Indian Journal of Chemical Technology

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VOLUME 13

NUMBER 6

NOVEMBER 2006

CODEN:ICHTEU

 

ISSN:0971-457X

 

CONTENTS

 

Papers

 

 

Sorption of water soluble dyes using inorganic materials as sorbents

539

        IPC Code: C02F1/00, C02F1/42

 

        Amit Jayswal & Uma Chudasama

 

 

Determination of serum glucose with glucose oxidase immobilized onto affixed egg membrane

544

        IPC Code: C13K1/00, C07C

 

        Minakshi Sharma, Vijay Kumar & C S Pundir

 

 

Spectrophotometric and high performance liquid-chromatographic determination of lansoprazole in pharmaceuticals

 

549

        IPC Code: B01D15/00

 

        K Basavaiah, V Ramakrishna, U R Anil Kumar & Udaya Kumar

 

 

Corrosion inhibition of mild steel in 20% HCl by some organic compounds

555

        IPC Code: C23F11/00

 

        D Prakash, Rajesh Kumar Singh & Ranju Kumari

 

 

Synthesis of a new resin functionalized with xanthine moiety and its application for separation of nickel and cadmium in natural water

 

561

        IPC Code: C02F1/00, B01D

 

        Debasish Banerjee & Arabinda K Das

 

 

Kinetic and equilibrium modeling of adsorption of cobalt(II) from aqueous solutions onto surface modified lignocellulosics (Musa paradisiaca)

 

567

        IPC Code: B01D15/00

 

        I G Shibi & T S Anirudhan

 

 

Removal of Cr(VI) from aqueous solution by adsorption onto low cost non-conventional adsorbents

 

576

        IPC Code: B01D15/00

 

        A K Bhattacharya, S N Mandal & S K Das

 

 

Selective hydrogenation of menthone on Raney nickel catalyst

584

        IPC Code: C07B35/02

 

        A Rehman, M Kamil, A K Gupta & A K Bhatnagar

 

 

Studies on bacterial growth and lead(IV) biosorption using Bacillus subtilis

591

        IPC Code: C02F3/00, C12N1/02

 

        Sk Masud Hossain & N Anantharaman

 

Determination of thermo-physical properties of freeze-dried foodstuffs

597

        IPC Code: A23L1/00, A23L1/025

 

        R Chakraborty, A K Saha & P Bhattacharya

 

 

Catalytic activity of anion-modified zirconia, alumina and silica in the esterification of benzyl alcohol with acetic acid

 

605

        IPC Code: C07C27/22, C07C27/00

 

        Joyce D’Souza & N Nagaraju

 

 

Laminar flow heat transfer in concentric equilateral triangular annular channels

614

        IPC Code: C09K5/00

 

        M Venkateswara Rao, P V Ravi Kumar & P S Sankara Rao

 

 

Neural modeling of biochemical systems using CDTA with adaptive learning rate

623

        IPC Code: C09K5/00

 

        K Yamuna Rani & V S Ramachandra Rao

 

 

Application of optimum ANN architecture for heat exchanger modeling

634

        IPC Code: C09K5/00

 

        S A Mandavgane & S L Pandharipande

 

 

Notes

 

 

Vapour phase transesterification over modified ZrO2-Al2O3 and ZrO2-SiO2 for the synthesis of isoamyl salicylate

 

640

        IPC Code: B01J31/00, B01J31/22

 

        Joyce D’Souza & N Nagaraju

 

 

Acridine orange and chlorite reaction-An indicator reaction for the trace determination of Ru(III)

 

644

        IPC Code: B01J23/46

 

        V W Bhagwat, Rajani Vijay, S B Jonnalgadda & Brijesh Pare

 

 

Chem-Tech Scan

 

649

List of referees

 

653

Annual Author Index

 

655

Annual Keyword Index

 

658

Guidelines for authors

661

 

 

 

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 539-543

 

Sorption of water soluble dyes using inorganic materials as sorbents

 

Amit Jayswal & Uma Chudasama*

 

