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INTERNATIONAL JOURNAL OF ENVIRONMENTAL SCIENCES Volume 3, No 5, 2013

© Copyright by the authors - Licensee IPA- Under Creative Commons license 3.0

Research article ISSN 0976 – 4402

Received on January 2013 Published on April 2013 1711

Removal of basic dyes from aqueous solutions using mustard waste ash and

buffalo dung ash Harminder Singh, Samiksha, Sameena Roohi

Department of Chemistry, Lovely Professional University, Punjab 144402, India

[email protected]

doi: 10.6088/ijes.2013030500039

ABSTRACT

The ability of the low cost materials viz. mustard waste ash (MWA) and buffalo dung ash

(BDA) to remove two basic dyes, Methylene Blue (MB) and Crystal Violet (CV) in aqueous

solution, was studied by the method of batch mode adsorption process. Effect of contact time,

initial dye concentration (mg/L), adsorbent dosage (g/L) and pH was studied and results

showed that amount of the dye adsorbed increase with increase in all the parameters studied.

Data was fitted to Langmuir and Freundlich models and it showed that the both isotherm

fitted well to the adsorption data. The Langmuir adsorption capacity of the MWA was 245.76

mg/g and 1079 mg/g respectively for MB and CV whereas this value for BDA was found to

be 294.11 and 1063.38 for MB and CV respectively. Apart from this, adsorbents were

characterized by Electron Dispersion X-ray Spectroscopy (EDS) and Scanning Electron

Microscopy (SEM).

Keywords: Biowastes, buffalo dung, crystal violet, methylene blue, mustard waste, sorption.

1. Introduction

Pollution caused by textile industry is the major concern for the developing countries.

Considering both volume-discharged and effluent combustion, the wastewater from the

textile industry is rated as the most polluting among all industrial sectors. Dyes present even

in low concentrations are highly visible. They affect the photosynthetic activity of the aquatic

life due to the reduced light penetration. Hence, dyes disturbing biological process of the

aquatic life especially the photosynthesis activity (Gücek et al. 2005). Dyes may be

carcinogenic, mutagenic, or teratogenic. Additionally it may also cause severe damage to

human beings such as dysfunction of kidney, reproductive system, liver brain and central

nervous system. The dyes are generally resistant to environmental conditions like light, effect

of pH and microbial attack. The removal of dyes from industrial effluents in an economical

way is a growing concern these days. There are various methods for the removal of dyes

including sedimentation and flotation, membrane separation, coagulation and ion exchange.

The cost of operation is the main drawback of these techniques (Garg et al. 2003).

The adsorption process is an efficient method for the removal of dyes from the waste

effluents. It is preferred over other techniques due to its less initial cost, flexibility and

simplicity of design, ease of operation and insensitivity to toxic pollutants. Activated carbon

adsorption is one of the widely used techniques but because of the high cost and regeneration

problems, there has been a constant search and demand for potential low cost adsorbents. A

number of low-cost adsorbents such as neem leaves (Velmurugan et al. 2011), sphagnum

moss peat (Luisa et al. 2008), treated guava seeds (Joseph et al. 2007), gypsum (Rauf and

Bukallah 2009), palm kernal coat (Gimba et al. 2011), tamarind fruit shell powder and

Removal of Basic Dyes from Aqueous Solutions Using Mustard Waste Ash and Buffalo Dung Ash

Harminder Singh et al

International Journal of Environmental Sciences Volume 3 No.5, 2013 1712

almond tree bark powder (Patil et al. 2011), cucumber peel (Thirumalisamy and Subbain 2010),

waste sludge from biodiesel plant (Gottipati and Mishra 2010) have been employed for the

removal of basic dyes via adsorption. In the present study, the potential of two low cost bio-

sorbents, viz. buffalo dung ash (BDA), mustard waste ash (MWA) for the removal of

methylene blue and crystal violet from the aqueous solution is studied.

2. Materials and methods

2.1 Adsorbent preparation

The adsorbents used in this study are BDA and MWA, waste materials and abundantely

available in rural areas of India.

BDA: Buffalo dung cakes were collected from Rama Mandi, a town near Jalandhar (India)

and the cakes were burnt in Muffle furnace at a temperature of 500˚ C for three hours and

stored in air tight container for further use.

MWA: Mustard waste was collected from Jalandhar (India) and was burnt in muffle furnace

at 500˚ C for three hours and stored in air tight container for further use. Both the adsorbents

were sieved through an I.S.70 mesh screen (70 µm) prior to their use.

