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RJCES Vol 5 [2] April 2017 58 | P a g e © 2017 AELS, INDIA

OORRIIGGIINNAALL AARRTTIICCLLEE

Adsorption of Methylene Blue Using Passiflora foetida Activated Carbon on Various Parameters

Dheeban Shankar P 1,2*, Basker S3 Karthik k4 and Karthik S5

1 Research and Development Centre, Bharathiar University, Coimbatore-46 , TN, India. 2&5 Department of Biotechnology, Nandha Arts and Science College, Erode-52 , TN, India.

3 Department of Botany, Government Arts College, Salem-07, TN, India. 4 Department of Chemistry, Nandha Arts and Science College, Erode-52, TN, India.

Email id: 1, 2*[email protected] * Corresponding author

ABSTRACT

The nature of the water is affected by the color where it inhibits the sunlight penetration into the stream and thereby reduces the photosynthetic action. The dyes are mostly produced from different chemicals and not suitable for biological degradation. Activated carbon is widely used in waste water treatment to remove organic and inorganic pollutant with effective removal of dye. By having these concepts in mind, the current study was aimed to prepare activated carbon from the stem of Passiflora foetida. Surprisingly, the uniqueness found in the current research was that the carbon activated at 180ºC had shown best adsorption like the carbon prepared at 800º C. The pattern of adsorption of Methylene blue was visualized to various parameters such as contact time, adsorbent dose, initial dye concentration, temperature and pH. The adsorption was observed to be very effective with gradual increase in the adsorbent dose and time. Further, the activated carbon was characterized with FTIR ,SEM and XRD studies. Key words: Passiflora foetida, Activated carbon, adsorption, FTIR, SEM and XRD. Received 20.01.2017 Accepted 18.03.2017 © 2017 AELS, INDIA

INTRODUCTION The industries such as paper, textiles, pharmaceutics, rubber, plastics, leather, cosmetics, and food use dyes as the important group of chemicals to colour the products. The normal function of aquatic life will become impaired when wastewater is released without proper treatment into water bodies and also it causes changes in food web [1]. The complex structure of the dyes and their synthetic origin made it tough to degrade easily, which then difficult for conventional methods to remove the dye efficiently from waste water [2]. At present, there is a growing interest in using low-cost and non conventional alternative materials instead of traditional adsorbents. Several researchers have been reported on the use of alternative materials with low costs. Activated carbon is the most widely used adsorbents because it has excellent adsorption efficiency of the organic compound. But, commercially available activated carbon is very expensive [3]. This led to further study for cheaper substitutions in the removal of dyes. The activated carbon materials can be prepared by physical and chemical methods. The temperature used in chemical activation is lower than that used in the physical activation process. As a result the development of a porous structure is better in the case of chemical activation method. The chemical activation can be done in a single step by carrying out thermal decomposition of raw material with chemical reagents [4].

The acidic reagents used in the chemical activation processes are ZnCl2 [5], H3PO4 [6], HCl [7] and H2SO4 or with basic reagents KOH [8], K2CO3

[9] and Na2CO31 [10]. The most commonly used dye in colouring the

cotton, wood and silk is the Methylene blue but it may cause a lot of health issues [11, 12, 13]. Using Methylene Blue as the model basic dye, numerous alternative materials have been analyzed to adsorb dyes from aqueous solution, such as giant duckweed[14], Bombax cieba tree[15], wheat shell[16], guava leaf [17] , activated carbon from sugar beet molasses [18],bamboo charcoal [19], teak tree bark

[20] ,Water hyacinth [21], Rice husk [22], raw grass and grass modified with citric acid [23], coir of Cocos nucifera [24] Neem leaf and orange peel [25] Apart from this, several other low cost activated carbons derived from agricultural and industrial wastes were reported[26]. In this current work, the stem of Passiflora foetida was employed for the preparation of activated carbon by chemical method. The activated carbon i.e., Adsorbent prepared were characterized and applied for

Research Journal of Chemical and Environmental Sciences Res J. Chem. Environ. Sci. Vol 5 [2] April 2017:58-66 Online ISSN 2321-1040 CODEN: RJCEA2 [USA] ©Academy for Environment and Life Sciences, INDIA Website: www.aelsindia.com/rjces.htm

