ADSORPTION OF CONGO RED DYE USING COBALT FERRITE … · dyes from wastewater. Reactive blue 19 (RB...

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International Journal of Civil Engineering and Technology (IJCIET) Volume 9, Issue 9, September 2018, pp. 1335–1347, Article ID: IJCIET_09_09_129

Available online at http://www.iaeme.com/ijciet/issues.asp?JType=IJCIET&VType=9&IType=9

ISSN Print: 0976-6308 and ISSN Online: 0976-6316

© IAEME Publication Scopus Indexed

ADSORPTION OF CONGO RED DYE USING

COBALT FERRITE NANOPARTICLES

Dr. K.R. Aswin Sidhaarth

Associate Professor Department of Civil Engineering,

Veltech Dr Rangarajan Dr.Sagunthala R&D Institute of Science and Technology,

Avadi, Chennai – 62

Dr.J.Jeyanthi


Government College of Technology, Coimbatore – 13

S.Baskar

Assistant Professor, Department of Civil Engineering,


Avadi, Chennai – 62

Dr. M. Vinod Kumar



Avadi, Chennai – 62.

ABSTRACT

The present study involves the applicability of cobalt ferrite Nanoparticles as an

adsorbent for the removal of Congo red dye from the aqueous solution. The

Nanoparticles were synthesized by co-precipitation method. X-Ray diffraction and

Transmission electron microscope studies confirm the formation of single phase cobalt

ferrite nanoparticle showing the size range of 16-60nm. The scanning electron

microscope studies reveal that the structure were agglomerated. From the batch studies

the removal was 99.9% at the optimum conditions. Further the results were subjected

to isotherm and kinetic studies.

Keywords: Cobalt Ferrite Nanoparticles, X-Ray Diffraction, Transmission Electron

Microscope.

Cite this Article: Dr. K.R. Aswin Sidhaarth, Dr.J.Jeyanthi, S.Baskar and Dr. M. Vinod

Kumar, Adsorption of Congo Red Dye Using Cobalt Ferrite Nanoparticles,

International Journal of Civil Engineering and Technology, 9(9), 2018, pp. 1335–1347.

http://www.iaeme.com/IJCIET/issues.asp?JType=IJCIET&VType=9&IType=9

Dr. K.R. Aswin Sidhaarth, Dr.J.Jeyanthi, S.Baskar and Dr. M. Vinod Kumar


1. INTRODUCTION

Environment embraces a vast and varied field of observation and research. The current study

is a benign effort to deal with Congo red dye generated as industrial effluents discharged into

the environment. Textile industries consume the largest volumes of water and chemicals for

wet processing of textiles. Worldwide annual textile production is 30 million tons with

expected growth of 3% per annum [14]. Wastewater coming out from dyeing industry is one

of the major environmental problems due to its acute and chronic effects on organisms

depending upon the exposure time and dye concentration [16]. In this study among the various

dyes Congo red dye has been given prime importance regarding their removal from wastewater.

It is the sodium salt of benzidinediazo-bis-1-naphthylamine-4-sulfonic acid (formula:

C32H22N6Na2O6S2; molecular weight: 696.66g/mol). It is a secondary diazo dye. λmax = 497nm

[17]. It is a toxic to many organisms and is a suspected carcinogen and mutagen. Benzidine, a

human carcinogen, and CR are, however, banned in many countries because of health concerns.

But, it is still widely used in several countries. The adsorption process is especially suitable for

countries like India as it involves simple process control steps. Among the treatment

technologies discussed above in relation to removal of heavy metals and dyes, adsorption

technique has been taken into consideration in which incorporation of nanotechnology by

applying nanomaterials as adsorbents has been given prime importance in this research work.

