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Indian Journal of Chemical Technology

 

ISSN: 0971-457X

 

CODEN: ICHTEU 10(3) 241-340

VOLUME 10

NUMBER 3

MAY 2003

 
CONTENTS
Research Articles

An efficient liquid phase mono acylation of alcohols, diacylation and dimethoxylation of aldehydes over ZSM-35

247

R Srivastava & N Venkatathri

 

 

 

Photophysical studies of N-phenylanthranilic acid in polymer films

251

S R Pujari, P N Bhosale, P M R Rao & S R Patil

 

 

 

Modification of epoxy system for industrial applications: Preparation and characterization

257

M Suguna Lakshmi & B S R Reddy

 

 

 

Sucrose conferred stability of fructosyl transferase at elevated temperatures

265

V B Patil & N B Patil

 

 

 

Organization of amphiphiles, Part-III: Effect of hydrophobicity and hydrophilicity on the phase behaviour of some ethoxylated surfactants

269

Lingaraj Sahoo, Garudadhwaj Hota & Pramila Kumari Misra

 

 

 

Removal of zinc from wastewater by water hyacinth

274

S H Hasan, S Rai & D C Rupainwar

 

 

 

Removal of arsenic from water by ferrous sulphide

281

E K Unnikrishnan, A K Basu, N Chattopadhyay & B Maiti

 

 

 

Spectrophotometric determination of palladium(II) using piperonal thiosemicarbazone

287

Prakash Shetty, A Nityananda Shetty & R V Gadag

 

 

 

Rapid determination of molybdenum and titanium in uranium based alloys

291

M K T Bassan, K V Iyer & M Sudersanan

 

 

 

Determination of silver at submicrogram levels by absorption spectrophoto-metry

295

Jyoti Pandey, Padmaja Sudhakar & V J Koshy

 

 

 

Carbon molecular sieves (CMS) from coconut shell by carbonization and carbon dioxide activation

298

KimTae-Hwan, S Vijayalakshmi, Son Seok Jin & Kim Jee Dong

 

   

Catalytic wet air oxidation of pulp and paper mill effluent

305

Anurag Garg, Somen Saha, Vinayak Rastogi & Shri Chand

 

 

 

Mass transfer analysis of the extraction of Nickel(II) by emulsion liquid membrane

311

Mousumi Chakraborty, Chiranjib Bhattacharya & Siddhartha Datta

 

 

 

Thermal analysis of tri-ethylene glycol di-methacrylate

321

J S Notay, S M Dahiwale & S D Pradhan

 

 

 

Selective esterification of triethylene glycol with methacrylic acid using methane sulphonic acid

324

J S Notay, S M Dahiwale & S S Bhagade

 

 

 

Educator
 
 
 

Raoul-Pierre Pictet-The liquefaction of oxygen and achievement of low temperature

326

Jaime Wisniak

 

 

 

Chem-Tech Scan

337

 

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 247-250

 

 

An efficient liquid phase mono acylation of alcohols, diacylation and dimethoxylation of aldehydes over ZSM-35

R Srivastava & N Venkatathri*

ZSM-35, a medium pore zeolite has been synthesized using ethylene diamine as an organic template. The catalyst was found to be an active catalyst for chemoselective catalytic acylation of alcohols and diacetylation and dimethoxylation of aldehydes.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 251-256

 
Photophysical studies of N-phenylanthranilic acid in polymer films

S R Pujari, P N Bhosale, P M R Rao & S R Patil*

Photophysical properties of bifunctional N-phenylanthranilic acid (NPAA) have been studied as a dopant in polystyrene (PS) films. The PS films containing fluorescent NPAA were prepared from the solutions in non-polar and polar solvents. The fluorescence spectra of PS films prepared by using non-polar solvents depend on the concentration of NPAA in the film. The films containing lower concentration have exhibited sharp emission band at 412 nm corresponding to normal emission while the films containing higher concentration of NPAA have shown broad emission band peaking at 466 nm. The broad emission band is attributed to as arising due to formation of dimeric species by hydrogen bonding between two neighbouring NPAA molecules in the films. The modification observed in the fluorescence excitation and absorption spectra of the films with dopant concentration allows to consider the interaction between dopant molecules. In case of NPAA doped poly(vinyl acetate) films, there is an evidence for the destabilization of dimeric species as the fluorescence corresponds to the normal emission only.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 257-264

