Indian Journal of Chemical Technology


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VOLUME 13

NUMBER 1

JANUARY 2006

CODEN: ICHTEU

 

ISSN:0971-457X

 

CONTENTS

Papers

 

Titrimetric and spectrophotometric determination of lamivudine in pharmaceuticals

   IPC Code: G01J3/00

  K Basavaiah & B C Somashekar

7

    

 

 

 

 

A chloride ion-selective potentiometric sensor based on a polymeric schiff base complex

   IPC Code: C07C251/02

K Girish Kumar, K Saji John & C J Indira

13

    

 

       

 

 

 

Use of jackfruit peel carbon (JPC) for adsorption of rhodamine-B, a basic dye from aqueous solution

  IPC Code: C09B61/00

   B Stephen Inbaraj & N Sulochana

 

17

       

 

    

 

 

 

Bioprocessing and resource recovery of solid waste by low-income citizens

  IPC Code: C05F9/00

S Gajalakshmi, P. Sankar Ganesh and S A Abbasi

24

       

 

       

 

 

 

Quantification of polycyclic aromatic hydrocarbons in fruits and vegetables using high performance liquid chromatography

IPC Code: C07C15/00

Narsi R Bishnoi, Urvashi Mehta & G G Pandit

 

30

       

 

       

 

 

 

Spectrophotometric determination of arsenic in environmental and biological Samples

  IPC Code: G01J3/00

B Narayana, Tom Cherian, Mendalin Mathew & Chand Pasha

36

       

 

       

 

 

 

Alternate method for synthesis of 1,3,3-trinitroazetidine (TNAZ): Next generation melt castable high energy material

IPC Code: C06B25/00

H S Jadhav, M B Talawar, D D Dhavale, S N Asthana & V N Krishnamurthy

 

41

       

 

       

 

 

 

Quickly design CO2 – amine absorber

  IPC Code: C01B31/00; B01D15/00

Prakash D Vaidya & Vijaykumar V Mahajani

47

       

 

       

 

 

 

Leaching of non-treated ilmenite by HCL-CH3OH-H2O mixture and its Kinetics

  IPC Code: B01D21/00

M A Habib, R K Biswas, M R Ali & A K M Hasan

53

       

 

       

 

Kinetic studies on mineralization of p-nitrophenol by Pseudomonas putida at low and high concentration

  IPC Code: C12P1/04

Meenal Kulkarni & Ambalal Chaudhari

 

60

       

 

       

 

Preparation and properties of composite membranes composed of non-conductive membranes and polypyrrole

IPC Code: C08J5/24

  S S Madaeni

 

65

       

 

       

 

 

 

Volume and transport properties of binary liquid systems of acrylonitrile with aromatic ketones at 308.15 K

  IPC Code: G05D23/13

  Savitha Jyostna Tangeda & Satyanarayana Nallani

 

71

       

 

       

 

 

 

Notes

 

 

 

Interelemental interference correction by computational method in flame atomic absorption spectroscopy (FAAS): Study of Fe-Mn system in silico-manganese ferro-alloy

IPC Code: C22C9/05

A S Rao, K K Gupta, M Singh, A K Upadhyay & J K Sircar

 

77

       

 

       

 

 

 

Simultaneous spectrophotometric determination of formoterol fumarate and budesonide in their combined dosage form

  IPC Code: G01J3/00

  A V S S Prasad

81

       

 

       

 

 

 

Metal ion chromatography on sodium diethyldithiocarbamate

  IPC Code: B01D15/00

H S Rathore, M Kumar & K Ishratullah

84

       

 

       

 

 

 

Chem-Tech Scan

89

 

 

Author Index

93

 

 

Keywords Index

94

 

 

Guidelines for Authors

95

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 7-12

 

Titrimetric and spectrophotometric determination of lamivudine in pharmaceuticals

 

K Basavaiah* & B C Somashekar

 