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the decolourization of Methylene blue as a model dye with involvement of various parameters viz., concentration of dye, effect of carbon dose, time of incubation or contact time, temperature and pH etc., The plant materials of Passiflora foetida are found to be abundant, widely distributed, easily available and not grazed over by the cattle which might be due to the presence of secretory trichomes and were reported as rich in fibre content [27]. Moreover the activated carbon from Passiflora foetida was proved to have antimicrobial efficacy [28]. So that it could be exploited for the adsorption of dyes in wastewater treatment where the dyes are adsorbed along with the removal of microbial contaminants may be observed. Though there were many reports on the pharmacological studies over this plant, it is the first and novel report in this genus for applying in dye removal process. MATERIAL AND METHODS EXPERIMENTAL Collection of Plant materials and authentication The plant, Passiflora foetida (Fig.1.) was collected from in and around Erode District, Tamil Nadu. The plant materials were taxonomically identified and authenticated by the Botanical survey of India [BSI] at Tamil Nadu Agricultural University, Coimbatore and registered with no: BSI/SRC/5/23/2014-15/Tech-1085. The leaves were detached from plants and the stem materials were washed with tap water followed by sterile distilled water, cut into smaller pieces and then shade dried for about 15 days. The dried stem was powdered using electric blender which was then stored in airtight container for further experiments. Preparation of Activated carbon The powdered stem materials weighing about 200g was immersed in excess of concentrated sulphuric acid and incubated at room temperature for 10 days with constant stirring. After incubation, the material obtained was washed with tap water following distilled water for 5 - 6 times to remove the free acid residues. Finally the material was activated at 180 ºC in hot air oven and stored in air tight container. Batch adsorption experiments The adsorption of MB dye on Passiflora foetida activated carbon was carried out in a batch system according to the method described [29]. On the aspect of adsorption kinetics and adsorption isotherm study, batch adsorption experiments were conducted by varying the operational parameters such as contact time, adsorbent dose, initial dye concentration, pH and temperature at predetermined time interval. The initial and final dye concentration of the supernatant was measured using the UV-Visible Spectrophotometer. RESULTS AND DISCUSSION Characterization of Activated Carbon The physico-chemical properties of Passiflora foetida Activated carbon (PFAC) were analyzed to have the yield of Conc.H2SO4 treated carbon of ratio 1:3 found to be 51.5% following 0.6538 g/ml as the bulk density with pH 2.0 FT-IR transmission spectrum (Figure 1) was used to investigate variations in the functional groups of Passiflora foetida activated carbon. This technique has been used for the characterization of functional groups in various mixtures[30,31] The porosity as well as chemical reactivity of functional groups at the adsorbent surface determines the adsorption capacity of adsorbent [32].The PFAC exhibit O-H and C-H stretching in between 3470.06 - 3080.42 cm-1. The band in between 2800 - 3100 cm-1 shows C-H aromatic & C-H aliphatic bonds. The absorption band at 1707.06 cm-1 indicates the anhydride C=O bond. The C=O stretching in between 1718 - 1635 cm-1 attributed to phenolic ester, carboxylic acid and conjugated ketonic structures. The peak at 1608.69cm-1 reveals the presence of C=C bonds. The peak between 1155.40 – 1217.12 cm-1 indicates the existence of C-F stretch. The region in between 700 - 900 cm-1 contains various bands related to aromatic, out of plane C-H bending with different degrees of substitution[33]. The peak at 852.56 represent C-Cl stretching followed by C-I stretching between the peaks 418.57 – 491.86 cm-1

.Some weak bands were also observed in the range of 700 – 400 cm-1, indicates C-C stretching. The acidic groups present in Passiflora foetida activated carbon such as phenolic ester, carboxylic acid and conjugated ketonic structures might contributed to an acidic surface of the activated carbon, which was responsible for the adsorption of basic dyes especially methylene blue chosen for this study. Figure 2 a. and 2 b. illustrates the XRD pattern of adsorbents before and after adsorption respectively. X-ray diffraction analysis was performed to determine the degree of crystalline or amorphous nature of the Activated Carbon [34].The well defined or sharp peaks denote the crystalline nature of the material whereas broad peaks determine the non-crystalline or amorphous nature of the material as reported [35]. The Sharp peak obtained in the current study indicated the crystalline nature of the material and was observed to have no change in the crystalline nature of the adsorbent before and

