utilization of zncl2 activated jatropha husk carbon for...

139

Utilization of ZnCl activated Jatropha husk carbon for the 2

removal of reactive and basic dyes: Adsorption equilibrium and kinetic studies

Kumaravel Karthick, Chennamallan Dineshand Chinnaya Namasivayam*

Department of Environmental SciencesBharathiar University

Coimbatore 641046, India

Key Words: Adsorption, Jatropha husk carbon, dyes, kinetics

*Corresponding authorEmail: [email protected]

ABSTRACT

INTRODUCTION

Jatropha curcas is an important plant for production of bio-diesel. Huge volume of Jatropha husk is generated in bio-diesel industries and it was used for the production of activated carbon (ZAJHC) by zinc chloride activation method. ZAJHC was employed for adsorption of reactive dye, Procion Orange (PO) and basic dye, Rhodamine B (RB) from water. Effects of various parameters such as initial dye concentration, adsorbent dose, contact time and initial solution pH on adsorption were carried out. Adsorption kinetics followed pseudo second order. The adsorption isotherm was described using Langmuir, Freundlich, and Dubinin-Radushkevich isotherm models. The Langmuir

-1adsorption capacity for PO and RB was found to be 21 and 50 mg g , respectively. .

Industrial development resulted in the disposal of large quantity of various toxic pollutants into the aquatic environment, which are hazardous to human as well as animal health [1]. Dyes are the most common water pollutants. Various sources of dye effluents are from pickling industries, paper and pulp industries, dye stuff industries, tanning, and textile industries [2]. Procion Orange (PO) is a reactive dye and Rhodamine B (RB) is a fluorescent cationic dye which are used in dyeing industries. Of the current yearly world dye production of 10 million kg, between 1 and 2 million kg of reactive dyes enter into the biosphere either in dissolved or suspended form in water [3]. Dyes are difficult to degrade due to their complex structure and synthetic origin [4]. Various treatment methods include biological treatment, catalytic oxidation, sonocatalytic degrada-tion, ozonation, adsorption [4]. photocatalytic degrada-tion [5], electrochemical oxidation [6], and coagula-tion/flocculation for dye removal [7]. Among various methods, adsorption is the most efficient method for the removal of dyes from waste water. It also provides an attractive, alternative treatment especially if the adsorbent is inexpensive and readily available [4].

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The conventional methods for the removal of dyes using coal based activated carbon (AC) are not cost-effective in India. An inexpensive and more easily available adsorbent would make the removal of pollu-tants an economically viable alternative. Different sources of adsorbent materials for ACs are coir pith, orange peel, saw dust, oil palm shell, pistachio-nut shells, sunflower seed hull, cashew nut shell, pome-granate peel, sugarcane bagasse pith, Indian rosewood, maize waste, mango seed kernel, coconut waste, avo-cado kernel [4], and rice husk ash [8]. Jatropha curcus is a multipurpose non-edible oil yielding perennial shrub and is a drought tolerant plant. Its seeds are used to produce bio-diesel. Indian railways uses 2 million kL diesel per year. The Indian government has decided to use bio-diesel at 5% level in the regular diesel. Several international funding agencies such as World Bank, Rockefeller Foundation, Appropriate Technology International, Intermediate Technology Development Group, USA, UK and Biomass Users Network are supporting the promotion of Jatropha for bio-diesel purpose [4]. Jatropha husk (JH) is generated in large quantities as an agro-industrial solid waste in the bio diesel production industries. JH constitutes nearly 80% of the dried vegetable. Lignocellulosic biomasses are attractive

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Sustain. Environ. Res., 24(2), 139-148 (2014)

140

sources for the development of ACs in adsorption process. Activation of JH with ZnCl generates more inter-2

spaces between carbon layers leading to micro porosity and more surface area [9]. It causes electrolytic action termed as “swelling” in the molecular structure of cellulose which leads to the breaking of lateral bonds in the cellulose molecule resulting in increased inter-and intra voids. It promotes the development of porous structure of the AC because of the formation of ele-mentary crystallites [9]. The adsorption capacity of ZnCl activated JH carbon (ZAJHC) is higher com-2

pared to thermal activated JH carbon, because of in-crease in surface area and porosity [10]. The intention of the present work was to explore the feasibility of using ZAJHC for removal of reactive dye, PO and basic dye, RB present in water.

