Removal of indigocarmine from industrial effluents using low cost adsorbent

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1 Journal of Scientific & Industrial Research Vol. 65, March 2006, pp Removal of indigocarmine from industrial effluents using low cost adsorbent Rajeev Jain*, Megha Mathur and Shalini Sikarwar Department of Environmental Chemistry, Jiwaji University, Gwalior Received 06 September 2005; revised 28 December 2005; accepted 03 January 2006 In the present paper, adsorption technique was employed for removal of indigocarmine and the technique was found to be very useful and cost effective for a better removal of dye. The operating variables such as adsorbent dose, adsorbate concentration, particle size, ph, contact time and temperature were optimized. Keywords: Adsorption, Charcoal, Indigocarmine, Rice husk IPC Code: B01D17/05 Introduction Indigo dyes (Fig. 1) are widely used for dyeing and printing protein and cellulose fibers 1. In conventional indigo dyeing process, significant quantity of excess indigo was found in wash water from rinsing operation, which becomes part of the effluent 2. Textile individual process generates large quantities of wastewater, which are very toxic and difficult to be disposed by physical, chemical and microbiological methods. Textile wastewater is characterized by high chemical oxygen demand (COD), low biological oxygen demand (BOD) and heavy colour. COD and colour of wastewater are resistant to conventional wastewater treatment 3-8. Activated carbon has been widely used in wastewater treatment to remove organic and inorganic pollutants Possessing high surface area, activated carbon frequently exhibits high removal efficiency for most dissolved compounds. Activated carbon is expensive, therefore, development of low cost alternative adsorbent has been the focus of recent research. A number of workers have used different materials as the adsorbent for the removal of different pollutants In the present work, a low cost adsorbent rice husk was used for the removal of indigocarmine from wastewater. Materials and Methods Adsorption studies of indigocarmine were carried out using charcoal and rice husk as adsorbents. The effect of concentration, ph, adsorbent dose, temperature and contact time were evaluated. *Author for correspondence Tel: rajeevjain54@yahoo.co.in Adsorption isotherms were run at 40, 50 and 60 o C. The effect of ph on the adsorption of dyes has been studied by changing ph ( ) of the medium. The effect of amount of adsorbent has also been studied by varying the amount of adsorbent at constant concentration of dye, ph and temperature. The variation in the uptake of dye with different particle size (<106, , , , , , >300 mesh size) was investigated. Initial dye concentration was 1.0 x x 10-4 M for charcoal and rice husk. Rice husk after converting into an adsorbent was selected as low cost adsorbent and activated charcoal was used for comparing the results. For measuring pollutional load, COD was determined using COD digestion apparatus (Spectra lab S). COD was determined by preparing a dye solution (4.0 x 10-4 M) for blank, thereafter a solution was used for adsorption study and COD was determined after adsorption. Dye concentration was determined on Spectronic 20D+thermospectronic spectrophotometer at 707 nm. Optical density was measured after filtration of the dye by whatman No. 1 filter paper. ph of the solution was maintained using B R buffers and measured by Digital ph meter DB Adsorption Fig. 1 Structure of indigocarmine

