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Chemical Engineering Journal 222 (2013) 259264

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Chemical Engineering Journal


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Batch adsorption of semi-aerobic landll leachate by granular activated carbon prepared by microwave heating
K.Y. Foo a,b,, L.K. Lee b,c, B.H. Hameed d
a

Environment and Occupational Health Programme, School of Health Sciences, Health Campus, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan, Malaysia River Engineering and Urban Drainage Research Centre (REDAC), Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia c Nutrition Programme, School of Health Sciences, Health Campus, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan, Malaysia d School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia
b

h i g h l i g h t s
" Highlight the renewable use of " "

g r a p h i c a l a b s t r a c t
100 COD 80 Removal (%) Color

"

"

tamarind fruit seed. Explore the efcient use of microwave irradiation. To examine the physical and chemical characteristics of the adsorbent. To evaluate the potential for the adsorptive treatment of landll leachate. Outline the adsorption isotherms, kinetics and thermodynamics.

60

40

20

Tamarind Fruit Seed Activated Carbon


0 2 4 6 8 10 Dosage (g) 12 14 16

a r t i c l e

i n f o

a b s t r a c t
In this work, tamarind fruit seed derived granular activated carbon (TSAC) was prepared by microwave heating for the adsorptive treatment of semi-aerobic landll leachate. TSAC was examined by pore structural analysis and determination of surface acidity/basicity. The effects of adsorbent dosage, contact time, and solution pH on the adsorptive removal of color and non-biodegradable constituents, expressed in term of chemical oxygen demand (COD) were quantied. The experimental results manifested that the adsorptive removal of color and COD increased with increasing the adsorbent dosage and contact time, with the adsorptive removal of color and COD of 91.23% and 79.93%, respectively, at the adsorbent dosage of 6 mg/200 mL and pH 6. The adsorption kinetic was satisfactory tted to the pseudo-second-order kinetic model. Equilibrium data were favorably described by the Langmuir isotherm model, showing a monolayer adsorption capacity for color and COD of 168.57 PtCo/g and 64.93 mg/g at 30 C, respectively. 2013 Elsevier B.V. All rights reserved.

Article history: Received 13 October 2012 Received in revised form 7 February 2013 Accepted 9 February 2013 Available online 18 February 2013 Keywords: Adsorption Chemical oxygen demand Color Isotherm Landll leachate Microwave

1. Introduction Landll leachate is a heterogeneous mixture of complex organic and inorganic contaminants, formed by excess water percolating
Corresponding author at: Environment and Occupational Health Programme, School of Health Sciences, Health Campus, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan, Malaysia. Tel: +60 45945874/97677824; fax: +60 45941011/ 97677515. E-mail addresses: redacfoo@eng.usm.my, k.y.foo@kk.usm.my (K.Y. Foo).
1385-8947/$ - see front matter 2013 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.cej.2013.02.032

through the waste layers in the landlls [1]. The raw leachate generated from young acidogenic landlls is commonly characterized by a high biochemical oxygen demand (BOD) (400013,000 mg/L), high concentrations of chemical oxygen demand (COD) (30,000 60,000 mg/L), a moderately high strength of NH3N (500 2000 mg/L) and a high ratio of BOD/COD ranging from 0.4 to 0.7 [2]. With the increasing age of a landll, the produced leachate is featured by the presence of recalcitrant, difcult-to-treat, hard COD and a low BOD/COD ratio of less than 0.2. Typically, most of the organic materials present in the stabilized leachate are

