Indian Journal of Chemical Technology


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Volume 12

Number 4

July 2005

CODEN:ICHTEU 12(4) 387-506

 

ISSN:0971-457X

 

CONTENTS

 

Research articles

 

 

 

Micellar-enhanced ultrafiltration of chromate [Cr(VI)] ion from aqueous streams by using cationic surfactant

 

393

        IPC Code: B01D61/14; C02F

 

        S B Kamble & K V Marathe

 

 

 

Sensitive micro analysis of frusemide (furosemide) in bulk drug and formulations by visible spectrophotometry and high performance liquid chromatography (HPLC)

 

401

        IPC Code: B01D15/00; A61K

 

        K Basavaiah & U Chandrashekar

 

 

 

Agricultural solid waste for the removal of inorganics: Adsorption of mercury(II) from aqueous solution by Tamarind nut carbon

 

407

        IPC Code: B01D17/00; C02F101/20

 

        A Ramadevi & K Srinivasan

 

 

 

Solid phase extraction of lead using modified cellulose in natural wastewater and egg Samples

413

        IPC Code: C22B13/00; B01D; C02F1/00

 

        Bibhesh Kumar Singh, Deo Nandan Kumar & Bhagwan S Garg

 

 

 

Extraction of Zn(II) from sulphate media using organophosphine oxides, cyanex-923 and cyanex-925

 

419

        IPC Code: C22F1/053

 

        S D Pawar & P M Dhadke

 

 

 

Studies on equilibrium and kinetics of ACRY Red 4G removal from aqueous solutions using low cost adsorbents

 

425

        IPC Code: B01D15/00; C02F1/00

 

         Kiran Prajapati, Kalpesh Sidhpuria, Dharmesh Mahajan & Mousumi Chakraborty

 

 

 

Detection, isolation and reconstruction of faulty sensors using principal component analysis

430

        IPC Code: G01N; G21C17/00

 

        M S R K Bose, G Sathyendra Kumar & Ch Venkateswarlu

 

 

 

Removal and recovery of lead from aqueous solution using supported liquid membrane

436

         IPC Code: B01D61/38

 

         R Anupama & K Palanivelu

 

 

 

Pervaporation of chloroform-acetone mixtures through DCP crosslinked poly(ethylene-co-vinyl acetate) membranes

 

441

        IPC Code: B01D61/36

 

        M N Muralidharan & S Anil Kumar

 

Pinacol-Pinacolone rearrangement over solids supported metal ion catalysts

447

         IPC Code: B01J21/00

 

        S Z Mohamed Shamshuddin, George Kuriakose & N Nagaraju

 

 

 

Studies on ionic mass transfer on to a target surface with submerged impinging jet in a closed cell

 

455

        IPC Code: C21D1/00

 

        P King, V S R K Prasad & G Hanumantha Rao

 

 

 

Inhibition of corrosion of mild steel in hydrochloric acid by N-cyclohexyl-N¢-phenyl thiourea

462

        IPC Code: C23F11/00

 

        S Divakara Shetty, Prakash Shetty & H V Sudhaker Nayak

 

 

 

Corrosion behaviour of electrochemically joined aluminum and stainless steel

466

        IPC Code: G01N17/02; C23F11/00

 

        G Sheela, V S Muralidharan & Malathy Pushpavanam

 

 

 

Corrosion inhibition of carbon steel by adipic acid-Zn2+ system

472

         IPC Code: C23F11/00

 

        G Ruba Helen Florence, A Noreen Anthony, J Wilson Sahayaraj, A John Amalraj & Susai Rajendran

 

 

 

Notes

 

 

QA/QC aspects of GC-MS analytical instrument for environmental analysis

477

        IPC Code: B01D15/08; G01N30/00

 

        Sanjay M Kashyap, Girish H Pandya, Sudheer D Wachasunder & Vivek K Kondawar

 

 

 

Educator

 

 

Borax, Boric acid, and Boron-From exotic to commodity

488

        Jaime Wisniak

 

 

 

Chem-Tech Scan

501

 

 

Author Index

505

 

 

Keywords Index

506

 

 

 

 

 

 

 

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 393-400

 

Micellar–enhanced ultrafiltration of chromate [Cr(VI)] ion from aqueous streams by using cationic surfactant