Ion exchange technique has been used for treatment of wastewater containing dyes. Zirconium molybdate (ZM) an inorganic cation exchanger of the class of tetravalent metal acid salt has been used for the purpose. Sorption of dyes namely crystal violet (CV), methyleneblue (MB) and rhodamine6G (R6G) has been carried out on zirconium molybdate by varying pH and flow rate. The dyes can be effectively recovered by using dilute acids such as HCl, HNO3 and H2SO4. Similar studies have also been carried out using zirconia (ZO) for comparison. Considerable differences in the binding of the dyes tested, have been observed. In general, heteropolycyclic dyes exhibit more affinity towards ZM as compared to ZO.

Keywords: Wastewater treatment, Cation exchanger, Zirconium molybdate, Crystal violet, Methylene blue, Rhodamine 6G

IPC Code: C02F1/00, C02F1/42

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 544-548

 

 

Determination of serum glucose with glucose oxidase immobilized onto affixed egg membrane

Minakshi Sharma, Vijay Kumar & C S Pundir*

 

A reusable strip of glucose oxidase (GOD) from Aspergillus niger was prepared by immobilizing the enzyme onto egg albumin membrane affixed on a plastic strip with a conjugation yield of 1.5 mg/cm2 and 66% retention of their initial specific activity. The immobilized enzyme showed maximum activity at pH 7.0 when incubated at 37°C for 15 min. A method for discrete analysis of serum glucose was developed employing this strip. The minimum detection limit of the method was 5 mg/dL. Within and between assay coefficient of variation (CV) for serum were <5 and <6%. A good correlation (r=0.972) was found between glucose values obtained by commercial enzymic colorimetric method employing free GOD and the present method. No significant loss in the strip activity was observed after its 150 regular uses for a period of 40 days, when stored in reaction buffer at 4°C. The method has advantage over commercial enzymic colourimetric method that it provides reuse of glucose oxidase with ease.

Keywords: Glucose, Glucose oxidase, Immobilization, Egg membrane

IPC Code: C13K1/00, C07C

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 549-554

 

 

Spectrophotometric and high performance liquid-chromatographic determination of lansoprazole in pharmaceuticals

K Basavaiah*, V Ramakrishna, U R Anil Kumar1 & Udaya Kumar

 

Two rapid assay procedures based on visible spectrophotometry and high performance liquid chromatography (HPLC) have been developed for lansoprazole in bulk drug and in capsules. Spectrophotometric method is based on the formation of a charge-transfer (CT) complex between chloranilic acid (CAA) as a π-acceptor and lansoprazole (LPZ) as an n-donor in acetonitrile solvent, the absorbance of the complex being measured at 520 nm. Beer’s law is obeyed for 5-80 mg mL-1 with an apparent molar absorptivity of 3.45´103 L mol-1 cm-1 and a Sandell sensitivity of 0.0011 µg cm2-. The HPLC determination was performed on a reversed phase column (Hypersil C18 5 µm; 250´4.6 mm, i.d) using a mobile phase (1 mL min-1) consisting of acetonitrile-0.1% phosphoric acid (pH 3)-70:30(v/v) with UV-detection at 284 nm. A reactilinear relationship between mean peak area and concentration of LPZ was observed in the range 6-248 mg mL-1 with a detection limit of 0.62 mg mL-1 and a quantitation limit of 1.86 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 LPZ in tablet preparations with recoveries varying from 97.14 to 102.3% with standard deviation in the range of 0.57-1.65%. The results were statistically compared with those of the reference method by applying Student’s t-test and F-test. Accuracy, evaluated by means of the spike recovery method was in the range 97.66-106.6%, with precision (RSD) better than 3%.

