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© 2019 JETIR February 2019, Volume 6, Issue 2 www.jetir.org (ISSN-2349-5162)

JETIRAB06067 Journal of Emerging Technologies and Innovative Research (JETIR) www.jetir.org 381

RHODAMINE 6G REMOVAL USING PROSOPIS SPICIGERA L. WOOD(PSLW)CARBON-IRON

OXIDE COMPOSITE

[1]R. Dhana Ramalakshmi,[2] V. Jeyabal,[3]M. Murugan

[1]Reg.No: 12583, Department of Chemistry, Rani Anna Government College for Women, Tirunelveli-627008,Research centre (St. Xavier's College, Tirunelveli-627002), affiliation of Manonmaniam

Sundaranar University, Abishekapatti, Tirunelveli-627012, Tamil Nadu, India. [2]Associate professor, Department of Chemistry, St. Xavier's College, Palayamkottai,Tirunelveli-

627002, Tamil Nadu, India. [3]Associate professor, Department of Chemistry, Sri K.G.S. Arts College, Srivaikuntam-628619,

Thoothukudi, Tamil Nadu, India. mail:[1][email protected], [2][email protected], [3][email protected]

Abstract:

Rhodamine 6G, a cationic dye is used to dyeing silk, cotton, wool, baste fiber, paper, leather, and

plastic. It is toxic and carcinogenic in nature. Hence it is essential to remove Rhodamine 6G from dyeing

industrial discharge and contaminated drinking water resources. In this present work, a waste plant

material Prosopis spicigera L.wood is carbonised (by natural process) and its composite with iron oxide,

is used for the removal of Rhodamine 6G from aqueous solutions by batch and column methods. The

PSLW carbon-iron oxide compositeis characterized by FTIR for functional group, scanning electron

microscope for surface morphology and potentiometric titration for pHzpc. Batch experiments have

been carried out to investigate the influence of sorption parameters such as initial dye concentration,

pH, contact time, in the presence of other ions and temperature on the removal of Rhodamine 6G. The

batch experiments were carried out at pH 6.0. The adsorption equilibrium fits Langmuir isotherm. The

kinetic data follows pseudo second order model. The thermodynamic study indicated that the

adsorption of dye is spontaneous and endothermic in nature. In order to apply this process to industrial

and domestic applications, column analysis was performed. Column data was analysed using Thomas

model.

Keywords: Adsorption, Kinetics, PSLW carbon, Langmuir Isotherm, Rhodamine 6G,Thomas model. Introduction

Dyes are colored compounds which are widely used in textiles, printing, cosmetics, plastics,

rubber and leather industries. These industrial effluents contain a large amount of colored wastewater

and pollute the environment. The usage of natural dye which is isolated from natural materials is limited.

The discovery of synthetic dyes and its wide range of uses such as fastness and brightness produce a

massive industrial effluents[1]. However, synthetic dyes have toxic behavior and adverse effect.

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The presence of dyes or their degradation products in water even at low concentration can cause

human health disorders like nausea, haemorrhage, ulceration of the skin, damage kidneys,

reproductive system, liver,brain and central nervous system[2]. It is difficult to remove these dyes using

conventional water treatment method because they are designed to have high water solubility [3]. Many

physical, chemical and biological methods are available for the removal of dye from aqueous system.

Among various physical methods, adsorption is one of the best method to successively remove them.

In sorption technique, adsorbents have a prominent role. The common adsorbents like activated

carbon, peat, wood, fly ash, coal and silica are used. Activated carbons are most widely used to remove

pollutants from aqueous solutions due to their high surface area, adsorption capacity and easily

availability. The adsorption capacity of activated carbon stillcan be increased by modifying the surface

of carbon. One such process is composite formation with iron metal oxides. The magnetic particle

technology have received more attention to solve the environmental problems[4]. Compared to other

adsorbents, the magnetic composites are good adsorbents because of their large surface area, high

adsorption capacity and after adsorption, it can be easily separated from the medium by a simple

magnetic process. In our present study, a low-cost adsorbent i.e., Prosopis spicigera L. wood (PSLW)

carbon and its iron oxide composite which is used for Rhodamine 6G removal. The effect of pH, contact

time, initial concentration, adsorbent dosage, presence of other ions and temperature of Rhodamine

6G solution on PSLW carbon-iron oxide composite were examined. The equilibrium and kinetic data of

the adsorption process were then analyzed to study the adsorption isotherms, kinetics and

thermodynamic parameters.