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MATERIALS AND METHODS

1. Pre-treatment Step

JH was collected from Tamilnadu Agricultural University, Coimbatore, India. The dry JH was washed with tap water and then washed with double distilled water to remove earthy impurities. Then it was dried in a hot air oven at 105 ± 5 °C for 8 h and AC was developed using ZnCl . 2

2. Adsorbent: Chemical Activation with Zinc Chloride

ZAJHC was prepared as reported in literature [4]. Characteristics of ZAJHC are shown in Table 1.

3. Adsorbates

PO and RB were supplied by S. D. Fine Chemi-cals, Mumbai, India and used as such without further purification. All the other chemicals used were of AR

-1grade. A stock solution of 1000 mg L of PO and RB was prepared by dissolving the dye in double distilled water. Solutions of various concentrations were prepared by using the above solution. The solutions

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..

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Table 1. Characteristics of ZAJHC

S. No

1

2

3

4

5

6

7

Characteristic

pHzpc

Specific gravity-1Bulk density (g L )

Porosity (%)2 -1S (m g )BET

-1Ion exchange capacity (meq g )-1Iodine number (mg g )

Value

6.8

1.03

0.20

81

822

Nil

91Fig. 1. Structure of dyes (a) PO and (b) RB in acidic (I), neutral (II) and alkaline (III) aqueous media.

were stored in brown glass bottles to avoid degradation in light. Absorbance measurements were carried out for PO and RB using UV-Vis Spectrophotometer (Specord 200, Analytic Jena, Germany). The absorp-tion maxima at 488 nm for PO and 555 nm for RB were used as the monitoring wavelengths for the measurement of absorbance. Calibration graphs were made for PO and RB and the concentrations were estimated using calibration graphs.

4. Structure of Dyes

4.1. PO

PO has one azo, three sulphonic acid groups and contains triazinyl amine group that has two liable chlorine atoms activated by the electron-with drawing action of the three N atoms [11]. The solubility of reactive dyes depends on the number of sulphonic groups (-SO Na) present in the dye molecule. The 3

triazinyl group is responsible for the formation of covalent bonds between the dye and the adsorbent [12]. The rate of adsorption may be lowered by thedye's structural complexity that is inversely propor-tional to the number of sulfonate groups present (Fig. 1a) [13].

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Karthick et al., Sustain. Environ. Res., 24(2), 139-148 (2014)

141

4.2. RB

RB has two diethyl amine groups, four N-ethyl groups on either side of xanthene rings and carboxy-phenyl group. RB exists in two forms (cationic and zwitterionic) in polar solvents. The transformation of the cationic to zwitterionic form occurs at pH values of greater than 3.7 (pKa of RB = 3.7) by deprotonation

+of the carboxyl group of the cationic (RB ) form. An electrostatic interaction between the xanthene and the carboxyl group of RB monomers causes the aggrega-tion of RB to form dimers and hinders the adsorption of dye molecules into the pores (Fig. 1b) [14]. There-fore, the chemical structure (shape, number of active groups, stability of charge and molecular size) of the dye gives the difference in the affinity of PO and RB towards ZAJHC (Table 2).

5. Instrumental Analysis of ZAJHC

The surface morphology of loaded and unloaded ZAJHC was examined using scanning electron micro-scope (SEM-JSM, 840A, JEOL, Japan). After adsorp-tion, PO and RB loaded ZAJHC carbon samples were filtered using a suction pump on qualitative filter paper and stored in a vacuum desiccator, which was later used for instrumental analysis.

6. Batch Mode Adsorption Studies

Adsorption experiments were carried out for PO and RB to investigate the effect of various parameterssuch as initial concentration of adsorbate, contact time, adsorbent dose and initial pH. Solutions containing desired concentrations of PO at pH 2.0 or RB at pH 4.0 and ZAJHC were placed in 100 mL conical flasks and agitated at 200 rpm, 35 °C on a thermo stated rotary shaker (Scientific Systems, Chennai, India). After the predetermined time intervals, the samples were withdrawn and the supernatant was separated from the ZAJHC by centrifugation at 2500 rpm for 30 min. Then the concentration of the residual dye was determined as said earlier. Effect of pH was studied in the pH range 2-11 by adjusting the pH of solutions