Keywords: Lansoprazole, Assay, Spectrophotometry, HPLC, Chloranilic acid

IPC Code: B01D15/00

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 555-560

 

Corrosion inhibition of mild steel in 20% HCl by some organic compounds

 

D Prakash*, Rajesh Kumar Singh & Ranju Kumari

Mild steel is very important material for petroleum industry and it is used in several processing units like oil recovery, refining of crude oil, transportation, storage and petroleum products. Processing of crude oil is done in environment having strong acids and at high temperature, hence, rate of corrosion increases during this process. The corrosion inhibitors are used to reduce corrosion damage in sub-surface equipments in oil well field. In this study corrosion inhibition activity of four inhibitors namely 2-mercaptobenzoxazol, 2-mercaptobenzimidazol, N-cetylpyridiniumbromide and propargylbenzene-sulphonate was studied by gravimetric (viz. weight loss) and potentiostatic polarization methods in the temperature range of 30-70şC in presence of 20% HCl.

Keywords: Mild steel, Gravimetric analysis, Potentiostatic polarization, Corrosion inhibition

IPC Code: C23F11/00

 

Indian Journal of Chemical Technology

Vol 13, November 2006, pp. 561-566

 

 

Synthesis of a new resin functionalized with xanthine moiety and its application for separation of nickel and cadmium in natural water

 

 Debasish Banerjee & Arabinda K Das*

 

A new chelating resin has been synthesized by functionalization of polystyrene-divinylbenzene (8%) with xanthine through -N=N- bonding. The resulting resin has been characterized by elemental analysis, thermogravimetric analysis, infrared spectroscopy, hydrogen ion capacity and capacity of metal ions. The separation and mesurement of Ni(II) and Cd(II) were carried out with this resin and the maximum exchange capacity of Cd(II) was found to be 0.73 mmol g-1 and that for Ni(II) was 0.57 mmol g-1 at pH 1.0 for both. The eluents 10% thiourea in 0.1 M HClO4 and 1.0 M sulphosalicylic acid have been used for separation of Cd(II) and Ni(II), respectively. The detection limits for Ni(II) and Cd(II) were found to be 3.6 and 4.1 ng mL-1, respectively . The optimum flow rate and sample breakthrough volume of column operation for both the metal ions were found to be 1.2 mL min-1 and 3000 mL, respectively. The developed method was applied for determination of these two metal ions in synthetic binary mixtures. The developed method was also applied to natural water sample and compared with the results of previously developed method

Keywords: Solid phase extraction, Chelating resin, Xanthine, Nickel (II), Cadmium (II), Natural water

IPC Code: C02F1/00, B01D

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp.- 567-575

 

Kinetic and equilibrium modeling of adsorption of cobalt(II) from aqueous solutions onto surface modified lignocellulosics (Musa paradisiaca)

 

I G Shibi & T S Anirudhan*

 

Banana (Musa paradisiaca) Stalk (BS), an agricultural waste, modified by graft copolymerization reaction might be the basis of a new approach to remove the metal pollutants from water. The treatment process involves graft copolymerization of acrylamide onto BS using ferrous ammonium sulphate/H2O2 redox initiator system followed by functionalization of carboxylate group (PGBS-COOH). In this paper, the efficiency of the PGBS-COOH in the removal of Co(II) from aqueous solutions has been investigated using batch experiments. The influence of different experimental parameters such as pH, contact time, initial concentration of Co(II), adsorbent dose and temperature on the adsorption process has been studied. The maximum adsorption capacity is observed at the pH range 6.5-8.0. Maximum removals of 99.7 and 97.2% are observed at Co(II) concentration of 25.0 and 50.0 mg/L, respectively. A kinetic model based on empirical relationship has been derived to predict the percentage Co(II) removal at any time for known amount of sorbent and initial Co(II) concentration. The surface mass-transfer coefficient as a function of temperature has been determined. Kinetic parameters are also evaluated. The Langmuir isotherm model fitted the experimental equilibrium data. The PGBS-COOH had adsorption capacities for Co(II) from 166.66 mg/g at 30°C to 181.46 mg/g at 60°C. Graft copolymerization of BS—an agricultural waste which is found in abundance and has otherwise no significant use and results in a low cost—value-added product which can benefit industry.

