Indian Journal of Chemical Technology

 

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VOLUME 13

NUMBER 4

JULY 2006

CODEN:ICHTEU

 

ISSN:0971-457X

 

CONTENTS

 

Papers

 

 

Physico-chemical and surface characterization of adsorbent prepared from groundnut shell by ZnCl2 activation and its ability to absorb colour

319

        IPC Code: B01D15/00, C01B31/00

 

        R Malik, D S Ramteke & S R Wate

 

 

Methylation of toluene over MnAPO-11 and ZAPO-11

329

        IPC Code: C12P5/00, CO2F11/04

 

        K Joseph Antony Raj, A Dayalan & V R Vijayaraghavan

 

 

Alkylation of benzene with aqueous solution of ethanol over ZSM-5 catalysts

334

        IPC Code: C07B37/00

 

        Jun-Jun Yuan & Borje S Gevert

 

 

Synthesis, characterization and photocatalytic studies of some metal phthalocyanines

341

        IPC Code: C07D487/22

 

        Pritam Borker & A V Salker

 

 

Development and characterization of groundnut shell lignin modified phenol formaldehyde wood adhesive

347

        IPC Code: C09J5/00

 

        M A Khan & S M Ashraf

 

 

Sensitive bromatometric methods for the assay of metaprolol tartrate in dosage forms

353

        IPC Code: A61K9/08

 

        K Basavaiah, B C Somashekar & V Ramakrishna

 

 

Application of bromate-bromide mixture and methyl orange in the titrimetric, spectrophotometric and kinetic assay methods for cyproheptadine in pharmaceuticals

360

        IPC Code: G01J3/00

 

        K Basavaiah

 

 

Electrosynthesis and photoelectrochemical studies on (CdHg)S

367

        IPC Code: C25B1/00

 

        Kehar Singh & Sameer S D Mishra

 

 

Preparation and some properties of lithium vanadium bronzes

372

        IPC Code: C01G31/00

 

        A M El-Sayed & S M A Mousa

 

Mass integration for recovery of zinc from galvanizing and metal finishing industry using supertargeting approach

378

        IPC Code: C22B9/00

 

        Shabina Khanam & Bikash Mohanty

 

 

Dissolution kinetics of iron from diasporic bauxite in hydrochloric acid solution

386

        IPC Code: C21B15/00

 

        Gulsemin Gulfen, Mustafa Gulfen & Ali Osman Aydin

 

 

Determination of the optimum conditions for dissolution of magnesite with H2SO4 solutions

391

        IPC Code: C01B6/21

 

        Yuksel Abali, Mehmet Copur & Mesut Yavuz

 

 

Enhancement of viscosity index of mineral base oils

398

        IPC Code: G01N, C07C7/00

 

        Sabiha Tanveer & Ram Prasad

 

 

Studies on yield improvement of High Melting Explosive (HMX)

404

        IPC Code: C06B

 

        S Das, V D Raut, N M Gawande, R S Khopade & V L Narasimhan

 

 

Notes

 

 

Cetyldimethyl benzyl ammonium cerium nitrate as a phase-transfer oxidant in the oxidation of alcohols to carbonyl compounds

411

        IPC Code: C07B33/00

 

        Smriti Rekha Baruah & Dilip Kumar Kakati

 

 

Study of deflouridation of drinking water by impregnation of metal ions in activated charcoal

414

        IPC Code: C02F1/28, C02F1/00

 

        C Janardhana, G Nageswara Rao, R Sai Sathish & V Sai Lakshman

 

 

Book Review

 

417

Chem-Tech Scan

 

419

Author Index

 

423

Keyword Index

 

424

Guidelines to Authors

425

 

 

 

 

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 319-328

 

Physico-chemical and surface characterization of adsorbent prepared from groundnut shell by ZnCl2 activation and its ability to adsorb colour

R Malik, D S Ramteke* & S R Wate

 

Physico-chemical and surface characterization of activated carbon prepared from groundnut shell, an abundantly available carbonaceous solid waste from oil processing mills in India, by chemical activation were carried out. The effect of various activation conditions viz. time, temperature and ZnCl2 / char ratio on the % yield of product and adsorption efficiency in terms of iodine number was studied. Changes in surface morphology of char before and after activation were examined by scanning electron microscopy which showed well developed pore structure in activated carbon demonstrating corrosive effect of ZnCl2. Surface modifications through chemical changes were studied by FTIR spectroscopy which showed considerable development and increase of surface functional groups in activated carbon as compared to char. The developed adsorbent was utilized for the removal of acid dye from aqueous solution and its adsorption capacity was found to be 55.5 mg/g of the adsorbent for 100 ppm initial concentration of dye solution. Adsorption parameters for Freundlich and Langmuir isotherm models were examined for dye adsorption and for the validity of models to analyze the equilibrium data, it was found that Freundlich model fitted better than Langmuir. The results indicate that Groundnut Shell based Powdered Activated Carbon (GSPAC) could be employed as low-cost alternative adsorbent to commercial activated carbon in the wastewater treatment for removal of acid dyes.

