Iranica Journal of Energy & Environment 5 (4): 446-452, 2014

ISSN 2079-2115
IJEE an Official Peer Reviewed Journal of Babol Noshirvani University of Technology
DOI: 10.5829/idosi.ijee.2014.05.04.12
BUT

Heavy Metal Removal Efficiency of Paper Mulberry Biochar and Commercially

Available Silica Powder from Simulated Industrial Wastewater
1
Sawaira Adil, 2Azhar Mashiatullah, 1Maliha Asma, 1Jawaria Abid and 1Abdul Ghaffar

1
Department of Environmental Science, International Islamic University Islamabad, Pakistan
2
Isotope Application Division, Directorate of Technology,
Pakistan Institute of Nuclear Science and Technology, Islamabad, Pakistan

Received: August 21, 2014; Accepted in Revised form: October 10, 2014
Abstract: Paper mulberry bio-char produced was characterized and evaluated for heavy metals removal from
simulated industrial wastewater in compare to silica powder. The batch adsorption study was conducted
under different conditions like, the effects of solution pH, contact time and temperature. The paper mulberry bio-
char (PMB) was more effective and exhibited a higher adsorption potential for cadmium, copper, chromium, lead
and zinc than commercially available silica powder. Experiments conducted with an initial metal concentration
of 50 mg/l at pH 2, 4, 8, 12. Maximum removal of cadmium, copper, chromium, lead and zinc by PMB was
higher than silica powder. Contact time of 2, 3, 4 h showed maximum removal of cadmium, copper, chromium,
lead and zinc removal for PMB and was found higher than that of silica powder. The thermodynamic parameters
such as G°, H° and S° were calculated for predicting the nature of sorption. The results
showed that plant-residue bio-char can act as effective alternative sorbent instead of silica powder for the
removal of heavy metal ions from industrial wastewater.

Key words: Paper mulberry Bio-char Wastewater Heavy metals Voltammeter

INTRODUCTION the population growth [1]. It is necessary to remove

heavy metal from industrial sources before they enter
The pollution of surface and underground water to environment. Many processes are developed to
has been gradually increased; that is worldwide address these stringent environmental regulations
concern due to the disposal of heavy metals for last which necessitate removal of heavy metal compounds
few decades [1]. Heavy metals coming from from wastewater.
municipal waste and agriculture runoff to the earth’s Common contaminants removal processes are
surface from industrial process can pollute surface known as chemical precipitation, ion exchange,
water and underground water. Heavy metals are adsorption, membrane filtration, electrochemical filtration,
usually released into water bodies from etc. [3-5]. Most of these processes are difficult to
industrial/domestic effluents such as metal plating implement on large scale due to expensiveness and
industries, mining and tanneries, etc. Heavy metals ineffectiveness at low concentration (<100 mg/l) and
from polluted water bodies can then diffuse into the production of toxic sludge and other waste products
surrounding soil, surface water and groundwater. that also need disposal [6, 7]. The disadvantages have
When the polluted water is consumed by living increased the need of developing alternative and low-cost
organisms, the toxic heavy metals can accumulate and water treatment technologies for treatment of heavy
become harmful [2]. The human health and ecological metal contaminants. Among these technologies for the
systems are threatened to get worse. Harmful heavy removal of heavy metal, adsorption is considered as
metals are abundant in the water bodies due to the rapid simple, user-friendly technique and efficient method.
industrial and agricultural development together with Adsorption is a fundamental process in the

Corresponding Author: Azhar Mashiatullah, Isotope Application Division, Directorate of Technology,

