Indian Journal of Chemical Technology

Total visitors: 43  since 16-05-06

 

VOLUME 13

NUMBER 3

MAY 2006

CODEN: ICHTEU

 

ISSN:0971-457X

 

 

 

CONTENTS

Papers

 


Conventional and non-conventional adsorbents for removal of pollutants from water — A review

 

203

        Amit Bhatnagar & A K Minocha

 

 

Adsorption of cadmium(II) from aqueous solutions by an indigenous clay mineral

218

        IPC Code: B01D21/00

 

        Y C Sharma & V Srivastava

 

 

A new system for spectrophotometric determination of trace amounts of selenium

222

        IPC Code: C01B19/00, G01J3/00

 

        Tom Cherian & B Narayana

 

 

Modelling of a fixed-film tubular photobioreactor for conversion of hydrogen sulphide to elemental sulphur

226

        IPC Code: C01B17/16: 17/027

 

        Murtuza A Syed & Paul F Henshaw

 

 

Recycling of polyethylene/nylon 6 based waste oil pouches using compatibilizer

233

        IPC Code: D06M101:34

 

        Arup Choudhury, Mandira Mukherjee & Basudam Adhikari

 

Stability-indicating HPLC determination of tolterodine tartrate in pharmaceutical dosage form

242

        IPC Code: B01D15/08

 

        Vinay Saxena, Zahid Zaheer & Mazhar Farooqui

 

 

Holdup and solids circulation rate in liquid-solids circulating fluidised bed

247

        IPC Code: B01J8/00

 

        P Natarajan, R Velraj & R V Seeniraj

 

 

Interaction of tartaric acid during hydration of Portland cement

255

        IPC Code: C04B7/02

 

        Sarita Rai, N B Singh & N P Singh

 

 

Removal of total dissolved solids with simultaneous recovery of acid and alkali using bipolar membrane electrodialysis – Application to RO reject of textile effluent

 

262

        IPC Code: C02F1/44

 

        M Nisha Priya & K Palanivelu

 

Electrochemical behaviour of some industrially important azonaphthol derivatives at glassy carbon electrode

269

        IPC Code: C07C245/02

 

        H Jayadevappa, Y Shivaraj, K M Mahadevan, B E Kumaraswamy, A K Sathpathi &
B S Sherigara

 

Ternary inhibitor system containing phosphonate, molybdate and Zn2+ in corrosion control of carbon steel

 

275

        IPC Code: C23F13/00

 

        B V Appa Rao & K Christina

 

 

Photoinitiated copolymerization of α-terpineol and methylmethacrylate

283

        IPC Code: C08F2/00

 

        Sarika Yadav & A K Srivastava

 

 

Prediction of vapour-liquid pseudo-equilibrium data for pervaporation of benzene-cyclohexane system

 

290

        IPC Code: B01D61/00

 

Debarati Mitra (‘nee Sarkhel), Debashis Roy, Madhusree Bandyopadhyay &
Pinaki Bhattacharya

 

 

Notes

 

 

 

An extractive colorimetric method for determination of pentachlorophenol (PCP) 

294

        IPC Code: G01J3/00

 

        Aruna Sao, Ajai K Pillai & V K Gupta

 

 

Potential of leaf litter for phenol adsorption- A kinetic study

298

        IPC Code: C02F3/00, B01D15/00

 

        Susmita Mishra & J Bhattacharya

 

 

A simple HPLC method for determination of 2-diazonaphtho-quinone-5-sulphonic acid phenyl ester used in positive photoresists

 302

        IPC Code: B01D15/08

 

        Maruthi Janaki Ram Reddy, V Venkat Reddy, B Ananda Rao & V Jayathirtha Rao

 

 

 

Chem-Tech Scan

 305

 

 

Author Index

309

 

 

Keyword Index

310

 

 

Guidelines for Authors

311

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 203-217

 

Conventional and non-conventional adsorbents for removal of pollutants from water – A review

Amit Bhatnagar* & A K Minocha

 

In the present article, the suitability of activated carbon and other alternative adsorbents for wastewater treatment has been reviewed. It is evident from literature survey of last 20-25 years that researchers have gained success to some extent in developing inexpensive adsorbents for water pollution control utilizing naturally available and waste materials. However, still there is a need to find out the practical utility of such developed adsorbents on large-scale and safe and eco-friendly disposal of spent adsorbents.