Keywords: Activated carbon, Groundnut shell, Porosity, FTIR, Fuchsin acid, Adsorption isotherms

IPC Code: B01D15/00, C01B31/00

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 329-333

 

Methylation of toluene over MnAPO-11 and ZAPO-11

 

K Joseph Antony Raj, A Dayalan & V R Vijayaraghavan*

 

Methylation of toluene with methanol in the vapour phase has been studied over MnAPO-11 and ZAPO-11. The reactions were carried out in a fixed bed reactor in the temperature range of 250-400ºC. p-Xylene is produced in greater concentrations than the other products. The selectivity for p-xylene is a function of acidity, specific surface area of the catalyst, reaction temperature and toluene to methanol ratio. ZAPO-11 was found to be more active than MnAPO-11. Maximum conversion (25.8%) was observed at 400ºC over ZAPO-11. The selectivity to p-xylene was found to increase with time on stream possibly due to partial reduction in the pore size of the catalyst by coke deposition.

Keywords: Methylation, AlPO-11, Xylene, Toluene, Molecular sieves

IPC Code: C12P5/00, C02F11/04

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 334-340

 

Alkylation of benzene with aqueous solution of ethanol over ZSM-5 catalysts

 

Jun-Jun Yuan & Börje S Gevert*

 

 

Alkylation of benzene with aqueous solution of ethanol (commercial 95 % purity) has been done in a laboratory scale reactor with ZSM-5 zeolite diluted with silica as a catalyst. The experiments have been done using different ratios of SiO2/Al2O3 catalysts in the reactor to study the change of activity and selectivity of desired product. Alkylation of benzene with aqueous ethanol yielded ethylbenzene as the primary product and lower amount of diethylbenzene isomers. With changing silica to alumina ratio in unmodified ZSM-5 catalysts, it was supposed that the influence caused by the existence of water in the reactants on acid-catalysed reaction is also changed. Modified B- and Mg- types of ZSM-5 zeolites were also examined. There were only small differences between 100% ethanol and 95% aqueous solution of ethanol in the experiments related to alkylation. Thus, it was inferred that it is possible to use 95% ethanol and water mixture as alkylating agent and ZSM-5 catalyst as a catalyst.

Keywords:          Alkylation, Benzene, ZSM-5 zeolite, SiO2/Al2O3 ratios, Selectivity, Aqueous ethanol, Ethylbenzene, Diethylbenzene

IPC Code: C07B37/00

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 341-346

 

Synthesis, characterization and photocatalytic studies of some metal phthalocyanines

Pritam Borker & A V Salker*

 

Metal phthalocyanines (MPc) (M = Cu, Ni, Co and Fe) have been synthesized and characterized by XRD, IR, ESR and thermal technique. The solid state studies such as magnetic susceptibility, electrical resistivity and electron spin resonance have been carried out. Solar induced degradation of a textile dye Naphthol Blue Black (NBB) has been studied employing metal phthalocyanines.

Keywords: Photocatalysis, Metal phthalocyanines, Naphthol Blue Black, Solid state studies, Semiconductors

IPC Code:  C07D487/22

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 347-352

 

Development and characterization of groundnut shell lignin modified phenol
formaldehyde wood adhesive

M A Khan & S M Ashraf*

 

Lignin modified phenol formaldehyde wood adhesives have been prepared by replacing phenol with the groundnut shell lignin (GNSL) at varying weight percentages. The optimization of weight percent incorporation of GNSL was carried out in respect to mechanical properties. It was found that a maximum of up to 50 wt.% of phenol in the phenol formaldehyde (PF) adhesive can be substituted by GNSL to obtain lignin substituted phenol formaldehyde (LSPF) adhesive with improved adhesive and shear strength in comparison with PF adhesive. The adhesive composition having 50 wt.% of phenol substituted by GNSL, termed as LSPF50 showed highest adhesive strength. LSPF50 and PF were further characterized by IR, DSC and TGA. Gel time measured and DSC showed higher rate of curing / hardening in LSPF50 than in PF. Thermo-gravimetric analysis (TGA) suggests C stage curing of LSPF50 adhesive at about 150/160 °C while for PF at about 160/185°C.