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Table 2. Physical characteristics of dyes

S. No

1

2

3

4

characteristic

Molecular formula

Molecular weight

ë (nm)max

Color index name

PO

C H C N O S24 16 l2 6 10 3

715.5

488

Reactive Orange

1,5-Naphthalenedisulfonic acid, 2-[[6-

[(4,6-dichloro-1,3,5-triazin-2yl)

methylamino]-1-hydroxy-3-sulfo-2-

naphthalenyl]azo], trisodium salt

RB

C H N O Cl28 31 2 3

479.0

555

Basic Violet 10

[9-(2-carboxyphenyl)-6-diethylamino-3-

xanthenylidene]-diethylammonium chloride5 IUPAC name

using 1 M H SO and 1 M NaOH solutions by means of 2 4

a pH meter (Elico, Mode LI-107, Hyderabad, India).

RESULTS AND DISCUSSION

1. SEM Observations

The SEM picture of the thermally activated JH carbon (JHC) is shown in (Fig. 2a) for comparison with SEM picture of the ZAJHC prepared using ZnCl2

(Fig. 2b). There is no uniform and well developed pore structure on the surface of the JHC. High surface area and pore structure are the basic parameters for an effective adsorbent. When the porosity increases the surface area also increases. ZAJHC show tremendous, perfect and constructed pore structures on the surface. The micrograph of ZAJHC shows a compressed and lanky structure due to the formation of more inter-spaces between the mono layers by the activation of ZnCl . Higher volume of pores developed from the 2

ZnCl activation acts as a route for the contaminants 2

to enter into the micro pores. After adsorption, the surface of ZAJHC was loaded by PO and RB (Figs. 2c and 2d). It clearly shown that the dyes were strongly adsorbed on the surface of the ZAJHC and it turned to irregular and unrecognizable structures.

2. Effects of Agitation Time and Adsorbent Dose

A series of contact time experiments for adsorp-tion of PO and RB dyes were carried out at different

-1 initial concentrations (PO 10-50 mg L and RB 30-70 -1mg L ) at 35 °C. Adsorption of PO and RB reached

equilibrium at 120 min for all concentrations. The per cent removal decreased with increasing initial dye concentration and the actual amount of dye adsorbed per unit mass of carbon increased with increase in dye concentration. It means that the adsorption is highly dependent on initial concentration of dye. At lower concentration, the ratio of the initial number of dye molecules to the available surface area is low. Subse-quently the fractional adsorption becomes independent of initial concentration. However, at high concentration

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Fig. 2. SEM images for JHC and ZAJHC: (a) raw Jatropha husk carbon, (b) ZAJHC and (c) ZAJHC after adsorption of PO (d) ZAJHC after adsorption of RB.

of dyes the available sites of adsorption becomes fewerand hence the per cent removal of dye is dependent upon initial concentration [15].

3. Adsorption Kinetics

Adsorption of PO and RB was analyzed using the Lagergren first order rate equation [16].

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(1)

(2)

where q and q are the amounts of dye adsorbed (mg e-1g ) at equilibrium and at time t (min) respectively. k is 1

the Lagergren rate constant of first order adsorption -1(min ). Values of the q and k , respectively, were e 1

where k is the equilibrium rate constant of pseudo 2-1 -1second order adsorption (g mg min ). Values of k and 2

q were calculated from the plots of t/q versus t (figure e

not shown). The computed results obtained from the first and second order kinetic models along with the experimental q values are presented in Table 3. Thee

calculated q values of the pseudo second order e

kinetics are generally closer to the experimental q e

values compared to the calculated q values from first e

order kinetics for both PO and RB. So the adsorption process follows pseudo second order kinetic model for both reactive and basic dyes [17].

4. Adsorption Isotherms

In order to quantify the adsorption capacity of the ZAJHC for the removal of PO and RB, the equilibrium data were fit in to Langmuir, Freundlich and Dubinin-Radushkevich (D-R) isotherm equations.

