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Corresponding Author: Azhar Mashiatullah, Isotope Application Division, Directorate of Technology, Pakistan Institute of Nuclear Science and Technology, Islamabad, Pakistan. Tel: +92-51-2207221.

1 2 1 1 1

Department of Environmental Science, International Islamic University Islamabad, Pakistan1

Isotope Application Division, Directorate of Technology, 2

Pakistan Institute of Nuclear Science and Technology, Islamabad, Pakistan

Received: August 21, 2014; Accepted in Revised form: October 10, 2014Abstract: Paper mulberry bio-char produced was characterized and evaluated for heavy metals removal fromsimulated industrial wastewater in compare to silica powder. The batch adsorption study was conductedunder different conditions like, the effects of solution pH, contact time and temperature. The paper mulberrybio-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 metalconcentration of 50 mg/l at pH 2, 4, 8, 12. Maximum removal of cadmium, copper, chromium, lead and zinc byPMB 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 thermodynamicparameters such as G°, H° and S° were calculated for predicting the nature of sorption. The resultsshowed that plant-residue bio-char can act as effective alternative sorbent instead of silica powder for theremoval 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

The pollution of surface and underground water to environment. Many processes are developed tohas been gradually increased; that is worldwide address these stringent environmental regulationsconcern due to the disposal of heavy metals for last which necessitate removal of heavy metal compoundsfew decades [1]. Heavy metals coming from from wastewater.municipal waste and agriculture runoff to the earth’s Common contaminants removal processes aresurface 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 toindustrial/domestic effluents such as metal plating implement on large scale due to expensiveness andindustries, mining and tanneries, etc. Heavy metals ineffectiveness at low concentration (<100 mg/l) andfrom polluted water bodies can then diffuse into the production of toxic sludge and other waste productssurrounding soil, surface water and groundwater. that also need disposal [6, 7]. The disadvantages haveWhen the polluted water is consumed by living increased the need of developing alternative and low-costorganisms, the toxic heavy metals can accumulate and water treatment technologies for treatment of heavybecome harmful [2]. The human health and ecological metal contaminants. Among these technologies for thesystems are threatened to get worse. Harmful heavy removal of heavy metal, adsorption is considered asmetals 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

heavy metal from industrial sources before they enter

Sawaira Adil, Azhar Mashiatullah, Maliha Asma, Jawaria Abid and Abdul Ghaffar

Heavy Metal Removal Efficiency of Paper Mulberry Biochar and Commercially Available Silica Powder from Simulated Industrial Wastewater

Iranica Journal of Energy & Environment 5 (4): 446-452, 2014ISSN 2079-2115 IJEE an Official Peer Reviewed Journal of Babol Noshirvani University of TechnologyDOI: 10.5829/idosi.ijee.2014.05.04.12

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

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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 theefficient 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= (C - C )/ C X 100Therefore, especially assessment of biomass is gettingincreased attention in all over the world as it is renewable, Where, C is quantity of metals before adsorptionwidely available, cheap and environmental friendly. experiment; C is quantity of metals after adsorptionThere are a number of biomass sources, such as forest experiment. In addition, C is the initial metal ionresidues, low grade plants, agricultural residues and concentration (mg/l), C is the equilibrium concentrationmunicipal solid wastes, which can be utilized for activated of the metal ion (mg/l).carbon precursor. Biomass is a renewable energy resourceand 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 andporous substance, similar in its appearance to charcoal PMB Biochar Preparation: Paper mulberry (Broussonetiaproduced by natural burning which results from papyrifera) locally grown in Pakistan, were obtained fromcombustion of organic materials under oxygen-limited a plantation in Islamabad, Pakistan was used forconditions (Pyrolysis). Because of its high surface-to- producing bio-char. Bark/wood thoroughly washed involume ratio and strong affinity for non-polar substances water to remove any dust, sand, leaves, dirt and adhesivebiochars can be a potential sorbent for organic pollutants insoluble materials. Conversion of paper mulberry toand 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 wereheating rate, temperature, surrounding atmosphere and crushed and ground small particles in electric grinder toresidence time. Bio-char is extensively used for water obtain homogenous powder and the resultant powdertreatment process, adsorption potential of almond shell was sieve to a size no larger than 0.00141 mm (1.4µm) inbio-char for Ni and Co removal from aqueous solution. size. Sieved sample of paper mulberry biomass wereCharacterization and investigation of bio-chars produced pyrolyzed in a tube furnace at 350°C. The biochar wasthrough 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-charsconverted from anaerobically digested biomass to sorb Biochar Characterizationheavy metals used in a range of laboratory sorption and SEM Analysis: For SEM analysis PMB biocharcharacterization 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 discsinvestigate the ability of paper mulberry derived biochar (diameter= 9mm, thickness= 3mm) to fit in the especiallyin 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 sampleschromium, lead, zinc) from simulated industrial conductive before scanning electron microscopy.wastewater. The maximum thickness of Au coating ranged from