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refractory compounds such as humic substances and fulvic-like fractions, which are not easily degradable [3]. As a result, stabilized leachate cannot be effectively treated either by biological processes such as activated sludge, anaerobic ltration and anaerobic lagoons, or by natural systems such as leachate recirculation or constructed wetland [4]. In view with the above matter, a wide range of new tertiary treatment technology has been abounded [58]. In particular, activated carbon adsorption process has emerged to be a plausible circumstance for leachate treatment, main hinges on its simplicity of design, ease of operation, insensitivity to toxic substances, and superior ability for removing a broad range of pollutants, even from the gases environment [9]. Despite its prolic use in water treatment, a major limitation of the use of activated carbon is the high production cost, associated with the long processing time and high energy consumption [10]. Therefore, it is necessary to nd an alternative route for the preparation of activated carbons. In our previous work, the preparation of granular activated carbon from tamarind fruit seed derived by microwave heating has been reported [11]. This research was undertaken to provide an insight into its feasibility for the adsorptive treatment of COD and color of the semi-aerobic landll leachate in a batch mode study. Textural and surface characterization of the prepared adsorbent was performed. The effects of adsorbent dosage, contact time, and solution pH on the adsorptive removal of color and COD were evaluated. Moreover, the adsorption isotherms, kinetics and thermodynamics are elucidated. 2. Materials and methods 2.1. Adsorbate Leachate samples were collected from a municipal waste semi-aerobic landll (Pulau Burung Landll Site, PBLS), situated within the Byram Forest Reserve at 5240 N, 100240 E, in Penang, Malaysia. The site has a natural marine clay liner with the total area of 33 ha. The PBLS was developed semi-aerobically employed a controlled tipping technique into a leachate recirculation system in March, 2001 and is one of the only three sites of its kind in Malaysia. The samples were collected from the active detention pond with the leachate age of less than 5 years, and instantaneously transported to the laboratory, and stored in darkness at 4 C prior to use to minimize the chemical and biological changes. The characteristics of the leachate samples are listed in Table 1. The chemical oxygen demand (COD) of the leachate varied between 2060 and 2700 mg/L, while the biological oxygen demand (BOD5) was less than 200 mg/L. This gives a BOD5/COD ratio of 0.06, which indicates that most of the organic compounds in the landll leachate were poorly biodegradable. Chemical analysis was performed according to the Standard Method of Water and Wastewater [12]. All experiments were undertaken in triplicates.

2.2. Preparation of activated carbon The preparation procedure has been reported elsewhere [11], where the raw precursor was thoroughly washed, air-dried and sieved to obtain a fraction of 12 mm. The dried TS was loaded into a tubular furnace, and heated up to a carbonization temperature of 700 C under puried N2 gas ow (150 cm3/min), at the heating rate of 10 C/min [13]. The char produced was mixed with potassium hydroxide solution in a char/KOH impregnation ratio of 1:1.50 (wt%) with occasional stirring. Microwave heating was conducted in a 2.45 GHz commercial microwave oven with suitable modications [14]. The reaction was performed in a Pyrex glass reactor xed in the chamber of microwave oven. The microwave power was set at 600 W and the irradiation time of 7 min was selected as the heating period based on preliminary runs. Nitrogen gas at a pre-set ow rate of 300 mL/min was used to purge air in the reactor before the start of microwave heating and it continued to ow during the cooling intervals. The resultant activated carbon was washed sequentially with 0.1 M of hydrochloric acid and rinsed repeatedly with hot and cold distilled water until the pH of the washing solution reached 67. 2.3. Characterization of activated carbon The surface acidity was estimated by mixing 0.20 g of TSAC with 25 cm3 of 0.05 M NaOH solution in a closed ask, and agitated for 48 h at room temperature. The suspension was decanted, and the remaining NaOH was titrated with 0.05 M HCl. The surface basicity was measured by titration with 0.05 M NaOH after incubation 0.20 g of TSAC with 0.05 M HCl. 2.4. Batch equilibrium studies The batch adsorption experiments were undertaken in a series of Erlenmeyer asks containing 200 mL of leachate solution. The asks were kept in an isothermal water bath shaker at 30 C with an agitation speed of 120 rpm. In each experiment, the same sample was used and the initial characteristics were determined as to reduce the background interferences. The samples were collected at prescribed time intervals, and the chemical oxygen demand (COD) and color was measured using the dichromate closed reuxed calorimetric and APHA PlatinumCobalt standard methods, with a spectrophotometer (HACH DR2500) at the maximum wavelength of 620 and 455 nm, respectively. All samples were ltered using a syringe lter (Whatman 0.45 lm) prior to analysis to minimize the interference of carbon nes with the analysis. The adsorptive uptake of COD (mg/g) and color (PtCo/g) at time t, qt and equilibrium, qe was calculated by:

