Removal of Colour (Direct Blue 199)

Removal of Colour (Direct Blue 199) from Carpet Industry Wastewater Using Different Biosorbents (Maize Cob, Citrus Peel and Rice Husk) Sudhakar Saroj, Satya Vir Singh & Devendra Mohan

Arabian Journal for Science and Engineering ISSN 1319-8025 Volume 40 Number 6 Arab J Sci Eng (2015) 40:1553-1564 DOI 10.1007/s13369-015-1630-0

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Author's personal copy Arab J Sci Eng (2015) 40:1553–1564 DOI 10.1007/s13369-015-1630-0

RESEARCH ARTICLE - CHEMICAL ENGINEERING

Removal of Colour (Direct Blue 199) from Carpet Industry Wastewater Using Different Biosorbents (Maize Cob, Citrus Peel and Rice Husk) Sudhakar Saroj1 · Satya Vir Singh1 · Devendra Mohan2

Received: 16 October 2014 / Accepted: 3 March 2015 / Published online: 26 March 2015 © King Fahd University of Petroleum & Minerals 2015

Abstract Direct Blue 199 is used to colour carpets. In this study, adsorbents prepared from maize cob, citrus peel and rice husk (agricultural wastes) were used to study removal of Direct Blue 199 from its aqueous solution and a carpet industry’s effluent. The adsorption equilibrium studies were carried out by varying the adsorbent dosage at a constant temperature of 28 ◦ C. Adsorption of the dye varied with different adsorbents. Equilibrium adsorption data were correlated using Langmuir isotherms for all the three adsorbents. Kinetic study showed that it took about 2 h for 80–90 % removal. Kinetic data for all the systems studied could be correlated satisfactorily by pseudo-second-order rate equation. It is confirmed by statistical t test (paired two samples for means) that the predicted and observed data were not significantly different statistically. The studies indicated that the adsorbents, maize cob, citrus peel and rice husk powders can be used as low-cost alternatives for the dye removal. Keywords Rice husk

Direct Blue 199 · Maize cob · Citrus peel ·

1 Introduction A large group of dyes and pigment are used in carpet and textile industries. About 10,000 types of dyes are used in

B

Satya Vir Singh [email protected]; [email protected]

1

Department of Chemical Engineering and Technology, Indian Institute of Technology IIT-BHU Varanasi, Banaras Hindu University Campus, Varanasi 221005, India

2

Department of Civil Engineering, Indian Institute of Technology IIT-BHU Varanasi, Banaras Hindu University Campus, Varanasi 221005, India

various industries like textile, carpet, food and pharmaceutical [1]. The trade in world market for Direct dyes and their preparations increased from 53,848 tonnes in 1992 to 1,81,998 tonnes in 2011 [2]. Water contaminated with residual dyes is ultimately discharged in nearby water bodies, and this causes ecological disturbances. Therefore, there is an urgent need for an advanced treatment of dye-contaminated water, for which primary and secondary treatments are found insufficient [3]. For treatment of dye-laden wastewaters, physico-chemical methods used are coagulation, electro-coagulation, flocculation, electro-flotation, precipitation, ion-exchange, membrane-filtration, irradiation and ozonation. To treat the wide range of dye-contaminated wastewaters, all these processes are relatively costlier. Bio-adsorbent, which are readily available and inexpensive, may be an attractive alternative for dye wastewater treatment. Activated carbon has widely been used for treatment of the wastewater due to its high adsorption properties, including the capacity for colour removal, but the manufacturing cost and its regeneration make it more expensive [4]. Consequently, removal of various dyes and many pollutants applying low-cost adsorbents have been studied by many investigators [5–16]. Most of the reported works are related to removal of colours on activated carbon obtained from various biosorbents such as rice husk for acid dye removal [17], groundnut shell for removal of Malachite green [18], sawdust for removal of Malachite green [10], pine saw dust for removal of Malachite green [19], Borassus bark for removal of Malachite green [20], pine needles biochar for removal of Reactive Black-5 [21] and orange peel for removal of basic dyes methylene blue and Rhodamine B [22], methylene blue [23], Direct Blue-86 and Direct Yellow 12 [24,25]. However, some work has been reported for adsorption on organic support adsorbents like dried biogas waste slurry for removal of Direct Red 12B [26] and duckweed powder for removal of