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after adsorption [36]. The average crystallite size was calculated using the Scherrer’s formula and found to be approximately 1.25nm. The surface morphology of the PFAC before and after adsorption was examined using Scanning Electron Microscope. SEM micrograph of the chemically activated carbon by H2SO4 was depicted in Figure 3. Many pores in honey comb shapes were clearly observed on the surface of the adsorbent which was found similar to the adsorbents prepared using agricultural wastes [37], Jatropha husk [38] and wood activated charcoal of Bombax cieba tree reported by Fazlullah et al.,2005.The pore development was noticed to be same to the activated Carbon prepared from gelam wood bark by employing zinc chloride as the impregnant solution [39].The SEM image of the adsorbent before adsorption at 3000X had shown irregular groove and ridges in fibrous network that was found to be helpful for the accessibility of metal ions to the adsorbent surface as reported earlier [40].Apart from the above observation, rosette like appearances with non uniform sizes were also revealed before adsorption and observable differences in the pore sizes were noticed in the adsorbent after adsorption at 2000x of Scanning Electron Micrograph. Investigation of Adsorption Parameters Effect of Contact Time and Initial Concentration of Dye The colour of the dye before and after treatment with the adsorbent is depicted in the figure 4. Effect of contact time on adsorption of MB dye on PFAC is shown in Fig.5. The dye removal percentage increased with the increase in contact time. As the initial MB concentration increased from 20 to 40ppm, the dye removal percentage decreased from 91.59 to 40.48% & 99.95 to 93.66% for 250mg and 500mg PFAC respectively. This may be attributed to the fact that at low concentrations the ratio of surface active sites to the total dye molecules in the solution is high and hence all dye molecules may interact with the activated carbon. Effect of adsorbent dosage and initial dye concentration The adsorption of Methylene Blue on PFAC was studied by changing the quantity of adsorbent (50, 100, 150, 200 and 500 mg/50mL) in the test solution. While keeping the initial MB concentration from 10 to 40ppm at temperature (28 ± 20C), the adsorption percentage was increased from 70.86 % to 98.07%, 43.35% to 93.86%, 15.31% to 63.12% and 12.64% to 55.71% as the PFAC dose increased from 50mg to 500mg at equilibrium time (60 minutes) for 10, 20, 30 and 40ppm respectively. The amount of MB adsorption increased with increase in dosage of adsorbent but the percentage removal of MB decreased with increase in concentration of dye which is shown in the figure 6 and it indicated the effective dosage of adsorbent for the removal of dye. Effect of temperature When the effect of temperature on the adsorption of Methylene blue at 500 mg adsorbent concentration in 50 ml of 20 & 40 ppm dye concentration was investigated, the removal of dye percentage decreased from 97.22 to 95.74% & 96.02 to 95.63% for 20 and 40ppm respectively with increase in temperature from 400C to 700C which were picturized in figure 7. It suits to the report that changing the temperature may change the equilibrium capacity of the adsorbent for a particular adsorbate [41, 42]. Effect of pH An important factor needed for controlling the adsorption of dye onto adsorbent is pH. The adsorption of MB with the concentration of 20 & 40 ppm on PFAC was studied by varying the pH from 2 to 10. The dye removal percentage as 88.09% at lower pH 2 was increased to 98.5% with increase in pH up to 6 and decreased to 96.2% with neutral pH following increases in removal percentage as 98.7% when the pH raised to 9, then again decreased to 96.8% with increase in pH at 10 and is shown in the Figure 8. The study revealed the maximum dye removal percentage at pH 6 and pH 9. Langmuir isotherm The data obtained on the adsorption of the dye have been analyzed on the basis of the Langmuir isotherm model,

Ce/qe = 1/Qo b + Ce/Q0 Where Ce is the equilibrium concentration of the dye solution (mg L-1), qe is the amount of dye adsorbed per unit mass of adsorbent (mg g-1), and Qo (mg g-1) and b (L mg-1) are the Langmuir constants related to the maximum adsorption capacity and the rate of adsorption respectively. The adsorption of dye onto PFAC was subjected to Langmuir plot (Figure 9). The Linear plot of Ce/qe vs Ce confirmed that the present investigation was suitable in explaining the adsorption process for Langmuir isotherm model. The essential characteristics of Langmuir equation can be expressed in terms of a dimensionless separation factor RL, as follows,

RL = 1/ (1+ b C0) Where, C0 is initial concentration of adsorbate and ‘b’ is the constant related to the energy of adsorption (Langmuir constant). The values of RL indicate the type of the isotherm (either Unfavourable (RL > 1),

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RJCES Vol 5 [2] April 2017

Linear (RL = 1), Favourable (0 < Rwas less than one which indicated that the process w CONCLUSION In the study undertaken, a new potential and cheap adsorbent has been prepared by chemical modification of Passiflora foetidaMethylene blue. Batch adsorption method was employed to optimize the process parameters of dye concentration, adsorbent dosage, contact time, pH and temperature. The results showed an effectdependent adsorption with respect to contact time, dye concentration, optimum temperature at 40ºC and pH at 6 and 9. Taking into consideration of all the above obtained results, it can be concluded that PFAC would be an alternative material to comavailable material for the preparation of activated carbon utilized for dye removal and antibacterial efficacy where it controls the water born diseases and water pollution. Thus the presenrevealed that the activated carbon obtained from the stem of for the removal of MB dye from wastewater.