Pakistan Institute of Nuclear Science and Technology, Islamabad, Pakistan.
Tel: +92-51-2207221, E-mail: [email protected] - [email protected].
Please cite this article as: Sawaira Adil, Azhar Mashiatullah, Maliha Asma, Jawaria Abid and Abdul Ghaffar, 2014. Heavy Metal Removal Efficiency of
Paper Mulberry Biochar and Commercially Available Silica Powder from Simulated Industrial Wastewater. Iranica Journal of Energy and Environment,
5 (4): 446-452.
 Iranica J. Energy & Environ., 5 (4): 446-452, 2014

physiochemical treatment of wastewaters because of its volumetric flask and make volume by distilled water.
relative low cost. The removal efficiency of the contaminants
Great efforts have been made to use the economically (Cd, Cu, Cr, Pb and Zn) was calculated using the
efficient and unconventional adsorbents to adsorb heavy following expression:
metals from aqueous solutions, such as aquatic plants,
plant wastes, agricultural and industrial by-products. Removal efficiency= (Cf - Ci)/ Cf X 100
Therefore, especially assessment of biomass is getting
increased attention in all over the world as it is renewable, Where, Ci is quantity of metals before adsorption
widely available, cheap and environmental friendly. experiment; Cf is quantity of metals after adsorption
There are a number of biomass sources, such as forest experiment. In addition, Ci is the initial metal ion
residues, low grade plants, agricultural residues and concentration (mg/l), Ce is the equilibrium concentration
municipal solid wastes, which can be utilized for activated of the metal ion (mg/l).
carbon precursor. Biomass is a renewable energy resource
and has a growing interest as a chemical feedstock Adsorbents: The adsorbents that were studied were:
source [8, 9]. PMB biochar; commercially available silica powder (SP).
Bio-char is a fine-grained, carbon rich material and
porous substance, similar in its appearance to charcoal PMB Biochar Preparation: Paper mulberry (Broussonetia
produced by natural burning which results from papyrifera) locally grown in Pakistan, were obtained from
combustion of organic materials under oxygen-limited a plantation in Islamabad, Pakistan was used for
conditions (Pyrolysis). Because of its high surface-to- producing bio-char. Bark/wood thoroughly washed in
volume ratio and strong affinity for non-polar substances water to remove any dust, sand, leaves, dirt and adhesive
biochars can be a potential sorbent for organic pollutants insoluble materials. Conversion of paper mulberry to
and pesticides, particularly planar aromatic compounds biochar was conducted in a high Helium Diffusion
[10, 11]. The distribution of products depends upon Furnace (SLM-1). Air and oven dried samples were
heating rate, temperature, surrounding atmosphere and crushed and ground small particles in electric grinder to
residence time. Bio-char is extensively used for water obtain homogenous powder and the resultant powder
treatment process, adsorption potential of almond shell was sieve to a size no larger than 0.00141 mm (1.4µm) in bio-
char for Ni and Co removal from aqueous solution. size. Sieved sample of paper mulberry biomass were Characterization
and investigation of bio-chars produced pyrolyzed in a tube furnace at 350°C. The biochar was through pyrolysis of
hardwood for the removal of Cu and then air dried and held for further characterization.
Zn from aqueous solution. The ability of bio-chars
converted from anaerobically digested biomass to sorb Biochar Characterization
heavy metals used in a range of laboratory sorption and SEM Analysis: For SEM analysis PMB biochar
characterization experiments [13-15]. samples were processes by compacting bio-chars sample
The primary objective of this study was to in the locally designed pellet press to make discs investigate
the ability of paper mulberry derived biochar (diameter= 9mm, thickness= 3mm) to fit in the especially in
comparison with commercially available silica powder fabricated Aluminum (Al) stubs (O.D= 10 mm, I.D= 9mm, for
the removal of heavy metals (cadmium, copper, depth= 3mm) to make the surface of bio-char samples
chromium, lead, zinc) from simulated industrialconductive before scanning electron microscopy.
wastewater. The maximum thickness of Au coating ranged from 10-
20 µM. The conductive layer helps in passing of
MATERIALS AND METHODS electron charge through the sample. A series of electron
micrographs were recorded of each sample at various
Adsorbates: The adsorbates in this study were cadmium, magnifications SEM (Model: Leo 440I).
copper, chromium, lead and zinc by dissolving cadmium
chloride (CdCl2.H2O), copper chloride (CuCl2.2H2O), BET Surface Area Measurement: The method of
potassium dichromate (K2CrO7), lead chloride (PbCl2) Brunauer, Emmett and Teller (BET) is commonly used to
and zinc sulphate (ZnSO4.7H2O) salts in 1000ml of determine the total surface area of materials. One gram of
distilled deionized water used as stock solution bio-char samples was degassed at 350°C for 24 hours
concentrations of 1000 mg/l of each metal. Mixture of under pressure of 7 Pa before adsorption measurements.
cadmium, copper, chromium, lead, zinc solutions were The degassed samples were introduced in an automated
prepared by taking 50ml (50ppm) of each solution in 500ml nitrogen adsorption apparatus at 77 K. The equilibrium