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methyl violet 2B [27]. The dyes such as Direct Red 23 and Direct Red 80 have been removed from wastewater using orange peel [28], removal of colour Direct Red 23 by biosorption on rice husk [29]. The maize cob has been used as biosorbent to adsorb Direct Blue 6 [30]. The acid-treated rice husk was used as adsorbent for removal of Reactive Red dye [31]. The crop residues like maize cob, rice husk and citrus peel may be effectively used as adsorbents for colour removal. These low-cost materials may serve as adsorbents with or without treatments. Objective of the present study was to assess the capability of rice husk, maize cob and citrus peel as economically attractive and efficient adsorbents for removal of Direct Blue 199 from dye-contaminated wastewaters. In most of the reported research works, simulated solutions of dyes have been used for the adsorption studies. In the present work, the simulated aqueous solutions as well as effluent collected from a carpet industry have been used to study adsorption of Direct Blue 199.

In all the three cases, the adsorbent materials were prepared into suitable sizes. Maize cobs were cut to small pieces of about 8 cm3 , citrus peels were cut to 2 × 2 cm2 pieces, and rice husk was taken as such. Each of these materials was washed with distilled water. Then, these were air-dried at 60 ± 5 ◦ C for 24 h. Subsequently, dried materials were powdered in crusher. The powders obtained were sieved, and the materials 40/60 mesh size were collected and used as adsorbents. The idea behind conducting studies on these adsorbents is that after use of these adsorbents for colour removal, the adsorbents along with the adsorbed dye can be briquetted and possibly burnt as a fuel to solve the problem of disposal. These may be burnt in boiler. The combustion products are likely to be CO2 , SO2 , H2 O and CuO which are non-toxic. However, in boiler, the chance of fumes escaping is negligible due to very high temperature and sufficient supply of air. The proximate analysis for fuel value is given in Table 1. 2.2 Chemicals Used

2 Materials and Methods 2.1 Materials For making simulated solution of dye, the Direct Blue -199 (Colour Index Number 74190, CAS Number 12222-04-7) was purchased from Jalil Dye and Chemicals, Godaulia, Varanasi, U.P., India, with purity of 99 %. It is a powder with blue appearance. Bhadohi, near Varanasi, is famous for carpet industries. Here, carpet yarns are coloured in various colours and shades. As informed by persons in the industry, for colouring carpet yarn in blue colour, Direct Blue 199 dye is preferred. Dyeing is commonly carried out in vats. So, the effluent was collected from such a vat after colouring the carpet yarn containing only Direct blue 199. 20 l effluent of Direct Blue 199 was collected from Champa Dyeing Industries Ltd., Bhadohi, UP, India, before the treatment process being applied. In the present work, studies are conducted to remove/reduce the dye (Direct Blue 199) from its solution as well as from the effluent obtained from the industry containing the same dye using adsorbents, dried powders of maize cob, citrus peel and rice husk after preliminary experimental confirmation that these adsorbents would work. In these experiments, the adsorbent powders in the range of 1–2 g were added to 100 ml (250 ppm concentration) dye solutions, and for comparison 100 ml solution was kept (as control) without adsorbent. It was observed that the dye concentration reduced appreciably in solution by the adsorbents in 24 h, when compared with the control. To confirm the cellulose presence which is mainly responsible for sorption activity of dye, the XRD analysis of all three adsorbents was also carried out.

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The chemicals used were sulphuric acid, manganese sulphate, silver sulphate, potassium permanganate, potassium iodide, potassium dichromate, potassium oxalate, ferrous ammonium sulphate, sodium thiosulphate and ferroin indicator in the experiments. All the chemicals were LR grade. For preparation of all the solutions, distilled water was used.