 

S B Kamble & K V Marathe*

 

Hexavalent chromium [Cr(VI)] in industrial effluent is one of the most serious environmental problems in India and also in other countries. Micellar-Enhanced Ultrafiltration (MEUF) of the chromate anions from aqueous solutions has been studied at room temperature (28±2°C) using cationic surfactants, cetyltrimethylammonium bromide (CTAB) and cetylpyridinium chloride (CPC), micelles of which adsorb the chromate ions by electrostatic interactions. The solution is processed by ultrafiltration, using a membrane with a pore size small enough to block the passage of the micelles and the adsorbed ions. The process is highly efficient in removing the chromate ions. In the absence of other electrolytes, chromate ion rejection up to 99% was observed at optimal conditions of pH, pressure, temperature, feed chromate and surfactant concentrations. The presence of added NaCl reduces the chromate rejection, but it was still considerable (up to 82%), even in the presence of 100 mM NaCl. The rejection rate of chromate was found to be highly dependent on the pH of the feed solution. The solute rejection is also affected by anion charge density, and interaction of fixed membrane charge sites with ionic solutes.

Keywords : Chromate ions removal,  surfactant, cetyltrimethylammonium bromide, cetylpyridinium chloride, micelles, membrane process, wastewater treatment, micellar-enhanced ultrafiltration

IPC Code: B01D61/14; C02F

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 401-406

 

Sensitive micro analysis of frusemide (furosemide) in bulk drug and formulations by visible spectrophotometry and high performance liquid chromatography (HPLC)

 

K Basavaiah* & U Chandrashekar

 

Two rapid and sensitive methods using visible spectrophotometry and HPLC are described for the determination of frusemide (FRU) in bulk drug and formulations. Spectrophotometry is based on a redox reaction involving FRU followed by complexation reaction and uses iron(III) and ferricyanide(III) as reagents. The resulting Prussian blue is measured at
760 nm. The HPLC determination was carried out on a reversed phase Accurasil ODS C18 column (250
´ 4.6 mm, 5 mm) using a mobile phase consisting of acetonitrile – 0.1% orthophosphoric acid (pH 3) (60 + 40) at a flow rate of 1.0 mL min-1 with UV detection at 233 nm. Working conditions of both methods have been optimized and the methods validated as per the ICH guidelines. In spectrophotometry, a regression analysis of Beer’s law plot showed a good correlation in the concentration range 0.4 - 4.0 mg mL-1 with an apparent molar absorptivity of 4.03 ´ 104 L mol-1 cm-1 and a Sandell sensitivity of 7.85 ng cm-2. The limits of detection and quantification were calculated to be 0.09 and 0.28 mg mL-1 respectively. The linear range of determination by HPLC was 1.01 - 121.8 mg mL-1. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found to be 0.3 and 0.6 mg mL‑1, respectively. Within-day accuracies and precisions were £ 3% and between-days precisions were less than 5% for all the concentrations tested. The methods were applied to the assay of FRU in tablets and injections. The label claim percentages and relative standard deviations were in the 98.28- 103.24 and 0.36 - 2.04% range, respectively. The validity of the methods was further ascertained by parallel determination by a reference method and by recovery studies via standard addition technique. The results showed that the procedures are suitable for routine analysis of the diuretic.

Keywords: Frusemide, assay, spectrophotometry, HPLC, prussian blue, formulations

IPC Code:B01D15/00; A61K

 

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 407-412

 

Agricultural solid waste for the removal of inorganics: Adsorption of mercury(II) from aqueous solution by Tamarind nut carbon

 

A Ramadevi & K Srinivasan*

 

The adsorption of Hg(II) on modified tamarind nut carbon (Bicarbonate treated tamarindnut carbon – BTNC) was investigated to assess the possible use of this adsorbent for the processing of mercury removal from wastewater. The influence of various factors such as agitation time, pH and carbon dosage on the adsorption capacity has been studied. Adsorption isothermal data could be interpreted by Langmuir and Freundlich equations. In order to understand the reaction mechanism, kinetic data has been studied using reversible first order rate equation.