2 JAIN et al.: REMOVAL OF INDIGOCARMINE FROM INDUSTRIAL WASTES USING RICE HUSK 259 Fig. 2 Effect of adsorbent amount on the uptake of indigocarmine (a) charcoal (b) rice husk of dye on glass surface of the electrode did not cause any problem. All chemicals and reagents were of analytical grade. Double distilled water was used for preparing different dilutions. Rice husk was cleaned and thoroughly washed with distilled water and dried. It was treated with acetic acid and again washed with distilled water. Thereafter, rice husk was treated with hydrogen peroxide (100 vol) to remove all adhering organic particulates and other impurities, washed with distilled water and dried at 60 o C for 1 h in vacuum oven. The material was grounded and sieved to desired particle size. Results and Discussion Effect of Adsorbent Dose The effect of adsorbent dose on the removal of indigocarmine was studied by varying the amount of charcoal ( g/l) and rice husk ( g/l). Experiments were carried out at fixed ph, concentration and at different temperatures. Adsorption decreases with increase in temperature for both the cases. The adsorption increases from 0.06 g/l to 0.26 g/l, thereafter it becomes constant for Fig. 3 Effect of contact time on the uptake of indigocarmine (a) charcoal (b) rice husk at conc. (7.0 x 10-4 M), temp. (40 o C) charcoal, while in case of rice husk initially adsorption was constant from 0.66 g/l to 2.0 g/l thereafter it increases (Fig. 2). Effect of Contact Time Adsorption was also studied for different contact time with fixed adsorbent dose for charcoal (0.13 g/l) and for rice husk (0.66 g/l), at fixed ph and temperature (40 o C). Increase in time has significant effect on the adsorption of indigocarmine (Fig. 3). Adsorption increases as the contact time increases, and after 20 min adsorption become constant for charcoal, whereas in case of rice husk initially adsorption was constant up to 40 min and then increases. Effect of ph Adsorption of indigocarmine over ph (Fig. 4) with charcoal is almost constant. Colour removal (96.9%) at ph 2.0 decrease at ph 12.0 (95.3%) for charcoal. Colour removal (90%) at ph 2.12 decreases at ph 12.0 (72%) for rice husk. Initially, colour removal was constant, thereafter it decreases at ph 7.0 and then adsorption became constant.

3 260 J SCI IND RES VOL 65 MARCH 2006 Fig. 4 ph profiles for (a) charcoal and (b) rice husk Fig. 6 Effect of particle size on adsorption of indigocarmine (a) charcoal (b) rice husk at conc. ( M), temp. (30±0.1 o C) Fig. 5 Effect of initial dye concentration on the uptake of indigocarmine (a) charcoal (b) rice husk at temp (30 ± 0.1 o C) Effect of Initial Dye Concentration The adsorption studies were carried out at fixed ph, adsorbent dose and room temperature. The adsorbent and dye solution of different initial concentration ( x 10-4 M) contacted for 30 min for charcoal and 60 min for rice husk (Fig. 5). The rate of uptake of indigocarmine decreases with increase in concentration with both the adsorbents. Effect of Particle Size At fixed concentration ( M), ph, and temperature and fixed adsorbent dose for charcoal (0.13 g/l) and rice husk (3.33 g/l), maximum adsorption was observed for charcoal (96%) at mesh size <106 and for rice husk (80.7%) at mesh size <106 (Fig. 6). Effect of Temperature Adsorption for charcoal and rice husk decreases with increase in temperature in the order 40 > 50 > 60 o C (Fig. 7). Adsorption Isotherms The adsorption of indigocarmine was analyzed by models given by Langmuir and Freundlich. The linear form of Langmuir isotherms is given as 1/qe = 1/Q o + 1/bQ o Ce (1) where, qe is the amount adsorbed (mol/g), Ce is the equilibrium concentration of the adsorbate (mol/l), Q o and b are the Langmuir constants related to maximum adsorption capacity and energy of adsorption relatively. When 1/qe is plotted against 1/Ce, a straight line with slope 1/bQ o is obtained (Fig. 8) which shows that the adsorption of indigocarmine follows the Langmuir isotherm. The Langmuir constants are calculated (Table 1) at different temperatures (40, 50, 60 o C). Freundlich Isotherms is given as Log qe = log K f + 1/n log C e (2) where, qe is the amount adsorbed (mol/g), C e is the equilibrium concentration (mol/l) K f and 1/n are