Table 1 Proximate analysis of adsorbents Adsorbent

Moisture content %

Volatile matter %

Ash content %

Fixed carbon %

Maize cob

0.567

4.767

5.431

89.235

Orange peel

0.802

4.266

5.001

89.931

Rice husk

0.106

4.314

5.444

90.136

Table 2 Characterization of effluent Testing parameters

Value of parameter (before treatment)

pH

7.6

Conductivity

846 milli Siemens (ms/m)

λmax

594 nm

BOD5 at 20 ◦ C

358 mg/l

COD

656 mg/l

Total dissolved solids

368 mg/l

Total suspended solid

240 mg/l

Temperature

30.1 ◦ C

Dye content

221 ppm

Appearance

Blue

The dye content was determined after filtration with filter paper. Other parameters were determined for effluent as obtained

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Fig. 1 XRD diagram of adsorbent powders a maize cob, b citrus peel and c rice husk

12.000

2.3 Effluent Characterization

System 2 System 4 System 6

8.000

qe (mg/g)

The effluent collected was characterized by determining the temperature using thermometer of least count 0.1 ◦ C, pH by an electronic pH meter and conductivity by electronic conductivity meter. Total dissolved solids (TDS), total suspended solids (TSS), biochemical oxygen demand (BOD) and chemical oxygen demand (COD) were determined by Standard Methods [32]. The concentration of unknown sample was determined from absorbance using a calibration curve drawn between absorbance vs. concentration for standard solutions at 594 nm.

System 1 System 3 System 5

10.000

6.000

4.000

2.000

0.000

0

50

100

150

200

250

Concentraon (ppm)

Fig. 2 Adsorption equilibrium study qe versus Ce for system 1–6

2.4 Adsorption Equilibrium and Kinetic Studies Equilibrium studies were carried out to determine the amount of adsorbate (Direct Blue 199), which can be adsorbed per unit weight of the adsorbents. Known amounts of adsorbents

were brought in contact with measured volumes of solution of predetermined concentrations and placed on shaker to reach equilibrium for 24 h. The concentration of dye solution was determined at equilibrium.

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Table 3 Values of Langmuir adsorption isotherm constants for all the systems studied System

a (l/g)

b (l/mg)

R 2 value of best fit line of the plot between 1/qe versus 1/Ce

1

0.086

5.313 × 10−3

0.940

16.187

2

0.054

4.362 × 10−3

0.954

12.379

3

0.095

5.114 × 10−3

0.935

18.576

4

0.085

6.729 × 10−3

0.971

12.632

0.020

2.044 × 10−3

0.992

9.784

0.017

1.987 × 10−3

0.968

8.555

5 6

qe max (a/b) mg/g

The kinetic studies were carried out to determine the rate at which the adsorption took place. A known volume of solution of already known concentration of the dye was put in

Fig. 3 a Adsorption kinetic study Ct versus t for dry maize cob powder and aqueous solution of dye (SYSTEM 1). b Regenerated curve Ct versus t for dry maize cob powder and aqueous solution of dye (SYSTEM 1)

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contact with the weighed adsorbent, the contents were well stirred, and samples of the solution were drawn at different time. Then, concentrations of dye in the drawn samples were determined. The amount of dye adsorbed on adsorbent was determined using mass balance in adsorption equilibrium and kinetic data, and it can be calculated using Eq. (1).

qt =

(Ci − Ct ) v w

(1)

where qt = concentration of adsorbate on the adsorbent at any time (mg/g); Ci = initial concentration of adsorbate in solution (mg/L); Ct = concentration of adsorbate in solution at any time (mg/L); v = volume of solution in litre; and w = weight of adsorbent used (g).


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Fig. 4 a Adsorption kinetic study Ct versus t for dry maize cob powder and effluent (SYSTEM 2). b Regenerated curve Ct versus t for dry maize cob powder and effluent (SYSTEM 2)

At equilibrium, qt = qe and Ct = Ce , where qe = equilibrium concentration of adsorbate on the adsorbent (mg/g) and Ce = equilibrium concentration of adsorbate in solution (mg/L). In the present case, the adsorption studies (equilibrium and kinetic) were carried out for six systems: maize cob powder and aqueous dye solution (System 1), maize cob powder and effluent obtained from the carpet industry (System 2), citrus peel powder and aqueous dye solution (System 3), citrus peel powder and effluent obtained from the carpet industry (System 4), rice husk powder and aqueous dye solution (System 5) and rice husk powder and effluent obtained from the carpet industry (System 6).

