Indian Journal of Chemical Technology

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VOLUME 16

NUMBER 3

MAY 2009

CODEN : ICHTEU

 

ISSN : 0971-457X

 

CONTENTS

 

Papers

 

 

Kinetics and mechanism of esterification of isoamyl alcohol with acetic acid by immobilized lipase

209

Sumbita Gogoai & N N Dutta

 

 

 

Characterization of corrosion resistance properties of sol-gel alumina coating in

216

mine water environment

 

G Ruhi, O P Modi, A K Jha & I B Singh

 

 

 

Corrosion inhibition of brass in presence of sulphonamidoimidazoline and
hydropyrimidine in chloride solution

221

Ranjana, M Maji & M M Nandi

 

 

 

Corrosion inhibition of aluminium by 2-chloronicotinic acid in HCl medium

228

J Ishwara Bhat & Vijaya Alva

 

 

 

Kinetics and thermodynamics of copper ions removal from aqueous solution by

234

use of activated charcoal

 

Pragnesh N Dave, N Subrahmanyam & Surendra Sharma

 

 

 

Adsorption of dye Green B from a textile industry effluent using two different

240

samples of activated carbon by static batch method and continuous process

 

Rita Kant & V K Rattan

 

 

 

Removal of Ni(II) from water and wastewater using modified Duolite XAD-761 resin

245

V Tharanitharan & K Srinivasan

 

 

 

Synthesis, characterization and analytical applications of zirconium (IV) diethanolamine

254

D K Singh & Vijay Kumar

 

 

 

Selective complexometric determination of palladium with sodium metabisulphite

259

as releasing agent

 

Prakash Shetty & A Nityananda Shetty

 

 

 

Determination of amoxycillin in pharmaceutical forms by visible spectrophotometry

265

and HPLC

 

K Basavaiah, Kalsang Tharpa, N Rajendra Prasad, S G Hiriyanna & K B Vinay

 

 

 

Notes

 

 

 

Influence of preparation method on the performance of Pd/ZrO2-Al2O3 catalysts for HDS

272

Sufen Chen, Laitao Luo & Xinsun Cheng

 

 

 

Interfacial area measurement in a gas-liquid ejector for a sodium chloride -air system

278

P T Raghuram

 

 

 

Author Index

283

 

 

Keyword Index

284

 

 

Guidelines for Authors

285

 

 

   

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 209-215

 

Kinetics and mechanism of esterification of isoamyl alcohol with
acetic acid by immobilized lipase

 

Sumbita Gogoi & N N Dutta*

Chemical Engineering Division, North East Institute of Science and Technology, CSIR

Jorhat 785006, India

 

In this study, the effects of the rate enhancement of isoamyl acetate formation by immobilized Mucor miehei lipase catalysed esterification of isoamyl alcohol with acetic acid were investigated. The esterification reaction was studied in ten different solvents and n-heptane was found to be most suitable. The rate of the reaction was affected by the addition of molecular sieves (3) and temperature. The effects of different reaction parameters such as lipase and substrate concentrations were studied. The activity of immobilized lipase was found to be maximum at lipase concentration of
12 mg/mL and at a reaction temperature of 55C; retained about one third of its initial activity up to seven reaction cycles after repeated use. The kinetics of the reaction can be described by Ping-Pong Bi-Bi mechanism with acid inhibition. The parameter values were estimated by non-linear regression analysis.

Keywords: Immobilized, Isoamyl acetate, Lipase, Esterification

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 216-220

 

Characterization of corrosion resistance properties of sol-gel alumina coating in mine water environment

G Ruhi, O P Modi, A K Jha & I B Singh*

Advanced Materials and Processes Research Institute, CSIR, Hoshangabad Road, Bhopal 462 026, India

Email: ibsingh58@yahoo.com

 

Sol-gel alumina coating was developed on mild steel surface by using dip coating technique. Prior to the sol-gel coating, the substrate was treated with zinc-phosphating solution to improve the bonding of the coating. The corrosion resistance properties of the sol-gel alumina coated, uncoated and surface pre-treated substrates were evaluated in an artificial mine water solution. Electrochemical measurements like OCP variation with time, partial polarisation and electrochemical impedance analysis were carried out to evaluate corrosion resistance properties of the coatings. The microstructure and compositional analysis of the sol-gel coated specimens were investigated by SEM and XRD, respectively. The experimental results exhibited a significant improvement in the corrosion resistance of the sol-gel coated specimens as compared to the uncoated and surface pre-treated specimens. The SEM micrographs showed the presence of a compact coating of thickness 20 micron (approx). The XRD spectrum of the sol-gel coated specimens suggested the presence of α-alumina phase in the coating.