Keywords: Tamarind nut carbon, mercury(II) adsorption, Langmuir and Freundlich isotherm, first order kinetics

IPC Code: B01D17/00; C02F101/20

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 413-418

 

Solid phase extraction of lead using modified cellulose in natural,
wastewater and egg samples

 

Bibhesh Kumar Singh, Deo Nandan Kumar & Bhagwan S Garg*

 

2-Pyridyliminosalicylcellulose has been used for the sorption and estimation of lead(II) by column and batch techniques. The distribution coefficient (D) was found to be 4.3´102 for the lead ion. The detection limit was found to be 3.82 ng mL-1 and the breakthrough volume was 20 mL. The present matrix coupled with FAAS has been used to enrich and determine the lead ions in natural and wastewater (RSD ~ 2.52-3.50%) and egg samples (RSD ~ 2.73%). The method is simple, rapid and relatively free from interference and satisfactorily applied for the estimation of lead (~98% recovery) in natural, wastewater and egg samples.

Keywords: Lead(II), extraction, 2-pyridyliminosalicylcellulose, preconcentration, FAAS

IPC Code: C22B13/00; B01D; C02F1/00

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 419-424

 

Extraction of Zn(II) from sulphate media using organophosphine oxides, cyanex-923 and cyanex-925

 

S D Pawar & P M Dhadke*

 

Extraction of Zn(II) with phosphine oxides cyanex-923 and cyanex-925 from sulphate solution is described. Extraction was found to be quantitative with 0.01M cyanex-923 and 0.03 M cyanex-925 in toluene in the pH range 8.0-10.0. From organic phase of cyanex-923 and cyanex-925, Zn(II) was stripped out with 1.0 M HCl and 1.0 M H2SO4 respectively and determined spectrophotometrically. Effect of various parameters such as reagent concentration, equilibration period, effect of various diluents and diverse ions on the extraction of Zn(II) was also studied. The stoichiometry of the extracted species was determined on the basis of slope analysis method.

 

Keywords: Zn(II), extraction, cyanex-923, cyanex-925, stripping

IPC Code: C22F1/053

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 425-429

 

Studies on equilibrium and kinetics of ACRY Red 4G removal from aqueous solutions using low cost adsorbents

 

Kiran Prajapati, Kalpesh Sidhpuria, Dharmesh Mahajan & Mousumi Chakraborty*

 

Applications of low cost adsorbents have been investigated as a replacement for the current expensive methods of reducing COD and colours from dyes/intermediate industrial wastewaters. Presently, PAC (powdered activated charcoal) is widely used in the industries. However, it is costly. Hence, other options have been explored which are low in cost. Effective adsorbents have been developed from bagasse fly ash, thermal fly ash, rice husk, jute thread and sawdust and successfully employed for the removal of dye, ACRY red 4G from aqueous solutions. Factors influencing the adsorption process, e.g., pH, contact time, adsorbent doses and adsorbent particle size are investigated. The experimental data fits well to the second-order kinetic model, which indicates that the chemical sorption is the rate-limiting step. A continuous method for removal of ACRY red 4G from industrial wastewater without prior treatment using all solid adsorbents such as bagasse fly ash, thermal fly ash, rice husk, jute thread and sawdust has also been proposed. An important aspect of the proposed method is that the removal is performed at a pH range in which the dye ACRY red 4G undergo an adsorption process, making the method useful for wastewater treatment.

Keywords: Adsorption, ACRY red 4G, fly ash, dye removal, sawdust, jute tread, rice husk

           IPC Code: B01D15/00; C02F1/00

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 430-435

 

Detection, isolation and reconstruction of faulty sensors using
principal component analysis+

 

M S R K Bose, G Sathyendra Kumar & Ch Venkateswarlu*

 

A strategy based on principal component analysis (PCA) is presented for detection, identification and reconstruction of faulty sensors. In this strategy, sensor fault detection is carried out by using multivariate statistics, faulty sensors are isolated using principal component score contributions and reconstruction of faulty sensors is accomplished through the analysis of fault direction vector. The performance of the strategy is evaluated by applying to a closed-loop controlled CSTR system. The simulation results demonstrate the ability of the strategy for detection, identification and reconstruction of single and multiple faulty sensors.