Three new methods are described for the assay of lamivudine in bulk drug and in tablet dosage forms using chloramine-T and two dyes, methyl orange and indigo carmine, as reagents. In titrimetry, aqueous solution of lamivudine is treated with a measured excess of chloramine-T in sulphuric acid medium and after the oxidation of lamivudine is judged to be complete, the unreacted oxidant is determined iodometrically. Spectrophotometric methods entail the addition of a known excess of chloramine-T to lamivudine in hydrochloric acid medium followed by determination of residual oxidant by reacting it 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 chloramine-T reacted corresponds to the amount of lamivudine. Titrimetric method is applicable over 3.5-10 mg range. In spectrophotometric methods, the systems obey Beer’s law for 0.1-1.0 and 0.25-3.5 mg mL-1 for method A and method B, respectively. Intra-day and inter-day precision and accuracy of the developed methods were evaluated. The methods were successfully applied to the assay of lamivudine in tablet formulations and the results were compared with those of a reference method by applying Student’s t- and F-tests. No interference was observed from common tablet adjuvants.

Keywords: Lamivudine, Assay, Titrimetry, Spectrophotometry, Chloramine-T, Tablets

IPC Code: Int. Cl.7 G01J3/00

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 13-16

 

A chloride ion-selective potentiometric sensor based on
a polymeric schiff base complex

K Girish Kumar*, K Saji John & C J Indira

 

This paper describes the fabrication of an ion-selective electrode in which a polymeric schiff base complex of cobalt(II) is used as the ionophore. The main advantage of the electrode is that it is mechanically stable upto 3 months. The electrode shows a linear response in the range of 2.5 ´ 10-5-0.5 ´ 10-1 mol dm-3. The response time of the electrode is 30 s. The pH range at which the electrode works is 3.8 to 6.8. The electrode was found to be selective towards chloride ion in the presence of ions like Na+, Ca2+, Mn2+, Fe3+, Co2+, Ni2+, Cu2+, Zn2+, CH3COO-, NO3-, SO42-, Br- and NO2-.

Keywords: Ion selective electrodes, Chloride ion, Amino methylated  polystyrene

IPC Code: Int. Cl.7 C07C251/02

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 17-23

 

Use of jackfruit peel carbon (JPC) for adsorption of rhodamine-B, a basic dye from aqueous solution

 

B Stephen Inbaraj* & N Sulochana

 

A carbon sorbent derived from an agricultural waste, jackfruit peel was applied to study the removal of a basic dye, rhodamine-B from aqueous solution. Batch experiments were performed as a function of process parameters like agitation time, initial dye concentration, temperature, carbon dose and pH. Modified Ritchie second order equation better predicted the kinetic results compared to other rate equations (pseudo first order and pseudo second order) tested. Among the isotherm models applied to the equilibrium data Redlich-Peterson model better predicted the experimental values. The adsorption capacity was 121.47 mg g-1 at an initial pH of 6.0 and at 32 ± 0.5°C. The adsorption capacity increased with increase in temperature. The influence of pH on dye removal was not significant. An optimum carbon dose of 1.2 g L-1 was required for the maximum removal (96%) of dye from its 60 mg L-1 solution. A significant portion of the dye was recovered from the spent carbon using 50% acetic acid.

Keywords: Adsorption, Rhodamine-B, Jackfruit peel, Carbon, Kinetics, Isotherms

IPC Code: Int. Cl.7 C09B61/00

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 24-29

 

Bioprocessing and resource recovery of solid waste by low-income citizens

 

S Gajalakshmi, P Sankar Ganesh & S A Abbasi*

 

The know-how developed earlier by the authors for resource recovery from household wastes, crop wastes, and weeds was extended to subsistence farmers and householders in rural Pondicherry, India, with an objective of identifying technological, operational, and sociological problems which may be faced when transferring this know-how to similar rural populations in the developing countries. The aim of the study was also to refine the know-how for eliminating the problems. In this paper the results of solid waste management by composting-vermicomposting at 53 sites in four villages of Pondicherry are presented. At all sites the pH, temperature, and C/N ratio were systematically measured for process monitoring and control. The results establish the suitability of the know-how for easy adoption by low-income householders and its propensity to achieve pollution control with income generation.