Keywords: Water pollution, Wastewater treatment, Adsorption, Activated carbon, Low-cost adsorbents

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 218-221

 

Adsorption of cadmium(II) from aqueous solutions by an indigenous clay mineral

 

Y C Sharma* & V Srivastava

 

Removal of cadmium, a priority pollutant, has been investigated by a locally available clay mineral, China clay. The removal depends on initial concentration of cadmium in solution and higher removal has been obtained in lower concentration ranges. The removal increased from 41.0 to 80.3% by decreasing the concentration of cadmium in solution from 2.0´10-4 to 0.5´10-4 M at 6.5 pH, 100 rpm and 0.01 M NaClO4 ionic strength. The pH of the solution plays an important role in the removal of cadmium. Rate of the removal was calculated by Lagergren’s model and was found to be 5.10´10-2 min-1 in optimum conditions. The process of removal proceeds with intraparticle diffusion and the value of the coefficient of intraparticle diffusion was found to be 3.25´10-10 cm2 s-1. The parameters can be used for designing a plant for treatment of Cd(II) rich water and wastewater economically.

Keywords: Cadmium(II), Adsorption, China clay

                IPC Code: B01D21/00

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 222-225

 

A new system for spectrophotometric determination of
trace amounts of selenium

 

Tom Cherian & B Narayana*

 

A simple and selective spectrophotometric method for the determination of trace amounts of selenium(IV) is described based on the oxidation of phenylhydrazine-p-sulphonic acid and coupling reactions. Selenium(IV) oxidizes phenylhydrazine-p-sulphonic acid into its diazonium salt in an acid medium. The diazonium salt is then coupled with acetylacetone or ethylacetoacetate in an alkaline medium, which gives azo dyes with absorption maximum at 490 or 470 nm, respectively. The method obeys Beer’s law in the concentration range of 0.5-20 μg mL-1 of selenium with phenylhydrazine-p-sulphonic acid-acetylacetone and 1-24 μg mL-1 of selenium with phenylhydrazine-p-sulphonic acid-ethylacetoacetate couples. The molar absorptivity, Sandell’s sensitivity of the systems with phenylhydrazine-p-sulphonic acid-acetylacetone and phenylhydrazine-p-sulphonic acid-ethylacetoacetate couples were found to be 1.02´104 Lmol-1cm-1, 7.69´10-3 mg cm-2 and 1.18´104 L mol-1cm-1, 6.67´10-3 μg cm-2, respectively. The developed method has been successfully applied for the determination of selenium in plant material, water and soil samples.

Keywords: Spectrophotometry, Selenium determination, Phenylhydrazine-p-sulphonic acid, Acetylacetone, Ethylacetoacetate

IPC Code: C01B19/00,G01J3/00

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 226-232

 

Modelling of a fixed-film tubular photobioreactor for conversion of
hydrogen sulphide to elemental sulphur

 

Murtuza A Syed* & Paul F Henshaw

 

Relationships were developed to establish the theoretical basis for scale-up of a fixed-film continuous-flow tubular photobioreactor for removal of hydrogen sulphide from synthetic industrial wastewater and its conversion to elemental sulphur. These are based on experiments with a bench scale reactor where the active part of the reactor was sixteen 150 mm length Tygon tubes. Three different tube sizes (internal diameters of 6.4, 3.2 and 1.6 mm) were used to investigate the effect of tube size on reactor performance. In addition, the washout velocity (the velocity at which fixed-film biomass started to washout) for the 1.6 mm diameter tube reactor was determined. Three models were developed to predict reactor performance and establish the basis for scale-up of the process. All three models predicted reactor performance with a reasonable degree of accuracy.