Keywords: Sensor, principal component analysis, controlled CSTR system

           IPC Code: G01N; G21C17/00

 

Indian Journal of Chemical Technology  

Vol 12July 2005, pp. 436-440

 

Removal and recovery of lead from aqueous solution using
supported liquid membrane

 

R Anupama & K Palanivelu*

 

A laboratory study was conducted to remove and recover lead from aqueous solution using supported liquid membrane (SLM) process. Preliminary solvent extraction studies, on lead revealed the iodo system with tributyl phosphate (TBP) as liquid membrane and sodium hydroxide as strippant to be an efficient one. Using synthetic lead(II) solution, the process parameters like feed side pH, strippant concentration, KI concentration and stirring speed were optimized. The initial lead concentration of 25 mg/L gave satisfactory result with complete removal and recovery in 4 h of operation with a permeability coefficient of 1.146 × 10-5 m/s.

Keywords: Liquid membrane, recovery, lead, iodo system, tri butyl phosphate

           IPC Code: B01D61/38

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 441-446

 

Pervaporation of chloroform-acetone mixtures through DCP crosslinked poly(ethylene-co-vinyl acetate) membranes

 

M N Muralidharan & S Anil Kumar*

 

Membranes of poly (ethylene-co-vinyl acetate) crosslinked with dicumyl peroxide (DCP) were prepared. The permeation characteristics in the pervaporation process were examined using chloroform-acetone mixtures. The DCP modified membranes exhibited chloroform permselectivity. The sorption characteristics, effects of feed concentration and crosslinking density on pervaporation were also examined. The separation was found to be maximum at high concentrations of chloroform in the feed mixture. The maximum separation and flux were found to be associated with a moderate amount of crosslinking agent in the membrane. As the crosslinking density was increased, flux and selectivity were found to decrease.

Keywords: Pervaporation, poly(ethylene-co-vinyl acetate), dicumyl peroxide

           IPC Code: B01D61/36

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 447-454

 

Pinacol-Pinacolone rearrangement over solids supported metal ion catalysts

 

S Z Mohamed Shamshuddin, George Kuriakose & N Nagaraju*

 

Catalytic activity of hydrated Al2O3, SiO2, ZrO2, AlPO4, zeolite-HY and Fe(III) ions supported on these solids has been evaluated in pinacol-pinacolone rearrangement (2,3-dimethyl-2,3-butanediol to 3,3-dimethyl-2-butanone). The effect of method of preparation of catalysts on their catalytic activity has been evaluated. Studies on catalytic activity have been performed in vapour phase at different reaction temperatures. Pinacolone and 2,3-dimethyl-1,3-butadiene were formed as the major products. The percentage conversion of pinacol and the selectivity of the products have been found to be influenced by the reaction temperature, the nature of the support, the metal ion present on the support and the method of preparation of supported catalysts. Al2O3 and AlPO4 containing 5% Fe ions on their surface are found to convert pinacol to pinacolone to an extent of 88% with a selectivity of 83% for ketone at 200 °C with 10 mL/h flow rate of the reactant. A comparative study of the catalytic activity of the materials containing 5% Fe ions on Al2O3 and those containing same percentage of Ni or Co ions in the chosen reaction at 200 °C, revealed a good correlation between the redox potential of the metal ions and their selective catalytic activity in the formation of pinacolone.

Keywords: Pinacol rearrangement, dehydration, solid acids, supports and supported metal ion catalysts

           IPC Code:B01J21/00

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 455-461

 

Studies on ionic mass transfer onto a target surface with submerged impinging jet in a closed cell

P King*, V S R K Prasad & G Hanumantha Rao

 

Mass transfer studies onto a target surface (disc type) with a submerged impinging jet in a closed cell were carried out in the present work. The limiting current technique for reduction of ferricyanide ion was employed. For varying parameters like nozzle sizes, the experimental mass transfer data were analyzed for two ranges of heights from target surface, Hn < 0.05 m and Hn ³ 0.05m.

