Indian Journal of Chemical Technology

VOLUME 8

NUMBER 4

JULY 2001

CONTENTS

 

Solvent extraction and separation of Bi(III) and Sb(III) from HCl and HBr media using tri-n-octyl phosphine oxide (TOPO)

239

 

      Kamaruddin Abdar Ali & Ajay K Vanjara

 

 

 

 

 

Investigation of the migration behaviour of aromatic amines on silica layer using nonionic surfactants containing mobile phases: Mixed surfactants assisted separations

244

 

      Ali Mohammad & Iftkhar Alam Khan

 

 

 

 

 

Arsenazo III test strip for rapid detection of hardness of water

252

 

      N B Tulsani, H vikram, Hemant Kumar, Suman, Reeti Chaudhary, Kirti Rani & Ashok Kumar

 

 

 

 

 

A method of separation of lime from high or low calcium oxide containing limestone

255

 

      S C Sarker

 

 

 

 

 

Development of a simple method for separation of  a- pinene and b-pinene from turpentine oil and designing milticomponent batch distillation columns

260

 

      J K Sama & P Bandopadhyay

 

 

 

 

 

Beta-correction spectrophotometric investigation of aluminium complex solution with new ligand, dibromo-o-nitrophenylfluorone

273

 

      Hong-Wen GAO, Shu-Ren SHI and Yu-Cheng LI

 

 

 

 

 

Studies on adsorption of selected organophosphorous pesticides by clays

278

 

      K Rama Mohan, A Ramesh & K Seshaiah

 

 

 

 

 

Identification and removal of bacteria E.coli from drinking water by ascorbic acid

281

 

      Ishwar Das, Alpana Bajpai & U K Singh

 

 

 

 

 

Sorption recovery of metal ions from aqueous solution using humus-boehmite complex

286

 

      Beena T Abraham & T S Anirudhan

 

 

 

 

 

Importance of small amount of water in solid-liquid phase transfer catalysis: Reaction of benzyl chloride with solid sodium sulphide

293

 

      Narayan C Pradhan

 

 

 

 

 

Catalysis by heteropoly acids: Formation of bisphenol A from phenol and acetone

298

 

      V N Sheemol, I R Unni & C Gopinathan

 

 

 

 

 

Synthesis of polymethylmethacrylate by using triphenyl-bismuthoniumylide: Kinetics and mechanism

301

 

      Radha Bajpai & A K Srivastava

 

 

 

 

 

A numerical solution to enzyme emulsion liquid membrane reactor model for sequencial bienzymatic reaction

307

 

      Parimal Pal, Siddhartha Datta & Pinaki Bhattacharya                                               contd

 

 

Immobilization of  a-L-rhamnosidase of Aspergillus terreus on bagasse particles based matrix

314

      Sarita Yadav & K D S Yadav

 

 

 

Educator

 

Candle: A light into the past

319

      Jaime Wisniak

 

 

 

Book Review

 

 

 

Chemistry of Advanced Materials

327

      Reviewer: G S Mukherjee

 

 

 

Announcement

330

 

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 239-243

Solvent extraction and separation of Bi(III) and Sb(III) from HCl and HBr media using tri-n-octyl
phosphine oxide (TOPO)

Kamaruddin Abdar Ali & Ajay K Vanjara*

Applied Chemistry Division, Department of Chemical Technology, University of Mumbai, Matunga, Mumbai 400 019, India

Received 9 November 2000; accepted 24 March 2001

The solvent extraction and separation of Bi(III) and Sb(III) from aqueous acidic media was investigated using Tri-n-octyl phosphine oxide (TOPO) in toluene. Quantitative extraction of Bi(III) was observed in acid range of 0.001-0.01M of HCl and 0.01-0.1M of HBr and that for Sb(III) extraction was incomplete in HCl media over the entire concentration range studied. The extraction of Sb(III) was quantitative in range 0.01-0.1M of HBr media. Effect of various other parameters such as reagent concentration, type of diluents, stripping agents, effect of diverse ions were studied to ascertain optimum conditions for the quantitative extraction and separation of Bi(III) and Sb(III). After equilibration Bi(III) from organic phase was stripped with 3M HNO3 and determined spectrophotometrically by thiourea method at 470 nm, while Sb(III) was stripped with 9M H2SO4 and determined spectrophotometrically by iodide method at 425 nm. The effect of temperature on the extraction of Bi(III) and Sb(III) from HCl and HBr media has also been studied. The method is applicable to the analysis of pharmaceutical samples and alloys.