2. LITERATURE REVIEW

2.1. Removal of Congo red dye using Nanoparticles: A detailed Citation

Abbas Afkhami et al. (2010) [3] studied the adsorption of Congo red (CR) onto maghemite

nanoparticles and its desorption was investigated. The maghemite nanoparticles were

synthesized using co-precipitation method. The synthesized nanoparticles were characterized

using Scanning electron microscopy and X-ray diffraction method. The characterization studies

showed that the crystallite size was 8.78nm, mean pore diameter of 10.37nm and the surface

area was found to be 81.61m2g-1. From the adsorption studies the maximum adsorption capacity

of maghemite Nanoparticles was found to be 208.33mg/g. The effect of contact time and pH

were given consideration. At 30 minutes and pH 5.9 maximum removal was observed. The

desorption studies was carried out in the alkaline range, 5ml of EtOH, DMF and 0.01molL-1

NaOH solutions were taken as eluents. The desorption efficiency for them was calculated as

4%, 13%, and 95% respectively.

Ghaedi et al. (2011) [9] investigated the applicability efficiency and performance of gold

nanoparticle loaded activated carbon (Au-NP-AC) adsorbent for the removal of (congo red)

from wastewater. The adsorption characteristics and dye removal efficiency of adsorbent have

been determined by investigating the influence of variables including pH, contact time,

concentration of the dye, amount of adsorbent and temperature. The nanoparticles were

prepared by one step reduction method. The TEM and SEM result revealed that the Au

nanoparticles were semi-spherical in shape and quite uniform size distribution in the range 20-

60nm. From the adsorption experiment it was observed that rapid uptake of 98% of Congo red

dye was observed at the initial period of contact of 15minutes. The same trend of order was

followed in the case of adsorbent dosage. The maximum removal was obtained at pH4 due to

the electrostatic phenomenon. From the temperature studies it was found that the process is

endothermic in nature also at higher concentration of congo red the removal efficiency reached

saturation level.

Gholamreza Moussavi et al. (2009) [10] focused on the preparation of MgO nanoparticles

and investigations into its efficiency as an adsorbent for the removal of azo and anthraquinone

Adsorption of Congo Red Dye Using Cobalt Ferrite Nanoparticles


dyes from wastewater. Reactive blue 19 (RB 19) and reactive red 198(RR 198) were taken as

models for azo and anthraquinone dyes, respectively, for removal investigation. The effect of

different variables, including dosage of MgO, concentration of dye, pH of the liquid and

reaction time, on removal of the two model dyes was evaluated. The magnesium oxide

nanoparticles was synthesized by the Sol-Gel method. From the SEM result it was found that

the size of MgO particles was found to range between 38 and 44nm. The results of the BET

method showed that the average specific surface area MgO nanoparticles was 103.5m2/g. The

dosage experiment revealed that 36 and 36.4% of RB 19 and RR 198 were removed at the

initial dosage of 0.05g, respectively. The pH experiment revealed that the removal of RB 19

increased from 86 to 100% when the pH was increased from 3 to 8. In case of RB198 the result

showed that the removal of RR198 was almost independent of pH and stayed higher than 99%

over the entire range of the experimental pHs. In the contact time experiment the removal

efficiency of RB 19 rapidly increased from 60% in the first minute of contact to 100% as the

stirring was increased to 5 minutes, when the equilibrium condition was attained. For RR 198,

the percentage of removal obtained in the first minute of stirring was 93% and complete

removal was attained when the stirring was continued to 5 minutes. The same trend of order

was followed in the concentration experiments. The maximum predicted adsorption capacities

were 166.7 and 123.5mg of dye per gram of adsorbent for RB19 and RR 198 respectively.