3 Results and Discussion 3.1 Characterization of Effluent and Adsorbents The characterization parameters related to effluent (as mentioned earlier) are shown in Table 2. The adsorbents’ characteristics were determined for moisture content, volatile matter, ash content and fixed carbon. The values are given in Table 1. XRD diagrams for all the three adsorbents are presented in Fig. 1. The XRD patterns of the adsorbents show main peaks at 2θ of 22, which is a typical spectrum of highly organized crystalline cellulosic material [33,34].

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Fig. 5 a Adsorption kinetic study Ct versus t for dry citrus peel and aqueous solution of dye (SYSTEM 3). b Regenerated curve Ct versus. t dry citrus peel and aqueous solution of dye (SYSTEM 3)

3.2 Adsorption Equilibrium and Kinetic Studies Adsorption equilibrium data (qe versus Ce ) for all the systems are shown in Fig. 2. The data could be correlated well using Langmuir adsorption isotherm for all the systems by the following Eq. (2). qe =

aCe 1 + bCe

(2)

The values of Ce and qe are in mg/L (ppm) and mg/g. The value of constants ‘a’ and ‘b’ for the correlating equation and R 2 values between ‘1/qe versus‘1/Ce ’ for Langmuir equation are presented in Table 3. The adsorption capacities for different system are presented in Table 3. From above data, it can be seen that in comparison with the synthetic solution,

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the adsorption is less from effluent. It may be due to the fact that effluent may have many other components, which may also compete for the sorption sites. Expressing the data in terms of percentage removal of dye, if initial condition is not given, is not a valid way because adsorptive removal by an adsorbent depends on initial concentration of dye, volume of solution and weight of adsorbent. However, most of researchers have reported value in percentage removal. The adsorption equilibrium data using untreated maize cob as adsorbent for removal of reactive dyes like Orange-16 [35], Direct Red 23 [36], Direct Orange 34 [36], Reactive Violet 2 [36] and Reactive Blue 19 [36] from their respective aqueous solution also followed the Langmuir isotherm.


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Fig. 6 a Adsorption kinetic study Ct versus t for dry citrus peel and effluent (SYSTEM 4). b Regenerated curve Ct versus t for dry citrus peel and effluent (SYSTEM 4)

Removal of Malachite green, Congo red and methyl red by maize cob from their respective aqueous solutions follows the Freundlich isotherm [37]. Present adsorption equilibrium data follow the Langmuir isotherm with adsorption capacities from aqueous solution being 16.2 mg/g and from the effluent 12.7 mg/g. With activated carbon obtained from citrus peel, the removal of dye Direct Blue 86 from its aqueous solution was 96 % and it followed the Langmuir isotherm with adsorption capacity of 33.78 mg/g [24]. Removal of Direct Yellow 12 from its aqueous solution by activated carbon derived from orange peel followed the Langmuir isotherm with adsorption capacity of 75.76 mg/g [25]. Treatment of aqueous solution of Direct Red 23 and Direct Red 80 by orange peel followed the Langmuir isotherm with 92 and 91 % removal, respectively, of the dyes at pH 2 [28]. Orange peel was also used

to remove Congo red, Procion orange and Rhodamine B. The equilibrium data were fitted to both Langmuir and Freundlich isotherms, and adsorption capacities of dye on orange peel were 22.4, 1.3 and 3.22 mg/g, respectively, [38]. In the present case, the removal of Direct Blue 199 with citrus (Kinnow) peel powder followed the Langmuir isotherm. The dye sorption capacity of adsorbent from aqueous solution was 18.6 mg/g and from effluent, 12.6 mg/g. This is relatively less, much about one-fourth of the adsorption capacity of citrus peel-based activated carbon applied for Direct Yellow dye. This is because the activated carbon had much higher surface area per unit mass in comparison with the citrus peel powder. The capacity of adsorbent derived from rice husk-activated carbon for removal of Direct Red 23 from its aqueous solution has been reported to be 13 mg/g of dry rice husk [29]. Activated rice husk treated with phosphoric acid was used to