Keywords: Groundnut shell lignin, Lignin substituted phenol formaldehyde, Wood adhesive

IPC Code: C09J5/00

 

 

Journal of Chemical Technology

Vol. 13, July 2006, pp. 353-359

 

Sensitive bromatometric methods for the assay of metaprolol tartrate in dosage forms

 

K Basavaiah*, B C Somashekar & V Ramakrishna

 

One titrimetric and two spectrophotometric methods are described for the determination of metaprolol tartrate (MPT) using bromate-bromide mixture and two dyes, methyl orange and indigo carmine, as reagents. In titrimetry, an acidified solution of MPT is reacted with a known excess of bromate-bromide mixture and after a pre-determined time, the unreacted bromine is determined by iodometric titration. The spectrophotometric methods involve the addition of a known excess of bromate-bromide mixture to MPT in acidic medium followed by determination of the residual bromine by reacting with 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, amount of bromine reacted corresponds to the amount of MPT. The working conditions of the methods have been optimised. Titrimetry allows the determination of MPT in 2.5 - 7.5 mg range and the calculations are based on a 1:1(MPT : KBrO3) reaction stoichiometry. In the spectrophotometric methods, Beer’s law is valid over the concentration ranges 0.5 -5.0 and 1.5 - 15.0 mg mL-1 MPT for method A and method B, respectively. Method A with a molar absorptivity of 8.17 ´ 104 L mol-1 cm-1 is more sensitive than method B (€ = 2.70 ´ 104 L mol-1 cm-1). The limits of detection and quantification are reported for both the methods. The methods could usefully be applied to routine quality control of tablets containing MPT. No interference was observed from common pharmaceutical adjuvants. Statistical comparison of the results with those obtained by an established UV-spectrophotometric method showed excellent agreement and indicated no significant difference in accuracy and precision. The reliability of the methods was further ascertained by recovery studies.

Keywords: Metaprolol tartrate, Assay, Bromate-bromide, Dyes, Dosage forms

IPC Code: A61K9/08

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 360-366

 

Application of bromate-bromide mixture and methyl orange in the titrimetric, spectrophotometric and kinetic assay methods for cyproheptadine in pharmaceuticals

 

K Basavaiah*

 

Three new methods have been developed for the assay of cyproheptadine in bulk drug and in tablet formulation based on the bromination of cyproheptadine hydrochloride (CPH) by bromine generated in situ by the action of acid on bromate-bromide mixture. In titrimetry, the drug is treated with a known excess of bromate-bromide mixture in hydrochloric acid medium followed by the determination of unreacted bromine iodometrically. Spectrophotometry involves the addition of a measured excess of bromate-bromide reagent in acid medium to CPH, and after the reaction is ensured to be complete, the residual bromine is determined by reacting with a fixed amount of methyl orange, and measuring the absorbance at 520 nm. In kinetic method, a mixture containing CPH and methyl orange dye in 1 M sulphuric acid is mixed with bromate-bromide reagent at 4-5°C and time required for bleaching of methyl orange colour is measured. In titrimetry and spectrophotometry, the amount of bromine reacted corresponds to the amount of CPH, and in the former method, quantitation is based on a 1:1 reaction stoichiometry (CPH:KBrO3) and the method is applicable over 2-15 mg range. The spectrophotometric method permits the determination of CPH in 0.5-4.0 μg mL-1 range with an apparent molar absorptivity of 5.25× 104 L mol-1 cm-1 and a Sandell sensitivity of 0.0062 μg cm-2. The limits of detection (LOD) and quantification (LOQ) are calculated to be 0.04 and 0.12 μg mL-1, respectively. Quantitation in kinetic method is based on the linear relationship that exists between the CPH concentration and the time for bromination as indicated by the bleaching of methyl orange acid color. The method is applicable over 10-50 μg mL-1 range with LOD and LOQ values being 1.42 and 4.74 μg mL-1 , respectively. The methods were statistically evaluated by calculating the relative error for accuracy and intra-day and inter-day coefficients of variation for precision, and were applied successfully to the determination of CPH in tablets and syrup with mean recoveries in the range of 97.58-100.9%. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition technique. There was no interference from tablet excipients and additives.