MATERIALS AND METHODS

Materials

PSLW plant material used in the present work was collected from the dry land area of

Palayamkottai in Tirunelveli district, Tamilnadu state, India. The branch and roots of the plant were cut

into pieces and piled up on a firing hearth. Before firing, the heaped wood pieces were enclosed by

fresh plantain pith and the whole mass was covered and plastered with layers of wet clay. This

arrangement prevented the direct entry of air into wood pieces and hence prohibited burning of wood

and its becoming ash. After 48 h of continuous firing and subsequent natural cooling, the activated

carbon was obtained. After removing the non-carbonaceous materials the carbon was isolated,

crushed and sieved to 75 micron particles. The composite adsorbent was prepared using the slightly

modified literature procedure [5],[6]. 20 g of PSLW carbon was suspended in 400 mlof FeCl3(7.8 g, 28

mmol) and FeSO4 (3.9 g, 14 mmol) at 70℃. The above solution was stirred well using a magnetic stirrer

for 3 hours. Sodium hydroxide solution (100 ml, 5 mol/L) was added dropwise to precipitate the iron

oxides. Again the stirring was continued for another two hours at 70℃. Later the solid material was




separated, washed with de-ionised water until the washings became neutral. Further the washings

were tested for iron with 1:10 phenonthroline for reddish color or precipitates. The final productwas

dried in an air oven at 100℃ for 8 hours and finally stored in air tight containers.

Characterisation of the adsorbent

The standard procedure [7], [8] was adopted to study the characteristics of PSLW carbon-iron

oxide composites.Surface functional groups and surface morphology of these adsorbent have been

analysed using FT-IR (JASCO FT/IR-4700 type A) and SEMrespectively. The morphological studies

SEM was performed on Jeol, JSM 6390, Oxford instruments, UK. Potentiometric titration with

acid/alkali was made to determine the zero point charge [9].

Batch Adsorption studies

The stock solution was prepared by dissolving 1 g of Rh 6G in 1000 mL of distilled water. The

stock solution was diluted with distilled water for further experimental studies. A digital pH meter with

glass electrode model (Roy instruments RI 501) was used for the measurement of pH of the dye

solution. The initial pH of the solution was varied (1-10) using 0.1 M NaOH or 0.1 M H2SO4 solutions.

Batch adsorption studies were carried out in 10 ml of dye solution. After adsorption, the solution was

centrifuged and absorbance was measured at 524 nm using UV–Visible spectrophotometer. The batch

experiments were studied to determine the effect of pH (1-10), initial concentration (10, 15 and 20

mg/L), contact time (5-150 min), in the presence of other ions (chloride, carbonate, nitrate and sulphate

ions) and temperature (20–50°C).

The amount of adsorbate adsorbed at equilibrium, qe (mg/g) was calculated as:

WVCCq ee (1)

Where, Co and Ce (mg/L) are the initial and equilibrium concentration of adsorbate respectively. V is

the volume of the solution (L) and W is the mass of adsorbent (g).

Column study

In column study, 5 g of PSLW carbon-iron oxide composite was packed in a glass column (2.5

cm diameter and 48 cm height) for a bed height of 3.5 cm. The dye solution was dropped into the

column at a rate of 2 mL/min from a separatory funnel fixed at a height of 1 meter. Effluents were

collected at regular intervals and analysed.

Results and Discussion

Characterisation of adsorbent




The FTIR spectrum of PSLW carbon and its iron composite (Fig. 2) show that both of their

surface have very few bands with very weak intensities. This indicates the presence of meagre amount

of acidic and basic groups on their surface. Further the composite formation has little interaction with

the surface functional groups. SEM study is used to understand the changes of morphological features

during adsorption process. The comparative study of SEM images of free PSLW carbon and PSLW

carbon-iron composite (Fig. 3) reveals that the PSLW carbon powder has irregularly shaped particles

with porous structure whose size is further reduced in the composites. Further a coating of white

patches of iron oxide is seen on the surface of the PSLW carbon.