Keywords: Graft copolymerization, Banana stalk, Adsorption, Co(II) removal, Langmuir isotherm

IPC Code: B01D15/00

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 576-583

 

Removal of Cr(VI) from aqueous solution by adsorption onto low cost non-conventional adsorbents

 

A K Bhattacharya, S N Mandal & S K Das

 

Adsorption behavior of chromium, Cr(VI) from wastewater has been investigated using clarified sludge (a steel plant waste material), rice husk ash and sawdust as non-conventional adsorbents. The studies were carried out at room temperature (30oC) following batch adsorption technique in a reciprocating shaker. Factors affecting the adsorption characteristics such as agitation time, initial metal ion concentration, adsorbent dose and pH were studied. Maximum adsorption of Cr(VI) was observed at pH 3. The experimental data fitted to Langmuir and Freundlich isotherms. The adsorption process found to follow Lagergren first order kinetics model. Adsorption capacity has been observed to follow the order clarified sludge > rice husk ash > sawdust. At pH 3 and initial Cr(VI) concentration of 3 mg/L more than 99% removal of Cr(VI) may be possible. The maximum amount of adsorbed metal (qmax) value is significantly influenced by liquid/solid ratio and by the pH values of the metal solutions.

Keywords: Adsorption, Non-conventional adsorbent, Lagergren model, Chromium(VI)

IPC Code: B01D15/00

 

 

Indian Journal of Chemical Technology

Vol 13, November 2006, pp. 584-590

 

Selective hydrogenation of menthone on Raney nickel catalyst

 

A Rehman, M Kamil*, A K Gupta & A K Bhatnagar

 

The present study deals with the selective hydrogenation of menthone to menthol in a Parr reactor. The reactions are carried out in the temperature range of 100-200°C, pressure range of 5-20 kg/cm2, 100 mL solvent and catalyst to substrate ratio ranging from 0-10% for a reaction time of 4-5 h. The samples are then analyzed using a gas chromatograph for determining the conversion and then selectivities are determined. The effect of various parameters such as reaction temperature, pressure, reaction time, type of solvent, type of catalyst, catalyst to substrate weight ratio, preactivation of the catalyst and precalcination of the catalyst on the selectivity and conversion was investigated. Optimization of process parameters was attempted to maximize the yield of menthol.

Keywords: Hydrogenation, Menthone, Menthol, Raney nickel catalyst

IPC Code: C07B35/02

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 591-596

 

 

Studies on bacterial growth and lead(IV) biosorption using Bacillus subtilis

 

Sk Masud Hossain* & N Anantharaman

 

Gram-positive bacterium Bacillus subtilis biosorbs lead(IV) ion from its aqueous solution. The maximum biosorption of lead is 97.68% (w/w) within 48 h of incubation time with optimum pH 4.5 and optimum temperature 40°C for 700 ppm initial loading of lead in a shake flask (optimum rpm 60). 7 days old and 30% (v/v) of suspension inoculum culture is used in the studies. Lead is measured by using atomic absorption spectrophotometer (AAS) into an air-acetylene flame and absorbance is measured at 283.3 nm. The maximum bacterial growth is noticed as 4.90´108 cells/mL at optimum bioprocess conditions.

Keywords: Bacteria, Biosorption, Incubation, Lead

IPC Code: C02F3/00, C12N1/02

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 597-604

 

Determination of thermo-physical properties of freeze-dried foodstuffs

R Chakraborty*, A K Saha &  P Bhattacharya

 

The thermo-physical properties of some important foodstuffs have been estimated and are correlated with temperature and pressure using semi-empirical technique. For determination of thermal conductivities (k) of paneer and mango samples, ‘Uniformly Retreating Ice Front’ (URIF) model has been used at two different methods of freezing conditions i.e. conventional slow freezing and rapid cryogenic freezing. In all the cases, linear equation expressing k as dependent variable with chamber pressure (P) [ranging from 0.003 to 0.05 mbar] and average temperature of dried layer (T) [ranging from 275 to 295 K] as independent variables has been established. The heat capacity, Cp of different freeze-dried foodstuffs have been determined experimentally using ‘Differential Scanning Calorimeter’ for a wide range of temperature at specific values of moisture content of practical significance. The equations of the best fit curves are also presented, enabling one to estimate the heat capacity value for freeze dried foodstuff (with specified moisture content) at any temperature within the range of 258 to 319 K. 