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 244-251

Investigation of the migration behaviour of aromatic amines on silica layer
using nonionic surfactant containing mobile phases: Mixed surfactants
assisted separations

Ali Mohammad* & Iftkhar Alam Khan

Analytical Research Laboratory, Department of Applied Chemistry, Faculty of Engineering and Technology,
Aligarh Muslim University, Aligarh 202 002, India.

Received 27 September 2000; accepted 23 February 2001

Migration behaviour of important aromatic amines on silica gel layers has been investigated using mobile phases containing a nonionic surfactant (Triton X-100) over a wider concentration range (0.001-0.1M). Effect of factors such as pH of mobile phase and the presence of electrolyte (NaCl, NaBr), non-electrolyte (urea) and alcohol (MeOH, EtOH, PrOH, BuOH) additives on the mobility of amines was also examined. The results obtained with surfactant containing mobile phases were compared with those obtained in the absence of surfactant. The main chromatographic characteristics and separation conditions for mixtures of amines on silica plates with Triton X-100 containing mobile phases were determined. As a first attempt, aqueous solutions of mixed surfactants (Triton X-100 plus sodium dodecyl sulphate, SDS) have been utilized for superior thin layer chromatographic separations of aromatic amines.

 

Indian Journal of Chemical Technology

Vol. 8, July 2001. pp. 252-254

 

Arsenazo III test strip for rapid detection of hardness of water

N B Tulsani , H Vikram, Hemant Kumar , Suman, Reeti Chaudhary, Kirti Rani & Ashok Kumar*

Centre for Biochemical Technology (CSIR), Delhi University Campus, Mall Road,  Delhi 110 007, India

Received 14 August 2000; accepted 20 March 2001

In this article development and optimization of visually evaluable dry-reagent test strip technique for qualitative and semi-quantitative estimation of hardness of water has been described. The hardness of water is based on its alkaline earth content i.e. calcium and magnesium ions and their salts. The estimation of hardness of water in industry as well as in private sector is essential. Presently, calorimetric assay and test kit methods are commonly used , however, they are expensive and require trained persons to perform the test. The dry reagent strip developed in the laboratory is quick, simple and economical. It is based on specific chromogen immobilized on to a pad which reacts with calcium present in water and thereby changes the colour of the strip from purple to blackish blue. The change in colour is visible with naked eyes and can be compared with the colour chart.

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 255-259

 

A method of separation of lime from high or low calcium oxide
containing limestone

 

S C Sarker

Analytical Laboratory, DMR Risa Colony, Shillong 793 003, India

Received 11 May 2000; accepted 20 March 2001

A method of separation of lime (CaO) from limestone either by treating with water or by treating with concentrated hydrochloric acid at pH 9-10. This method will help to enrich the concentration of various other elements associated with limestone and pure CaO may be used for industrial purpose.

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 260-272

 

Development of a simple method for separation of a-pinene and b-pinene from turpentine oil and designing
multicomponent batch distillation columns

J K Sama*a & P Bandopadhyay b

aChemical Engineering and Design Division, Regional Research Laboratory, Canal Road, Jammu Tawi 180 016, India

bFuel and Mineral Engineering Department, Indian School of Mines, Dhanbad 826 004, India

Received 25 May 2000; accepted 26 February 2001

A simple graphical method has been developed for designing batch fractionating towers for the fractionation of multicomponent mixtures. It can predict with accuracy the amount of high purity cut one can have, with optimum number of plates at optimum reflux ratio. This eliminates the rigorous determinations by computer. The method is equally good in predicting the amount and composition of subsequent cuts of high purity. The accuracy of the method has been established with the practical results from a pilot scale batch fractionating column.