2.2 Surface characterisation

Surface morphology and chemical constitution of both the adsorbents were studied by

Scanning Electron Microscopy (SEM) (model: FEI Quanta 450 FEG) and Energy dispersive

X-ray spectroscopy (EDS).

2.3 Adsorption studies

A stock solution of both Methylene blue (MB) and Crystal violet (CV) were prepared by

dissolving 1 g of the respective dye in 1 L of the double distilled water (1000 mg/L)

separately. This solution was further used to make desired concentrations using double

distilled water. The pH adjustments were made using hydrochloric acid and sodium

hydroxide. Batch mode experimental studies were carried out with a known weight of the

adsorbent in 50 mL working solution of different concentration range (100-800 mg/L) in 100

mL conical flask with stoppers. Although this concentration range is much higher than the

dyes would be in most effluents, but high concentrations helped in minimizing the error in the

estimation of dyes spectrophotometrically. These flasks were kept in a thermostatic shaker

maintained at a temperature of 30oC and 200 rpm for sufficient time to achieve equilibrium.

After equilibration, the adsorbent was separated by filtration using Whatman’s paper no. 40

and the aqueous phase concentration of the dyes was analyzed using UV-VIS

spectrophotometer (Shimadzu-1800) by observing optical density at different wavelengths for

MB and CV respectively at 662 and 591 nm. The above mentioned process repeated to find

the effect of different adsorption parameters like adsorbent dose (0.1-0.5 g/50mL), pH (2-9),

contact time etc. by keeping all other parameters at a fixed value.

2.4 Adsorption isotherms




The adsorption isotherm is relatively simple method for determining the feasibility of using

an adsorbent for a particular application. It is a plot of the amount of adsorbate adsorbed per

unit weight of adsorbent (Qe) versus the equilibrium concentration of adsorbate (Ce).

The sorption equilibrium (Qe) uptake capacity in mg/g, for each sample is calculated

according to mass balance and is expressed as

Q e = Vm

CC eo

Where Co and Ce are initial and equilibrium concentrations of dyes respectively, m is the

mass of adsorbent and V is the volume of solution in litres (Krishnaiah et al. 2006).

Adsorption isotherms on different adsorbents are usually presented as Langmuir and

Freundlich isotherms. The former shows initial rapid adsorption tending to be almost constant

at higher concentrations.

The linear form of the Langmuir isotherm is represented as:

CebQQQe

1111

The plots of eQ

1and

Ce

1for both the dyes were drawn for the data obtained in this study.

From the slope and intercept, the values of constants Q and b can be calculated. Where Q

signifies the adsorption capacity (mg/g) and b signifies the energy of adsorption (L/mg).

An important characteristic of the Langmuir adsorption is expressed in terms of a

dimensionless separation factor RL (Namasivayam et al. 2001) and is defined as

RL = obC1

1

Where Co is the highest initial dye concentration (mg/L) and b is the Langmuir constant. This

parameter indicates the isotherm shape according to the adsorption characteristics:

RL > 1, the process is unfavourable

RL = 1, the process corresponds to linear

0 < RL > 1, Process is favourable

RL = 0, Irreversible process

The linearized Freundlich isotherm is given by

Log eQ = Log KF + n

1log Ce

Values of Log eQ and Log Ce were plotted for both the dyes separately. From the intercept

and slope the values of Freundlich constants KF and n can be calculated. The KF represents

adsorption capacity and n refers to the process intensity (Gupta and Ali 2000). This isotherm

is frequently used for the interpretation of adsorption from solutions because of its simplicity.

Generally, straight-line plots can be obtained by making use of the empirical Freundlich

equation.

3. Results and discussion

3.1 Characterization of adsorbents

3.1.1 Scanning electron microscopy




Surface morphology of adsorbents was analysed by scanning electron microscopy which

showed a clear view of the grains of the materials used as adsorbent in this study. Scanning

electron micrograph of MWA and BDA are shown in Fig. 1 a & b respectively. It is clear

from Fig. 1a that MWA has a rough and uneven surface having small pores which have

diameter in the range from 0.182 µm to 3.5µm. These pores can serve as adsorption sites for

the removal of dyes. On the other hand BDA has fibrous structure and having small pellet

which are distributed throughout and the size of these fibres varies from 1.66 µm to 52 µm.

Space between these fibres and pellets may serve as adsorption sites.