 

Modification of epoxy system for industrial applications:
Preparation and characterization

M Suguna Lakshmi & B S R Reddy*

Modified DGEBA epoxy resin system was prepared using epoxy phenolic novolac (EPN), bisphenol A cyanate ester prepolymer and polyether sulphone (PES). DGEBA epoxy resin modified with cyanate ester prepolymer offers process advantage in making prepregs for the preparation of structural composite materials. Further, the DGEBA epoxy resin modified with EPN and PES along with cyanate ester prepolymer was fully polymerised by curing at 200°C for 4 h. The cured resin was characterised by FT-IR, thermogravimetric analysis and differential scanning calorimetric methods. The moisture resistance properties were studied for the cured resins. The morphology studies were done for cyanate ester monomer, cyanate ester-epoxy polymer and PES-modified cyanate ester-epoxy polymers. Carbon fibre laminates were made based on PES-modified cyanate ester and epoxy polymer. Mechanical properties of the laminates were evaluated.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 265-268

 

Sucrose conferred stability of fructosyl transferase at elevated temperatures

V B Patil* & N B Patil

Sucrose is one of the abundant bio-mass on the earth, which can be easily processed for the production of edible nondigestive sweetener fructo-oligosaccharide(s) using an enzyme fructosyl transferase. The physicochemical properties of fructosyl transferase can be exploitable for the industrial operations. The direction of efforts was to study the factors like heavily glycosylated nature of enzyme, presence of sugars like sucrose, glucose, fructose and their mixtures responsible for stability of the fructosyl transferase at elevated temperatures. Effects of different metals on enzyme activity were also studied.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 269-273

 

Organization of amphiphiles, Part-III: Effect of hydrophobicity
and hydrophilicity on the phase behaviour of
some ethoxylated surfactants

Lingaraj Sahoo, Garudadhwaj Hota & Pramila Kumari Misra*

The phase behaviour of pseudoternary systems of the type H2O-Oil-non-ionic surfactant-co-surfactant(1:4) have been investigated. The non-ionic surfactants selected are polyoxyethylated alkyl phenols and polyoxyethylated alkyl ethers with varying hydrophobicity and hydrophilicity. The phase diagram is found to consist of a smaller isotropic domain and a larger anisotropic domain. The isotropic domain grows in size with increase in both hydrophilicity and hydrophobicity of the surfactants. These results have been attributed to the solubilization of oil or water in W/O microemulsion with increase in hydrophobicity and hydrophilicity of the surfactants respectively. The percentage of water intake by the microemulsion increases with increase in emulsifier percentage with a break when the overall concentration of emulsifier is about 70-80%.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 274-280

 

 

Removal of zinc from wastewater by water hyacinth

S H Hasan, S Rai & D C Rupainwar*

The water hyacinth (Eichchornia crassipes) has been successfully utilized for the removal of Zn from simulated wastewater samples. It has been found that growth rate in general and relative growth rate in particular of the plant decreases with the increase of metal ion concentration. The process of metal uptake by the plant is monophasic in nature with the increase of metal ion concentration whereas it is biphasic in nature with the time of exposure. The rate of mobility of the metal is slow in the root than that for the top of the plants. However amount of metal accumulated in the root is larger as compared to the top of the plants. It has also been found that the percentage removal of the metal from the aqueous solution decreases with increasing initial concentration of the metal. The overall removal capacity of the plant has also been evaluated and found to fit the mathematical model. Thus the process can be recommended for the treatment of zinc-loaded wastewater.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 281-286

 

Removal of arsenic from water by ferrous sulphide

E K Unnikrishnan, A K Basu, N Chattopadhyay & B Maiti*

A simple, rapid and cost-effective method for the removal of arsenic from water has been developed. Both As(III) and As(V) could be removed quantitatively by treating the polluted water with ferrous sulphide in granular form. Ferrous sulphide is cheap and easily available commercially and very effective for this purpose. Various factors influencing the treatment procedure have been studied and the mechanism of the removal process has been discussed. It has the additional advantage that the heavy metals like Pb, Hg, Cu, etc. that form insoluble sulphide are also removed along with arsenic. Analysis of arsenic content in the treated water by spectrophotometry and neutron activation analysis suggests that the method could successfully bringdown the concentration of arsenic below the permissible limit of 10 g/L as recommended by WHO.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 287-290