Keywords: Mild steel, X-Ray diffraction, SEM, Sol-gel alumina coating

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 221-227

 

Corrosion inhibition of brass in presence of sulphonamidoimidazoline and hydropyrimidine in chloride solution

 

Ranjana, M Maji & M M Nandi*

Department of Chemistry, National Institute of Technology, Durgapur 713 209, India

 

Four sulphonamido derivatives namely 2(β-benzenesulphonamido) ethylbenzoxazole (I), 2(β-benzenesulphonamido) ethylbenzimidazole (II), 2(β-benzenesulphonamido) ethylimidazoline (III) and 2(β-benzenesulphonamido)ethyl-1,4,5,6-tetrahydropyrimidine (IV) have been synthesized and various physicochemical properties of these compounds have been recorded. These compounds were investigated as corrosion inhibitors of brass in 0.6 M NaCl solution using gravimetric, potentiodynamic polarization, AC impedance and EDS methods. The studies indicated that the ligands inhibit the corrosion of brass in chloride solution effectively. The inhibiting efficiency increases with the increase in basic character of the ligands. It was also observed that the inhibition efficiency increased in the presence of inhibitors in solution than surface coated with self-assembled film on the brass surface under identical condition.

Keywords: Brass, Polarization, Impedance, Imidazoline, Hydropyrimidine, EDS, Mixed ligand complex

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 228-233

 

Corrosion inhibition of aluminium by 2-chloronicotinic acid in HCl medium

 

j ishwara Bhat* & Vijaya Alva

Department of Chemistry, Mangalore University, Mangalagangothri 574 199, India

 

The inhibiting effect of 2-chloronicotinic acid on the dissolution of aluminium in various concentrations of HCl has been studied using weight loss and polarization measurements. The inhibition efficiency was found to increase with increasing concentration of the inhibitor. The effect of temperature on corrosion inhibition was investigated. The results indicate the decreased inhibition efficiency for the increase in temperature. The inhibitor was found to be adsorbed on aluminium surface probably following Langmuir adsorption isotherm at higher concentrations of HCl.

Keywords: Corrosion inhibition, Aluminium, 2-Chloronicotinic acid, Weight loss method, Polarisation method

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 234-239

 

Kinetics and thermodynamics of copper ions removal from aqueous solution by use of activated charcoal

 

Pragnesh N Dave*, N Subrahmanyam & Surendra Sharma

Institute of Technology, Chemical Engineering Department,
Nirma University of Science & Technology, Gandhinagar-Sarkhej Highway, Ahmedabad 382 481, India

Email: pragneshdave@gmail.com

 

A study on the adsorption of copper from aqueous solutions on activated charcoal has been carried out with an aim to obtain information on treating effluents from metal finishing industries. The effects of various experimental parameters like contact time, dosage of activated charcoal, initial concentration of metal ions, pH etc. have been investigated. The percentage removal of metal ions increased with the decrease in initial concentration and increase in contact time, dosage of adsorbent and initial pH. Adsorption data were modeled with the Freundlich and Langmuir adsorption isotherms, various first order kinetic equations viz. Lagergren, Natarajan-Khalaf and Bhattacharya and Venkobachar equations and intra particle diffusion model. These isotherms, first order equations and models were found to be applicable. The kinetics of adsorption is found to be first order with intra particle diffusion as the rate determining step. Removal of metal ions using activated charcoal is found to be favourable and hence it could be used as an adsorbent for the treatment of effluents from metal finishing industries, especially for the removal of metal ions.

