Indian Journal of Chemical Technology

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VOLUME 14

NUMBER 2

MARCH 2007

CODEN:ICHTEU

 

ISSN:0971-457X

 

CONTENTS

 

Papers

 

 

Synthesis of PAN nanoparticles via nonconventional microemulsion technique using Co(II)/EDTA in situ complex

 

119

        IPC Code: C08F2/00, C08J3/00

 

        Trinath Biswal & Prafulla K Sahoo

 

 

Synthesis, characterization and kinetic studies of PEMA grafted acacia gum

126

        IPC Code: C08F246/00

 

        S Samui, A K Ghosh, Md A Ali & P Chowdhury

 

 

Chemical modification of Norway spruce (Picea abies (L) Karst) wood with melamine formaldehyde resin

 

134

        IPC Code: C08G63/00, B27K1/02

 

        Manabendra Deka, Wolfgang Gindl, Rupert Wimmer & Christian H

 

 

Photodegradation of methylene blue dye using UV/BaTiO3, UV/H2O2 and UV/H2O2/BaTiO3 oxidation processes

 

139

        IPC Code: C09B, C07B33/00

 

        G M Madhu, M A Lourdu Antony Raj, K Vasantha Kumar Pai & Shreyas Rao

 

 

Parametric optimization of photocatalytic degradation of catechol in aqueous solutions by response surface methodology

 

145

        IPC Code: B01J21/00

 

        S K Kansal, M Singh & D Sud

 

 

Synthesis and characterization of LaCoO3 based cathode and its chemical compatibility with CeO2 based electrolytes for intermediate temperature solid oxide fuel cell (ITSOFC)

 

154

        IPC Code: C22B59/00, H01M8/00

 

        A Samson Nesaraj, I Arul Raj & R Pattabiraman

 

 

Electro catalytic amorphous nickel alloy

161

        IPC Code: C22C45/04, C25B1/44

 

        V S Muralidharan

 

 

Studies on sulphonates for enhanced oil recovery

166

        IPC Code: C07C9/00, C10G7/10

 

        A K Singh & O N Anand

 

 

Alkaline hydrolysis of poly(ethylene terephthalate) in presence of a phase transfer catalyst

173

        IPC Code: C08F4/00, C08G77/445

 

        J Das, A B Halgeri, V Sahu & P A Parikh

 

Prediction of vapour-liquid equilibrium of some binary liquid systems by Generalized London Potential method

 

178

        IPC Code: B30B9/00

 

        A Guha & Rupa Pal

 

 

Solubility of acenaphthene in pure non-aqueous solvents between 298.15 and 333.15 K

183

        IPC Code: C10H35/00

 

        M Thenmozhi, S Parvin Banu & T Karunanithi

 

 

Viscometric studies of binary non-aqueous liquid mixtures at 303.15 K

189

        IPC Code: G01N9/00

 

        A Ali & M Tariq

 

 

Concentration control of silica in water chemical regime for natural circulationhigh pressure drum boiler unit of thermal power station

 

195

        IPC Code: C08K3/36, B01B1/00, B01J21/08

 

        M Azad Sohail & A Ismail Mustafa

 

 

Titrimetric and spectrophotometric determination of zidovudine in pharmaceuticals using chloramine-T and two dyes

 

200

        IPC Code: G01J3/00, A61K9/00

 

        K Basavaiah & U R Anil kumar

 

 

Notes

 

 

Solid phase extraction and estimation of cadmium using glycine immobilized cellulose chelating resin

 

204

        IPC Code: C22B17/00, A61K

 

        Parul Singh, S Mittal & R K Sharma

 

 

Complexometric determination of mercury(II) using 2-thiobarbituric acid as a releasing agent

209

        IPC Code: C22B43/00, B01

 

        J Karthikeyan, P Parameshwara, A Nityananda Shetty & Prakash Shetty

 

 

Author Index

 

213

Keyword Index

 

214

Guidelines for Authors

215

 

 

 

 

 

 

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 119-125

 

Synthesis of PAN nanoparticles via nonconventional microemulsion technique using Co(II)/EDTA in situ complex

Trinath Biswal & Prafulla K Sahoo*

 

Synthesis of polyacrylonitrile nanoparticles was carried out under the catalytic effect of in situ developed Co(II)/EDTA complex with ammonium persulphate as initiator, in the absence of added emulsifier. The microemulsion polymerization was studied at varying concentrations of initiator, monomer, complex and solvent over a temperature range of 30-70°C. The overall activation energy (Ea, 49.79 kJ/mol), energy of dissociation of initiator (Ed, 82.68 kJ/mol), number of micelles
(0.163
´ 1018) and the viscosity average molecular weight of the polymer were computed. The distribution of particle sizes was determined by transmission electron microscopy (TEM). It was found that the oil-in-water polymerization was stabilized by the presence of the CoCl2/EDTA in situ complex reducing the particle size into nano order. The average diameters of PAN nano particles, obtained by TEM, were in the range of 50-150 nm at maximum conversion. The experimental particle size was mainly dependent on the concentration of complex and temperature.