MATERIALS AND METHODS electron charge through the sample. A series of electron

Adsorbates: The adsorbates in this study were cadmium, magnifications SEM (Model: Leo 440I).copper, chromium, lead and zinc by dissolving cadmiumchloride (CdCl .H O), copper chloride (CuCl .2H O), BET Surface Area Measurement: The method of2 2 2 2

potassium dichromate (K CrO ), lead chloride (PbCl2) Brunauer, Emmett and Teller (BET) is commonly used to2 7

and zinc sulphate (ZnSO .7H O) salts in 1000ml of determine the total surface area of materials. One gram of4 2

distilled deionized water used as stock solution bio-char samples was degassed at 350°C for 24 hoursconcentrations 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 automatedprepared by taking 50ml (50ppm) of each solution in 500ml nitrogen adsorption apparatus at 77 K. The equilibrium

f i f

i

f

i

e

10-20 µM. The conductive layer helps in passing of

micrographs were recorded of each sample at various

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points inside the 0.00-0.22 P/P0 range were determinedby the BET equation to calculate the surface area of thebio-char samples [16]. The porosity of the bio-char suchas pore diameter and pore volumes was also determinedfrom BET analysis.

RESULTS AND DISCUSSION

Effect of pH on Adsorption: pH of the solution is one ofthe most important parameters in the removal of heavymetals from aqueous solution. The pH of the solutionhas an ability to affect the surface charges of thebiosorbent, the degree of ionization of the biosorbent Fig 1: Removal efficiency of PMB bio-char at different pHduring biosorption and the forms of the metal ions inaqueous solutions [17-19]. The effect of pH on heavymetals (Cd, Cr, Cu, Pb and Zn) ions by PMB bio-charand silica powder were evaluated at four pH levelsviz 2, 4, 8 and 12 (Figures 1 and 2). Cadmium, copper,lead and zinc adsorption increased with increase inpH. Maximum removal efficiency of these metalswere recorded at pH of 12 (see Figures 1 and 2). One ofthe potential factors for the considerable lowadsorption 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 pHcations are completely released under circumstancesof extreme acidic conditions [20, 21]. However removalefficiency of chromium was decreased as the pH isincreased and maximum removal efficiency wasachieved in acidic pH. This is because of the fact underacidic condition the metal surface is highly protonatedthat favors the uptake of Cr in anionic form. By increasingthe pH of the solution surface protonation ofadsorbent gradually reduces and hence adsorptiondecrease.

Effect of Contact Time on Adsorption: Contact time is Fig 3: Removal efficiency of PMB bio-char at differentanother important factor in batch sorption process [22]. contact timeThe effect of contact time on the sorption of Cd, Cu, Cr,Pb, Zn was determined at three contact times viz 2, 3 and4hours (Figures 3 and 4). For adsorption of Cd, Cr and Zn,PMB bio-char reached to near asymptotic removal within3h. Maximum removal of Cu and Pb by PMB bio-charobserved at contact time of 4h and 2h, respectively.While, removal efficiency of Cd and Cu by SiO was below2

50% at contact time of 3h. Maximum removal efficiencyfor Zn was 12.6% at contact time of 4h. Removal efficiencyof cadmium, copper, chromium, lead and zinc by papermulberry biochar were higher than commercially availablesilica powder. Fig 4: Removal efficiency of silica at different contact time

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Fig 5: Removal efficiency of PMB bio-char at differenttemperature

Fig 6: Removal efficiency of silica at different temperatures

Effect of Temperature on Adsorption: The effect oftemperature variation on the sorption of Cd, Cu, Cr, Pband Zn was determined at four temperature levels viz 28,32, 36, 40 and 42°C (Figures 5 and 6). For cadmium,copper, zinc PMB showed maximum heavy metal removalof 75.6, 58.8 and 52.2% at 40°C; that was far greater thanheavy metal removal at 42, 40 and 36°C. For chromiummaximum removal efficiency of SiO was (99%) at 28°C;2

that is greater than the adsorbed on PMB (88%) at 42°C.Maximum removal of Pb by paper mulberry was 89%.An increase in removal of metals by PMB withincreasing temperature indicates an endothermic process.The increase in adsorption with temperature may beattributed to either increase in the number of activesurface sites available for adsorption on the adsorbentor the desolvation of the adsorbing species and thedecrease in the thickness of the boundary layersurrounding the adsorbent with temperature, so that themass transfer resistance of adsorbate in the boundarylayer decreases [23].

Table 1: Physical properties of bio-chars

Char samples S (m g ) V (cc/g) av (nm)a 2 1 b cBET T

Paper mulberry 1.84 5.37x10 11.73

a (S BET surface area ; b (v : Total pore volume) ;c (average poreBET: T

diameter)

Since diffusion is an endothermic process, greateradsorption will be observed at high temperature.Thus, the diffusion rate of ions in the external masstransport process increases with temperature. Whilesorption of chromium was recorded to be decreased withan increase in temperature and show maximum removalof 99% at 28°C, after which further increase in temperaturedid not bring about any further improvement for the metalions, but resulted in desorption of some of the metal ionsfrom the adsorbent surface.