Keywords: Chlorobium limicola, Fixed-film, Photobioreactor, Phototrophic, Green sulphur bacteria

IPC Code: C01B17/16:17/027

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 233-241

 

Recycling of polyethylene/nylon 6 based waste oil pouches using compatibilizer

Arup Choudhury, Mandira Mukherjee & Basudam Adhikari*

 

The present investigation deals with the viability of the use of recycled oil pouch material, which is a coextruded film of LDPE/LLDPE blend and nylon 6, and the scope for improvement of its properties by addition of compatibilizers. In fact, the use of reactive compatibilizers in recycling of mixed polymer waste was well proposed. Two efficient reactive compatibilizers, viz., zinc salt of ethylene methacrylic acid copolymer (Surlyn ionomer) and polyethylene grafted maleic anhydride (Fusabond) were used for this purpose. The effectiveness of the use of compatibilizer during recycling was evaluated by infrared spectroscopy, melt flow index, scanning electron microscopy, differential scanning calorimetry, X-ray diffraction analysis and mechanical properties. It was found that both thermal stability and mechanical properties of the recycled blend were remarkably improved by the addition of compatibilizing agent. Surlyn ionomer gave the best compatibilizing effect. However, the overall performances of compatibilized recycled oil pouch materials indicate their suitability in several demanding applications.

Keywords: Recycling, Polyethylene-nylon 6 blend, Compatibilization, MFI, Morphology, Thermal and mechanical properties

IPC Code: D06M101:34

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 242-246

 

Stability-indicating HPLC determination of tolterodine tartrate in
pharmaceutical dosage form

Vinay Saxena*, Zahid Zaheer & Mazhar Farooqui

 

A simple, selective, precise and stability-indicating high-performance liquid chromatographic (HPLC) method of analysis tolterodine tartrate in pharmaceutical dosage form was developed and validated. The chromatographic conditions comprised a reversed-phase C18 column (250 ´ 4.6 mm), 5 µ with a mobile phase consisting of a mixture of buffer solution (2.88 g ammonium dihydrogen orthophosphate in 1 L of water) and methanol in the ratio of 40 : 60. Triethylamine (5 mL /L) was added to it and pH of mobile phase was adjusted to 7.0± 0.1 with orthophosphoric acid at a flow rate of 1.5 mL/min. Detection was carried out at 220 nm. The retention time of tolterodine was 6.49 min. The linear regression analysis data for the calibration plots showed good linear relationship with coefficient of regression value, r2 = 0.99 in the concentration range 200.60-601.80 µg per mL. The value of correlation coefficient, slope and intercept were 1.0, 20.87 and –6.87, respectively. The method was validated for precision, recovery, ruggedness and robustness. The drug undergoes degradation under acidic, basic, photochemical and thermal conditions. All the peaks of degraded product were resolved from the active pharmaceutical ingredient with significantly different retention time. The samples degraded with hydrogen peroxide showed no additional peak. This indicates that the drug is susceptible to acid-base hydrolysis, photochemical and thermal degradation. Statistical analysis proves that the method is reproducible and selective for the estimation of said drug. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one.

Keywords: Tolterodine tartrate, HPLC, Stability indicating, Degradation

IPC Code: B01D15/08

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 247-254

 

Holdup and solids circulation rate in liquid-solids circulating fluidised bed

 

P Natarajan*, R Velraj & R V Seeniraj

 

Experimental data, obtained using liquid-solids circulating fluidised bed, are presented to study the influence of liquid flow rate and the solids properties on the solids velocity and holdup in the riser. The influence of the auxiliary liquid flow facilitating the solids feed into the riser, and that of primary liquid flow providing the solids transport in the riser are clearly examined and correlations are presented for the holdup and the solids circulation rate based on the present data and the data reported in literature.