Keywords: Microemulsion, CoCl2/EDTA in situ complex, Nano particle, Kinetics, TEM

IPC Codes: C08F2/00, C08J3/00

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 126-133

 

Synthesis, characterization and kinetic studies of PEMA grafted acacia gum

S Samui, A K Ghosh, Md A Ali & P Chowdhury*

 

Graft polymerization of ethyl methacrylate (EMA) onto acacia gum (AG) has been studied. The grafting was found to be optimal under the following reaction conditions: gum 0.4 g/dL, monomer 0.066 mol/dL, H2SO4 0.037 mol/dL, ceric ammonium sulphate 0.0009 mol/dL, temperature 50°C and time 3.5 h.  FTIR spectroscopy was used for the confirmation of grafting. Thermal, physical and biodegradation properties of the copolymer were studied. A probable mechanism of polymerization has been suggested based on reaction kinetics.

Keywords: Acacia gum, Graft polymerization, Reaction kinetics, FTIR, Biodegradation

IPC Code: C08F246/00

 

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 134-138

 

Chemical modification of Norway spruce (Picea abies (L) Karst) wood with melamine formaldehyde resin

 

Manabendra Deka*, Wolfgang Gindl, Rupert Wimmer & Christian H

 

Impregnation of Norway spruce soft wood with melamine formaldehyde (MF) resin under vacuum-pressure process showed promising potential to improve number of properties, such as, dimensional stability and surface hardness. In this study, MF resin impregnated wood was evaluated at different levels of weight percent gain (WPG) compared to untreated one, mainly for dimensional stability and surface hardness. The modified wood, at 22.9 level of WPG possessed increase in dimensional stability in terms of anti-swelling efficiency and surface hardness by 17.5% and 124% over untreated, control. Chemical adherence and/or reaction takes place onto wood cell wall components other than cell lumens, which was proved by vertical density profile (VDP), UV microscopic and scanning electron microscopic (SEM) studies.

Keywords: Norway spruce soft wood, Melamine formaldehyde resin, Picea abies, Dimensional stability, Surface hardness, Impregnated wood

IPC Codes: C08G63/00, B27K1/02

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 139-144

 

Photodegradation of methylene blue dye using UV/BaTiO3, UV/H2O2 and UV/H2O2/BaTiO3 oxidation processes

 

G M Madhu, M A Lourdu Antony Raj*, K Vasantha Kumar Pai & Shreyas Rao

 

The photocatalytic degradation of methylene blue (MB) in aqueous solution was studied using UV source in presence of synthesized BaTiO3 as photocatalyst and in combination with different concentrations of H2O2. The experiments were carried at different catalyst loading (0.05 & 0.1 wt %), pH (3, 7 & 9) and H2O2 dosage (0.5 – 6 mL/L). The degradation rate was found to be strongly dependent upon various experimental parameters such as catalyst loading, pH, and dosage of H2O2. There was no appreciable degradation seen in presence of catalyst alone. Discoloration of the dye was very nearly complete using UV/H2O2. Neither UV radiation nor H2O2 alone was able to decolourize the dye. The best degradation results were observed under optimum conditions of catalyst loading of 0.05 wt%, pH 9 for BaTiO3/UV system. The optimum dosage of H2O2 for 12 ppm concentration of the dye was found to be 2 mL/L for UV/H2O2. The experimental kinetic data on the degradation of the dye followed the pseudo first order rate. Tests were further carried out for degradation of the dye using BaTiO3/UV/H2O2 system. An enhancement in the degradation rate was observed with this system compared to UV/H2O2 system.

Keywords: Methylene blue, BaTiO3, Photocatalytic, Discolouration

IPC Codes:                C09B; C07B33/00

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 145-153

 

Parametric optimization of photocatalytic degradation of catechol in aqueous solutions by response surface methodology

 

S K Kansal*, M Singh & D Sud

 

In this paper, performance of a photocatalytic process for degrading catechol with titanium dioxide and zinc oxide catalysts is described. Response surface methodology (RSM) has been used to plan and analyze the experiments. The factors investigated include catalyst dose, pH and amount of oxidant. The performance of photocatalytic process was investigated in terms of percentage degradation (residual catechol concentration). The experimental results indicated that the proposed mathematical model could adequately describe the performance of the factors being investigated. Further the results showed that catalyst dose and amount of oxidant have significant effect on the degradation process. Photodegradation efficacy was confirmed under optimized conditions. The study was further extended to explore the degradation process under sunlight using titanium dioxide and zinc oxide as photocatalysts.