Figure 1 ((a), (b)): Scanning electron micrographs of MWA and BDA respectively

3.1.2 Energy dispersive X-ray spectroscopy (EDS)

The chemical constitution of both the adsorbents was studied by EDS. EDS spectra is shown

in figures 2 (a and b) for MWA and BDA respectively and elemental constitution is

represented in Table 1. It can be observed that carbon content was found to be more in MWA

(75.93) than BDA (55.57). Both the adsorbent have very different elemental constitution.




1 2 3 4 5 6 7 8 9

keV

0

2

4

6

8

10

12

14

16

18

cps/eV

C O K K

Ca

Ca

Mg Ir Ir Ir

Ir

S

S

1 2 3 4 5 6 7 8 9

keV

0

2

4

6

8

10

12

14

16

cps/eV

C O Si K K

Ca Ca

Cl

Cl

Mg

N Na

Figure 2 ((a), (b)): EDS Spectra of MWA and BDA respectively

Table 1: Characterization of MWA & BDA using EDS

S.No. Element

MWA BDA

Atomic

composition

(at. %)

Error

(wt. %)

Atomic

composition

(at. %)

Error

(wt. %)

1 C 75.93 8.7 55.57 4.4

2 O 22.01 4.2 15.70 1.2

3 K 0.47 0.1 4.02 0.3

4 Ca 0.36 0.1 1.22 0.1

5 Mg 0.20 0.1 1.03 0.1

6 S 0.85 0.1 - -

7 Ir 22.01 4.2 - -

8 Si - - 18.97 0.9

9 Cl - - 1.23 0.1

10 Na - - 0.95 0.1

11 N - - 1.30 0.2

3.2 Effect of contact time

For the evaluation of adsorption as a function of time, amount of dye adsorbed per gram (Qe)

and the percentage removal was calculated at regular intervals of 10 minutes until

equilibrium was achieved. The first phase was interpreted to be the instantaneous adsorption




stage or external surface adsorption. The plots of adsorption percentage versus time (Figure

3a and b) indicate that the adsorption become asymptotic to the time axis representing nearly

an equilibrium pattern. The equilibrium time for MB using both the adsorbents was found to

be 150 minutes whereas for CV it was 120 minutes and 140 minutes with BDA and MWA

respectively. For the further batch studies the equilibrium time was set to be three hours for

both the dyes.

Figure 3 ((a), (b)): Effect of contact time on the adsorption process for MB and CV

respectively. (Temperature = 30o ±1, adsorbent dose= 0.1g/mL, rotations per minute=200±1,

Concentration of dyes= 600 mg/L, pH=6.0 for MB and pH=6.5 for CV)

3.3 Effect of pH

pH is one of the most important factors in controlling the adsorption process. To evaluate the

effect of pH on the adsorption process, the adsorption of the dyes with pH values from 2-9

were studied keeping all other variables constant. It was observed after analyzing Fig. 4a & b

for methylene blue and crystal violet respectively that the amount of dye adsorbed per unit

weight of adsorbent (Qe) increased with increasing pH values. As the pH of the solution

increases, the surface charge density decreases and the electrostatic repulsions between the

adsorbent and the positively charged basic dyes is less, thereby increasing the extent of

adsorption. Similar results have been reported elsewhere (Patel and Vashi 2010).




Figure 4 ((a), (b)): Effect of pH on the amount of dyes adsorbed per unit weight (Qe) for the

two adsorbents for MB and CV respectively. (Temperature = 30o ±1, adsorbent dose=

0.1g/mL, rotations per minute=200±1, Concentration of dyes= 600 mg/L, equilibrium time =

3hrs).

3.4 Effect of adsorbent dose

The effect of adsorbent dose was studied by varying the amount of adsorbent dose from 0.1g

to 0.5g in 50 mL solution of both the dyes having 600 mg/L of initial concentration keeping

all other parameters at a constant value. The results are shown in figures 5a & b for the dyes

methylene blue and crystal violet respectively.




Figure 5 (a and b): Effect of adsorbent dose on the amount of dyes adsorbed per unit weight

(Qe) and % removal of dyes for the two adsorbents for MB and CV respectively.

(Temperature = 30o ±1, rotations per minute=200±1, Concentration of dyes= 600 mg/L,

equilibrium time = 3hrs pH=6.0 for MB and pH=6.5 for CV).

From obtained data it was observed that with increasing amount of adsorbent, percentage

adsorption also increases accordingly because maximum surface area is available for

adsorption which increases exchangeable number of sites on the surface of the adsorbent.