4.1. Langmuir isotherm

The Langmuir isotherm is represented by the following equation [18]:

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Table 3. Comparison of Lagergren first order and second order kinetic data for adsorption of PO and RB onto ZAJHC

Dye

PO

RB

10

20

30

40

50

30

40

50

60

70

7.2

14.4

17.0

18.4

19.7

27.5

31.6

37.2

40.8

44.4

-1k (min )1

0.02

0.02

0.02

0.02

0.03

0.03

0.21

0.02

0.02

0.03

-1q (mg g )e(cal)

6.4

12.9

13.4

13.7

15.1

26.6

31.1

28.3

32.7

32.2

2R

0.99

0.99

0.98

0.97

0.95

0.99

0.99

0.99

0.99

0.99

-1 -1k (g mg min )2

0.003

0.001

0.002

0.002

0.003

0.01

0.01

0.01

0.01

0.01

-1q (mg g )e(cal)

8.8

17.5

19.6

20.8

22.2

37.0

38.5

43.5

47.6

52.6

2R

0.97

0.97

0.98

0.99

0.99

0.97

0.96

0.98

0.99

0.99

First order kinetic model Second order kinetic model-1Conc. (mg L )

-1q (mg g )e(exp)

calculated from the slope and intercept of the plots of log (q - q) versus t (figure not shown). e

The pseudo second order kinetic model can be repre-sented as

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(3)

-1where C is the equilibrium concentration (mg L ), q is e e-1the amount adsorbed at equilibrium (mg g ) and Q o

and b are Langmuir constants related to adsorption efficiency and energy of adsorption, respectively. The


143

linear plots of C /q vs C suggest the applicability of e e e

the Langmuir isotherms (figure not shown). Values of Q and b were determined from slope and intercepts of o

the plots (Table 4). The values of Q and b indicate that o

the maximum adsorption corresponds to a saturated monolayer of adsorbate molecules on adsorbent sur-face with constant energy and no transmission of adsorbate in the plane of the adsorbent surface. To confirm the favourability of the adsorption process, the separation factor (R ) was calculated. L

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Table 4. Langmuir, Freundlich and Dubinin- Radushkevich isotherm constants for PO and RB

Dyes

PO

RB

Q0-1(mg g )

20.8

50.0

b-1(L mg )

0.44

0.3

Conc -1mg L

10

20

30

40

50

30

40

50

60

70

2R

0.997

0.980

RL

0.19

0.1

0.07

0.05

0.04

0.11

0.08

0.07

0.06

0.05

Äq (%)

5.5

16.1

kf1- l/n l/n -1mg L g

7.9

21.8

n

3.6

4.8

2R

0.97

0.94

Äq (%)

3.4

11.0

qm-1(mg g )

15.8

106.3

â 2 -2 -9(mol kJ x 10 )

2

1

2R

0.98

0.93

Äq (%)

8.5

28.6

The R values obtained were between 0 and 1 L

(0.04 to 0.19 for PO and 0.05 to 0.11 for RB) (Table 4). This indicates that the adsorption process is favourable [19].

The Freundlich isotherm is represented by [20]:

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4.2. Freundlich isotherm.

(4)

(5)

where k and n are constants incorporating the factors f

affecting the adsorption capacity and intensity of adsorption, respectively. Linear plots of log q vs log e

C shows that the adsorptions of RB dye obey e

Freundlich adsorption isotherm (figure not shown). The values of n are between 1 and 10 indicating favourable adsorption (Table 4). Comparison of Langmuir and Freundlich constants for various adsorbents from literature are presented in Table 5.

4.3. D-R isotherm

The D-R isotherm is represented as:

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(6) ln q = ln q - âå²e m

where â is a constant related to the mean free energy 2 -2of adsorption (mol kJ ), q is the theoretical saturation m

-1capacity (mg g ), å is the polyani potential, and calcu-lated as follows: .

(7)

(8)

The slope of the plot of ln q vs å² gives â and the in-e

tercept yields the adsorption capacity (figures not shown). The mean free energy of adsorption (E) (kJ

-1mol ) is calculated from the equation: .

-1If the value of E is less than 8 kJ mol , the adsorption follows physical sorption. If the value of E is between

-18 and 16 kJ mol , the adsorption follows ion exchange. -1If the E value is above 40 kJ mol the adsorption

follows chemisorption. Values of E obtained for PO -1and RB are 16 and 22 kJ mol , respectively. Hence

adsorption involved seems to be ion exchange mech-anism [21]. Figures 3a and 3b represent different adsorption isotherms along with the experimental data for adsorption of PO and RB. In order to compare thevalidity of isotherm equations, a normalized deviation, Äq (%) was calculated using the following equation: .