Keywords: Composting, Vermicomposting, Resource recovery, Water hyacinth, Earthworms

IPC Code: Int. Cl.7 C05F9/00

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 30-35

 

Quantification of polycyclic aromatic hydrocarbons in fruits and vegetables using high performance liquid chromatography

Narsi R Bishnoi , Urvashi Mehta & G G Pandit

 

This paper describes a method for determination of 16 polycyclic aromatic hydrocarbons (PAHs) in vegetables and fruits. In the present study reversed phase high-performance liquid chromatography with UV-VIS detection was optimized for separation and quantification of individual PAHs in fruit and vegetable samples. Concentration of total PAHs in different vegetable and fruit samples varied from 59.6 to 194.3 µg/kg and 25.5 to 51.7 µg/kg, respectively. The mean recovery of PAHs in different samples was in range of 70-86% with relative standard deviation in the range of 0.4-7%.

Keywords: Polycyclic aromatic hydrocarbons, HPLC, UV-VIS

IPC Code: Int. Cl.7 C07C15/00

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 36-40

 

Spectrophotometric determination of arsenic in environmental and
biological samples

B Narayana*, Tom Cherian, Mendalin Mathew & Chand Pasha

 

A simple and sensitive spectrophotometric method has been developed for the determination of arsenic using variamine blue as a chromogenic reagent. The method is based on the reaction of arsenic(III) with potassium iodate in acid medium to liberate iodine, which oxidizes variamine blue to form a violet coloured species having an absorption maximum at 556 nm. Beer’s law is obeyed in the range 0.2-14 μg mL-1 of As(III). The molar absorptivity, Sandell’s sensitivity, detection limit and quantitation limit were found to be 1.43´104 L mol-1cm-1, 5.26´10-2 μg cm-2, 0.022 and 0.072 μg mL-1, respectively. The optimum reaction conditions and other analytical parameters were evaluated. The proposed method has been successfully applied for the determination of arsenic in various environmental and biological samples.

Keywords: Arsenic, Spectrophotometry, Iodate, Variamine blue

IPC Code: Int. Cl.7 G01J3/00

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 41-46

 

Alternate method for synthesis of 1,3,3-trinitroazetidine (TNAZ): Next generation melt castable high energy material

H S Jadhav, M B Talawar*, D D Dhavale, S N Asthana & V N Krishnamurthy

 

The synthesis of 1,3,3-trinitroazetidine (TNAZ) from 2,2-dinitropropane-1,3-diol precursor derived from nitromethane is described. The cyclization of 1,3-dichloro-2,2-dinitropropane in presence of t-butyl amine to t-butylated azetidine ring, followed by its nitration afforded target molecule TNAZ in minimum number of synthesis steps. TNAZ was characterized by elemental analysis, Spectral Energy Dispersive Analyser-X-ray (EDAX), and Scanning Electron Microscope (SEM) techniques. Thermolysis studies on TNAZ were undertaken using Differential Scanning Calorimetry (DSC) and Thermo Gravimetric (TG) techniques. The Fourier Transform Infrared (FTIR) of decomposition products of TNAZ revealed the evolution of oxides of nitrogen and –CN containing species suggesting the cleavage of C/N-NO2 bond accompanied with the collapse of the ring structure. The sensitivity data obtained for the TNAZ indicated its sensitive nature towards external stimuli (Impact height (h50%) for explosion > 47 cm; Friction insensitive up to > 36 kg). The theoretically predicted performance parameters suggest that TNAZ is energetically superior in terms of velocity of detonation (VOD: 8.6 km/s) and power index (PI: 182) compared to the conventionally used melt castable high explosive 2,4,6-trinitrotoluene (TNT) (VOD-6.66 km/s and PI-125).