4 JAIN et al.: REMOVAL OF INDIGOCARMINE FROM INDUSTRIAL WASTES USING RICE HUSK 261 Freundlich constants (Table 2) related to adsorption capacity and intensity respectively 28. A linear relationship was observed between -log qe and -log C e (Fig. 9) from plotted parameters indicates the applicability of Freundlich equation. Thermodynamic Parameters The change in standard free energy ( G o ), enthalpy ( H o ), and entropy ( S o ) for the adsorbates were evaluated (Table 3) using following equations 29 : G o = -RT ln b ln b 2 /b 1 = ( H o /R) (T 2 T 1 /T 2 /T 1 ) S o = - ( G o - H o )/T (3) (4) (5) Adsorption Kinetics Adsorption kinetics was carried out at room temperature with fixed amount of adsorbent and ph with different contact time (Table 4). The data of indigocarmine was tested for the first order reaction. K = 2.303/t log 10 Ci/Ce where, Ci = initial concentration (mg/l), Ce = equilibrium concentration (mg/l), t = time in min, K = rate constant. Plot between log Ci /Ce and t results in straight line with slope K/2.303 (Fig. 10). This shows that the adsorption of indigocarmine follows the first order rate equation. Fig. 7 Effect of temperature on adsorption of indigocarmine (a) charcoal (b) rice husk at conc. ( M) Fig. 8 Langmuir adsorption isotherms of (a) charcoal (b) rice husk, at different temperatures Temperature o C Table 1 Langmuir constants for the adsorption of indigocarmine Charcoal Rice husk b, mol g -1 Q o, L mol -1 R 2 b, mol g -1 Q o, L mol -1 R

5 262 J SCI IND RES VOL 65 MARCH 2006 Temperature o C Table 2 Freundlich constants for the adsorption of indigocarmine Charcoal Rice Husk K f n R 2 K f n R Fig. 9 Freundlich adsorption isotherms of (a) charcoal (b) rice husk, at different temperatures Table 3 Thermodynamic parameters for adsorption of indigocarmine Adsorbents G o, KJmol -1 H o, KJmol -1 S o, JK -1 mol -1 Charcoal Rice husk Table 4 Adsorption kinetics (K 10-3 min -1 ) constants for indigocarmine Adsorbents 40 o C 50 o C 60 o C Charcoal Rice husk Fig. 10 Adsorption kinetics at different temperatures (a) charcoal (b) rice husk COD Determination COD of treated/adsorbed dye solution gets considerably reduced after adsorption on charcoal and rice husk. COD of the solutions after adsorption shows significant decrease from 1126 mg/l to 280 mg/l for charcoal and from 1126 mg/l to 480 mg/l for rice husk. Conclusions Adsorption of indigocarmine by charcoal and rice husk follows first order kinetics. Thermodynamic parameters indicate that the process is spontaneous