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Fig. 7 a Adsorption kinetic study Ct versus t for dry rice husk powder and aqueous solution of dye (SYSTEM 5). b Regenerated curve Ct versus t for dry rice husk powder and aqueous solution of dye (SYSTEM 5)

treat the Acid Yellow and Acid Blue and showed the kinetic process fit in the Langmuir adsorption isotherm [17]. Aqueous solution of reactive dye showed 96.33–95.63 % removal, when it was adsorbed on nitric acid-treated rice husk [31]. In this case, capacity of rice husk powder for removal of Direct Blue 199 from its aqueous solution is 9.8 mg/g and from effluent, 8.6 mg/g. The values are almost comparable to the adsorption capacity values in case of rice husk- based activated carbon obtained for Direct Red 23. To investigate kinetics of the adsorption process, two kinetic models have been used. For correlating the data, pseudo-first-order Lagergren [39] kinetic model was tried, but data could not be fitted with the model for any of the systems studied. Then, pseudo- second-order kinetic model [40] was applied for which the equation is given below (Eq. 3). dqt = ks (qe − qt )2 dt

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(3)

where ks is pseudo-second-order rate constant (g/mg/min). When Eq. (3) is integrated, the following Eq. (4) is obtained. t 1 1 = + t qt ks qe2 qe

(4)

When t/qt versus t graph is drawn, it gives a straight line. Intercept of the line is equal to 1/ks qe2 and the slope, equal to 1/qe . From these values, value of ks was calculated. Figure 3 shows observed Ct versus t and generated Ct versus t graph for system 1. For systems 2, 3, 4, 5 and 6, the Ct versus t and generated Ct versus t graphs are shown in Figs. 4, 5, 6, 7 and 8. The values of R 2 , rate constant (ks ) and qe were calculated for all the experimental runs for all the systems, and these values are given in Table 4. The average values of ks for the systems 1, 2, 3, 4, 5 and 6 are 0.0081, 0.0088, 0.0122, 0.0109, 0.0093 and 0.0205 (g/mg/min), respectively. For any system, the value of ks must be unique. These average values of ks were used to regenerate the data for Ct versus T .


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Fig. 8 a Adsorption kinetic study Ct versus t for dry rice husk powder and effluent (SYSTEM 6). b Regenerated curve Ct versus t for dry rice husk powder and effluent (SYSTEM 6)

Adsorption of Reactive Orange-16 [35] and Malachite green [41] from their respective aqueous solutions also followed the pseudo-second-order kinetics, when treated by maize cob. In the present study, adsorption on maize cob from both aqueous solution of dye and effluent was observed to follow the second-order kinetics. The adsorption of Direct Blue 86 [24] and Direct Yellow 12 [25] from their respective aqueous solutions on citrus peel- based activated carbon followed the pseudo-secondorder kinetics. Adsorption process on Direct Red 23 [28] and Direct Red 80 [28] on untreated orange peel from their aqueous solutions followed the pseudo-second-order kinetics. In the present study, removal of Direct Blue 199 with citrus (Kinnow) peel powder also followed the pseudo-secondorder kinetics. Rice husk-based activated carbon for removal of Direct Red 23 from its aqueous solution followed the first-order

Table 4 Value of parameters ks and qt for different systems ks (g mg−1 min−1 )

qe cal (mg/g)

R2

1st (2g)

0.0028

15.625

0.989

2nd (4g)

0.0113

10.75

0.993

3rd (6g)

0.011

8.13

0.993

4th (8g)

0.0072

7.633

0.994

1st (2g)

0.005

7.75

0.995

2nd (4g)

0.005

6.024

0.979

3rd (6g)

0.009

5.181

0.993

4th (8g)

0.0165

4.386

0.992

1st (2g)

0.0078

11.341

0.993

2nd (4g)

0.0221

9.434

0.991

Run System 1

System 2

System 3

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Table 4 continued (g mg−1 min−1 )

qe cal (mg/g)

R2

Run

ks

3rd (6g)

0.0087

8.197

0.900

4th (8)

0.0103

7.246

0.991

1st (2g)

0.007

8.196

0.989

2nd (4g)