However, a decrease in the value of Qe was observed from 274.5 mg/g to 66.3 mg/g,

247.6mg/g to 58mg/g with BDA for MB and CV respectively and on the other side the

decrease was from 182 mg/g to 52.88 mg/g, 239.5 mg/g to 54 mg/g in the value of Qe when

MWA is used with MB and CV respectively. The decrease in the amount of dye adsorbed per

gram of the adsorbents (Qe) with increase in the adsorbent dose is mainly because of

unsaturation of adsorption sites through the adsorption process (Kovacevic et al. 2000).

3.5 Effect of initial concentration of adsorbate

The amount of dyes adsorbed per gram of the two adsorbents used in this study was observed

at different dye concentrations (100 – 800 mg/L). The result showed that the amount of dye

adsorbed per gram of adsorbent (Qe) increased and percentage removal of the dye decreased

(Fig 6a & b). It was observed that with the increase in concentration of adsorbate, percentage

removal decreases, as after some concentration there is less number of adsorbing sites

available for the dye adsorption on the surface of adsorbent. The reason is that during the

adsorption of dye initially the dye molecules rapidly reached the boundary layer by mass

transfer and then they slowly diffuse from boundary layer onto the adsorbent because many

of the available sites have been occupied, and they finally diffuse into the porous structure of

the adsorbent. On the other hand the value of Qe was observed to be increased from 48.63

mg/g to 344.9 mg/g, and 39.9 mg/g to 302.4 mg/g respectively for MB and CV using BDA.

For MWA value of Qe increased from 42.9 mg/g to 250.3 mg/g for MB and it increased from

37.2 mg/g to 286.9 mg/g for CV. When initial concentration of the dye is increased, it

contributes to the driving force to overcome mass transfer resistance of ions between the

adsorbent and bulk fluid phases thereby increasing the uptake of dye molecules. Not only this,

increase in the concentration of dyes also increases number of collisions between adsorbate

and the adsorbent which results in increase of the adsorption (Krishnaiah et al. 2006).




Figure 6 (a and b): Effect of initial dye concentration on the amount of dyes adsorbed per

unit weight (Qe) and % removal of dyes for the two adsorbents for MB and CV respectively.

(Temperature = 30o ±1, rotations per minute=200±1, adsorbent dose= 0.1g/mL, equilibrium

time = 3hrs pH=6.0 for MB and pH=6.5 for CV).

3.6 Adsorption isotherm

The adsorption data are usually described analyzed and modeled using an adsorption

isotherm. It relates the amount of dye adsorbed per unit weight of the adsorbent to the

equilibrium concentration of the bulk phase. Data obtained in the study was fitted to the

Langmuir (Figure 7a & b) and Freundlich models (Figure 8a & b) which are often used to

describe equilibrium adsorption isotherms. The results obtained from Langmuir and

Freundlich isotherms indicate the strong adsorption capacity of adsorbents for the dyes.

Adsorption constant for Langmuir isotherm (b and Q) and Freundlich isotherm (KF and n)

were calculated from slope and intercept and are given in Table 2 for both the dyes. Data

fitted very well to both the isotherm as indicated by the ‘R’ values in table 2. A special

parameter ‘RL’ was also calculated for the two adsorbents used in this study on both the dyes.




Figure 7 (a and b): Langmuir adsorption isotherm for the two adsorbents for MB and CV

respectively. (Temperature = 30o ±1, rotations per minute=200±1, adsorbent dose= 0.1g/mL,

equilibrium time = 3hrs pH=6.0 for MB and pH=6.5 for CV).

Figure 8 ((a), (b)): Freundlich adsorption isotherm for the two adsorbents for MB and CV

respectively. (Temperature = 30o ±1, rotations per minute=200±1, adsorbent dose= 0.1g/mL,

equilibrium time = 3hrs pH=6.0 for MB and pH=6.5 for CV). Table 2: Langmuir and

Freundlich constants

Langmuir and Freundlich constants for MB

Langmuir constants Freundlich constants

Parameter MWA BDA Parameter MWA BDA

Q (mg/g) 248.756 294.11 KF 9.537 28.8071

b (L/mg) 0.0142 0.0696 n 1.741 1.826

R 0.9906 0.980 R 0.9985 0.9916

SD 9.53 x 10-4

0.0013

SD 0.0148 0.0404

RL 0.081 0.0176 - - -

Langmuir and Freundlich constants for CV




Parameter MWA BDA Parameter MWA BDA

Q (mg/g) 1079.252 1063.382 KF (mg/g) 3.7480 2.083

b (L/mg) 0.001594 0.00188 n 1.2709 1.0421

R

0.95619 0.9846 R

0.967 0.986

SD 0.00244 0.0014 SD 0.0789 0.053

RL 0.44 0.6614 - - -

Its value for methylene blue was found to be 0.081 and 0.0176 for MWA and BDA

respectively whereas for crystal violet it was found to be 0.44 and 0.6614 respectively for