Keywords: Liquid-solids circulating fluidised bed, Solids circulation velocity, Solids holdup, Stable operating range

IPC Code: B01J8/00

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 255-261

 

Interaction of tartaric acid during hydration of Portland cement

 

Sarita Rai, N B Singh* & N P Singh

 

Hydration of Ordinary Portland cement (OPC) in the presence of tartaric acid has been studied by using different techniques. Calorimetric studies have shown a rapid enhanced heat evolution within 5 min of hydration in presence of 1.0 wt% tartaric acid with a strong retardation of silicate phase hydration. DSC and X-ray diffraction studies have confirmed the formation of calcium tartarate hydrate in presence of 20.0 wt% tartaric acid. This compound is separated in the form of crystals as identified by SEM studies. I.R. studies confirmed the interaction of tartaric acid with mineral phases of the cement. The retardation of hydration has been explained on the basis of precipitation of calcium tartarate hydrate at the surface of cement grains.

Keywords: Hydration, Portland cement, Tartaric acid, SEM

IPC Code: C04B7/02

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 262-268

 

Removal of total dissolved solids with simultaneous recovery of acid and alkali using bipolar membrane electrodialysis–Application to RO reject of textile effluent

M Nisha Priya & K Palanivelu*

 

The present paper focuses on the application of electrodialysis process with bipolar membranes (EDBPM) for the treatment of reverse osmosis (RO) reject. The purpose of this work includes investigation on the reduction of total dissolved solids (TDS) of the RO reject process with the recovery of acids and bases. Preliminary studies were conducted with sodium chloride solutions in batch recirculation mode. The effect of process parameters such as electrolyte concentration in the electrode compartments (sulphuric acid and NaOH in anode and cathode compartments respectively), current density, flow rate, feed concentration on the process efficiency such as acid and alkali production, current efficiency and energy consumption were evaluated. The transport of co-ions to the electrode compartments was also studied. The optimum conditions of the process were found to be with electrolytes of 0.05 N concentration in electrode compartments (sulphuric acid and sodium hydroxide in anode and cathode compartments, respectively), with current density of 0.83A/ dm2 at 10, 000 mL/h flow rate. At these conditions the treatment was applied to a RO reject of textile effluent for the removal of TDS with acid and alkali recovery. On treatment the conductivity of the solution decreased to about 99.6% with recovery of acid and alkali concentrations of 0.274 N and 0.258 N, respectively. The energy consumption and current efficiency of the process were found to be 0.310 KWh/L and 56.8%, respectively. The transport number of chloride and sodium ions during the treatment of RO reject was found to be 0.0389 and 0.0161, respectively.

Keywords: Electrodialysis, Bipolar membranes, Textile dye effluent, RO reject, TDS removal, Acid/alkali recovery

IPC Code: C02F1/44

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 269-274

 

Electrochemical behaviour of some industrially important azonaphthol derivatives at glassy carbon electrode

H Jayadevappa, Y Shivaraj, K M Mahadevan, B E Kumaraswamy, A K Sathpathi & B S Sherigara*

 

Electroreduction of – N = N – and – NO2 groups of azodyes, 1-(4-nitro phenyl) -azo-2-naphthol (A), 1-(3-nitrophenyl)-azo-2-naphthol (B), 1-(2-nitrophenyl)-azo 2-naphthol (C) has been studied. The azo compound not containing - NO2 group taken for the study was 1-(2-hydroxyphenyl)-azo-2-naphthol (D). The studies were carried out in partial aqueous media containing organic co-solvents such as acetonitrile, DMF and methanol. The substituent effect on cathodic reduction potentials Epc in case of dyes A, B, C were studied and it was found to be in increasing order i.e. Epc(A) < Epc(B) < Epc(C). During electroreduction of dyes A, B, and C, two separate quasireversible peaks, one for reductive cleavage of – N = N – groups, the other one due to reduction of – NO2 group into – NH2 groups were observed. The redox process has been compared with the cyclic voltammetry of the trial compounds, 2-nitroaniline and 4-amino-3-hydroxy naphthalene-1-sulphonic acid. The other data such as effect of pH, concentration of active species, supporting electrolyte, scan rate on cathodic reduction peak potential and cathodic peak current has been determined. The process is found to be diffusion controlled.