Keywords: Thermal conductivity, URIF model, Heat capacity, Freeze dried foodstuffs

IPC Code: A23L1/00, A23L1/025

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 605-613

 

Catalytic activity of anion-modified zirconia, alumina and silica in the esterification of benzyl alcohol with acetic acid

 

Joyce D’Souza & N Nagaraju*

 

The catalytic activity of zirconia, alumina and silica and their sulphate, phosphate and borate modified forms has been studied in the liquid phase esterification of benzyl alcohol with acetic acid for the synthesis of benzyl acetate. All these catalysts have been found to be active for the formation of benzyl acetate with 100% selectivity. A small amount of dibenzyl ether was formed only in the case of sulphated zirconia when refluxed for more than 12 h. The active sites with ‘weak to intermediate’ acid strengths may be responsible for the catalytic activity towards the esterification. Sulphated zirconia is the most suitable catalyst providing 53 to 90% yield of benzyl acetate when refluxed for 30 min to 24 h with 0.1 to 3 g of the catalyst. This catalyst has been found to be effective in catalyzing the esterification of n-propanol, iso-propanol, n-butanol and iso-butanol with acetic acid to form the respective esters in good yields.

Keywords: Esterification, Benzyl acetate, Solid acids, Sulphate-, Borate-, Phosphate-modified zirconia, Alumina and silica

IPC Code: C07C27/22, C07C27/00

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 614-622

 

 

Laminar flow heat transfer in concentric equilateral triangular annular channels

M Venkateswara Rao*, P V Ravi Kumar & P S Sankara Rao

 

The problem of laminar flow heat transfer in channels of annular cross section formed by concentric equilateral triangles is studied. Numerical solutions for friction factor, and magnitude of minimum limiting Nusselt numbers for both constant heat input per unit length and constant wall temperature are obtained. The results obtained by the numerical method are compared with the available solutions for the limiting geometries of equilateral triangle and parallel plates. Experimental data for isothermal pressure drop and constant wall temperature boundary condition at the outer wall are presented. Test sections with length to equivalent diameter ratios of 13.85, 15.12 and 20.8 are employed in the present investigation. The Prandtl numbers are varied from 4 to 65 applying Glycerol-water mixture as coolant. Empirical correlations for isothermal friction factor and Nusselt number for constant wall temperature boundary conditions are presented.

Keywords: Laminar flow, Equilateral triangular annulus, Friction factor, Limiting Nusselt number

IPC Code:  C09K5/00

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 623-633

 

Neural modelling of biochemical systems using CDTA with
adaptive learning rate+

 

K Yamuna Rani* & V S Ramachandra Rao

 

Artificial neural networks are becoming increasingly popular as tools to represent chemical/biochemical process dynamics. A combined design and training algorithm (CDTA) is proposed in this study to simultaneously perform network architecture selection and training of the network weights. The proposed CDTA uses a modified back propagation learning method based on a new adaptive learning rate mechanism. The performance of the CDTA is illustrated through application to two typical fermentation systems, namely a SISO anaerobic digester and a MIMO continuous stirred tank fermenter. The adaptive learning rate method is shown to achieve faster convergence than the fixed learning rate method. The network generated is able to represent the fermentation processes accurately, which is illustrated through the reproduction of the training data set as well as through generalization data sets of responses to combinations of load disturbances and set point changes in both SISO and MIMO cases. This study demonstrates that the proposed CDTA can be used to find a neural network representation of chemical/biochemical process dynamics.