Fig. 1 structure of Rhodamine 6GFig.2 The FTIR spectrum of (a) pure PSLW carbon

(b) PSLW carbon-iron oxide composite (c) Rh 6G loaded carbon

4000 3600 3200 2800 2400 2000 1600 1200 800 400

(c)

(b)

(a)

Tran

sm

itta

nce (

%)

Wave number (cm-1)




Fig.3 SEM images of (a) pure PSLW carbon (b) PSLW carbon-iron oxide composite (c) Rh 6G loaded

carbon

Effect of pH

The adsorbate and the surface charge of the adsorbent in aqueous solution are pH dependent,

which makes pH be one of the most important factors affecting dye

Fig. 4 Effect of pH Fig. 5 Effect of initial concentrations and contact time

adsorption ontothe adsorbent [10].Fig.4 shows, the removal of dye which increases with increase in

pH and maximum sorption is noted above pH = 8.0. The maximum adsorption above pH = 8.0 may be

due to electrostatic attraction between adsorbent and dye molecule [11], [12].The pHzpc of the

composite is 8.22 and it reveals that the surface of the adsorbent is positively charged. Therefore the

adsorption of Rhodamine 6G cationic dye on the PSLW carbon-iron oxide composite above pH=8.0

may be due to electrostatic interaction. But the desorption study with 0.1 N NaOH shows 90.5 % of the

Rhodamine 6G dye is desorped. Therefore the adsorption may involve weak interaction between the

dye molecule and the composite. This is evident from the IR spectral study. In the IR spectrum there

is no shift in the stretching frequencies of the PSLW carbon composite (Fig. 2c) and the spectrum is

only due to the adsorbed Rhodamine 6G molecule. Further SEM analysis after adsorption of

Rhodamine 6G onto the composite (Fig. 3c) shows the presence of aggregated larger size particles

0 2 4 6 8 10

0

2

4

6

8

10

12

14

16

Adsorbent dose 0.5 g/L

Concentration 50 mg/L

pH 1-10

Am

ount

adso

rbed

(m

g/g

)

pH

0 20 40 60 80 100 120 140 160

0

4

8

12

16

20

3

2

1


pH 6

Concentration of Rh 6G

1. 10 mg/L

2. 15 mg/L

3. 20 mg/L

q (

mg/g

)

Time (min)




with filled pores. This indicates the asorption of Rhodamine 6G molecule onto the composites. But as

an optium pH=6.0 is maintained throughout the adsorption study to apply this process to treat polluted

drinking water.

Effect of initial concentration and contact time

Fig.5shows the effect of initial concentration and contact time. The sorption process increases

with increase in contact time and attains equilibrium in 150 minutes. The maximum adsorption capacity

at three differentconcentrations of 10, 15 and 20 mg/Lare found to be 11.6, 16.4 and 18.3 mg/g

respectively for an adsorbent dose 0.5 g/L.

Effect of Temperature

Fig.6 depicts that the adsorption capacity of adsorbentincreases with increase in temperature

due to increase in dye mobility that may occur at high temperature between the adsorbent and the

adsorbate [13]. This indicates that the adsorption of dye is an endothermic process [14].

Fig. 6 Effect of temperature

Adsorption of dye in the presence of other ions

Adsorption capacity of PSLW carbon-iron oxide composite of the dye was examined in the

presence of mixture of chloride, carbonate, nitrate and sulphate ions of concentration 0.001 M each.

The adsorption capacity increases with time and equilibrium is reached at 60 min which is similar to

that of adsorption of dye in the absence of above ions. But the adsorption capacity decreases and this

may be due to competition between the ions and dye molecules for the same number of adsorption

sites.