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 273-277

 

Beta-correction spectrophotometric investigation of aluminium complex solution with new ligand,
dibromo-o-nitrophenylfluorone

Hong-Wen GAOa*, Shu-Ren SHIb & Yu-Cheng LIa

a School of Chemistry and Chemical Engineering, Anhui University, Hefei 230039, P.R. China

bSchool of Life Science, Anhui University, Hefei 230039, P.R. China

Received 13 March 2000; accepted 23 February 2001

The new ligand, dibromo-o-nitrophenylfluorone (DBNPF) was found to sensitively complex aluminium (Al3+) at pH 8.5. The ordinary spectrophotometry was limited for use because of the serious interference of excess of DBNPF. The b-correction theory was applied to the analysis of this reaction instead of the single wavelength spectrophotometry. It gave the simple determination of the complex characteristic factors. Results showed that the formed complex can be expressed as Al(DBNPF)5 at pH 8.5, the cumulative stability constant of complex equaled to 1.48´1020. For analysis of water samples, the detection limit of aluminium was 0.005 mg/L and the recoveries vary between 92.0 and 108% with the relative standard deviations less than 4.4%.

 

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 278-280

Studies on adsorption of selected organophosphorus pesticides by clays

K Rama Mohan, A Ramesh & K Seshaiah*

Department of Chemistry, Sri Venkateswara University, Tirupati 517 502, India

Received 1 May 2000; accepted 9 April 2001

Adsorption of the organophosphorus pesticides, malathion and dimethoate on clays (viz. montmorillonite and kaolinite) saturated with cations, from aqueous solution was studied. The extent of adsorption was more on montmorillonite saturated with Fe3+ and Ca2+ than the montmorillonite saturated with Na+ and kaolinite saturated with the same cations for both the pesticides. The adsorption isotherms are fit into Freundlich adsorption equation.

 

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp.281-285

 

Identification and removal of bacteria E.coli from drinking water

by ascorbic acid

 

Ishwar Das a * , Alpana Bajpai a & U.K. Singh b

aChemistry Department, D D U Gorakhpur University, Gorakhpur 273 009, India

bDepartment of Microbiology, B R D Medical College, Gorakhpur 273 012, India

Received 7 January 2000; accepted 8 March 2001

Drinking water has been analysed and found to contain the bacteria predominantly E.coli with a large total count more than 1800 per 100 mL. It has been disinfected by several low cost alternative disinfectants which are safe and hazardless and reduce the total count considerably. Ascorbic acid (Vitamin C) is a low cost substance, easily soluble in water. It has been observed that ascorbic acid treatment was superior to that by uv, activated charcoal or other methods. These treatments were cumbersome and costlier as well. The kinetics of disinfection has been studied. The data obey the empirical equation N=b-a.t, where N is the total bacterial count at any time t, a and b are constants.

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 286-292

 

Sorption recovery of metal ions from aqueous solution using

humus-boehmite complex

 

Beena T Abraham & T S Anirudhan*

Department of Chemistry, University of Kerala, Kariavattom, Trivandrum 695 581, India

Received 25 November 2000; Accepted 12 February 2001

Humic acid (HA) was immobilized on boehmite (AlOOH) by batch equilibration. Removal of Pb(II), Hg(II) and Cd(II) from aqueous solution was studied using the batch equilibrium method. Experiments were carried out as a function of pH and concentration of metal ions. It was shown that the maximum adsorption of 96.7 % for Pb(II) occurred at an optimum pH of 5.5 whereas the maximum adsorption of 91.7% for Hg(II) and 80.8% for Cd(II) was observed at pH 6.0. The adsorption of metal ion proceeds predominently by the cation-exchange mechanism. Adsorption isothermal data could be interpreted by the Langmuir and Freundlich isotherm equations. Langmuir and Freundlich constants have been determined. Adsorption experiments were carried out to investigate the competitive effect on the uptake of metal ions from binary mixtures. Sheindorf - Rebhun - Sheintuch (SRS) model was used to study the competitive interactions for the adsorption of Pb - Hg, Pb - Cd and Cd - Hg mixtures by the adsorbent.

 

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 293-297

 

Importance of small amount of water in solid-liquid phase transfer catalysis: Reaction of benzyl chloride with solid sodium sulphide

 

Narayan C Pradhan*

Department of Chemical Engineering, Indian Institute of Technology, Kharagpur 721 302, India

Received 5 September 2000; accepted 19 March 2001

The reactions of benzyl chloride with solid sodium sulphide were carried out in the presence of two different phase transfer catalysts. The rate of reaction was found to vary non-linearly with catalyst concentration in both the cases. This was explained in terms of phase transfer catalyst-promoted dehydration of the solid reactant. The phenomenon was also explained theoretically which proved the importance of small amount of water in solid-liquid phase transfer catalysis.