Keywords: Voltammetry, Azo dyes, Azonaphthol derivatives, Glassy carbon electrode

IPC Code: C07C245/02

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 275-282

 

Ternary inhibitor system containing phosphonate, molybdate and Zn2+ in corrosion control of carbon steel

B V Appa Rao* & K Christina

 

With the objective of developing a new environmental friendly inhibitor formulation for corrosion of carbon steel in nearly neutral aqueous environments, phosphonic acid viz., N-(2-hydroxyethyl) imino-bis(methylphosphonic acid) [HEIBMPA] was chosen as the inhibitor. Zn2+ was chosen as the first synergist. A maximum inhibition efficiency of 99.3% was obtained with the binary system containing 70 ppm HEIBMPA and 80 ppm Zn2+. Molybdate ion, which is inorganic in nature but environmental friendly, was used as the second synergist. The binary inhibitor formulation containing relatively low concentrations, viz., 30 ppm HEIBMPA and 40 ppm Zn2+ offered an inhibition efficiency of only 23%. To the above combination, when 200 ppm molybdate was added, the inhibition efficiency was found to increase to 95%. The potentiostatic polarization studies revealed that this ternary inhibitor system controlled the anodic reaction predominantly. A large increase in the polarisation resistance (Rp) value indicated the formation of a non-porous protective film on the metal surface. The reflection absorption FT-IR spectrum and X-ray photoelectron spectra of the film suggested that the film consisted of [Fe(III)-HEIBMPA-molybdate] complex, [Fe(III), Zn(II)-HEIBMPA-molybdate]complex, oxides and hydroxides of iron and Zn(OH)2. A plausible mechanism of inhibition of corrosion is proposed, which explains all the above experimental results.

Keywords: N-(2-hydroxyethyl)imino-bis(methylphosphonic acid), Molybdate, Corrosion inhibition

IPC Code: C23F13/00

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 283-289

 

Photoinitiated copolymerization of a-terpineol and methylmethacrylate

 

Sarika Yadav & A K Srivastava*

 

Free radical copolymerization of a-terpineol and methylmethacrylate (MMA) in xylene at 30±0.2°C using azobisisobutyronitrile (AIBN) as the photoinitiator for 27 h has been carried out. The kinetic expression is {Rp a[AIBN]0.62, [a-terpineol]1.2, [MMA]1.5}. It is attributed to primary radical termination as well as degradative chain transfer reaction. Analysis of the copolymers by IR and NMR shows the presence of alcoholic and carboxyl group due to acrylate in the copolymer. The glass transition temperature of the copolymer, determined by differential scanning calorimetry, is 85°C. The alternating nature of the copolymer is confirmed by the product of the reactivity ratios r1 [MMA] = 0.12 and r2 [a-terpineol] = 0.08. The Alfrey-Price, Q-e parameter for a-terpineol has been calculated as 0.282 and 1.82, respectively. A possible mechanism of the copolymerization has been proposed.

Keywords:  a-Terpineol, Copolymerization, Photoinitiator, Kinetics

IPC Code: C08F2/00

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 290-293

 

 

Prediction of vapour-liquid pseudo-equilibrium data for pervaporation of benzene-cyclohexane system

Debarati Mitra (‘nee Sarkhel), Debashis Roy, Madhusree Bandyopadhyay & Pinaki Bhattacharya

 

In pervaporation operation pore diffusion model predicts that a vapour-liquid pseudo-equilibrium exists between the solute concentration in vapour and liquid phases during its flow through the pores of the membrane. In the present investigation, using pore diffusion model an attempt has been made to predict a semi-empirical vapour-liquid equilibrium relationship for benzene concentration in vapour and liquid inside the pore of the membrane while separating benzene-cyclohexane azeotropic mixture by pervaporation technique.