Keywords: Copper, Activated charcoal, Adsorption, Adsorption model, Kinetic model

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 240-244

 

Adsorption of dye Green B from a textile industry effluent using two different samples of activated carbon by static batch method and continuous process

 

Rita Kant1 & V K Rattan2*

1University Institute of Fashion Technology, Panjab University, Chandigarh 160 010, India

2Department of Chemical Engineering & Technolgy, Panjab University, Chandigarh 160 014, India

Email: vkrattanpu@yahoo.com

 

Removal of dye Green B using two different samples of activated carbon by static-batch method and continuous process was studied. Experimental data on optical density of blank solutions of different concentrations ranging from 10 to 100mg/L and optical density of solutions after adsorption on activated carbon samples were taken and analyzed. Calibration curves were plotted and the amount of dye adsorbed was calculated. The data was fitted to Langmuir and Freundlich isotherms for two different carbon samples and concentration values. Constants were calculated from the slope and intercept values of the isotherm. Coefficient of correlation R2 and standard deviation SD were also noted. The data fitted well to the isotherms. Carbon sample C1 showed considerably higher potential to adsorb the dye Green B as compared to carbon sample C2. Adsorption was better in batch process in respect to continuous flow method. From the analysis of the data it is shown that both activated carbon samples had a good capacity to remove the textile dye from the residue wastewater.

Keywords: Adsorption, Green B, Activated carbon, Textile industry effluent

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 245-253

 

Removal of Ni(II) from water and wastewater using modified
Duolite XAD-761 resin

 

V Tharanitharan & K Srinivasan*

Department of Chemistry, Government College of Engineering, Anna University-CBE, Salem 636 011, India

Email: srini_vasank@hotmail.com

 

Complete mixing of cross-linked phenol-formaldehyde polymeric resin (Duolite XAD-761) with anionic surfactant -sodium dioctyl sulphosuccinate (SDOSS) and EDTA-disodium salt (Chelating agent) in an aqueous solution led to the formation of a modified resin. FT-IR studies showed that the immobilization of the extractants results from hydrophobic interaction between the alkyl group of the extractants and phenyl group of the support, and also from other mechanisms like polar or electrostatic forces. The modified resin was used in batch adsorption experiments for the removal of Ni(II) were carried out as a function of agitation time, pH, adsorbent dosage and adsorption capacity. Adsorption data could be interpretated by Langmuir and Freundlich equations. The results showed that the adsorption kinetics of Ni(II) on modified XAD-761 resin could be best described by the pseudo-second-order model. SEM studies revealed the morphological observations of the pure resin, modified resin and Ni(II) adsorbed modified resin.The adsorbent was also tested for the removal of Ni(II) from synthetic wastewater.

Keywords: Ni(II) adsorption, Duolite XAD-761, SDOSS, EDTA, FT-IR, SEM, Adsorption isotherms, Kinetics

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 254-258

 

Synthesis, characterization and analytical applications of zirconium (IV) diethanolamine

 

D K Singh* & Vijay Kumar

Analytical Research Laboratory, Department of Chemistry
Harcourt Butler Technological Institute, Kanpur 208 002, India

 

A new chelating ion exchanger, zirconium(IV) diethanolamine has been synthesized, characterized and studied for sorption of eight heavy metal ions at different pH (1-6). Sorption capacity of zirconium (IV)-diethanolamine sample (ZDEA5) for Cu2+ and Hg2+ was found to be 1.2 and 0.7 mmol g1, respectively. The effect of pH on sorption revealed that capacity generally decreases with decrease in pH and optimum pH for maximum sorption is 6. The distribution coefficients of metal ions on ZDEA5 as a function of pH have been studied. Separations of Hg2+ from its mixture with Zn2+, Cd2+, Ni2+, Fe3+ and Cu2+ from its mixture with Fe3+, Ni2+ and Zn2+ have been achieved quantitatively on a mini-column of ZDEA5.On the basis of high selectivity and good sorption in acidic aqueous solutions a mini-column of ZDEA5 has also been tested for recovery of Hg2+ from dilute solutions.

Keywords: Ion exchanger, Zirconium(IV) dithanolamine, Sorption of metal ions, Separation of Hg2+ , Cu2+

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 259-264

 

Selective complexometric determination of palladium with sodium metabisulphite as releasing agent

 

Prakash Shettya* & A Nityananda Shettyb

aDepartment of Printing and Media Engineering, Manipal Institute of Technology, Manipal University,
Manipal 576 104, India

bDepartment of Chemistry, National Institute of Technology Karnataka, Surathkal,
Srinivasnagar 574 157, India

Email: prakash.shetty@manipal.edu

 

Sodium metabisulphite has been proposed as a selective releasing agent for the rapid and selective complexometric determination of palladium. Pd(II) present in a given sample solution is first complexed with excess of EDTA and the surplus EDTA is back titrated with standard zinc sulphate solution at pH 5-5.5 (acetic acid-sodium acetate buffer) using xylenol orange as indicator. Sodium metabisulphite solution is then added to displace EDTA quantitatively from the Pd-EDTA complex. The released EDTA is back titrated with standard zinc sulphate solution as before. The method works well in the concentration range 2-20 mg of Pd with a relative error ≤ 0.40% and relative standard deviation ≤ 0.65%. The method has been applied to the determination of palladium in catalysts, alloys and complexes.

