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Indian Journal of Chemical Technology

 

ISSN: 0971-457X   CODEN:ICHTEU 10(4) 341-440
Volume 10

Number 4

 July 2003

 

CONTENTS

Study of insecticidal activity of some pyrazole derivatives against American

 

cockroaches

347

Rajesh K Verma & Sanjay S Nayal

 

 

 

Preparation and characterization of lobster shell chitosan: Modification of

 

traditional method

350

S Chatterjee, A K Guha & B P Chatterjee

 

 

 

New titrimetric and spectrophotometric methods for the determination of

 

promethazine theoclate using metavanadate

355

K Basavaiah & V S Charan

 

 

 

Synthesis and spectral studies of macrocyclic mono- and binuclear gadolinium(III) complexes derived from schiff’s bases

 

363

P Akilan, M Thirumavalavan & M Kandaswamy

 

 

 

Chromatographic behaviour of metal ions on egg shell layers

367

Aditya K Misra

 

 

 

An improved method for the recovery of essential oil from Celery seeds

370

M P Jain, J K Sama, S M Jain, V K Sharma &  Baldev Singh

 

 

 

Determination of total sulphur in inorganic compounds-An overview

373

Y S Sayi, P S Shankaran, C S Yadav & G C Chhapru

 

 

 

Precipitation and complex formation reactions based titrimetric and

 

spectrophotometric methods for the determination of diphenhydramine

 

hydrochloride

382

K Basavaiah & V S Charan

 

 

 

Kinetic study of crystal colouration during crystallization of sucrose

386

Kaman Singh & Sudhanshu Mohan

 

 

 

Investigation on the equilibrium solubility of cesium chloride-hydrochloric acid-water ternary system and application

 

391

Yucheng Jiang, Mancheng Hu, Mei Meng, Shiyang Gao & Shuping Xia

 

 

 

Electrochemical degradation of resorcinol using mixed oxide coated titanium

 

electrode for wastewater treatment-A kinetic study

396

D Rajkumar, K Palanivelu & N Mohan

 

 

 

Kinetics of RuIII catalysed polymerization of methylmethacrylate by aliphatic

 

amines in presence of carbontetrachloride

402

Manisha Pachauri & Santosh K Upadhyay

 

 

 

Thermal behaviour of bismaleimides, allyl nadic-imides and their blends

408

Indrajeet Singh, Anju Srivastava & I K Varma

 

 

 

Effect of substituents on corrosion inhibition efficiency of arylisothiocyanates and their condensation products with thiosemicarbazide for corrosion of copper in aqueous chloride solution

 

 

414

M M Singh, R B Rastogi, B N Upadhyay & M Yadav

 

 

 

Notes

 

Kinetics of esterification of tri-ethylene glycol-methacrylic acid reaction system

420

J S Notay & S S Bhagle

 

 

 

Educator
 

James Dewar-More than a flask

424

Jaime Wisniak

 

 

 

Chem-Tech Scan

435

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 347-349

 

 

Study of insecticidal activity of some pyrazole derivatives against American cockroaches

Rajesh K Verma* & Sanjay S Nayal

 

Pyrazole derivatives are well-known biological active compounds. This paper deals with the insecticidal activity of some pyrazole derivatives, namely N1-4-(Fluorobenzoyl)-5,5'-dimethyl cyclohexane-4-(sulpha/substituted phenylazo)-1, 2-diazole against American cockroaches, Periplaneta americana. The results of the study indicate that the few synthesized pyrazole derivatives show significant insecticidal activity against American cockroaches.

 

 

 

Indian Journal of Chemical Technology

Vol.10, July 2003, pp. 350-354

 

 

Preparation and characterization of lobster shell chitosan: Modification of traditional method

S Chatterjee, A K Guha & B P Chatterjee*

 