Keywords: Ionic mass transfer, impinging jet, forced convective flow

           IPC Code: C21D 1/00

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 462-465

 

Inhibition of corrosion of mild steel in hydrochloric acid by
N-cyclohexyl-N/- phenyl thiourea

 

S Divakara Shetty, Prakash Shetty* & H V Sudhaker Nayak

 

The inhibition of corrosion of mild steel in 0.01-0.1 N HCl solutions by N-cyclohexyl-N/-phenyl thiourea (CPTU) has been studied using potentiodynamic polarization technique. Results obtained reveal that CPTU performs excellently as anodic inhibitor for mild steel in HCl solution. The inhibitor functions through adsorption following Temkins’ adsorption isotherm. The influence of parameters like temperature, hydrochloric acid concentration and inhibitor concentration on the corrosion of mild steel has also been studied.

Keywords: Mild steel, corrosion inhibitor, potentiodynamic polarization, hydrochloric acid, chemisorption

           IPC Code: C23F11/00

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 466-471

 

Corrosion behaviour of electrochemically joined aluminum and stainless steel

G Sheela, V S  Muralidharan & Malathy Pushpavanam*

 

Two dissimilar metals viz., aluminum and stainless steel (SS) were joined electrochemically by heavy nickel deposition. Potential-time behavior, Tafel extrapolation method and galvanic coupling experiments were conducted to study the corrosion behavior of the three individual metals in 5% aqueous sodium chloride acidified with acetic acid, alone and in combination. The systems behaved differently in simple immersion test and on coupling with each other. In simple immersion test, nickel and SS were nobler to aluminum. Coupling of aluminum and nickel (bi-metallic) resulted in dissolution of both metals, the rate of nickel being lower. Potentiodynamic polarization experiments showed that the aluminum-SS bi-metallic system has the highest corrosion rate than aluminum-Ni or SS-nickel. Aluminum exhibits pitting type corrosion when coupled to nickel. Experiments with electroplated specimens and SEM analysis confirmed that in aluminum-nickel couple both metals corrode, the corrosion of nickel being considerably lower. Formation of elemental nickel on aluminum surface also confirmed the above result.

Keywords: Electrochemical joining, mass loss, corrosion current, galvanic couple, polarization technique

           IPC Code: G01N17/02; C23F11/00

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 472-476

 

Corrosion inhibition of carbon steel by adipic acid – Zn2+ system

 

G Ruba Helen Florence, A Noreen Anthony, J Wilson Sahayaraj, A John Amalraj & Susai Rajendran*

The inhibition efficiency (IE) of adipic acid (AA)-Zn2+ system in controlling corrosion of carbon steel immersed in well water has been evaluated by weight-loss method. The formulation consisting of 50 ppm of AA and 50 ppm of Zn2+ has 95% IE. At lower pH value(pH=6) IE decreases and in alkaline medium (pH=8) IE increases. Polarization study reveals that AA- Zn2+ system functions as a mixed inhibitor. AC impedance spectra reveal that a protective film is formed on the metal surface. FTIR spectra reveal that the protective film consists of Fe2+-AA complex and Zn(OH)2.

Keywords: Carbon steel, corrosion inhibition, adipic acid, well water, zinc ion

           IPC Code: C23F11/00

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 477-487

 

 

QA/QC aspects of GC-MS analytical instrument for environmental analysis

Sanjay M Kashyap*, Girish H Pandya, Sudheer
D Wachasunder & Vivek K Kondawar

 

The study of the sources, effects, and transport of organic pollutants in the environment has been the subject of intense scrutiny in recent years. Since some of these compounds are considered to be toxic at very low concentrations, analysis methods are required that are capable of achieving accurate, precise determinations at lower than parts-per-billion concentrations. As environmental legislation in many countries is becoming stricter the quality control (QC) and quality assurance (QA) procedures are followed as per the specific methodologies employed.

Keywords:            QA/QC, GC/MS, analytical instrument, quantitative analysis

IPC Code: B01D15/08; G01N30/00

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 12, July 2005, pp. 488-500

 

Borax, Boric acid, and Boron¾From exotic to commodity

Jaime Wisniak*

           Since old times borax has been an important raw material used particularly in the metal and ceramic industries first for soldering and brazing, second as a flux to give certain glazes an appropriate fusibility. Here, we provide the historical background that led to the understanding of the nature and composition of boron compounds, isolation of the element, and establishment of a flourishing industry with an overall annual world output of more than 4.5 million tons of ore.