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 Iranica J. Energy & Environ., 5 (4): 446-452, 2014

points inside the 0.00-0.22 P/P0 range were determined

by the BET equation to calculate the surface area of the
bio-char samples [16]. The porosity of the bio-char such
as pore diameter and pore volumes was also determined
from BET analysis.

RESULTS AND DISCUSSION

Effect of pH on Adsorption: pH of the solution is one of

the most important parameters in the removal of heavy
metals from aqueous solution. The pH of the solution
has an ability to affect the surface charges of the
biosorbent, the degree of ionization of the biosorbent Fig 1: Removal efficiency of PMB bio-char at different pH
during biosorption and the forms of the metal ions in
aqueous solutions [17-19]. The effect of pH on heavy
metals (Cd, Cr, Cu, Pb and Zn) ions by PMB bio-char
and silica powder were evaluated at four pH levels
viz 2, 4, 8 and 12 (Figures 1 and 2). Cadmium, copper,
lead and zinc adsorption increased with increase in
pH. Maximum removal efficiency of these metals
were recorded at pH of 12 (see Figures 1 and 2). One of
the potential factors for the considerable low
adsorption capacity at pH 2.0 is the H+ ions compete with
metal cation for the exchange sites in the system;
thereby partially releasing the later. The heavy metal Fig 2: Removal efficiency of Silica at different pH
cations are completely released under circumstances
of extreme acidic conditions [20, 21]. However removal
efficiency of chromium was decreased as the pH is
increased and maximum removal efficiency was
achieved in acidic pH. This is because of the fact under
acidic condition the metal surface is highly protonated
that favors the uptake of Cr in anionic form. By increasing
the pH of the solution surface protonation of
adsorbent gradually reduces and hence adsorption
decrease.

Effect of Contact Time on Adsorption: Contact time is Fig 3: Removal efficiency of PMB bio-char at different
another important factor in batch sorption process [22]. contact time
The effect of contact time on the sorption of Cd, Cu, Cr,
Pb, Zn was determined at three contact times viz 2, 3 and
4hours (Figures 3 and 4). For adsorption of Cd, Cr and Zn,
PMB bio-char reached to near asymptotic removal within
3h. Maximum removal of Cu and Pb by PMB bio-char
observed at contact time of 4h and 2h, respectively.
While, removal efficiency of Cd and Cu by SiO2 was below
50% at contact time of 3h. Maximum removal efficiency
for Zn was 12.6% at contact time of 4h. Removal efficiency
of cadmium, copper, chromium, lead and zinc by paper
mulberry biochar were higher than commercially available
silica powder. Fig 4: Removal efficiency of silica at different contact time

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 Iranica J. Energy & Environ., 5 (4): 446-452, 2014

Table 1: Physical properties of bio-chars

a
Char samples SBET (m2g 1) b
VT (cc/g) c
av (nm)
3
Paper mulberry 1.84 5.37x10 11.7
a (SBET: BET surface area ; b (vT : Total pore volume) ;c (average pore
diameter)

Since diffusion is an endothermic process, greater

adsorption will be observed at high temperature.
Thus, the diffusion rate of ions in the external mass
transport process increases with temperature. While
sorption of chromium was recorded to be decreased with
an increase in temperature and show maximum removal
Fig 5: Removal efficiency of PMB bio-char at different of 99% at 28°C, after which further increase in temperature
temperature did not bring about any further improvement for the metal
ions, but resulted in desorption of some of the metal ions
from the adsorbent surface.