Preparation of chitosan from lobster shells by Hackman method and modified Hackman method was compared with respect to their physico-chemical properties, molecular weight, degree of deacetylation, polydispersity and crystallinity. In modified method maximum yield (78%) of chitosan with almost 91% degree of deacetylation determined by first derivative UV spectra was achieved. Molecular size distribution as well as average size of chitosan produced by Hackman method was higher (PI 1.205, particle size 1448.6 nm) and of wt 10  105 when compared to chitosan produced by modified Hackman method (PI 0.8832, particle size 95.3 nm) of wt 3.98  105. X-ray powdered diffraction showed that chitosan prepared by Hackman method was found to be more crystalline, Bragg refractions 13.32 (d = 6.66Å) and 19.72 (d = 4.51Å), respectively than chitosan produced by modified method, Bragg refraction 13.62 (d = 6.51Å). This method provides quality product in less time and is economical.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 355-362

 

 

New titrimetric and spectrophotometric methods for the determination of promethazine theoclate using metavanadate

K Basavaiah * & V S Charan

 

Four new methods (titrimetric and spectrophotometric, two each) which are accurate, precise and rapid are described for the determination of promethazine theoclate in bulk form and in tablets. The titrimetric methods are based on the oxidation of the drug by metavanadate in acidic condition followed by determination of the unreacted oxidant by titration with iron(II) ammonium sulphate (Method A) or titration of the vanadium(IV) formed, with cerium(IV) sulphate (Method B). The spectrophotometric procedures are also based on the oxidation of the drug with metavanadate followed by the estimation of unreacted oxidant after complexing with chromotropic acid and measuring the absorbance at 420 nm (Method C) or estimation of the vanadium(IV) formed, by reacting it with ferriin and measuring the resulting ferroin at 510 nm (Method D). Method A and Method B are applicable over the ranges 1-20 and 5-12 mg, respectively. Calculations in both methods are based on the reaction stoichiometry of 1:2 (drug: metavanadate). In spectrophotometry, Beer's law is obeyed over the ranges 0.0-125.0 and 10.0-60.0 g mL-1 for method C and method D, respectively and the corresponding molar absorptivity values are 2.64103 and 5.33103 L mol-1 cm-1, respectively. The methods were successfully applied to the determination of promethazine theoclate in avomine tablets, and the results obtained were in the range of 97.73-102.24% of declared content with a relative standard deviation of 1.51-2.22%.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 363-366

 

 

Synthesis and spectral studies of
macrocyclic mono- and binuclear gadolinium(III)
complexes derived from schiff's bases

P Akilan, M Thirumavalavan & M Kandaswamy*

 

A series of mono- and binuclear Gadolinium(III) macrocyclic complexes have been prepared by the condensation of schiff's bases with the precursor compound 4,4-dimethyl(2,2-diformyl-6,6-piperazine-1,4-di-yl-methylene)bis phenol in template method. All the binuclear complexes have been prepared in situ from their corresponding mononuclear complexes without isolation. The phenolate oxygen atom of the binucleating ligands behaves as a bridging group between two metals. The complexes have been characterized by elemental analysis, IR, NMR, UV spectra. The ESR spectral study was carried out for some complexes. The results of elemental analysis of the complexes are in good agreement with the theoretical value. Conductivity studies reveal that all the complexes are neutral.

 

 

 

Indian Journal of Chemical Technology

Vol.10, July 2003, pp. 367-369

 

Chromatographic behaviour of metal ions on
egg shell layers

Aditya K Misra

 

The thin layer chromatography of metal ion has been performed in twelve solvent system’s on egg shell layers. The separation of Mo6+ and W6+ from Ti4+, VO2+, Fe2+, Fe3+, UO22+, Ta5+ and Nb5+; Tl+ from Hg2+ and Pb2+; Hg2+ from Hg+ have been achieved on egg shell layers in distilled water, 0.1 M calcium nitrate and 0.1 M potassium thiocyanate, respectively. The separation on egg shell layers follow the ion exchange precipitation mechanism as evidenced by the X-ray analysis results and the solubility data of various carbonates.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 370-372

 

An improved method for the recovery of
essential oil from Celery seeds

M P Jain* , J K Sama , S M Jain , V K Sharma & Baldev Singh

 

Celery, Apium graveolens L is cultivated for its seeds and essential oil. An improved method has been developed for maximum yield of essential oil with higher content of phthalides (the valuable constituent of oil), in short time, making the process economical. The method involves hydrodistillation using electric, microwave as well as steam heating. Effect of addition of salt was also studied. Microwave contributed saving in energy, but did not improve yield.