Keywords:Bromate-bromide mixture, Methyl orange, Cyproheptadine, Pharmaceuticals

IPC Code: G01J3/00

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 367-371

 

Electrosynthesis and photoelectrochemical studies on (CdHg)S

 

Kehar Singh* & Sameer S D Mishra

 

Electrosynthesis of titanium supported (CdHg)S has been carried out with the objective of its photoelectrochemical characterization. Inclusion of Hg enhances photoelectroactivity of the composite somewhat. This is consistent with the observed lowering of the band gap of CdS due to the presence of Hg as inferred on the basis of photoaction spectral studies. Current-voltage studies show that (CdHg)S electrodeposits are also endowed with enhanced resistance towards electrochemical corrosion.

Keywords: Electrosynthesis, Sulphidization, Photoelectrochemical conversions, Action spectrum, Electrochemical corrosion

IPC Code: C25B1/00

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 372-377

 

 

Preparation and some properties of lithium vanadium bronzes

A M El-Sayed* & S M A Mousa

 

Lithium vanadium bronzes with composition formula LixV2O5 (0.04 ≤ x ≥ 0.92) have been prepared by solid-state reaction at 650oC in argon atmosphere. The products were characterized by X-ray powder diffraction and IR spectroscopy. The results reveal that four phases namely a-, ß-, ß/-, and γ-phase are present in the studied range. The magnetic susceptibility for the investigated samples was measured using Gouy,s method. The values of the effective magnetic moments as calculated from experimental data indicate the presence of V4+ ions in all samples. The electrical conductivity as a function of temperature and lithium content was measured in the temperature range from room temperature to 483 K. The electrical conductivity of the samples is found to be affected by lithium content. The values of the electrical conductivity increase with temperature for the investigated samples. The electronic and ionic conductions are discussed.

Keywords: LiV2O5, XRD, IR, Magnetic susceptibility, Electrical conductivity

IPC Code: C01G31/00

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 378-385

 

Mass integration for recovery of zinc from galvanizing and metal finishing industry using supertargeting approach

Shabina Khanam* & Bikash Mohanty

 

This paper presents an optimization technique, based on Supertargeting Approach, for the synthesis of solvent extraction and ion exchange network, which broadly falls under Mass Exchange Network (MEN). The present work is related to the recovery of zinc from spent pickle liquor and the rinse water, an effluent of galvanizing and metal finishing industry. The minimum composition difference of zinc, ¢e¢, between operating condition and equilibrium condition is found to be a key optimization variable. This paper describes the targeting as well as designing procedures for optimization of present MEN. During the design stage, it has been possible to achieve the targeted results.

Keywords: Mass exchange network, Minimum composition difference, Supertargeting

IPC Code: C22B9/00

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 386-390

 

Dissolution kinetics of iron from diasporic bauxite in hydrochloric acid solution

Gülsemin Gülfen*, Mustafa Gülfen & Ali Osman Aydın

 

The dissolution of iron in the bauxite ore including diasporite mineral from Kayaderesi region in Muğla-Milas city, Turkey was investigated in hydrochloric acid solution. The bauxite was calcined at different temperatures and periods, and then dissolved in hydrochloric acid solution. After determining the optimum calcination conditions as 1-hour period at     1173 K temperature and the optimum acid concentration as 8 M HCl, dissolution temperature and period for removal of iron from the bauxite were examined experimentally. In calculations of dissolution kinetics of iron, the experimental data showed that the dissolution process was controlled by interfacial chemical reaction with the apparent activation energy of 41.38 kJ/mol. First order reaction kinetics in shrinking core model was found to fit the experimental results. The dissolution of iron from the bauxite was achieved as 96.46% together with 23.40% aluminium.

Keywords: Bauxite, Iron, Acid leaching, Dissolution kinetics, Activation energy

IPC Code: C21B15/00

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 391-397

 

Determination of the optimum conditions for dissolution of
magnesite with H2SO4 solutions

 

Yüksel Abali*, Mehmet Çopur & Mesut Yavuz

 

Basic data on leaching of magnesite (MgCO3) with sulphuric acid are of interest from the point of view of the industrial process for obtaining pure MgSO4.  The Taguchi method was used to determine the optimum conditions for the dissolution of magnesite in H2SO4 solutions. The experiments were performed within the ranges mentioned herein i.e. 20-65°C for reaction temperature, 0.5/100-10/100 g/mL for solid-to-liquid ratio, 0.2-5 M for acid concentration, 5-60 min for reaction time and 150-750 rpm for stirring speed. The optimum conditions for these factors were found to be 65°C, 5/100 g/mL, 2 M, 60 min and 300 rpm, respectively. Under these conditions, the dissolution mass fraction of MgCO3 in H2SO4 solutions were w = 96.32%.