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001 pp.298-300

 

Catalysis by heteropoly acids : Formation of bisphenol A from phenol and acetone

V N Sheemol, I R Unni & C Gopinathan*

Inorganic and Catalysis Division, National Chemical Laboratory, Pune 411 008, India

Received 25 August 2000; aceepted 9 April 2001

A process for the production of p,p’-bisphenol A from phenol and acetone in the presence of heteropoly acid as catalyst has been described. Effect of various heteropoly acids, reaction time, and catalyst concentration have been studied. Results show that heteropoly acid catalysts give higher conversion and selectivity to the p,p’ isomer than conventional HCl catalyst.

 

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 301-306

 

Synthesis of polymethylmethacrylate by using triphenybis-muthoniumylide :
Kinetics & mechanism

Radha Bajpai & A K Srivastava*

Department of Chemistry, H. B.Technological Institute, Kanpur 208 002, India

Received 26 September 1999; accepted 13 November 2000

The polymerization of methylmethacrylate initiated by triphenyl- bismuthonium 1,2,3,4-tetraphenylcyclo­pentadienylide in benzene follows ideal radical kinetics. The activation energy (Ea) and k2p/kt values were 76 KJ mol-1 and 1.06 ´ 10-1 L mol-1s-1, respectively. The scanning electron microscopy and qualitative analysis shows that the little amount of bismuth has trapped in polymer matrix. The presence of 6 hyperfine lines in E.S.R. spectrum indicate that the system follows free radical polymerization and the initiation is brought about by phenyl radical.

 

 

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 307-313

A numerical solution to enzyme emulsion liquid membrane reactor model
for sequential bienzymatic reaction

Parimal Pala, Siddhartha Dattab & Pinaki Bhattacharyab*

a Department of Chemical Engineering, Regional Engineering College, Durgapur, India

b Department of Chemical Engineering, Jadavpur University, Calcutta 700 032, India

Received 18 April 2000; accepted 19 February 2001

Dynamic mathematical models of liquid membrane-immobilized multienzyme reaction systems involve a large number of algebraic, ordinary and nonlinear partial differential equations with different types of boundary conditions. Solutions of such model equations are often difficult and stand in the way of realistic modeling efforts in this field. In the present study, attempt has been made to numerically solve such model equations for a liquid membrane-immobilized sequential bienzymatic reaction system through development of a software (MEMBSOL). In the solution process, partial differential equations have been converted into ordinary differential equations by using a finite difference technique in which the spatial derivatives have been discretized while leaving the temporal derivatives unconverted. Through mathematical manipulations, use of fictitious points at the boundaries has been eliminated thereby making the solution-approach a general-purpose one. To integrate the differential equations, Runge-Kutta-Fehlberg method has been applied. An automatic step-size adjustment mechanism has been incorporated in the integration process to produce results with a reasonably desired level of accuracy. In the present computations, numerical solutions with 0.1 percent relative error have been obtained.

 

Indian Journal of Chemical Technology

Vol. 8, July 2001, pp. 314-318

 

 

Immobilisation of a-L-rhamnosidase of Aspergillus terreus on

bagasse particles based matrix

 

Sarita Yadav & K D S Yadav*

Department of Chemistry, D D U Gorakhpur University, Gorakhpur 273 009, India

Received 13 April 2000; accepted 27 March 2001

a-L-rhamnosidase from Aspergillus terreus has been immobilised on bagasse particles based matrix. Km, pH and temperature optima of the immobilized enzyme using narigin as the substrate have been found to be 0.24 mM, 4.0 and 55°C respectively. The corresponding values for the same enzyme in the solution phase are 0.16 mM, 4.0 and 55°C respectively. The immobilized preparation of a-L-rhamnosidase hydrolyses naringin present in Citrus sinansis juice indicating its applicability in the debittering of citrus fruit juices.

 

Indian Journal of Chemical Technology

Vol.7, July 2001, pp. 319-326

 

Candle: A light into the past

Jaime Wisniak*

Department of Chemical Engineering, Ben-Gurion University of the Negev, Beer-Sheva, Israel 84105

The historical development of the candle is a fascinating subject because it reflects the parallel development of chemical industry, the understanding of physical and chemical phenomena, and the ingenuity of the human being. Today, the burning of a candle is already being studied under microgravity conditions. A semicircular blue flame is found to result under microgravity, in sharp contrast to an oblong two coloured flame observed under gravity of the earth.

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