Lixia Wang et al. (2011) [18] compared the adsorption capacity of different MFe2O4

(M=Mn, Fe,Co, Ni) ferrite nanocrystals synthesized a by hydrothermal method for CR. It is the

first time to give a comprehensive comparison and analysis of the adsorption capacity of ferrite

nanocrystals with spinal structure for CR. Research indicates that the cations distribution of

MFe2O4 ferrites is the most important factor to decide their adsorption capacity. Electrostatic

absorption was conceived as the main adsorption mechanism. Meanwhile, the MFe2O4

nanoparticles exhibited a clearly ferromagnetic behaviour under applied magnetic field, which

allowed their high-efficient magnetic separation from wastewater. Furthermore, acetone is an

effective desorption agent for desorption of MFe2O4 nanoparticles loaded by CR. All of the

spinel ferrite nanocrystals possess good soft-magnetism, especially; CoFe2O4 nanocrystals

exhibit a higher saturation magnetization of 86.1 emu/g as well as the outstanding adsorption

capacity for CR. By the calculation of Langmuir isotherm model, the maximum adsorption

capacity of CoFe2O4 for CR is 244.5 mg g−1.

3. MATERIALS AND METHODS

3.1. Preparation of Congo red dye stock solution

The stock solution of 1000 ppm was prepared by dissolving 1 gram of congo red dye in 1 litre

of distilled water. The desired concentration for the adsorption study was prepared from the

stock solution.

3.2. Preparation of Cobalt Ferrite Nanoparticles

For the preparation of Cobalt ferrite Nanoparticles co-precipitation method has been adopted

in this work. This involves dissolving a salt precursor in water (or other solvent) to precipitate

the oxo hydroxide form with the help of a base. Very often, control of size and chemical

homogeneity in the case of mixed-metal oxides is difficult to achieve. However, the use of

surfactants, sonochemical methods, and high gravity reactive precipitation appear as novel and

viable alternatives to optimize the resulting solid morphological characteristics.



3.3. Characterization of Nanoparticles

The synthesized Cobalt Ferrite Nanoparticles were characterized using X-ray Diffraction

studies at PSG College of technology – Coimbatore (Schimadzu), for the determination of

crystallite size, microscopic analysis were performed using Scanning electron microscopy

(JSM-7600F) and Tunnelling electron microscopy (Philips CM200) at SAIF-IIT BOMBAY to

study the surface topography and also to determine the diffraction pattern and particle size. The

presence of Congo red dye was measured using Ultraviolet Spectrophotometer at their

characteristic detection limit wavelength of 400-500nm (Anna University, Regional Centre,

Coimbatore).

3.4. Adsorption studies -Batch Experiments

Batch adsorption experiments were carried out by mechanical agitation (agitation speed:

150rpm) at a temperature 30(±2)0C, where pre-determined quantities (50 ml) of desired

concentration of Congo red dye synthetic solution were agitated continuously with the known

weight of the Cobalt Ferrite Nanoparticles. After agitation, all sample solutions were filtered

through Whitman filter paper and, the filtrate was analyzed for Congo red using UV-

Spectroscopy.

4. RESULTS AND DISCUSSION

4.1. Synthesis of Cobalt Ferrite Nanoparticles

Cobalt ferrite Nanoparticles were synthesized by chemical precipitation method. 0.4M solution

of FeCl3 and 0.2M solution of CoCl2.6H2O were added together in a 100 ml beaker and it is

mixed vigorously using a magnetic stirrer. 3M NaOH solution was used as a pH stabilizer. It

is slowly added to the salt solution drop wise. NaOH solution was added until it reaches the

pH11 and the reactants were stirred vigorously for one hour. After an initial brown precipitate,

a black precipitate was formed. The precipitate was washed off several times by distilled water

to obtain pure and neutral pH and then with the ethanol until it shows pH7. The ferrofluid thus

formed was evaporated in oven at 1000C overnight. The CoFe2O4 nanoparticles thus formed

was weighed and stored in air tight containers.

4.2. Characterization of Cobalt ferrite Nanoparticles

The X ray diffraction studies showed that the final product is CoFe2O4 with the expected

inverse spinal structure. The reflection planes (311), (511), and (440) which confirm the

presence of single-phase in CoFe2O4 with a face centered cubic structure. And the same was

also reported in [19], and [20].