MWA and BDA. It is clear from these values that ‘RL’ is between 0 and 1, which indicates

that the adsorption process for these adsorbents was favourable. Table 3 a and b represents

adsorption capacities of various low cost adsorbents used for methylene blue and crystal

violet and it can be clearly observed that adsorbents used in this study have adsorption

capacities with the low cost absorbents reported in the literature. More over both these

adsorbents even outperformed in case of crystal violet dye adsorption.

Table 3 (a): Adsorption capacity of various adsorbents with MB

Adsorbent Name Qe (mg/g)

Sawdust (Ansari and Mosayebzadeh 2010)

19.41

Sawdust coated with polypyrole (Ansari and Mosayebzadeh 2010)

34.36

Gypsum (Rauf et al. 2009) 36

Palygorskite (Al-Futaisi et al. 2007) 50.8

Yellow Passion Fruit waste (Pavan et al. 2008) 44.7

Coffee hysks (Oliveira et al. 2008) 90

Waste from biodiesel plant (Gottipati and Mishra 2010) 40

Sargassum (Tahir et al. 2008)

145.55

Cucumber peel (Thirumalisamy and Subbaine, 2010) 46.73

Ulva lactuca (Tahir et al. 2008)

69.23

Rectorite (He et al. 2010) 81.2

Carbon prepared from Guava seeds (Joseph et al. 2007) 198.12

Ghassoul (Natural clay) (Elass et al. 2010) 290

MWA 248.756




BDA 294.11

Table 3 (b): Adsorption capacity of various adsorbents with CV

Adsorbent Name Qe (mg/g)

Jute fibre carbon (Porkodi and Vasanthkumar 2007) 27.99

Tamarind fruit shell powder (Patil et al. 2011) 142.85

Almond tree bark powder (Patil et al. 2011) 166.66

Mango leaf powder (Patil et al. 2011) 200

Mangrove plant leaf powder (Patil et al. 2011) 200

Teak tree bark powder (Patil et al. 2011) 200

Mangrove plant fruit powder (Patil et al. 2011) 250

carbon from Ricinus communis pericarp (Madhavakrishanan et al.

2009) 106.95

Activated carbon from sewage sludge(Graham et al. 2001) 68.13249

Activated carbon from coconut husk(Graham et al. 2001) 61.60483

Unexpanded perlite(Dogan and Alkan 2003) 3.30463

Expanded perlite(Dogan and Alkan 200 3) 1.142341

Bagasse fly ash(Mall et al. 2006) 26.23305

Activated carbon (PAAC)(Senthilkumaar et al. 2006) 60.74807

MCM-22(Wang et al. 2006) 48.95748

Palygorskite(Al-Futaisi et al. 2007) 57.93302

Raw sepiolite(Eren and Afsin 2007) 73.43622

Raw kaolin(Nandi et al. 2008 ) 44.87769

UNCAL BC(Monash et al. 2011) 48.95748

CAL BC(Monash et al. 2011) 40.49

BDA 1063.382

MWA 1079.252

4. Conclusion

Adsorption of two basic dyes methylene blue and crystal violet was investigated using two

low cost biowaste adsorbents, viz. MWA & BDA. Conclusion from this study can be

represented as follows

1. Surface morphology and surface particles size of the two adsorbents used in this study

were quite different from each other MWA has uneven surface with small pores

whereas BDA has fibrous character.

2. It was also concluded that pH of the solution has a marked effect on the adsorption

and adsorption increased with the increase in pH value.




3. It was found that adsorbent dose and initial concentration of dyes has a significant

effect on the adsorption of dyes.

4. Both Langmuir and Freundlich adsorption isotherm fitted well for the adsorbent.

Adsorption capacities were found to be 248.76 and 294.11 for MWA and BDA

respectively for methylene blue where as for crystal violet these values were found to

be 1079.25 and 1063.38 for MWA and BDA respectively.

5. It was also found that adsorption capacity of MWA & BDA were comparable to many

other low cost adsorbents reported in the literature. Therefore it can be concluded that

MWA and BDA can be used as adsorbents for the removal of cationic dyes.

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