 
Spectrophotometric determination of palladium(II) using
piperonal thiosemicarbazone

Prakash Shetty, A Nityananda Shetty* & R V Gadag

A simple, rapid, selective and sensitive spectrophotometric method for the determination of palladium is proposed using piperonal thiosemicarbazone (PATS) as a reagent. The reagent forms a 1:2 complex (Pd:Reagent) with palladium. The yellow complex is soluble in 32-40% ethanol and has an absorption maximum at 363 nm. Beer’s law is obeyed upto 3.85 ppm of palladium and the optimum concentration range is 0.5-2.45 ppm of Pd. The molar absorptivity and Sandell’s sensitivity are 3. 80  104 dm3 mol-1 cm-1 and 2.8  10-3 g cm-2, respectively. The experimental conditions for complete colour development and the interference from various ions are investigated. The method is used for the determination of palladium in its complexes and synthetic mixtures.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 291-294

 

Rapid determination of molybdenum and titanium in
uranium based alloys

M K T Bassan, K V Iyer & M Sudersanan*

A rapid method has been developed for the selective determination of molybdenum in uranium-molybdenum alloy by derivative spectrophotometry without any need for the separation of the matrix element. The measurements were carried out at 376 nm in presence of hydrogen peroxide, without any interference from uranium. The determination of titanium in uranium-titanium alloy was carried out by normal spectrophotometry at 510 nm using hydrogen peroxide as the chromophoric reagent without any interference from uranium. The proposed methods are precise and accurate besides being very simple and rapid.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 295-297

 

Determination of silver at submicrogram levels by
absorption spectrophotometry

Jyoti Pandey, Padmaja Sudhakar* & V J Koshy

A selective and sensitive spectrophotometric method is described for the determination of 15-700 ng of Ag(I). Silver is extracted as silver iodide into benzene and selectively stripped into ammonia. The iodide associated with silver in the ammonical stripping is oxidised to iodate and then treated with excess iodide to give iodine. The iodine formed is extracted into benzene and equilibrated with iodate in acidic medium in the presence of chloride and Rhodamine 6G for the formation of ICl2- Rh 6G+ ion-pair in benzene layer. Determination is completed by measuring the absorbance of the extract at 535 nm. The coefficient of variation is 1% for 10 determinations of 630 ng of silver. The method has been applied to establish the silver content of dental samples, ornamental washing and photographic sample.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 298-304

 

Carbon molecular sieves (CMS) from coconut shell by
carbonization and carbon dioxide activation

KimTae-Hwan, S Vijayalakshmi*, Son Seok Jin & Kim Jee Dong

Carbon Molecular Sieves (CMS) are specially treated micro porous adsorbents derived from carbonaceous precursors. Due to the molecular sieving property, coupled with thermal, mechanical and chemical stability under acidic/alkaline conditions, CMS have found many applications in the field of difficult gas, as well as liquid separations from their mixtures. CMS have been successfully synthesized from a wide variety of carbonaceous materials, by the carbonization followed by carbon dioxide or steam activation. The effect of carbonization temperature and activation temperature on the surface area as well as pore volume, calculated using the carbon dioxide adsorption data at room temperature is studied. The most suitable carbonization temperature is found to be in the range 750-850oC, beyond which the surface area is found to decrease due to sintering of the particles at high temperature. The samples prepared were found to give good adsorption selectivity for CO2 over H2 or N2. Kinetic and equilibrium adsorption data for gases like N2, O2, H2, CH4, and equilibrium adsorption of selected organic vapours are also reported.