Keywords:  Pervaporation, Vapour-liquid pseudo-equilibrium, Benzene-cyclohexane mixture, Pore-diffusion model

IPC Code: B01D61/00

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 294-297

 

An extractive colorimetric method for determination of pentachlorophenol (PCP)

Aruna Sao, Ajai K Pillai & V K Gupta

 

A new extractive spectrophotometric method, which is sensitive, is described for the determination of pentachlorophenol (PCP), a widely used insecticide and herbicide. The method is based on the reaction of pentachlorophenol with concentrated nitric acid at elevated temperature to form chloranil, which liberates iodine with potassium iodide. The liberated iodine then forms yellow brown coloured complex with cetyltrimethyl-ammoniumbromide (CTAB) having absorption maximum at 390 nm and extractable into isoamyl alcohol. Beer’s law is obeyed over the concentration range of 2.5-20 mg of PCP in a final solution 100 mL (0.025-0.20 ppm) and has molar absorptivity and Sandell’s sensitivity values of 9.6´105 L mol-1 cm-1 and 0.000277-mgcm-2, respectively. The detection limit and quantification limit for the proposed method is found to be 0.0018 and 0.0063 ppm, respectively. The method has been satisfactorily applied for the determination of PCP in water, plant material and biological samples.

Keywords:            Spectrophotometry determination, Pentachlorophe-nol, Cetyltrimethylammoniumbromide

IPC Code: G01J3/00

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 298-301

 

Potential of leaf litter for phenol adsorption ľA kinetic study

Susmita Mishra & J Bhattacharya

 

The present study envisages the use of plant material, Shorea robusta for the removal of phenol by adsorption process. The effect of pH, contact time, particle size and initial concentration of adsorbate on removal process was investigated. The maximum removal of phenols from their aqueous solutions occurred in the pH range of 4-6. Kinetic parameters as a function of concentration and pH were evaluated to predict the nature of adsorption. Equilibrium adsorption data were correlated with Freundlich adsorption isotherm model. The maximum adsorption capacity of leaf litter was found to be 0.06 mg/g.

Keywords: Adsorption, Equilibrium, Kinetics, Phenol

IPC Code: C02F3/00, B01D15/00

 

 

Indian Journal of Chemical Technology

Vol. 13, May 2006, pp. 302-304

 

A simple HPLC method for determination of 2-diazonaphthoquinone-5-sulphonic acid phenyl ester used in positive photoresists

 

Maruthi Janaki Ram Reddy, V Venkat Reddy, B Ananda Rao & V Jayathirtha Rao*

 

A simple high performance liquid chromatographic (HPLC) method for the determination of 2-diazonaphthoquinone-5-sulphonic acid phenyl ester (DNQ) is developed. 5-Amino naphthalene-1-sulphonic acid sodium salt is used as internal standard. A Polaris C18-5 m silica column (250´4.6 mm), 5 m particle size, was equilibrated with a mobile phase composed of methanol and water (80:20, v/v). Flow rate was 1.0 mL/min. The elution time for 5-amino naphthalene-1-sulphonic acid sodium salt and DNQ was approximately 2 and 4 min, respectively. Calibration curve of DNQ was linear in the concentration range of 10-50 mg/mL. Limit of detection and quantification were measured in the lowest concentrations of the replicates. Recovery is about 96%.

Keywords: 2-Diazonaphthoquinone-5-sulphonic acid phenyl ester, 5-Amino naphthalene-1-sulphonic acid sodium salt, Reverse phase HPLC, Quantification, HPLC method validation

IPC Code: B01D15/08