Keywords: Photocatalysis, Titanium dioxide, Zinc oxide, Response surface methodology, UV light, Catechol

IPC Code: B01J21/00

 

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 154-160

 

Synthesis and characterization of LaCoO3 based cathode and its chemical compatibility with CeO2 based electrolytes for intermediate temperature solid oxide fuel cell (ITSOFC)

A Samson Nesaraj*, I Arul Raj & R Pattabiraman

 

The use of alternate cathode materials with improved performance and without any chemical reaction with adjoining electrolyte is required for a reduction in operating temperature of SOFC from 1273 K to about 1073 K (ITSOFC). Cobalt containing perovskite oxides such as LaCoO3 tend to exhibit a higher ionic conductivity due to a greater concentration of oxygen vacancies than other perovskite oxides. The mixed ionic and electronic conducting cathode of the La1-xSrxCoO3-d systems has shown the lowest cathodic overpotential for an SOFC air electrode. In this research work, fine powders of La0.70Sr0.30CoO3-d (LSC) cathode and Ce0.90Gd0.10O2-d (GDC) and Ce0.80Sm0.20O2-d (SDC) are synthesized by glycine nitrate combustion synthesis and systematically characterized by XRD and particle characteristics. The electrical properties of LSC cathode and GDC and SDC electrolytes are also studied. But, the crucial requirement for applicability of LSC cathode is its chemical compatibility in conjunction with the alternate solid electrolytes, GDC and SDC without any phase formation. The XRD studies showed no reaction products when the La0.70Sr0.30CoO3-d cathode is mixed and calcined with GDC and SDC electrolyte at 1573 K. Hence, the LSC cathode may be combined with CeO2 based electrolytes in ITSOFC application.

Keywords: Solid oxide fuel cell, Perovskite oxide, Intermediate temperature

IPC Codes: C22B59/00, H01M8/00

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 161-165

 

Electro catalytic amorphous nickel alloy

 

V S Muralidharan

 

Nickel and nickel based alloy deposits are used as cathode materials for hydrogen evolution. Watt’s bath modified with thiourea was used to deposit Ni-S and Ni-S-Co alloys. In presence of thiourea, Watt’s bath offered amorphous Ni-S alloy. In presence of CoCl2 and thiourea, amorphous Ni-S-Co alloy was formed. Hydrogen evolution reaction occurred faster on amorphous Ni-S-Co alloy compared to amorphous Ni-S alloy from 28 wt% NaOH. Hydrogen evolution reaction rate increased with temperature on these amorphous alloys. A fast Volmer followed by slow Heyrovsky reaction occurred on the surfaces of these alloys. Heat treatment of amorphous Ni-S-Co alloy decreased the electro catalytic activity due to the disturbance in the amorphous structure.

Keywords: Amorphous alloy, Electro catalysis, Hydrogen evolution, Ni-S-Co alloy

IPC Codes: C22C45/04, C25B1/44

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 166-172

 

Studies on sulphonates for enhanced oil recovery

A K Singh* & O N Anand

 

The hydrocarbon/surfactant solution IFT characteristics for several commercial and synthesized sulphonates were studied with various alkanes and the crude oils. It was found that only sulphonates of specific structures and their combination in specific proportions produced ultra low interfacial tension (ULIFT) (<10-2 dynes/cm) with specific hydrocarbons and crude oils. The mixtures of sulphonates of specific structures in specific proportion, which produced ultra low tension with one or more crude oil also, gave higher tertiary recovery under laboratory conditions as compared to commercial sulphonates. The solubilization of hydrocarbons by sulphonates studied also show that very high solubilization (20 moles/g) of sulphonates is highly specific and depends upon the structure of sulphonates and their specific combinations in specific proportions. None of the commercial sulphonates solubilized crude oil in large quantities and only a few combinations of sulphonate solutions solubilized large quantities of different crude oils. These sulphonates produced much higher oil recovery of Ankleswar crude under laboratory conditions in low-tension floods. It is recommended that pilot studies be taken for synthesis of these sulphonates in large quantities for undertaking field trials to study the tertiary oil recovery from Indian oil fields and the economics of recovery and conditions of substantial recovery of crude oil established in view of high crude oil prices prevalent from time to time.