Thermodynamic behavior

0 30 60 90 120 150

0

4

8

12

16

4

3

2

1


pH 6

Concentration of Rh 6G 10 mg/L

1. 20

o C

2. 30o C

3. 40o C

4. 50o C

q (

mg

/g)

Time (min)




The thermodynamic parameters, standard free energy (∆G°), standard enthalpy (∆H°)and

standard entropy (∆S°) were calculated using equations (2), (3)and (4).

kRTG ln (2)

RTHRSk ln (3)

STHG (4) where, T is

the temperature (K), R is the gas constant (8.314 J/mol k) and K is the equilibrium constant. A plot of

ln k versus l/T gives a straight line with slope ∆H°and intercept ∆S°.The values of the thermodynamic

parameters are listed in table I. The negative value of ∆G° which indicates the adsorption of dye on

PSLW carbon-iron oxide composite is a spontaneous process. The positive value of ∆H° shows the

adsorption process is endothermic. This reveals that the adsorption capacity increases with increase

in temperature. The ∆S° value increases with temperature, which indicates the randomness of

adsorption of dye on adsorbent surface. From thermodynamic parameters, the adsorption process is

spontaneous and endothermic [15], [16]. Thus, temperature plays a vital role in adsorption of dye on

PSLW carbon-iron oxide composite.

I. Thermodynamic parameters: Adsorbent dose 0.5 g/L

Isotherm Analysis

Adsorption isotherm is used to predict the mechanism of sorption process. The adsorption

capacity of the adsorbent was examined by Langmuir[17] and Freundlich[18] models. Langmuir and

Freundlich models are expressed by equations (5)and (6)

QCbQqC ee 1 (5)

ef CnKq log1loglog (6)

Temperature

(K)

- ∆G°

(KJ/mol)

∆H°

(KJ/mol)

∆S°

(KJ/mol K)

293

120.34

512.14

2.16

303

313

115.88

164.46

2.07

2.16

323 172.40 2.12




where Ce is the equilibrium concentration of the adsorbate (mg/L), q is the amount of dye adsorbed at

equilibrium (mg/g), Qo and b are the Langmuir constants which represents the maximum monolayer

adsorption capacity and energy of adsorption respectively.Kf and 1/n are Freundlich constants related

to adsorption capacity and adsorption intensity respectively. Fig. 7 shows the linear plot Ce/q versus

Ceat different initial concentration and temperature. The slope and intercept of the plot gives the values

of Qo and b respectively. The adsorption process follows Langmuir isotherm and not Freundlich

isotherm.

Fig.7 Langmuir plot ofRh 6G adsorption at different concentrations and temperatures

The essential characteristics of the Langmuir isotherm can be described by the dimensionless

separation factor RL[19] calculated using equation (7).

bCRL 11 …. (7)

The values of Qo, b and RL are tabulated in table II. The observed values of RL lie between zero to one,

which establish the fact that the adsorption process is favorable under the studied conditions.

II. Langmuir isotherm constants: Adsorbent dose 0.5 g/L

Co

(mg/L)

Temp

(°C)

Langmuir isotherm constants

Qo

(mg/g)

B

(L/mg)

RL

10 30 3.2952 0.2517 0.2843

15 30 5.8213 0.1826 0.2674

20 30 5.9319 1.1650 0.0412

10 20 4.4436 0.3425 0.2259

10 30 3.0463 0.3623 0.2163

0 3 6 9 12

0.0

0.3

0.6

0.9

1.2

3

2

1


pH 6


1. 10 mg/L

2. 15 mg/L

3. 20 mg/L

Ce/q

(g/L

)

Ce ( mg/L)

4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5

0.0

0.2

0.4

0.6

0.8

1.0


pH 6


1. 20o C

2. 30o C

3. 40o C

4. 50o C

4

3

2

1

Ce/q

(g/L

)

Ce (mg/L)




10 40 5.5816 0.3761 0.2100

10 50 4.8655 0.3311 0.2019

Adsorption kinetics

The kinetics of dye adsorption on PSLW carbon-iron oxide composite was analyzedby pseudo-

first order [20]or pseudo- second order [21], [22] kinetic models,given by equations (8) and (9).

tKqqq ee 1lnln (8)

eet qtqKqt 2

21 (9)

Where, qeandqt is the amount of adsorbate, adsorbed at equilibrium (mg/g) and at particular time

intervals respectively. K1 and K2 are the rate constants. A plot of ln (qe-q) versus t gives a straight line

slope of k1 and intercept of ln qe. The rate constants (K1 and K2) and calculated equilibrium capacity

(qe cal) of pseudo first order and second order models were determined from the slope and intercept

of linear plotsof pseudo first order and second order models at different concentration and temperature.