Keywords: Artificial neural network, Combined design and training algorithm

IPC Code: C09K5/00

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 634-639

 

Application of optimum ANN architecture for heat exchanger modeling

 

S A Mandavgane* & S L Pandharipande

 

The shell and tube heat exchanger is a common type used for heating or cooling of process fluids. The various parameters to be taken into account for developing a model are inlet and outlet temperatures of shell and tube side fluids and their flow rates. Artificial Neural Networks (ANN) are effective in modeling of non-linear multi variable relationships and also referred as black box models. For modeling of shell and tube heat exchanger, ANN architecture has been optimized. In this paper the optimized ANN architecture is employed for water-20% glycerin and water-40% glycerin systems for estimation of exit temperature of both the fluids as a function of inlet temperature conditions and also flow rates. It is observed that ANN model with three hidden layers (4-15-15-15-2) has good level of accuracy (98-99.5%) for predicted values of training and test data set.

Keywords: ANN, Shell and tube heat exchanger and modeling, Optimization

IPC Code: C09K5/00

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 640-643

 

Vapour phase transesterification over modified ZrO2-Al2O3 and ZrO2-SiO2 for the synthesis of isoamyl salicylate

 

Joyce D’Souza & N Nagaraju*

 

Vapour phase transesterification of methyl salicylate with isoamyl alcohol in the presence of simple oxides, mixed oxides and their modified forms as catalysts was carried out. A systematic study was made with zirconia, alumina and silica and the complete series of zirconia-alumina and zirconia-silica mixed oxides for 10-100% composition of zirconia, as well as the sulphate, phosphate and borate treated forms to identify the most suitable catalyst for this reaction. All the catalysts used for the study exhibited catalytic activity for this transesterification reaction. The only side-product formed was phenol, apart from the primary byproduct methanol. The catalytic activity of zirconia, alumina and silica is in the range of 12 to 15%. There is a significant increase in the catalytic activity when these simple oxides are modified by sulphate, borate and phosphate ions. The trend in the increase in activity on modification is zirconia > alumina > silica. Among the anions, the trend in the increase in the activity is sulphate > phosphate > borate. However, the phosphated forms score over the sulphated forms for this reaction because (a) the activity of phosphated forms does not reduce with time on stream up to 2 h while there is a noticeable reduction in the catalytic activity of sulphated forms within 15 minutes from the start of the reaction and (b) there is no coke formation when the phosphated forms are used while sulphated forms lead to excessive coke formation and loss of reactants. The mixed oxide ZrO2-Al2O3 of 20% ZrO2 composition modified with phosphate ions is found to be the most suitable catalyst for this reaction.

Keywords: Transesterification, Sulphate-, Borate-, Phosphate-modified zirconia, Alumina, Silica, Solid acids, Isoamyl

                salicylate

IPC Code: B01J31/00, B01J31/22

 

 

Indian Journal of Chemical Technology

Vol. 13, November 2006, pp. 644-647

 

Acridine orange and chlorite reaction  — An indicator reaction for the trace
determination of Ru(III)

 

V W Bhagwat, Rajani Vijay, S B Jonnalgadda & Brijesh Pare*

 

Catalysis by transition metal ions plays an important role in understanding the mechanistic aspects of a particular redox reaction. Ru(III) acts as an efficient and potential catalyst in many redox reactions. Hence the use of Ru(III) chloride as a homogeneous catalyst in acidic medium is of present interest. Based on the highly selective catalytic efficiency of Ru(III) on the oxidation of acridine orange {3,6-bis (dimethylamino) acridine zinc chloride double salt}(AO+) by acidic chlorite, a fixed-time kinetic analytical procedure for determination of Ru(III) is developed. The lowest determination limit attainable with the developed method is 1.01 ng/mL. The method allows determination of Ru(III) with no interference from a wide range of cations. Tolerance ratios have also been computed. With excess concentration of reactants, both un-catalyzed and catalyzed reactions follow a pseudo-first order kinetics in [AO+], fractional order kinetics in oxidant and first order kinetics in catalyst [Ru(III)]. The rate coefficient of the un-catalyzed reaction is 4.45´10-4 s-1 while the catalytic constant for the catalyzed reaction is 8.00´10-4 s-1. Retarding effect of increasing ionic strength suggests the involvement of oppositely charged species in rate determining step. A tentative mechanism has also been proposed based on the results of variation of various factors.

Keywords: Ruthenuim(III) determination, Acridine orange, Acidic catalysis

IPC Code: B01J23/46