Biochar CharacterizationScanning Electron Microscope and Bet Surface Area:Table 1 shows surface area, total pore volume andaverage pore diameter of the paper mulberry bio-charsproduced. Single point BET surface area of the bio-charswas determined by the nitrogen sorption method.Paper mulberry bio-char has surface area of 1.84m g ,2 1

total pore volume of 5.37x10 and average pore diameter3

of 11.7nm. There is an inverse relationship betweensurface area and average pore diameter.

Figure 7 shows scanning electron microscopy(SEM) images of paper mulberry bio-char. Morphologicalanalysis was performed by scanning electron microscopy.SEM micrographs clearly show the amorphous andheterogeneous nature of paper mulberry bio-char.Scanning electron microscopy revealed that internal poresand cracks /mesopores are present in bio-chars materials.Due to importance of mesopores to many liquid-solidsorption processes these pores are of importance to manyliquid-solid sorption processes [24].

Thermodynamic Model: Temperature dependence ofthe adsorption process is associated with severalthermodynamic parameters. Thermodynamicconsiderations of an adsorption process are necessaryto conclude whether the process is spontaneous or not.The thermodynamic parameters, the values of enthalpy

H° and entropy S° and Gibbs free energy G° ofsorption are useful in defining whether sorption isendothermic or exothermic. Modelling temperaturedependence of the adsorption process is associated withseveral thermodynamic parameters. Thermodynamicconsiderations 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 and C is the equilibrium concentration of metalThe 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 beimportant criterion for spontaneity. Also, both energy and expressed by the following equationsentropy factors must be considered in order to determinethe Gibbs free energy of the process [25]. Thermodynamic G° = H° - T S° (6)parameters such as Gibbs free energy change ( G°),enthalpy change ( H°) and the entropy change ( S°) can Eq. (6) can be written asbe estimated using equilibrium constants changingwith temperature. The Gibbs free energy change of the lnK = - G°/RT = - H°/RT + S°/R (7)adsorption reaction can be determined from the followingequation. According to Eq. (7), H° and S° parameters can be

G° = -RT lnK (4) K versus 1/T, respectively [25-27]. Moreover, theL

Where R is gas constant (8.314 J/mol K), K is equilibrium shows a decrease in feasibility of sorption at higherL

constant and T is absolute temperature (K). The K value temperatures. The positive value of H° indicates thatL

was calculated using the following equation: the nature of adsorption process is endothermic in all

K = q /C (5) are more preferred for higher sorption. The positiveL e e

e e

L

calculated from the slope and intercept of the plot of lnL

decrease in G° values with increase in temperature

cases. This behavior indicates that higher temperatures

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 -0.09632 -1.246 -0.392 -2.195 -2.304 -0.09736 -1.262 0.397 -2.224 2.334 -0.09840 -1.279 -0.402 -2.253 -2.334 0.10042 -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

R 0.505 0.599 0.765 0.644 0.4632

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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 1.42832 -1.187 0.976 -5.063 -1.929 1.44736 1.203 0.989 -5.130 -1.954 1.46640 1.218 1.002 -5.196 -1.979 1.48542 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

R 0.254 0.732 0.715 0.192 0.312

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حصف یػگیبی ظغبل حبنل اظ زضذت تت PMB زض همبیؿ ثب پزض ؾیلیؽ ثطای حصف فلعات ؾگیي هضز اضظیبثی لطاض گطفت. اثط

زهب، ظهبى توبؼ pH زضخصة بپیؾت ثطضؾی گطزیس. خصة وبزهیم، هؽ، وطم ضی ثب شغبل PMB زض همبیؿ پزض ؾیلیؽ

ثؿیبض هثط تط ثز اؾت. آظهبیف ثب غلظت mg/l 50 زض pH 2، 4، 8 12 ادبم قس تبیح كبى زاز اؾت و زض ظهبى توبؼ 2 تب 4

ؾبػت حس اوثط خصة وبزهیم، هؽ، وطم ضی ثب ظغبل PMB زض همبیؿ ثب پزض ؾیلیؽ خصة ثیكتطی ثسؾت اهس اؾت. ثطضؾی

هحبؾجبت پبضاهتطبی تطهزیبهیىی اطغی آظاز گیجؽ، اتبلپی اتطپی كبى زاز اؾت عجیؼت ضفتبض خصة لبثل پیف ثیی اؾت.

تبیح خصة فلعات ؾگیي فبضالة نؼتی ظغبل ثیكتط هثط تط اظ پزض ؾیلیؽ ثز اؾت.

Persian Abstract

چىیس

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