SEM analysis revealed that the CoFe2O4 nanoparticles have uniform, monodispersive

spherical structure morphology with a narrow size distribution of particles and they were also

found to be agglomerated. TEM analysis revealed that the structure of the nanoparticle was

agglomerated and gives a cloudy appearance in its alkaline condition. From the XRD and TEM

analysis the size of the nanoparticle was found to vary from 16 to 60nm.



Figure 1 XRD pattern of Cobalt Ferrite Nanoparticles

Figure 2 SEM Image of Cobalt Ferrite Nanoparticles

Figure 3 TEM Image of Cobalt Ferrite Nanoparticles



4.3. Batch Studies

4.3.1. Influence of Contact Time

0.05g of cobalt ferrite Nanoparticles was added into a 50ml of congo red dye solution with a

concentration of 50mg/L. The contact time was varied from 10 to 200 minutes at interval of 10

minutes. The maximum removal efficiency was found to be 97.84% at contact time of 130

minutes. Further batch studies were carried out at this contact time.

Figure 4 Effect of contact time on the removal of Congo red dye from synthetic wastewater using

cobalt ferrite nanoparticles

4.3.2. Influence of Adsorbent dosage

In this study it was observed that there was a rapid uptake in the initial stages and the removal

efficiency percentage reached to a maximum 99.9% and it was followed by a slight dip and a

gradual decrease. The background phenomenon was as the adsorbent dosage increased the

active adsorption vacant sites simultaneously increased which resulted in the increase in the

rate of attraction of Congo red dye towards cobalt ferrite Nanoparticles. The optimum dosage

was found to be 0.30g.

Figure 5 Effect of adsorbent dosage on the removal of Congo red dye from synthetic wastewater

using cobalt ferrite nanoparticles



4.3.3. Influence of pH of the Synthetic Solution

The rate of influence of pH was investigated in the operating range from pH2 to pH11. In this

study it was observed that the level of affinity was found to be on a higher scale in the acidic

range marked by a sudden increase in the removal efficiency and it was followed by a gradual

decrease as the hydrogen ion concentration in the solution shifted to alkaline range. Here the

governing rate of affinity was observed to be anionic adsorption rather than cationic adsorption.

The optimum pH was observed to be 4 exhibiting a removal efficiency of 99.0%.

Figure 6 Effect of hydrogen ion concentration on the removal of Congo red dye from synthetic

wastewater using cobalt ferrite nanoparticles

4.3.4. Influence of initial concentration of Congo red dye in the synthetic solution

The optimum concentration was found out by varying the concentration from 10mg/l to

100mg/l. It was observed that the Congo red dye adsorption efficiency gradually increased as

the concentration increased from 10 to 60 mg/l attaining a peak absorption efficiency of 98.3%

at a concentration of 60mg/l.

Figure 7 Effect of initial concentration on the removal of Congo red dye from synthetic wastewater

using cobalt ferrite nanoparticles



4.3.5. Effect of Agitation Speed

The rate of contact between the adsorbent and the adsorbate is an important governing

parameter for optimum removal. The experiment was carried out in the operating speed range

of about 50-2000rpm. From the experiment the optimum value of speed was found to be

150rpm.

Figure 8 Effect of Agitation Speed

Table1 Optimization of batch parameters for Congo Red dye removal using Cobalt Ferrite

Nanoparticles

SI.No Parameter Experimental

Range Optimized value

1. Contact time 0-200 minutes 130 minutes

2. Dosage of Adsorbent (Cobalt Ferrite

Nanoparticles) 0.01-0.50g 0.30g

3. pH of the Lead Aqueous Solution 2-12 4

4. Initial ion Concentration of Lead in the

solution 10-100mg/l 60mg/l

5 Agitation Speed 50-250rpm 150

4.4. Isotherm Studies

4.4.1. Langmuir Isotherm

Langmuir isotherm quantitatively the formation of a monolayer adsorbate on the outer surface

of the adsorbent, and after that no further adsorption takes place. Langmuir represented the

following equation:

0 0

1 1 1

e L eq Q Q K C= +

From the graph and calculations the isotherms of Congo red dye on cobalt ferrite

Nanoparticles was found to be linear over the whole concentration range studies. The

adsorptive capacity was found to be 13.88mg/g.



