuric acid as a chemical activation Shadia Sakarnah for performing some of the

Brazilian Journal of Chemical Engineering

 Production and Characterization of Granular Activated Carbon from Activated Sludge 135

experimental work and Eng. Reema Jaradat for the ZnCl2 and H2SO4. Environmental Technology, 17,
analysis of the experiments. 667-672 (1999).
Khalili N. R., Campbell M., Sandi G. and Gola J.,
Production of micro and mesoporous activated
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