Keywords: Trinitroazetidine, Melt cast explosive, Synthesis, Thermolysis

IPC Code: Int.Cl.7 C06B25/00

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 47-52

 

Quickly design CO2 – amine absorber

 

Prakash D Vaidya & Vijaykumar V Mahajani*

 

An integral rate-based model is used to find a quick and reliable estimate of the height of packing in a CO2-alkanolamine absorber. Heat transfer in the gas phase is neglected. Due to the need to arrive at a quick estimate of the height of packing, this assumption is made. Starting from the bottom, the height of packing required for a small change in solute mole fraction in a differential section of the tower is calculated. An average of the enhancement factor calculated using film theory of mass transfer accompanied by chemical reaction for each boundary, is used. These calculations are repeated until at the top of the tower, the desired solute concentration is reached. The cumulative height gives total height of packing required. The method is illustrated.

Keywords: CO2, Absorption, Alkanolamine

IPC Code: Int. Cl.7 C01B31/00; B01D15/00

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 53-59

 

Leaching of non-treated ilmenite by HCl-CH3OH-H2O mixture and its kinetics

M A Habib*, R K Biswas, M R Ali & A K M Hasan

 

The effect of the addition of methanol to leachant hydrochloric acid on the dissolution of non-treated ilmenite has been investigated. The kinetics of the dissolution processes have also been investigated. The dissolution of ilmenite is enhanced by the addition of little amount of methanol in hydrochloric acid. The leaching with 6 M HCl -0.5 M CH3OH-H2O mixture at 110°C and solid to liquid ratio (S/L) of 0.02 g/mL results in the dissolution of 91% Ti and 95% Fe compared to dissolutions of 53.5% Ti and 60% Fe in 6 M HCl alone. Decrease in leaching temperature and HCl concentration and increase in S/L ratio result in decrease in the extent of dissolution percentages. The kinetics of dissolution have been investigated by measuring the dependences of rate of dissolution on HCl concentration and temperature of leaching. The values of activation energy have been evaluated from the temperature dependence rate data. The kinetic data could be fitted to the Shrinking Core model of dissolution.

Keywords: Leaching, Kinetics, Ilmenite, HCl-CH3OH-H2O mixture, Dissolution

IPC Code: Int. Cl.7 B01D21/00

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 60-64

 

Kinetic studies on mineralization of p-nitrophenol by Pseudomonas putida at low and high concentration

 

Meenal Kulkarni & Ambalal Chaudhari*

 

Pseudomonas putida isolated from ecological habitat, has been evaluated for its potential to mineralize high (2.143 mM) concentration of p-nitrophenol (PNP). The bacterium utilized PNP as the sole source of carbon, nitrogen and energy. Its half saturation constant (Ks values) of PNP degradation was 0.22 mM, as determined by Michaelis- Menten curve. Further, its maximum rate of PNP degradation as per Lineweaver-Burk plot was 4.5 µmol min-1g-1 dry biomass L-1. Its kinetics of growth in minimal medium containing low and high PNP concentrations was Monod type of curve. Various metabolic parameters like specific growth rate (µ), specific PNP uptake rate and specific degradation rate at initial concentrations of 0.143, 0.2143, 0.357, 0.714, 1.43, 2.143 and 3.75 mM PNP were determined.

Keywords: p-Nitrophenol, Mineralization, Kinetics

IPC Code: Int. Cl.7 C12P1/04

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 65-70

 

Preparation and properties of composite membranes composed of
non-conductive membranes and polypyrrole

S S Madaeni

 

Conductive composite membrane was prepared by oxidation of pyrrole in the commercial microfiltration membrane support using ferric ions and ascorbic acid as polymerization and oxidation agents, respectively. The concentrations for pyrrole and ferric chloride solutions were optimized as 0.745 and 2 molar, respectively. An acceptable conductivity resistivity equals to 42.1 Kohm.cm was obtained in these conditions. Filtration of BSA (bovine serum albumin-charged protein) solution was carried out to investigate the properties of prepared membrane. Higher fluxes were obtained for conductive membrane, exhibiting the effect of the membrane conductivity. Both BSA and membrane are negatively charged. This results in the partial repulsion of BSA from the membrane surface or membrane matrix due to the electrostatic barrier. Repulsion means less concentration polarization and fouling i.e. lower resistivity against the passage through the membrane or higher flux. For conductive membrane higher rejection was obtained compared to non-conductive membrane. This effect is attributed to the conductivity of the membrane. The negatively charged membrane surface acts as a barrier against BSA. A part of the protein is pushed back due to the electrostatic effect. This results in higher rejection.