Keywords: Enhanced oil recovery, Sulphonates, Interfacial tension, Crude oil, Reservoir

IPC Codes: C07C9/00, C10G7/10

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 173-177

 

Alkaline hydrolysis of poly(ethylene terephthalate) in presence of a
phase transfer catalyst

 

J Das, A B Halgeri, V Sahu & P A Parikh*

 

Poly(ethylene terephthalate) (PET) powder was hydrolyzed at atmospheric pressure in 5-10 wt% aqueous NaOH at 95°C for 100 min using some phase transfer catalysts (PTC) with an intention to recover the starting monomers from the waste PET. The intent behind attempting new PTC was to carry out the reaction at milder conditions than those reported in the literature. One of the monomers, terephthalic acid (TPA) was produced in the presence of a PTC during the alkaline hydrolysis of PET. The TPA yield agreed with the degree of hydrolysis of PET. Benzalkonium chloride (BKC) was found to be the most effective catalyst among the ones studied. Operating parameters such as NaOH concentration, catalyst concentration and reaction temperature were optimized.

Keywords: Poly(ethylene terephthalate), Benzalkonium chloride, Phase transfer catalyst

IPC Codes:                C08F4/00, C08G77/445

 

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 178-182

 

Prediction of vapour-liquid equilibrium of some binary liquid systems by Generalized London Potential method

 

A Guha* & Rupa Pal

 

A novel ab initio method (named the generalized London Potential method) has been developed by Homer et al.6,9 to predict vapour- liquid equilibrium data for binary mixtures. By this approach, the activity coefficients, vapour- phase composition and total vapour pressures of series of different kinds of binary liquid mixtures such as (i) C6H6-CCl4,
(ii) cC6H12-CCl4, (iii) cC5H10-CCl4, (iv) cC6H12-C6H6, (v) cC5H10-C6H6, (vi) C6H6-CH3OH, (vii) C6H6-C2H5OH
(viii) cC6H12-C2H5OH, (ix) CH3OH-C2H5OH, (x) water-C2H5OH are calculated and the result obtained are compared with experimental data. Reasonable agreement is found between predicted and experimental data for only non-polar simple systems.

Keywords: Vapour-liquid equilibrium, London potential method, Binary liquid mixture, Activity cofficient

IPC Code: B30B9/00

 

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 183-188

 

Solubility of acenaphthene in pure non-aqueous solvents
between 298.15 and 333.15 K

 

M Thenmozhi*, S Parvin Banu & T Karunanithi

 

Binary solid-liquid equilibria (SLE) for the systems acenaphthene +benzene, +methanol, +2-propanol, +2-methyl-propan-1-ol, +ethyl acetate, +methyl ethyl ketone, +acetone, +chloroform are reported in the temperature range of 298.15 K to 333.15 K. The predictive ability of UNIFAC model as applied to SLE data of these systems is evaluated by comparing with the experimental values using percent relative deviation (%RD). Scope for improvements in UNIFAC model is analyzed based on the application of this model to SLE involving polycyclic aromatic compounds.

Keywords: SLE, Acenaphthene, UNIFAC, Polycyclic aromatic hydrocarbons (PAHs)

IPC Code: C10H35/00

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 189-194

 

Viscometric studies of binary non-aqueous liquid mixtures at 303.15 K

 

A Ali* & M Tariq

 

Viscosities, h, of dimethylsulphoxide (DMSO), 1-butanol, 1-hexanol, 1-heptanol and those of their binary mixtures having DMSO as a common component have been experimentally measured at atmospheric pressure and 303.15 K. The experimental data have been used to calculate the deviation in viscosities, Dlnh, and excess Gibbs free energy of activation of viscous flow, DG*E. The experimental viscosity deviation, Dlnh, have also been compared with theoretically calculated, Dlnhth, using Bloomfield-Dewan theory. These parameters were used to study the nature and extent of interaction between the component molecules in the present binary mixtures. Moreover, various semi-empirical correlations were used to estimate the viscosities of the present binary mixtures. The results are given in terms of average standard percentage deviations from experimentally measured one.