(9)

where superscripts 'exp' and 'cal' are the experi-mental and calculated values, respectively, and 'n' is the number of measurements [22]. Lowest Äq (%) values obtained from the isotherm models indicate highest fitting with the adsorption data. In the present study the Äq (%) values obtained for both PO and RB are in


Langmuir Frendlich D-R

144

Adsorbate Adsorbent-1Q (mg g )o

1.3

*

3.1

3.8

2.6

20.83

4.8

3.23

8.5

*

2.6

50

-1b (L mg )

0.059

*

0.046

0.012

0.43

0.44

0.12

0.049

0.034

*

2.74

0.3

1- l/n l/n -1k (mg L g )f

0.16

0.86

*

0.059

0.33

0.84

7.94

1.22

0.24

0.16

1.10

1.56

21.8

n

2.07

1.30

*

1.21

1.26

0.013

3.6

0.792

1.57

1.17

1.56

0.90

4.79

ReferenceLangmuir isotherm Freundlich isotherm

Orange peel

Red mud

Chemically modified

orange peel

Waste Fe(III)/Cr(III) hydroxide

Coir pith carbon

Gobar gas waste slurry

ZAJHC

Chemically modified

orange peel

Orange peel

Banana pith

Biogas residual slurry

Coir pith carbon

ZAJHC

Procion

Orange

Rhodamine B

[23]

[24]

[25]

[26]

[27]

[28]

This work

[25]

[29]

[29]

[29]

[29]

This work

Table 5. Comparisons of Langmuir and Freundlich constants for adsorption capacity for various adsorbents from literature

*Not reported

the order: Freundlich < Langmuir < D-R (Table 4). Hence Freundlich isotherm fits most with the equilib-rium adsorption data for both PO and RB. Adsorption capacity values from Langmuir [Q ], Freundlich [k ] o f

and D-R [q ] isotherms for PO are found to be less m

than those of RB, which is due to the bulk structure of PO (higher molecular weight) compared to RB and PO also contains more sulphonate groups.

5. Effect of pH

Experiments were carried at different pH values varying from 2-11. The results show that the removal of PO is higher in acidic pH (pH = 2) (Fig. 4a). The solution pH affects both aqueous chemistry and sur-face binding sites of the adsorbent. Reactive dyes are known to ionize to a high degree in aqueous solutionsto form coloured anions due to the sulfonated groups in their structures. The three SO groups of PO are 3

easily dissociated and have negative charges in the aquatic environment. The higher uptakes obtained at very acidic pH can be attributed to the electrostatic interaction between the positively charged ZAJHC [pH , 6.8] and the negatively charged PO dye zpc

anions. When the pH of the system was increased, the number of negatively charged site increases and the number of positively charged site decreases. A nega-tively charged surface site on the ZAJHC does not favour the adsorption of dye anions due to the electro-

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static repulsion [30]. The percentage removal of RB at various pH values seems to be very close to each other (Fig. 4b). This indicates strong affinity of RB for ZAJHC. Simi-lar pH influence on removal was reported for adsorp-tion of RB onto jackfruit peel carbon [31]. However there was a small decreased removal at pH values < 3.7 (pKa of RB = 3.7) and a small increased removal at pH values > 10. At pH < 3.7, protonated RB is repelled by the positively charged adsorbent surface [pH , 6.8]. At pH > 10.0, transformation of the cati-zpc

+onic (RB ) form to zwitterionic form by deprotonation of the carboxyl group occurs. Dimerization of RB monomers is favoured. As a result, the amount of dye adsorbed on the AC decreased slightly with an increase in pH of the solution [32].

6. Intrapartical Diffusion

An empirically found functional relationship for intrapartical diffusion, common to the most adsorption

1/2processes, is that the uptake varies with t . According to Weber and Morris [33],

-1where q is the amount adsorbed (mg g ) at time, t t

(min) and k is the intra-particle diffusion rate con-id

stant. All the plots have the same general features: (i)

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(10)

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Fig. 3. Comparison of Langmuir, Freundlich and D-R isotherms for adsorption of (a) PO and (b) RB.