Figure 9 Langmuir isotherm for Congo red dye removal using Cobalt Ferrite Nanoparticles

4.4.2. Freundlich Isotherm

These data often fit the empirical equation proposed by Freundlich:

nefe CKQ

1

=

From the observation it was found that Freundlich is unsuitable model for interpreting

whole isotherm equation.

Figure 10 Freundlich isotherm for Congo red dye removal using Cobalt Ferrite Nanoparticles

4.4.3. Temkin Isotherm

The model is given by the following equation:

)ln( eTe CAb

RTq =

,

eT

T

T

e Cb

RA

b

RTq lnln

+=

, Tb

RTB =

,

eTe CBABq lnln +=

From the graph and calculations it was found that the temkin isotherm was not found to be

suitable.



Figure 11 Temkin isotherm for Congo red dye removal using Cobalt Ferrite Nanoparticles

Table 2 Isotherm constants for Congo red dye removal using Cobalt ferrite nanoparticles

Isotherms Constants R2 Range

Langmuir b = 0.875

qmax=13.88mg/g RL = 0.011 0.939 RL= 0 to 1

Freundlich n= 0.825 Kf = 4.613 0.908 1<n>10

Temkin A = 0.873 B = 23.51 0.839 B= 1 -50

4.5. Study of rate Constants

4.5.1. Pseudo First order Kinetic Model

The sorption kinetics may also be described by the pseudo first order reaction model, which is

expressed as

log (qe− q) = log qe− �

�.��

Here the experimental qe values were less than the calculated ones, qecal obtained from the

linear plots. Therefore pseudo first order kinetic model gave less fit to the sorption of Congo

red dye using cobalt ferrite Nanoparticles.

Figure 12 Pseudo First order kinetics for Congo red dye removal using Cobalt Ferrite Nanoparticles



4.5.2. Pseudo Second order Kinetic model

A pseudo second order reaction model may also be applicable to kinetics of sorption and the

equation for this reaction is

��

� = k(qe − q)2

The linear plot shows good agreement between experimental and calculated qe values.

Figure 13 Pseudo Second order kinetics for Congo red dye removal using Cobalt Ferrite

Nanoparticles

4.5.3. Intraparticle Diffusion Model

According to this theory, the intraparticle diffusion equation is expressed as follows:

CtKq difft +=2

1

Where diffK is the intraparticle diffusion rate constant (mg/gmin1/2) and C is the intercept.

If the mechanism of adsorption process follows the intraparticle diffusion, the plot of qt versus

t1/2 would be a straight line and diffK and C can be calculated from the slope of the plot. Values

of C give an idea about the thickness of boundary layer i.e., the larger the intercept the greater

the contribution of the surface sorption in the rate controlling step

Figure 14 Intraparticle diffusion kinetics for Congo red dye removal using Cobalt Ferrite

Nanoparticles



Table 3 Kinetic Constants for Congo red dye removal using cobalt ferrite nanoparticles

kinetics constants

pseudo first order qe = 16.150 mg/g

k = 0.011 g/mg-min

pseudo second order qe = 43.47 mg/g

k = 0.0088 g/mg-min

intra particle diffusion kid = 1.231min-1

ci=31.44

5. CONCLUSION

The prepared cobalt ferrite nanoparticles were subjected for the removal of colour from the

synthetic wastewater by considering congo red dye a contaminant of concern. The removal

efficiency of 98% was achieved at the optimum contact time of 130 minutes, adsorbent dosage

was found to be 0.10 g/50ml, the optimum pH and initial lead concentration was found to be 4

and 60 mg/ L respectively. And finally the optimum speed was found to be 150 rpm. Langmuir

and Temkin isotherms fitted well revealing that there is possible of homogenous multilayer

adsorption. Pseudo first and second order kinetics gave a very good fit among the kinetics

considered.

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