qt qe

C o C t V W C o C e V W

Table 1 Characteristics of the leachate samples based on ve samplings in May, 2012. Parameter COD BOD5 BOD5/COD Color NH3N Suspended solids pH Unit mg/L mg/L PtCo mg/L mg/L Values 20602700 40190 0.020.07 42505700 23102880 114360 7.98.5 Average 2336 147 0.055 5095 2550 181 8.2

where Co, Ct and Ce are the liquid-phase concentrations of COD (mg/ L) and color (PtCo) at initial, time t (min) and equilibrium, respectively. V is the volume of the leachate solution (L), and W is the mass of adsorbent used (g). The pollutant removal, R (%) was determined by:

C o C e 100% Co

The inuence of adsorbent dosage on the adsorptive uptake of COD and color was conducted by varying the TSAC dosage from 2.0 to 14.0 g, while keeping the other parameters constant. The

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effect of pH was examined by regulating the pH from 2 to 10, with a TSAC dosage of 6.0 g/200 mL and adsorption temperature of 30 C. The initial pH of the leachate solution was adjusted by addition of 0.10 M HCl or NaOH. The pH was measured using a pH meter.

3. Results and discussion 3.1. Characterization of the prepared adsorbent The surface acidity and basicity is an important criterion interpreting the surface chemistry of the carbon adsorbents [15]. Analysis of the acid/base titration indicates that TSAC exhibited an acidic behavior, with the surface acidity of 2.78 mmol/g and 1.05 mmol/g as surface basicity. From the result, it can be proposed that there were greater amounts of oxygen-containing groups (mainly carboxylic, anhydrides, lactones and phenols) than oxygen-free Lewis sites, carbonyls, pyrone and chromene type structures at the edge of the carbon layers. The presence of these surface acidic groups may impart a polar character to TSAC surface, which can effectively affect the preferential adsorption of COD and color onto TSAC. Nitrogen adsorption isotherm provides qualitative information on the porosity of the carbonaceous adsorbents. The isotherm resembles III hybrid shape as dened by the International Union of Pure and Applied Chemistry (IUPAC) classication. The BET surface area, external surface area, Langmuir surface area and total pore volume of TSAC was identied to be 1090.01 m2/g, 578.23 m2/g, 1616.84 m2/g and 0.594 cm3/g, respectively [11].

It is plausible to suggest that by increasing the adsorbent dosage, there would be a greater availability of surface area and exchangeable binding sites. However, further increment in adsorbent dosage beyond 6.0 g/200 mL illustrated a slight decline of adsorptive uptake of COD and color, consequence of the unsaturation of adsorption sites during the adsorption process. Moreover, higher adsorbent dosage could impose particle interactions, resulting from the aggregation and overcrowding of adsorbent particles. Such aggregation would lead to a decrease in the accessible surface area of TSAC, lowering the pollutant removal per unit of adsorbent [16]. Fig. 2 presents the adsorptive removal of COD and color onto TSAC with respect to time at the adsorbent dosage of 6.0 g/ 200 mL and operating temperature of 30 C. It is clear from Fig. 2 that the adsorption process increased sharply at the initial stage, indicating of the availability of readily accessible sites. The process was gradually slower as the equilibrium approached. This phenomenon is attributed to the reduction of immediate solute adsorption due to the lack available open sites for COD and color adsorption, which in turn supported lm diffusion [17]. The time required to attain this state of equilibrium is termed as equilibrium time (2.67 h). The time prole of COD and color uptake is a single, smooth and continuous curve leading to saturation, suggesting possible monolayer coverage of COD and color onto the surface of TSAC. 3.3. Effect of solution pH on the adsorptive uptake of COD and color Solution pH is a predominant factor affecting the degree of ionization of adsorbate and the surface charge of a solid adsorbent. Fig. 3 depicts the adsorptive behavior of COD and color as a function of pH onto TSAC at 30 C. Generally, a stabilized leachate may contain high amount of polar and nonpolar aggregated organic constituents, in the form of proteins, carbohydrates, detergents, tannins, lignin, humic acid, fulvic acid, melanic acid and dissolved organic compounds, usually expressed in term of COD [2]. The extent of adsorption of these colored impurities was depended primarily on their molecular weight, ionic charge, pH level, and hydrophobicity. The removal of these aggregated organic compounds may occur in two mechanisms, physical adsorption (non-polar attractions), which involves Van der Waals interactions between the non-ionic head and the hydrophobic matrix, and ion exchange (polar attractions), that involves counterion displacement and electrostatic interaction between the positively charged quaternary ammonium functional group, and the negatively charged carboxylic or sulfonic groups [18].