Biochar Characterization
Scanning Electron Microscope and Bet Surface Area:
Table 1 shows surface area, total pore volume and
average pore diameter of the paper mulberry bio-chars
produced. Single point BET surface area of the bio-chars
was determined by the nitrogen sorption method.
1
Paper mulberry bio-char has surface area of ,
3
total pore volume of and average pore diameter of
11.7nm. There is an inverse relationship between surface
area and average pore diameter.
Figure 7 shows scanning electron microscopy
Fig 6: Removal efficiency of silica at different temperatures (SEM) images of paper mulberry bio-char. Morphological
analysis was performed by scanning electron microscopy.
Effect of Temperature on Adsorption: The effect of SEM micrographs clearly show the amorphous and
temperature variation on the sorption of Cd, Cu, Cr, Pb heterogeneous nature of paper mulberry bio-char.
and Zn was determined at four temperature levels viz 28, Scanning electron microscopy revealed that internal pores
32, 36, 40 and 42°C (Figures 5 and 6). For cadmium, and cracks /mesopores are present in bio-chars materials.
copper, zinc PMB showed maximum heavy metal removal Due to importance of mesopores to many liquid-solid
of 75.6, 58.8 and 52.2% at 40°C; that was far greater than sorption processes these pores are of importance to many
heavy metal removal at 42, 40 and 36°C. For chromium liquid-solid sorption processes [24].
maximum removal efficiency of SiO2 was (99%) at 28°C;
that is greater than the adsorbed on PMB (88%) at 42°C. Thermodynamic Model: Temperature dependence of
Maximum removal of Pb by paper mulberry was 89%. the adsorption process is associated with several
An increase in removal of metals by PMB with thermodynamic parameters. Thermodynamic
increasing temperature indicates an endothermic process. considerations of an adsorption process are necessary
The increase in adsorption with temperature may be to conclude whether the process is spontaneous or not.
attributed to either increase in the number of active The thermodynamic parameters, the values of enthalpy
surface sites available for adsorption on the adsorbent H° and entropy S° and Gibbs free energy G° of
or the desolvation of the adsorbing species and the sorption are useful in defining whether sorption is
decrease in the thickness of the boundary layer endothermic or exothermic. Modelling temperature
surrounding the adsorbent with temperature, so that the dependence of the adsorption process is associated with
mass transfer resistance of adsorbate in the boundary several thermodynamic parameters. Thermodynamic
layer decreases [23]. considerations of an adsorption process are necessary

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Fig 7: Paper mulberry bio-char micrographs.

to conclude whether the process is spontaneous or not. Where q e and Ce is the equilibrium concentration of metal
The Gibbs free energy change is an indication of ions on adsorbent (mg/g) and in the solution (mg/l),
spontaneity of a chemical reaction and therefore is an respectively. Relation between G°, H° and S° can be
important criterion for spontaneity. Also, both energy and expressed by the following equations
entropy factors must be considered in order to determine
the Gibbs free energy of the process [25]. Thermodynamic G° = H° - S° (6)
parameters such as Gibbs free energy change G°),
enthalpy change H°) and the entropy change S°) can Eq. (6) can be written as
be estimated using equilibrium constants changing
with temperature. The Gibbs free energy change of the lnKL = - G°/RT = - H°/RT + S°/R (7)
adsorption reaction can be determined from the following
equation. According to Eq. (7), H° and S° parameters can be
calculated from the slope and intercept of the plot of ln
G° = -RT lnKL (4) KL versus 1/T, respectively [25-27]. Moreover, the
decrease in G° values with increase in temperature
Where R is gas constant (8.314 J/mol K), KL is equilibrium shows a decrease in feasibility of sorption at higher
constant and T is absolute temperature (K). The KL value temperatures. The positive value of H° indicates that
was calculated using the following equation: the nature of adsorption process is endothermic in all
cases. This behavior indicates that higher temperatures
KL = qe/Ce (5) are more preferred for higher sorption. The positive