Fig. 2. XRD Profile of PFAC before [B] and after [A]

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= 1), Favourable (0 < RL < 1) or Irreversible (RL = 0). In the present investigation, the value Rwas less than one which indicated that the process was favourable.

In the study undertaken, a new potential and cheap adsorbent has been prepared by chemical Passiflora foetida stem powder using concentrated sulphuric acid for the removal of

Methylene blue. Batch adsorption method was employed to optimize the process parameters of dye concentration, adsorbent dosage, contact time, pH and temperature. The results showed an effectdependent adsorption with respect to contact time, dye concentration, optimum temperature at 40ºC and

Taking into consideration of all the above obtained results, it can be concluded that PFAC would be an alternative material to commercial adsorbents. Therefore, the use of this lowavailable material for the preparation of activated carbon utilized for dye removal and antibacterial efficacy where it controls the water born diseases and water pollution. Thus the presenrevealed that the activated carbon obtained from the stem of Passiflora foetida are a promising material for the removal of MB dye from wastewater.

Fig.1.FTIR spectrum of PFAC

Fig. 2. XRD Profile of PFAC before [B] and after [A] adsorption

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© 2017 AELS, INDIA

= 0). In the present investigation, the value RL

In the study undertaken, a new potential and cheap adsorbent has been prepared by chemical stem powder using concentrated sulphuric acid for the removal of

Methylene blue. Batch adsorption method was employed to optimize the process parameters of dye concentration, adsorbent dosage, contact time, pH and temperature. The results showed an effective dose dependent adsorption with respect to contact time, dye concentration, optimum temperature at 40ºC and

Taking into consideration of all the above obtained results, it can be concluded that PFAC mercial adsorbents. Therefore, the use of this low-cost and easily

available material for the preparation of activated carbon utilized for dye removal and antibacterial efficacy where it controls the water born diseases and water pollution. Thus the present work had

are a promising material

adsorption


Fig.3. The images A,B,C and D depicts the surface of PFAC before adsorption and the images E ,F ,G and H shows the surface of PFAC after adsorption at different magnifications viz.,X1000,X2000,X3000 and X 7000 respectively.

A.)

B.)

C.)

D.)

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The images A,B,C and D depicts the surface of PFAC before adsorption and the images E ,F ,G and H shows the surface of PFAC after adsorption at different magnifications viz.,X1000,X2000,X3000 and X 7000 respectively.

E.)

F.)

G.)

H.)

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© 2017 AELS, INDIA

The images A,B,C and D depicts the surface of PFAC before adsorption and the images E ,F ,G and H shows the surface of PFAC after adsorption at different magnifications


Fig.4. The colour of Methylene blue dye solution

A.) Fig.5.Effect of contact time at 250mg adsorbent (A) & 500mg adsorbent(B) with methylene blue

Fig.6. Effect of carbon (Adsorbent dosage)

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of Methylene blue dye solutionBefore (A.) and After (B.) treatment with Adsorbent

B.) Fig.5.Effect of contact time at 250mg adsorbent (A) & 500mg adsorbent(B) with methylene blue

Fig.6. Effect of carbon (Adsorbent dosage) Fig.7. Effect of Temperature

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Before (A.) and After (B.) treatment with Adsorbent

Fig.5.Effect of contact time at 250mg adsorbent (A) & 500mg adsorbent(B) with methylene blue

of Temperature


Fig.9. Langmuir plot for the adsorption of Methylene Blue dye at different concentration REFERENCES 1. Aksu Z , Ertu S, Donmez G (2010). Methylene Blue biosorption by

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CITE THIS ARTICLE Dheeban Shankar P, Basker S, Karthik K, and Karthik S. Adsorption of Methylene Blue Using Passiflora foetida Activated Carbon on Various Parameters. Res. J. Chem. Env. Sci. Vol 5 [2] April 2017. 58-66

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