Fig. 4. (a) Effect of initial pH on adsorption of PO and (b) RB onto ZAJHC.

the initial curved portion is attributed to the bulk diffusion effect, (ii) the linear portion to the intrapar-ticle diffusion effect and (iii) the plateau to the equilib-rium. The linear portions of the plots do not pass through the origin indicating that intraparticle diffusion is not the only rate controlling step for adsorption process. According to Eq. 10, the slopes of the linear

1/2 portions of the plots of q vs t give the values of kt id

(Figs. 5a and 5b). Values of intercept give an idea about the thickness of boundary layer, i.e., larger the intercept the greater is the boundary layer effect. The linear portions are attributed to the instantaneous utilization of the most readily available adsorbing sites on the adsorbent surface.

7. FTIR Study

The FTIR spectra were recorded on pellets ob-tained by pressing mixture of 1 mg of the ZAJHC and 100 mg of dried KBr under pressure. The FTIR spec-trum of the ZAJHC shows weak and broad peaks in

-1 -1the region of 500-4000 cm . A broad band at 3424 cm is due to the O-H vibration of hydroxyl groups (Fig.

-1 6a). An intense band observed at 2923 cm for the sewage sludge precursor was attributed to the C-H stretching vibration, which disappeared for the ZnCl 2

AC due to the elimination of hydrogen to a large ex-tent. Also it was observed that the sharp bands at 1035

-1 cm for the sludge precursor shifted towards higher wave number for ZAJHC indicating some changes in the C-O-C group in carboxylic and alcoholic group [34]. An IR spectrum consists of two main regions: (i)

-1 There are absorption bands above 1500 cm that can be assigned to individual functional groups, whereas (ii)

-1 the region below 1500 cm (the fingerprint region) contains many bands which characterize the molecule as a whole. The bands within the fingerprint region, which arise from functional groups, can be used for identification, but such assignments should be consid-ered only an aid to identification and not as conclu-sive proof [35].

-1 For PO, a broad band at 3425 cm (OH group -1stretching) and bands at 2923 cm (=Ch with saturated 2

-1C-H stretching), 2846 cm (-O-CH with miscellaneous 3-1C-H stretching), and 1440 cm (N=N stretching) were

observed. Moreover, the IR spectrum of PO showed a -1 stronger band at 1440 cm of the azo group (-N=N-)

that contributed to the chromophoric group. The C=N group can be found in some reactive dyes. It may beoverlapped with the carbonyl compound and N-H bending in the IR spectrum. With reference to reactive dye, C=N often exists in a conjugated cyclic system.

-1For RB, a broad band at 3560 cm (H-bonded -OH -1with -O-H stretching) [36] and bands at 1048 cm (C-

-1O stretching vibration) [37] and 3680 cm (free OH oscillators) [38] were observed. They demonstrate the adsorption of PO and RB on to the surface of ZAJHC (Figs. 6b and 6c) [39].

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Fig. 5. Intrapartical diffusion plots for adsorption of (a) PO and (b) RB onto ZAJHC.

Fig. 6. FT-IR spectra of ZAJHC before (a) and after adsorption of PO (b) and RB (c).

8. Cost Benefit Analysis

The raw material for the carbon, namely, JH is disposed as waste in the bio-diesel production indus-tries and the ZAJHC developed from the agricultural waste material can be used for the economic removal of toxic ions, dyes and organics from waters. Approxi-mate calculations show that the cost of the ZAJHC

-1carbon is $0.5 kg , while that of the commercial -1carbon for dye removal is $3 kg [10].

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CONCLUSIONS

The present investigation showed ZAJHC can be effectively used as adsorbent for the removal of PO and RB. Adsorption reached equilibrium at 120 min. The equilibrium time is independent of initial dye con-centration. The equilibrium data were analyzed using Langmuir, Freundlich and D-R isotherms. Freundlich isotherm gave the best fit for PO and RB. Adsorption of PO and RB on ZAJHC obeyed pseudo second order kinetic model. As the raw material for the preparation of the AC is a waste material, the treatment process is expected to be economical. .

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Discussions of this paper may appear in the discus-sion section of a future issue. All discussions shouldbe submitted to the Editor-in-Chief within six monthsof publication. .

Manuscript Received: Revision Received:

and Accepted:

January 16, 2013May 23, 2013

July 2, 2013

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