Keywords: Liquid mixtures, Viscosity, Bloomfield-Dewan theory, Semi-empirical relations

IPC Code: G01N9/00

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 195-199

 

Concentration control of silica in water chemical regime for natural circulation high pressure drum boiler unit of thermal power station

M Azad Sohail* & A Ismail Mustafa

 

The effective relations of silica (SiO2) concentration in boiler drum and generated steam, with respect to pH and pressure for a natural circulation water wall tubes (WWTs) high-pressure (158 and 100 kGf cm-2) boiler, (Type TGME-206-COB, Russia) at Ghorasal Thermal Power Station (GTPS) Bangladesh, has been studied. Extensive analyses of different parameters of boiler water chemical regime (WCR) of the plant based experimental results revealed that on maintaining SiO2 0.35 (± 0.15) mgL-1 in boiler drum clean (evaporation) section [at pH 9.1 (± 0.1), temperature 330°C (± 10°C)] of boiler WCR provides excellent results with less corrosion or scale formation in interior surface of boiler WWTs and turbine blades. Such a procedure is effective for high softening of make up water SiO2 0.02 (± 0.01 mgL-1) ensuring high degree of purity of feed water cycle of the boiler and appropriate dosing of chemicals in boiler.

Keywords: Boiler drum, Silica, Corrosion

IPC Codes: C08K3/36, B01B1/00, B01J21/08

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 200-203

 

Titrimetric and spectrophotometric determination of zidovudine in pharmaceuticals using chloramine-T and two dyes

 

K Basavaiah*& U R Anil kumar

 

Three new methods using titrimetry and spectrophotometry are described for the assay of zidovudine (ZDV) in bulk drug and in dosage forms using chloramine-T (CAT) and two dyes, methyl orange and indigocarmine, as reagents. Titrimetry involves treating of ZDV with a measured excess of CAT in hydrochloric acid medium, and after the oxidation of ZDV is seemed to be complete, the unreacted oxidant is determined iodometrically. Spectrophotometric methods entail the addition of a known excess of CAT to ZDV in hydrochloric acid medium followed by determination of residual oxidant by reacting with a fixed amount of either methyl orange and measuring the absorbance at 520 nm (Method A) or indigo carmine and measuring the absorbance at 610 nm (Method B). In all the methods, the amount of CAT reacted corresponds to the amount of ZDV. In titrimetric method, the reaction follows a reaction stoichiometry of 1:1 (ZDV: CAT), and is applicable over a range 3-10 mg of ZDV. In spectrophotometric methods, the absorbance is found to increase linearly with concentration of ZDV. The systems obey Beer’s law for 0.5-5.0 and 2.5-20.0 mg mL-1 for method A and method B, respectively. The apparent molar absorptivities are calculated to be 3.4´104 and 7.4´103 L mol-1 cm-1 for method A and method B, respectively. The methods were successfully applied to the assay of ZDV in tablet and capsule formulations.

Keywords: Zidovudine, Assay, Titrimetry, Spectrophotometry, Chloramine-T, Formulations

IPC Codes: G01J3/00, A61K9/00

 

 

Indian Journal of Chemical Technology

Vol. 14, March 2007, pp. 204-208

 

Solid phase extraction and estimation of cadmium using glycine immobilized cellulose chelating resin

 

Parul Singh*, S Mittal & R K Sharma

 

A simple and rapid method of preconcentration and determination of cadmium by both batch and column techniques using glycine immobilized cellulose is presented. Cadmium ion is quantitatively retained on the column packed with immobilized cellulose in the pH range of 6.6-7.8. The distribution coefficient for cadmium is found to be 2.32´102 mL g-1. The method is successfully applied to the determination of cadmium content in water and cigarette samples.

Keywords: Solid phase extraction, Chelating resin, Cellulose, Glycine, Preconcentration

           IPC Codes: C22B17/00, A61K

 

Indian Journal of Chemical Technology

Vol. 14, March. 2007, pp. 209-211

 

Complexometric determination of
mercury(II) using 2-thiobarbituric acid as a releasing agent

 

J Karthikeyan, P Parameshwara, A Nityananda Shetty* & Prakash Shetty

 

A simple and selective complexometric method for the determination of mercury is proposed, based on the selective releasing ability of 2-thiobarbituric acid towards mercury(II). Mercury(II) present in a given sample solution is first complexed with an excess of EDTA and the unreacted EDTA is titrated against zinc sulphate solution at pH 5-6 (hexamine buffer) using xylenol
orange as the indicator. An excess of a 0.25% solution of 2-thiobarbituric acid is then added to displace EDTA from the Hg(II)-EDTA complex. The released EDTA is estimated. Reproducible and accurate results are obtained for 3-95 mg of mercury(II) with coefficient of variation not more than 0.34%. The effects of various ions were studied. The method is used for the analysis of mercury in its synthetic alloy mixtures and also in complexes.

 

Keywords: Mercury(II) determination, 2-Thiobarbituric acid, Masking reagent, Complexometric titration, EDTA

           IPC Codes: C22B43/00, B01