3.2. Effect of adsorbent dosage and contact time on the adsorptive removal of COD and color Adsorbent dosage is a profound parameter affecting the adsorption process due to the reason that it predicts the cost of pollutant to be treated. Fig. 1 shows the variation of adsorbent dosage on the adsorptive uptake and adsorptive removal of COD and color onto TSAC at 30 C. It is clearly revealed that the adsorptive removal of COD and color increased with increasing the adsorbent dosage from 2.0 g/200 mL to 6.0 g/200 mL, and thereafter, further increase in adsorbent dosage did not exert an appreciable increase in the adsorptive removal of COD and color. The optimum adsorptive uptake and adsorptive removal of COD and color are noted at 62.23 mg/g and 79.93%, and 154.94 PtCo/g and 91.22%, respectively.

160 100
COD (mg/g)

80

COD Color
160

Color (Pt-Co/g)

120

Removal (%)

120

qt
COD (mg/g) Color (Pt-Co/g) 0 2 4 6 8 10 12 14 16

60
qe

80

40

80

40

40

20
0

Dosage (g)

0 0 2 4 6 8 10 12 14 16

0 0 0.5 1 1.5 2 2.5 3

Dosage (g)
Fig. 1. Variation of adsorbent dosage on the adsorptive uptake and adsorptive removal of COD and color onto TSAC at 30 C.

Time (h)
Fig. 2. Effect of contact time on the adsorptive uptake of COD and color onto TSAC at 30 C.

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180 150 120


COD (mg/g) Color (Pt-Co/g)

Table 3 Thermodynamic parameters for the adsorption of COD and color onto TSAC at 30, 40 and 50 C. Adsorbate

DH (J/mol)

DS (J/mol K)

DG (J/mol)
30 C 40 C 58.49 1077.53 50 C 338.67 1517.15

90 60 30 0 0 2 4 6 8 10 12

COD Color

67.11 63.72

0.215 0.236

249.25 801.10

qe

pH
Fig. 3. Effect of solution pH on the adsorptive uptake of COD and color onto TSAC at 30 C.

COD and color onto TSAC was well described by the pseudo-second-order kinetic model, with the highest correlation coefcient, R2 (>0.99). Besides, the experimental qe values agreed satisfactory with the calculated qe values obtained theoretically. This suggested that the adsorption system followed the pseudo-second-order model, based on the assumption that the rate-limiting step may be chemisorption. 3.5. Adsorption thermodynamic Adsorption thermodynamic is a signicant criterion outlining the adsorption behavior of an isolated system [24]. The values of enthalpy change (DH), Gibbs free energy change (DG), and entropy change (DS) at the adsorption temperature of 30, 40 and 50 C were determined following the equations:

According to Cossu and Rossetti [19], the organic fraction preferentially removed by activated carbon is the fulvic fraction, with a molecular weight of 10010,000 g/mole. In another study in which the humic and fulvic acid content in the leachates were determined, it was found that fulvic acids may represent 59% of the initial COD of the landll leachate [20]. In the present work, it is apparently that increasing pH from 2 to 6 showed an enhancement of the adsorptive uptake for COD and color from 18.01 to 65.45 mg/ g, and from 60.14 to 156.36 PtCo/g, respectively, and then it gradually decreased. Lower adsorption in strong acidic pH of 24, can be attributed to the high mobility of H3 O ions competing with organic cations for the adsorption sites. Simultaneously, it is likely that a strong electrostatic repulsion force presents between H3 O cations with the positively charged quaternary ammonium functional groups of adsorbent, leading to a sharp reduction of adsorption. In the basic medium of 810, the abundance of OH ions would induce a strong hindrance to the diffusion of organic anions. This interaction may mutually inhibit the adsorptive uptake of COD and color onto TSAC. 3.4. Adsorption kinetic Adsorption kinetic describes the solute uptake, which governs the adsorption rate, retention time and mechanism of the adsorption process [21]. The pseudo-rst-order kinetic model [22] is dened as:

ln K d

DS DH R RT

6 7

DG RT ln K d

where R (8.314 J/mol K) and T (K) are universal gas constant and absolute temperature, and Kd is the distribution coefcient derived as:

Kd

C Ae Ce

log

qe qe qt

k1 t 2:303

where k1 is the adsorption rate constant (1/min). Pseudo-secondorder equation [23] is given by:

t 1 1 t qt k2 q2 qe e

where k2 (g/mg h) is the pseudo-second-order kinetic rate constant. The corresponding results are tabulated in Table 2. The results of the two tested models indicated that the adsorption of

where CAe (mg/L) is the amount adsorbed on solid at equilibrium and Ce (mg/L) is the equilibrium concentration. The computed values are summarized in Table 3. The positive value of DH indicated the adsorption process was endothermic in nature. The result implied that the adsorption of COD and color onto TSAC was highly temperature dependent, favorable at higher operating temperature. This endothermic process was due to the increase in temperature which enhanced the diffusion rate of the organic molecules across the external boundary layer, and in the internal pores of adsorbent. The positive value of DS revealed the afnity of TSAC for the adsorbate being tested and increasing randomness at the solidsolution interface during the xation of COD and color onto the active sites of TSAC. The negative values of DG illustrated spontaneous nature and feasibility of the adsorption process with high preference of COD and color onto TSAC. The values of DG was 249.25 and 801.10 J/mol for COD and color, respectively at 30 C, and this DG value turned lower at higher operating temperature of 40 (58.49 and 1077.53 J/mol) and 50 C (338.67 and 1517.15 J/mol). This shows that the reaction rate increased with increasing the operating temperature.

Table 2 Kinetic models parameters for the adsorption of COD and color onto TSAC at 30 C. Adsorbate Co qe,
exp

Pseudo-rst-order k1 (1/h) qe,calc 56.15 mg/g 124.33 PtCo/g R2 0.983 0.972

Pseudo-second-order

Dq (%)
9.76 19.75

k2 0.035 g/mg h 0.026 g/PtCo h

qe,calc 61.35 mg/g 151.52 PtCo/g

R2 0.998 0.996

Dq (%)
1.41 2.21

COD Color

2336 mg/L 2550 PtCo

62.23 mg/g 154.93 PtCo/g

1.18 1.62

K.Y. Foo et al. / Chemical Engineering Journal 222 (2013) 259264 Table 4 Isotherm parameters for the adsorption of COD and color onto TSAC at 30, 40 and 50 C. Adsorbate Temperature (C) Langmuir isotherm model Q0 (mg/g) COD 30 40 50 64.93 67.57 80.25 Q0 (PtCo/g) Color 30 40 50 168.57 182.78 194.92 KL (L/mg) 0.011 0.031 0.007 KL (L/PtCo) 3.96 103 4.40 103 3.91 103 R
2

263

Freundlich isotherm model KF (mg/g)(L/mg) 1.04 21.63 52.51 KF (PtCo/g)(L/PtCo)1/n 6.96 6.19 5.98
1/n