Keywords: Optimisation, Magnesite, Sulphuric acid, Taguchi method

IPC Code: C01B6/21

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 398-403

 

Enhancement of viscosity index of mineral base oils

 

Sabiha Tanveer & Ram Prasad*

 

Multigrade engine oils of high viscosity index (VI) are required for modern internal-combustion engines. Such a high VI is difficult to achieve by the conventional processing of petroleum fractions. Therefore, VI improvers are added in the mineral base oils to achieve the desired VI. The enhancement of VI of mineral base oils (100 N, 150 N and 500 N) by the addition of VI improvers [polyisobutylene(PIB), polybutadiene rubber (PBR)] has been studied. VI of blended oils, made from the mineral base oils 100 N, 150 N and 500 N by the addition of PIB and PBR, is found to pass through maximum. It was observed that the occurrence of maximum depends on the mineral base oil used and the type and concentration of VI improver.

Keywords: Viscosity index, Mineral base oil, Polyisobutylene, Polybutadiene rubber, VI improver

IPC Code: G01N, C07C7/00

 

 

Indian Journal of Chemical Technology

Vol. 13, July 2006, pp. 404-410

 

Studies on yield improvement of High Melting Explosive (HMX)

S Das, V D Raut, N M Gawande, R S Khopade & V L Narasimhan*

 

In India, octahydro-1,3,5,7-tetranitro-1,3,5,7-tetraazocine, commonly known as HMX (High Melting Explosive), is manufactured by the modified Bachmann combination method using continuous nitrolysis of hexamine in a cascade of four stirred tank reactors. In this laboratory, the technology was established more than three decades ago with an overall yield of about 40%. However, as the reported yield of HMX is around 55%, it was considered essential to systematically study the Bachmann reaction system to improve the yield. As such a detailed study on quantities/ratios of raw materials and process conditions was carried out to improve the yield. Optimized ratios of raw materials, use of nitric acid having strength >99%, proper control of temperature and optimal nitration and residence time gave an yield of 60-65%.

Keywords: Explosive, Bachmann reaction system

IPC Code: C06B

 

 

Indian Journal of Chemical Technology

Vol. 13, July. 2006, pp. 411-413

 

 

Cetyldimethyl benzyl ammonium cerium nitrate as a phase-transfer oxidant in the oxidation of alcohols to carbonyl compounds

 

Smriti Rekha Baruah & Dilip Kumar Kakati*

Oxidation of organic substrates by inorganic reagents is restricted by mutual insolubility of the two. However, this problem of mutual insolubility can be alleviated by the use of oxidants in the form of phase transfer reagents, like tetra-alkylammonium salts. Tetra-alkylammonium salt has a polar (N+) group and hydrocarbon side chains (alkyl groups). The ammonium salt allows a low concentration of oxidant to pass into the organic layer where they act as oxidizing agent. In the present case, the synthesis of a phase transfer oxidant cetyldimethyl benzyl ammonium cerium nitrate (CDBACN) and its use in the oxidation of alcohols to carbonyl compounds has been reported. CDBACN was synthesized from cetyldimethyl benzyl ammonium chloride (CDBACl) and ammonium ceric nitrate (CAN). The reagent was characterized by elemental analysis and spectral studies. The solubility and electronic spectra of the oxidant in various solvents were studied. This oxidant was successively utilized in the oxidation of different alcohols.

Keywords: Phase-transfer oxidant, Cetyldimethyl benzyl ammonium cerium nitrate (CDBACN), Ammonium ceric nitrate (CAN)

IPC Code: C07B33/00

 

Indian Journal of Chemical Technology

Vol. 13, July. 2006, pp. 414-416

 

Study on defluoridation of drinking water by impregnation of metal ions in activated charcoal

 

C Janardhana*, G Nageswara Rao, R Sai Sathish & V Sai Lakshman

 

Defluoridation of drinking water was carried out by the continuous down flow adsorption mode at room temperature. Five columns were prepared by the impregnation of ZrOCl2, CaO, Alum, CaCl2 and Borax in activated coconut shell charcoal. Known fluoride influent water was run into the column at a constant rate of 4.0 L/h and a constant level of water was maintained. Samples of the treated water were collected for analysis by the ion selective electrode method. In this study zirconium ion impregnated coconut shell charcoal (ZICSC) showed maximum fluoride uptake and proved to be the most effective defluoridating agent followed by CaO and Alum.

Keywords: Activated coconut shell charcoal, Alum, Calcium oxide, Continuous flow method, Defluoridation, Zirconium oxychloride

IPC Code: CO2F1/28, CO2F1/00