Fig. 8 shows that the linear plot of pseudo first order and second order models at different concentration

and temperature. The summary of kinetic parameters listed in table. III

Fig.8 Pseudo- second order plot of Rh 6G adsorption at different concentrations and temperatures

III. Pseudo first order and second order constants at different concentrations and temperatures:


Co Temp Pseudo first order constants Pseudo second order constants

0 20 40 60 80 100 120 140 160

0

2

4

6

8

10

12

14


pH 6


1. 10 mg/L

2. 15 mg/L

3. 20 mg/L

t/q

t

Time (min)

0 20 40 60 80 100 120 140 160

0

2

4

6

8

10

12

14

43

2 1

1. 20o C

2. 30o C

3. 40o C

4. 50o C


pH 6


t/q

t

Time (min)




(mg/L) (°C) qe(exp)

(mg/g)

K1

(min-1)

qe(cal)

(mg/g)

R2

K2(g/mg/m

in)

qe (cal)

(mg/g)

R2

10 30 11.6102 0.0091 1.6352 0.9616 0.01215 11.6265 0.9936

15 30 16.4832 0.0076 1.5503 0.8162 0.01777 16.4554 0.9983

20 30 18.3052 0.0077 1.0077 0.9671 0.02883 18.4060 0.9994

10 20 12.373 0.0921 1.9771 0.8543 0.00757 12.7064 0.9755

10 30 11.6102 0.1068 1.9176 0.9735 0.01215 11.6265 0.9936

10 40 13.1357 0.0108 1.7545 0.9953 0.01174 13.1961 0.9954

10 50 13.8985 0.01370 2.0713 0.9857 0.00852 14.1242 0.9926

From the experimental data, it is clearly seen that the adsorption of dye follows pseudo second order

kinetics. The comparision between qe(cal) and qe (exp) value and the closeness of R2 towards unity is

closer for pseudo second order kinetics than pseudo first order kinetics. Thus, the adsorption process

follows pseudo second order kinetics.

Pore diffusion

The intra particle diffusion method is used to study the mechanism of Rh 6G dye adsorption.

The plot of q versus t½ gives the information about the mechanism and the slope is the intra particle

diffusion constant (ki). The ki values are listed in table. IV for different concentration and temperature.

The ki value increases with increase in concentration and temperature and it indicates the increase in

boundary layer thickness and it leads to decrease in external mass transfer and increase the internal

mass transfer [23].

IV. The intra particle diffusion constant:Adsorbent dose 0.5 g/L

Co (mg/L) T °C Intra particle diffusion

(ki) (mg/g/min1/2)

10 30 2.2701

15 30 3.7976

20 30 4.5772

10 20 1.5636

10 30 1.7036

10 40 1.8595

10 50 1.9532

Column Study




The columnstudy provides the practical application of this process to industries. The observed

data fit to the linearised form of the Thomas model [24], [25] and are given in equation (10).

QVKCQMKqCC e 1log (10)

where, Co and Ce are the influent and effluent dyes concentrations (mg/L) respectively. K stands for

the Thomas rate constant (mL/min/mg), qo is the maximum solid phase concentration of solute (mg/g),

M is the mass of the adsorbent (g), and V is the throughput volume (ml/min). The linear plot of log

(Co/Ce-1) against V gives the value of K (slope) and qo (intercept).The column study was performed by

10 mg/L dye solution. The concentration of dye is gradually increases with bed volume. The value of

rate constant K (1.712 mL/min/mg) and the solute concentration qo (1.95 mg/g) are useful for designing

columns on large scale.

Conclusion

The present study describes the effective removal of Rh 6G dye from aqueous solution using

low-cost PSLW carbon-iron oxide composite as an adsorbent. Batch studies exhibits the adsorption

process follows Langmuir adsorption. The thermodynamic parameters show the adsorption process is

spontaneous, favorable and endothermic nature. The effective removal of dye can be obtained even

at high temperature. The kinetic data indicates the removal of dye follows the pseudo-second order

kinetics. In column study, Thomas model is used to assign the dye removal in industrial scale. From

the above results, it is concluded that the effective removal of Rh 6G from industrial effluents can be

achieved using PSLW carbon-iron oxide composite.

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