0.008

6.494

0.991

3rd (6g)

0.0148

4.785

0.993

4th (8)

0.0138

4.08

0.994

1st (2g)

0.0042

8.0

0.980

2nd (4g)

0.0049

5.376

0.979

3rd (6g)

0.0119

4.115

0.990

1st (2g)

0.0045

6.410

0.980

2nd (4g)

0.0108

4.524

0.991

4th (8)

0.0260

2.840

0.993

System 4

System 5

System 6

pseudo-second-order kinetics. Different kind of observations may due to differences in the adsorbate–adsorbent system. The generated (calculated) data are shown in smooth curve for system 1 in Fig. 3b. When predicted data vs. experimental data graph is drawn, slope of line passing through origin is near to 1.0. When the generated and experimental data obtained from each run of every system were subjected to t test (paired two samples for means) for significance of mean difference paired observation at 5 % level of significance, it was found that the values of t Stat were less than with tCritical. These data are summarized in Table 5. In case of all the systems, differences in the values predicted and the observed kinetic data were found to be non-significant (NS) for all the experimental runs. This means that concentration values could be reasonably predicted with time from adsorption equilibrium isotherm and the initially known conditions like those related to the adsorbent dosage, concentration of the dye in solution/effluent and volume of solution.

4 Conclusions kinetics [29]. Activated rice husk with phosphoric acid was used to treat the Acid Yellow and Acid Blue, which followed the first-order kinetics [17]. In the present case, removal of dye Direct Blue 199 with rice husk powder followed the Table 5 Statistical analysis of predicted (calculated) and experimental data

System

Run

Slope Ct Cal. versus Ct Exp.

R2

Degree of freedom (df)

t critical

1

1

0.9187

0.871

12

2.179

2

0.9376

0.967

12

3

0.9656

0.967

12

4

0.9676

0.996

1

0.9645

2 3

2

3

4

5

6

t Cal.

Inference

1.438

NS

2.179

1.644

NS

2.179

0.482

NS

12

2.179

1.178

NS

0.963

12

2.179

1.268

NS

0.9265

0.925

12

2.179

1.465

NS

0.9567

0.953

12

2.179

0.939

NS

4

0.9359

0.935

12

2.179

1.807

NS

1

0.9587

0.950

12

2.179

0.166

NS

2

0.8786

0.874

12

2.179

0.413

NS

3

0.9147

0.910

12

2.179

0.097

NS

4

0.9058

0.907

12

2.179

0.125

NS

1

0.9837

0.932

12

2.179

0.036

NS

2

0.9754

0.970

12

2.179

0.084

NS

3

0.9561

0.953

12

2.179

0.128

NS

4

0.9357

0.932

12

2.179

0.910

NS

1

0.9266

0.921

12

2.179

5.211

NS

2

0.9398

0.937

12

2.179

4.516

NS

3

0.8849

0.887

12

2.179

8.189

1

0.9430

0.973

12

2.179

2

0.9630

0.963

12

2.179

6.689

NS

3

0.9640

0.964

12

2.179

2.346

NS

NS not significant, S significant

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The present study shows that a non-conventional agro-wastebased biomaterials such as powdered dry maize cob, citrus peel and rice husk can be used effectively as adsorbents

10.52

NS NS


for removal of Direct Blue 199 from the effluent as well as simulated solution. The equilibrium data were correlated by Langmuir isotherm for maize cob, citrus peel and rice husk powders. Dye removal by these adsorbents was in the range 60–90 % in the experimental conditions. By maize cob powder, it was the maximum 90 %. However, the amounts of dye uptake (mg/g) at equilibrium (qe ) decreased with increasing adsorbent dosage. From the kinetic data, it was evident that more than 90 % adsorption took place within the first two hours. The kinetic data for all the systems studied could be correlated quite well by pseudo-second-order rate equation. It was confirmed also by statistical t test (paired two samples for means) of predicted and observed data, which were not significantly different statistically. Maize cob, citrus peel and rice husk are relatively inexpensive and locally available materials, and this study showed that these can be effectively used as alternatives of costly adsorbents applied earlier for dye removal in wastewater treatment processes.

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