 

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 305-310

 

Catalytic wet air oxidation of pulp and paper mill effluent

Anurag Garg, Somen Saha, Vinayak Rastogi & Shri Chand*

The catalytic wet air oxidation of pulp and paper mill effluent was studied using CuSO4, perovskite based oxides, zeolites and bagasse flyash as catalysts at atmospheric pressure using air as the source of oxygen. Among the catalysts studied the activity of CuSO4 was the best, having a reduction of 36.5 and 68.1% in BOD and COD values respectively. Among the insoluble catalysts, La0.3Ce0.7CoO3 was the best with a marginally lower activity in comparison to CuSO4. The performance of flyash was also closer to CuSO4 and La0.3Ce0.7CoO3. At a higher catalyst concentration of 5 g/L flyash (initial concentration 1 g/L), the reduction in BOD and COD values of the pulp and paper mill effluent were 48.9 and 77.4% respectively, whereas the BOD/COD value was increased to 0.56, a value much closer to 0.63, which is an indicator for the complete biodegradability of the effluent. The reactivity of the catalyst was found to be a strong function of the pH of the effluent solution, and a pH of 10 was found to be the best.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 311-320

 

 

Mass transfer analysis of the extraction of Nickel(II)
by emulsion liquid membrane

Mousumi Chakraborty*, Chiranjib Bhattacharya & Siddhartha Datta

A mathematical model for batch extraction of Nickel(II) with emulsion liquid membrane (ELM) from a dilute sulphate solution and from industrial wastewater, using di-(2-ethylhexyl) phosphoric acid (D2EHPA) as extractant and hydrochloric acid as stripping agent is reported. The model considers a reaction front within the emulsion globule and assumes an instantaneous and irreversible reaction between the solute and the internal reagent at the membrane internal droplet interface. Batch experiments are performed for separation of Nickel(II) from aqueous sulphate solution of initial concentration in the range of 100-75 mg/L. The influence of Nickel(II) concentration on the distribution coefficient at pH 3.5 is co-related by a semiempirical model, which has been used for simulation of the extraction process. The simulated curves are found to be in good agreement with the experimental data.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 321-323

 

Thermal analysis of tri-ethylene glycol di-methacrylate

J S Notay*, S M Dahiwale & S D Pradhan

Thermal characterization of tri-ethylene glycol di-methacrylate was carried out in view of its vast applications. The main objective of this paper is to investigate the thermal behaviour of the impurities present in the compound tri-ethylene glycol di-methacrylate and its effects during applications of the compound. Thermal characterisation was carried out under two different experimental conditions. One at low heat flux rate of 10C/min, and another at higher heat flux rate of 100C/min. At low heat flux rate, the ethers present as impurities in the compound tri-ethylene glycol di-methacrylate are stable below the temperature of 150C. This is desirable for applications in anaerobic adhesive and optical articles where exposure to temperature beyond 150C is not required. At higher heating rate of 100C/min, the endothermic decomposition of the impurities as ethers present in the compound tri-ethylene glycol di-methacrylate is observed, and the same is desired from the application point of view of using tri-ethylene glycol di-methacrylate as a moderant in single base propellants.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 324-325

 

Selective esterification of triethylene glycol with methacrylic
acid using methane sulphonic acid

J S Notay*, S M Dahiwale & S S Bhagade

The esterification of tri-ethylene glycol with methacrylic acid under identical conditions of catalyst concentration, for synthesis of tri-ethylene glycol di-methacrylate using sulphuric acid and methane sulphonic acid as catalyst is discussed. The reaction by-products are lesser in case of methane sulphonic acid catalyst, in comparison to sulphuric acid catalyst. Therefore the yield of ester product, tri-ethylene glycol di-methacrylate, achieved during the synthesis is higher with the use of methane sulphonic acid as a catalyst, than on use of sulphuric acid as catalyst. This concludes that methane sulphonic acid has better catalyst selectivity in comparison to sulphuric acid for the synthesis of tri-ethylene glycol di-methacrylate. Methane sulphonic acid when neutralized is easily bio-degradable which is also desirable from environmental point of view.

 

Indian Journal of Chemical Technology

Vol. 10, May 2003, pp. 326-336

 

Raoul-Pierre Pictet—The liquefaction of oxygen and
achievement of low temperatures

Jaime Wisniak

To Raoul Pictet (1846-1929) we owe the realization of the liquefaction of oxygen and the study of the effect of low temperatures on physical, chemical, and physiological phenomena. He developed Trouton’s law in a theoretical manner, years before Trouton did it by simple tabular means. The priority of oxygen liquefaction was and continues to be a matter of discussion.