Temkin isotherm model n 5.56 6.29 7.94 n 2.23 2.06 1.99 R


2

A (L/g) 0.986 0.948 0.635 A (L/g) 0.032 0.033 0.029

B 67.77 9.49 10.66 B 40.49 43.95 48.36

R2 0.934 0.823 0.739 R2 0.982 0.976 0.989

0.987 0.997 0.983 R2 0.991 0.995 0.992

0.841 0.798 0.754 R2 0.993 0.983 0.970

Table 5 Comparative evaluation of adsorption capacities onto various adsorbents. Adsorbent TSAC Sugarcane bagasse activated carbon Composite Zeolite Periwinkle shell activated carbon Commercial activated carbon TSAC Fungal Biomass Bygasse y ash Anionic resins Adsorbate COD COD COD COD COD COD Color Color Color Color Monolayer adsorption capacity 64.93 mg/g 20.16 mg/g 22.99 mg/g 2.35 mg/g 0.03 mg/g 0.08 mg/g 168.57 PtCo/g 84.99 PtCo/g 88.50 PtCo/g 71.43 PtCo/g Refs. Present study [29] [30] [30] [31] [31] Present study [32] [33] [34]

3.6. Adsorption isotherm Adsorption isotherm is a fundamental tool elucidating the relationship between adsorbate molecules and the adsorbent surface [25]. In this study, three common isotherm models were established: the nonlinear Langmuir [26], Freundlich [27], and Temkin and Pyzhev [28] isotherm models:

30 C, respectively, for COD and color as compared to some previous works as reported in the literature. 4. Conclusion This study revealed the versatility of tamarind fruit seed derived granular activated carbon prepared by microwave heating for the adsorptive treatment of semi-aerobic landll leachate. The prepared activated carbon attained the maximum BET surface area and total pore volume of 1112.88 m2/g and 0.594 cm3/g, respectively. The adsorption of COD and color onto TSAC was best described by the Langmuir isotherm model, with a monolayer adsorption capacity of 64.93 mg/g and 168.57 PtCo/g, respectively. The results indicated that the tamarind fruit seed derived granular activated carbon adsorption process was sufcient for removing these targeted contaminants, to reach to the industrial discharge limit of COD (500 mg/L) permitted by the World Health Organization (WHO). Acknowledgements The authors acknowledge the nancial support provided by the Ministry of Higher Education of Malaysia and Universiti Sains Malaysia under the LRGS (Project No. 203/PKT/6720004) and Universiti Sains Malaysia short term grant scheme. References
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qe

Q 0K LCe 1 K LCe
1

qe K F C n e qe B lnAC e

10 11

where Q0 (mg/g) and KL (L/g) are Langmuir constants related to adsorption capacity and energy of adsorption, KF (mg/g (l/mg)1/n) and n are Freundlich constants related to adsorption capacity and adsorption intensity of the adsorbent, respectively. B = RT/b, where b (J/mol) and A (L/g) are Temkin constant related to heat of sorption and Temkin equilibrium binding constant, respectively. The detailed parameters of these different forms of isotherm equations are listed in Table 4. The results were consistent with the earlier ndings, where the adsorption of COD and color onto TSAC was endothermic in nature. The equilibrium data for the adsorption of COD and color onto TSAC was getting valid for Langmuir isotherm model at the three tested temperatures, with R2 values higher than 0.98, while the correlation coefcient, R2 tted with Freundlich and Temkin isotherm models was found much lower than the Langmuir isotherm model. The applicability of Langmuir isotherm model suggests that the adsorption process is monolayer with each molecule poses equal enthalpies and activation energy. The results also demonstrated no interaction and transmigration of COD and color in the plane of the neighboring surface. Table 5 exhibits a comparison of maximum monolayer adsorption capacities of COD and color onto different adsorbents [2934]. The adsorbent prepared in this work showed relatively high adsorption capacities of 64.93 mg/g and 168.57 PtCo/g at

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