Table 2: Thermodynamic parameters of adsorption of heavy metals on PMB

G°
------------------------------------------------------------------------------------------------------------
Thermodynamic parameters Temperature (°C) Cd Cu Cr Pb Zn
28 -1.230 -0.387 -2.167 2.274 -0.096
32 -1.246 -0.392 -2.195 -2.304 -0.097
36 -1.262 0.397 -2.224 2.334 -0.098
40 -1.279 -0.402 -2.253 -2.334 0.100
42 -1.287 -0.405 -2.267 -2.379 -0.100
H° -0.132 0.078 0.54 -0.038 0.037
S° 414.7 251.03 186.4 112.1 116.5
R2 0.505 0.599 0.765 0.644 0.463

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Table 3: Thermodynamic parameters of adsorption of heavy metals on silica powder

G°
------------------------------------------------------------------------------------------------------------
Thermodynamic parameters Temperature (°C) Cd Cu Cr Pb Zn
28 -1.172 -0.963 -4.997 -1.903 1.428
32 -1.187 0.976 -5.063 -1.929 1.447
36 1.203 0.989 -5.130 -1.954 1.466
40 1.218 1.002 -5.196 -1.979 1.485
42 1.226 1.008 -5.229 -1.992 1.494
H° -0.166 0.069 -0.188 0.0168 0.0174
S° 557.0 212.2 595.3 65.8 43.0
R2 0.254 0.732 0.715 0.192 0.31

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Persian Abstract
‫ُسی ى‬
‫چ‬
‫ی‬
‫تذض ظا لنبح لبغظ یب ْگػیٍ فص‬ ٍ PMB ‫ فطگ اطل ییبیظ ا زصٍه يیگٍؾ اعلف فصح یاطث ؽیلیؾ ض ٍپ بث ؿ ِیبمه ض‬. ‫به طثا‬، ‫ ٍ ؼبو ىیهظ‬pH
‫سیزطگ یضطث ِتؾیپبٍ ةصخ ض‬. ‫میهززو ةصخ‬، ‫ؽه‬، ‫ لبغش بث یٍ ٍ مطو‬PMB ‫ؽیل یؾ ضپ ؿ ِیبمه ض‬
ً
‫تؾا ٍزث ط طثه ضبیؿ‬. ‫ تظلغ بث فیبهظآ‬mg/l 50 ‫ ض‬pH 2، 4، 8 ٍ 12 ‫ ؼزو ىبهظ ض ٍِو ؾا ضاض ىىیكٍ حیب ٍ سق مبدا‬2 ‫ ب‬4
‫مٍیززو ةصخ طثوا سح تػب‬، ‫ؽه‬، ‫ لبغظ بث یٍ ٍ مطو‬PMB ‫ ؾا سها تؾسث یطتكیث ةصخ ؽیل یؾ ض ٍپ بث ؿ ِیبمه ض‬. ‫ٍ یضطث‬
ً
‫ ؽ ى‬، ‫تؾا یٍیؾ فیپ لثبل ةصخ ضبتفذ ٍ تؼیجع تؾا ضاض ىىیكٍ یبٍط ا ٍ یپلبتٍا‬.
‫جیگ ضاظآ یعطٍا ییهبیز هط یىبٍطتهاضبپ تبجؾبح‬
‫تؾا ضٍث ؽیل یؾ ض ٍپ ظا ط طثه ٍ طتكیث لبغظ یؼٍن ةلاضبف يیگٍؾ اعلف ةصخ حیب‬.

452