 

 

 

Indian Journal of Chemical Technology

Vol.10, July 2003, pp. 373-381

 

 

Determination of total sulphur in
inorganic compounds—An overview

Y S Sayi*, P S Shankaran, C S Yadav & G C Chhapru

 

Sulphur is invariably present in all materials either as an impurity or as a major constituent. Several methodologies are available to determine the sulphur content both at trace level and percentage levels. Some of the techniques employed for the determination of total sulphur in inorganic materials have been briefly described in this paper.

 

 

 

Indian Journal of Chemical Technology

Vol.10, July 2003, pp. 382-385

 

 

Precipitation and complex formation reactions based titrimetric and spectrophotometric methods for the determination of diphenhydramine hydrochloride

K Basavaiah* & V S Charan

 

Two simple, accurate and selective methods for the determination of diphenhydramine in pharmaceutical grade sample and in dosage forms are described. The titrimetric method is based on the precipitation of the chloride content of the drug as AgCl with a known excess of silver nitrate and back titration of the residual silver nitrate with thiocyanate using iron(III) as indicator. The reaction stoichiometry and the range of determination have been evaluated. The spectrophotometric method involves the displacement of thiocyanate of mercuric thiocyanate from the ionized chloride and the subsequent reaction of the liberated thiocyanate with iron(III) to form the familiar red coloured complex, Fe(SCN)2+ which is measured spectrophotometrically at 460 nm. The Beer’s law is obeyed over the range 5-45 g mL-1 of diphenhydramine HCl, the molar absorptivity and Sandell sensitivity being 3.45 × 103 L moL-1 cm-1 and 84.5 ng cm-2, respectively at 460 nm. The reaction variables have been optimized. The methods have been found to be very simple, cost-effective and reliable for three dosage forms containing diphenhydramine hydrochloride.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 386-390

 

 

Kinetic study of crystal colouration
during crystallization of sucrose

Kaman Singh* & Sudhanshu Mohan

 

Although, existence of the coloured syrup layer surrounding the crystal surface is fait accompli, there is no definite explanation for the colour inside the crystal. In the present investigation, therefore, whether the colour is adsorbed or occluded or both, three types of artificial colouring matters; caramel, iron-phenol complex and reducing sugar-amino acid browning reaction products are used to examine the effect of each on crystal colouration. By static and dynamic analysis, it is concluded that different colourants have different affinities for the crystals and cause different colouration under the same condition; viz. caramel is the slowest, RS-AA browning product is intermediate and the iron-phenol complex is the fastest. At a slow rate of the crystallization (k=0.86-6.05105 mg/m2/h), colouration is caused mainly by adsorption. However, when the rate increases, this may also be accompanied by another mechanism such as occlusion, although adsorption is still in effect. The quantity of colouration decreases with rise in crystallization temperature, the extent of which decreases with increase in super-saturation. By reducing the amount of these colourants of higher affinity which are present in the mother liquor and under varying crystallization conditions, different effective measures may be adopted to overcome the colouration. Thermodynamic data of the crystal colouration are also evaluated and data indicate a loss in the entropy change in the process.

 

 

 

Indian Journal of Chemical Technology

Vol.10, July 2003, pp. 391-395

 

 

Investigation on the equilibrium solubility of
cesium chloride-hydrochloric acid-water
ternary system and the application

Yucheng Jianga,b, Mancheng Hub, Mei Mengb, Shiyang Gaoa,b * & Shuping Xiaa

 

Equilibrium solubility of cesium chloride-hydrochloric acid-water system is measured in the temperature range of -24 to 50°C. Based on this data and the solubility data of the cesium chloride-water system available in the literature, a simple and practical method for preparation and purification of cesium chloride is presented. A rapid and sensitive analytical system employing atomic absorption spectrometry (AAS) convenient to monitor the quality of the products is also described.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 396-401

 

 

Electrochemical degradation of resorcinol using
mixed oxide coated titanium electrode for
wastewater treatmentA kinetic study

D Rajkumar, K Palanivelu1* & N Mohan

 