Keywords: Palladium determination, Complexometry, Sodium metabisulphite, Releasing agent

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 265-271

 

Determination of amoxycillin in pharmaceutical forms by visible spectrophotometry and HPLC

 

K Basavaiah*, Kalsang Tharpa, N Rajendra Prasad, S G Hiriyanna & K B Vinay

Department of Chemistry, University of Mysore, Manasagangothri, Mysore 570 006, India

Email: basavaiahk@yahoo.co.in

 

Two rapid assay procedures based on visible spectrophotometry and high performance liquid chromatography (HPLC) have been developed for amoxycillin (AMX) in bulk drug and in dosage forms. Spectrophotometric method is based on the formation of a charge-transfer (CT) complex between chloranilic acid (CAA) as a π-acceptor and amoxycillin (AMX) as an n-donor in acetonitrile solvent, the absorbance of the complex being measured at 520 nm. Beers law is obeyed for
10-200
mg mL-1 with an apparent molar absorptivity of 1.3 103 L mol-1 cm-1 and a Sandell sensitivity of 0.2741 g cm-2. The HPLC determination was performed on a reversed phase column (Hypersil C18 5 m; 2504.6 mm i.d) using a mobile phase (1 mL min-1) consisting of acetonitrile-0.1% ortho phosphoric acid (pH 3.0)-60:40 (v/v) with UV-detection at 230 nm. A rectilinear relationship between mean peak area and concentration of AMX was observed in the range 7.2-396 mg mL-1 with a detection limit of 1.5 mg mL-1 and a quantitation limit of 4.5 mg mL-1. Intra-day and inter-day precision, and accuracy of the methods have been established according to the current ICH guidelines. The methods have been successfully applied to the assay of AMX in preparations and the results were statistically compared with those of the reference method by applying Students t-test and F-test.

Keywords: Amoxycillin, Assay, Spectrophotometry, HPLC, Chloranilic acid, Pharmaceuticals

 

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 272-277

 

Influence of preparation method on the performance of Pd/ ZrO2-Al2O3 catalysts for HDS

 

Sufen Chen, Laitao Luo*& Xinsun Cheng

Department of Chemistry, Nanchang University, Nanchang 330031, P.R. China

Email: luolaitao@163.com

 

ZrO2-Al2O3 (I) and ZrO2-Al2O3(S) mixed supports were prepared using impregnation and sol-gel methods, separately. Influences of preparation methods on the properties of Pd based catalysts for hydrodesulphurization (HDS) of thiophene were studied. The prepared samples were characterized by means of XRD, H2-TPD, H2-TPR, XPS, NH3-TPD, H2 chemisorption and BET surface area. Pd/ZrO2-Al2O3(S) catalyst supported on ZrO2-Al2O3 (S) exhibited much higher HDS activity than that of the Pd/ZrO2-Al2O3 (I) catalyst supported on ZrO2-Al2O3 (I). As compared with Pd/ZrO2-Al2O3 (I) catalyst, Pd/ZrO2-Al2O3(S) catalyst has higher dispersion, more acid sites and stronger interaction between palladium and mixed support, which presented an increasing driving-force toward the catalyzed conversion of thiophene.

Keywords: Hydrodesulphurization, Thiophene, Catalyst

 

 

Indian Journal of Chemical Technology

Vol. 16, May 2009, pp. 278-282

 

 

Interfacial area measurement in a gas - liquid ejector for a sodium chloride - air system

 

P T Raghuram

Department of Chemical Engineering

Indian Institute of Science, Bangalore 560 012, India

 

Interfacial area measurement has been carried out experimentally by measuring the bubble size and holdup for air-sodium chloride solution system. The size of the bubble is predominantly established by the air hold up. High speed photography technique for bubble size measurement and gamma ray attenuation method for holdup measurements are followed. The measured values are compared with the theoretically predicted values. Interracial area as a function of the liquid flow rate and also its distance from the nozzle of the ejector has been reported in this paper. The results obtained for this non-reactive system are also compared with those of air-water system.

 

Keywords: Gas-liquid ejector, High speed photography method, Air-sodium chloride system