Keywords: Membrane, Conductivity, Microfiltration, Polypyrrole

IPC Code: Int. Cl.7 C08J5/24

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 71-76

 

Volume and transport properties of binary liquid systems of acrylonitrile with aromatic ketones at 308.15 K

 

Savitha Jyostna Tangeda & Satyanarayana Nallani*

 

 

The densities and viscosities for the binary mixtures of acrylonitrile with aromatic ketones (acetophenone, propiophenone, paramethyl acetophenone and parachloro acetophenone) have been reported over the entire range of mole fraction at 308.15 K. The excess molar volume (VE) and deviation in viscosity (Dh) are fitted to a Redlich-Kister type equation. Other parameters like excess Gibbs free energy of activation of viscous flow (G*E) and Grunberg-Nissan interaction parameter (d') are also utilized in the qualitative analysis to elicit the information on the nature of the bulk molecular interactions of acrylonitrile + aromatic ketone binary mixtures.

 

Keywords: Density, Viscosity, Aromatic ketones, Acrylonitrile, Binary solvent mixtures

IPC Code: Int. Cl.7 G05D23/13

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 77-80

 

 

Interelemental interference correction by computational method in flame atomic absorption spectroscopy (FAAS): Study of Fe-Mn system in silico-manganese ferro-alloy

A S Rao, K K Gupta, M Singh, A K Upadhyay & J K Sircar*

 

An accurate method for the estimation of iron and manganese by flame atomic absorption spectrometry (FAAS), correcting the inter-elemental interference, using an ISO accepted two parameter computational method has been developed for silico-manganese samples. Iron and manganese are determined at 372 and 403.1 nm, respectively, using air-acetylene flame. Interelemental interferences can also be overcome by removing one of the interferant ion by precipitating it with zinc oxide. The evaluation of the methodology has been done using Fe-Mn synthetic mixtures, as well as in certified reference materials. The standard deviation is within 1% in majority of samples studied. Some real samples have also been analysed by the present method and the results compared with titrimetric method of analysis.

Keywords: Interference in flame AAS, Statistical model

IPC Code: Int. Cl.7 C22C9/05

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 81-83

 

Simultaneous spectrophotometric determination of formoterol fumarate and budesonide in their combined dosage form

A V S S Prasad

 

A new UV spectrophotometric method for the simultaneous determination of formoterol fumarate and budesonide in their combined dosage form has been developed. The lmax values for formoterol fumarate and budesonide in methanol medium were found to be 217 nm and 252 nm respectively. The results of analysis by this method have been found to be precise and accurate.

Keywords: Simultaneous determination, Formoterol fumarate, Budesonide, Combined dosage form

IPC Code: Int. Cl.7 G01J3/00

 

 

Indian Journal of Chemical Technology

Vol. 13, January 2006, pp. 84-87

 

Metal ion chromatography on sodium diethyldithiocarbamate

H S Rathore*, M Kumar & K Ishratullah

 

Metal ions such as Pb2+, Hg2+, Hg22+, Cd2+, Zn2+, Cu2+, Co2+, Ni2+, Fe3+, Fe2+ and Mn2+ have been chromatographed on paper strips impregnated with sodium diethyldithiocarbamate and its admixtures with SiO2, CaSO4, Na2CO3, NaCl, NH4Cl, EDTA, NaOH, CaCO3, Na2HPO4 and H3PO4. Common solvents namely acetone, acetonitrile, benzene, carbon tetrachloride, isopropanol, aqueous NaDDC and distilled water have been used as mobile phases. Several binary separations of heavy metal ions have been achieved experimentally.

Keywords: Chromatography, Sodium diethyldithiocarbamate, Metal ions

IPC Code: Int. Cl.7 B01D15/08