This study presents the theory and kinetics of electrochemical degradation of resorcinol in the presence of chloride using Ti/TiO2 - RuO2 - IrO2 electrode. The rate constant is affected by chloride concentration, initial resorcinol concentration and current density. The rate of electrochemical oxidation is found to be a pseudo first order kinetic process. The maximum rate of reaction is obtained at higher chloride concentration with low resorcinol concentration and high current density. The results obtained reveal the feasibility of application of electro-oxidation for the degradation of resorcinol.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 402-407

 

 

Kinetics of RuIII catalysed polymerization of methylmethacrylate by aliphatic amines in
presence of carbontetrachloride

Manisha Pachauri & Santosh K Upadhyay*

 

The kinetics of ruthenium(III) catalysed polymerization of methylmethacrylate(MMA) with aliphatic amines viz. ethylamine, diethylamine and triethylamine has been investigated in presence of carbontetrachloride in dimethylsulphoxide medium employing a dilatometric technique at 60oC. The rate of polymerization of MMA (Rp) is a function of [MMA], [amine], [CCl4] [RuIII]. In absence of either CCl4 or amine no polymerization of MMA was observed under the experimental conditions. The polymerization (Rp) was inhibited by hydroquinone suggesting a free radical mechanism. A mechanism involving the participation of charge transfer complex formed between {amine-RuIII} complex and CCl4 for the initiation of polymerization has been proposed.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 408-413

 

 

Thermal behaviour of bismaleimides,
allyl nadic-imides and their blends

Indrajeet Singh, Anju Srisvastava & I K Varma*

 

Synthesis and characterisation of bis(4-maleimidophenyl) sulphone (B) and its Michael adducts E and F, prepared by reacting 1 mol of B with 0.33 mols of 4,4-diaminodiphenyl ether and 9,9-bis(4-aminophenyl)fluorene is described. Curing characteristics of these resins and bis(4-allyl nadicimidophenyl) methane (S) and 1,6-diallyl nadicimidohexane (V) were studied in static air atmosphere by differential scanning calorimetry. Curing temperatures depended on the structure of the resins and highest curing temperatures were observed in S and V samples. Thermal behaviour of blends of B, E, and F with S and V resins was studied as a function of blends composition. Thermogravimetric analysis of cured resin blends showed an improvement in thermal stability.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 414-419

 

 

Effect of substituents on corrosion inhibition efficiency of arylisothiocyanates and their condensation products with thiosemicarbazide for corrosion of copper in
aqueous chloride solution

M M Singh*, R B Rastogi, B N Upadhyay & M Yadav

 

The inhibition of copper corrosion in 1.5% sodium chloride solution was studied at 25, 35 and 45C using different concentrations of thiosemicarbazide, p-methoxyphenyl isothiocyanate, p-methylphenyl isothiocyanate and p-chlorophenyl isothiocyanate and their corresponding condensation products with thiosemicarbazide. The inhibition efficiency IE of these compounds was evaluated by weight loss and electrochemical polarisation techniques. Substitution at p-position in the phenyl group resulted in change in IE in the following order for both the aryl isothiocyanates and their corresponding condensation products with thiosemicarbazide-p-chlorophenyl-< phenyl- < p-methylphenyl- < p-methoxyphenyl.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 420-423

 

 

Kinetics of esterification of tri-ethylene
glycol-methacrylic acid reaction system

J S Notay & S S Bhagade*

 

Catalysis of esterification reaction of triethylene glycol and methacrylic acid has been reported. A kinetic empirical expression correlating the fractional conversion of methacrylic acid, with catalyst concentration, mole ratio (glycol to methacrylic acid) and temperature is presented for tri-ethylene glycol-methacrylic acid reaction system using methane sulphonic acid and sulphuric acid as homogenous catalyst.

 

 

 

Indian Journal of Chemical Technology

Vol. 10, July 2003, pp. 424-434

 

 

James DewarMore than a flask

Jaime Wisniak

 

James Dewar (1842-1923) is widely known for his pioneering work in cryogenics, of being the first to achieve the liquefaction of hydrogen, by the flask that carries his name, and by his studies about the behaviour of living organisms and materials under conditions of extreme cold. Although he was an excellent experimentalist, he did not leave many significant theoretical contributions.