6 JAIN et al.: REMOVAL OF INDIGOCARMINE FROM INDUSTRIAL WASTES USING RICE HUSK 263 and exothermic in nature. Rice husk, a solid waste converted into an inexpensive adsorbent material, exhibits very good adsorption capacity for indigocarmine. References 1 Snell F D & Ettre L S, Encyclopedia of industrial chemical analysis, edn 5 (John Wiley and Sons, Inc. N Y) Reife A & Freeman H S, Environmental Chemistry of Dyes and Pigments (Wiley Interscience Publication, New York) Mittal A, Krishnan, L & Gupta V K, Removal and recovery of malachite green from wastewater using an agricultural waste material, de-oiled soya, Separation Purification Technol, 43 (2005) Gupta V K, Mittal A & Gajbe V, Adsorption and desorption studies of a water-soluble dye, Quinoline yellow, using waste materials, J Colloid Interface Sci, 284 (2005) Mittal A, Kurup L & Gupta V K, Use of waste materials - Bottom ash and de-oiled soya, as potential adsorbents for the removal of Amaranth from aqueous solutions, J Hazardous Mat, 17 (2005) Jain A K, Gupta V K, Bahtnagar A & Suhas, Utilization of industrial waste products as adsorbents for the removal of dyes, J Hazardous Mat, 101 (2003) Jain A K, Gupta V K, Bhatnagar A, Jain S & Suhas, A comparative assessment of adsorbents prepared from industrial wastes for the removal of cationic dye, J Indian Chem Soc, 80 (2003) Gupta V K, Mohan D, Sharma S & Sharma, Removal of basic dyes (Rhodamine B and Methylene blue) from aqueous solutions using bagasse fly ash, Separation Sci & Technol, 35 (2000) Ho Y S & Chiang C C, Sorption studies of acid dye by mixed sorbents, Adsorption, 7 (2001) Tseng R L, Wu F C & Juang R S, Liquid-phase adsorption of dyes and phenols using pinewood-based activated carbons, Carbon, 41 (2003) Meshko V, Markovska L, Mincheva M & Rodrigues A E, Adsorption of basic dyes on granular activated carbon and natural zeolite, Wat Res, 35 (2001) Wu F C, Tseng R L & Juang R S, Kinetic modeling of liquid-phase adsorption of reactive dyes and metal ions on chitosan, Wat Res, 35 (2001) Wu F C, Tseng R L & Juang R S, Adsorption of dyes and humic acid from water using chitosan-encapsulated activated carbon, J Chem Technol Biotechnol, 77 (2002) Yang X Y & Al-Duri B, Application of branched pore diffusion model in the adsorption of reactive dyes on activated carbon, J Chem Eng, 83 (2001) Chen J P & Lin M, Equilibrium and kinetics of metal ion adsorption onto a commercial H-type granular activated carbon: experimental and modeling studies, Wat Res, 35 (2001) Chiang H L, Tsai J H, Chang G H &. Jeng F T, Diffusion of hydrogen sulfide and methyl mercaptan onto microporous alkaline activated carbon, Chemosphere, 41 (2000) Cowan C E, Zachara J M & Resch C T, Cadmium adsorption on iron oxide in the presence of alkaline-earth elements, Environ Sci Technol, 25 (1991) Lee C K & Low K S Removal of copper from solution using moss, Environ Techno Lett, 89 (1989) Low K S & Lee C K, Cadmium uptake by the moss, Clympeters Delessertii Beach Biosour Technol, 38 (1991) Kesaoul-Qukel S, Cheeseman C & Perry R, Effect of conditioning and treatment of chabazite and clinoptilolite prior to lead and cadmium removal, Environ Sci Technol, 27 (1993) Rodda P D, Johnson B B & Wello J D, The effect of temperature and ph on the adsorption of copper (II), lead (II) and zinc (II) on geolite, J Colloid Interface Sci, 161, (1993) Gupta V K, Mittal A & Gajbe V, Adsorption and Desorption studies of a water-soluble dye, Quinoline yellow, using waste materials. J Colloid Interface Sci, 284 (2005), Mittal A, Kurup K L & Gupta V K, Use of waste materialsbottom ash and de-oiled soya, as potential adsorbents for the removal of Amaranth from aqueous solutions, J Hazardous Mat, 117 (2005) Gupta V K, Ali I, Suhas & Mohan D, Equilibrium uptake and sorption dynamics for the removal of a basic dye (basic red) using low cost adsorbents, J Colloid Interface Sci, 265 (2003) Gupta V K, Miital A, Krishnan L & Gajbe V, Adsorption kinetics and column operations for the removal and recovery of malachite green from wastewater using bottom ash, Sep Purif Technol, 40 (2004) Gupta V K, Srivastava S K & Mohan D, Equilibrium uptake, Sorption dynamics, process optimization and column operations for the removal and recovery of malachite green from wastewater using activated carbon and activated slag, Ind Engg Chem Res, 36 (1997) Gupta V K, Ali I, Saini V K & Suhas, Removal of Rhodamine B, fast green and methylene blue from wastewater using red mud-an aluminum industry waste, Ind Eng Chem Res, 43 (2004) Weber J R, Jr, Physicochemical Process for Water Quality Control (John Wiley and Sons, N Y) Gupta V K, Equilibrium uptake, sorption dynamics, process development and column operations for the removal of copper and nickel from aqueous solutions and wastewater using activated slag, a low cost adsorbent, Ind Eng Chem Res, 37 (1998)

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