Indian Journal of Chemical Technology

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VOLUME 15

NUMBER 1

JANUARY 2008

CODEN:ICHTEU

 

ISSN:0971-457X

 

CONTENTS

 

Papers

 

 

Photochemical treatment of rhodamine-B wastewater by photo-Fenton reagent

7

        Anil Kumar, Mukesh Paliwal, Rameshwer Ameta & Suresh C Ameta

 

 

Adsorption of chromium(VI) from aqueous solutions by chemically treated water hyacinth Eichhornia crassipes

 

12

        Sujana M Gude & S N Das

 

 

Adsorption of Fe(II), Co(II) and Cu(II) ions onto a low cost activated carbon: Equilibrium, kinetic and thermodynamic studies

 

19

        S Arivoli, M Sundaravadivelu & K P Elango

 

 

Influence of condensation product on electrodeposition of Zn- Mn alloy on steel

29

        S Shivakumara, Y Arthoba Naik, Ganesha Achary, H P Sachin & T V Venkatesha

 

 

Acetylation of anisole on TPA/ZrO2

36

        R Sakthivel & E Kemnitz

 

 

Combustion synthesis of LiMn2O4 by thermal decomposition of oxalate precursors

41

        Arunkumar Lagashetty, Vijayanand Havanoor, S Basavaraja & A Venkataraman

 

 

Preparation of semi-refined K-carrageenan: Recycling of alkali solution and recovery of alkali from spent liquor

 

45

        A S Mehta, K H Mody, Anita Iyer & P K Ghosh

 

 

Application of ANN for prediction of cellulase and xylanase production by Trichoderma reesei under SSF condition

 

53

        Aruna Singh, Divya Tatewar, P N Shastri & S L Pandharipande

 

 

Spectrophotometric determination of artemisinin and dihydroartemisinin

59

        T V Sreevidya & B Narayana

 

 

Radiation effects on MHD flow past an impulsively started infinite isothermal vertical plate

63

        P Chandrakala & S Antony Raj

 

 

Notes

 

 

Influence of formic acid addition on the electrochemical behaviour of mild steel in glacial acetic acid

 

68

        S K Singh, A K Mukherjee & M M Singh

 

Synthesis of physiologically important quinoxaline derivatives using conventional method and microwave irradiation

 

72

        G Bhattacharjee, S M Sondhi, Monica Dinodia & Sushanta K Mishra

 

 

Esterification of carboxylic acids by acid activated Kaolinite clay

75

        Dilip Konwar, Pradip K Gogoi, Pranjal Gogoi, Geetika Borah, Ruby Baruah, Neelakshi Hazarika & Rituraj Borgohain

 

 

Solvent extraction and spectrophotometric determination of copper(II) with 2-hydroxy-5-methylacetophenoneisonicotinoylhydrazone (HMAINH)

 

79

        A S Aswar & M D Joshi

 

 

Electrodeposition of nickel from dimethyl sulphoxide bath: Effect of nucleoside

82

        Ashutosh K Gupta, H K Srivastava, Jyotsna Singh, Priyanka Srivastava & Rahul Kashyap

 

 

Prediction of minimum slugging velocity, bubbling bed index and range of bubbling fluidization in cylindrical and non-cylindrical gas-solid fluidized beds

 

85

        R K Singh & G K Roy

 

 

Author Index

 

 91

Keyword Index

 

 92

Guidelines for Authors

 93

 

 

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 7-11

 

Photochemical treatment of rhodamine-B wastewater by photo-Fenton reagent

 

Anil Kumar, Mukesh Paliwal, Rameshwer Ameta & Suresh C Ameta*

 

Oxidation by photo-Fenton like reaction is an economically feasible process for degradation of a variety of hazardous pollutants in wastewater from dyeing and printing industries. Oxidation of rhodamine-B, (an acid dye of xanthene series) using photo-Fenton reagent has been carried out under ambient conditions. The effect of different parameters like the concentration of ferric ion, rhodamine-B, pH, hydrogen peroxide, light intensity etc. on the reaction rate has been observed. A tentative mechanism for the degradation of rhodamine-B by photo-Fenton’s reaction has been proposed.

Keywords: Photochemical degradation, Photo-Fenton, Rhodamine-B, AOPs

 

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 12-18

 

Adsorption of chromium(VI) from aqueous solutions by chemically treated Water hyacinth Eichhornia crassipes

 

Sujana M Gude*& S N Das

 

The adsorption potential of water hyacinth Eichhornia crassipes for the removal of Cr(VI) from aqueous solutions has been stidied. The influence of various parameters including contact time, temperature, solution pH, initial adsorbate and adsorbent concentrations and effect of competing anions were studied. Results obtained indicate that the treated weed Eichhornia crassipes has remarkable adsorption capacity for Cr(VI) at pH below 4. The rate of adsorption was rapid and equilibrium attained within 2 h. The method followed first order kinetics. The adsorption process does exhibit a Langmuir type behaviour which is affected by the temperature. The maximum Cr(VI) removal was found to be 7.5 mg/g of dry weight weed at pH of 3.0 in 120 min at 25°C. The calculated activation energy for the method studied was around 54.6 kJ/mol. About 500 mg weed could remove Cr(VI) successfully from 100 mL of chromite mine water containing 2.8 mg/L Cr(VI) at normal conditions.

Keywords: Adsorption, Water hyacinth, Cr(VI) removal, Mine water

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 19-28

 

Adsorption of Fe(II), Co(II), Ni(II) and Cu(II) ions onto a low cost activated carbon: Equilibrium, kinetic and thermodynamic studies

 

S Arivoli, M Sundaravadivelu & K P Elango*

 

Batch sorption system using activated carbon from Aegle marmelos fruits source as an adsorbent was investigated to remove Fe(II), Co(II), Ni(II) and Cu(II) ions from aqueous solutions. The system variables studied include initial concentration of the sorbate, agitation time, adsorbent dose, pH, co-ions and temperature. The experimental data fitted well to the Langmuir and Freundlich isotherms. The values of thermodynamic parameters such as DH°, DS° and DG° indicated that the adsorption was a spontaneous, endothermic and a physical process. Kinetic studies revealed that the adsorption is of first order. A two staged mechanism has been proposed for the adsorption of metal ions onto the adsorbent. FT-IR and SEM patterns of the adsorbent were used to understand the mechanism of the adsorption process. The order of adsorption of the metal ions was found to be Fe(II) > Cu(II) > Ni(II) > Co(II) which is in agreement with the intra-particle diffusion studies.

Keywords: Adsorption, Activated carbon, Aegle marmelos, Kinteics, Metal ions

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 29-35

 

Influence of condensation product on electrodeposition of Zn-Mn alloy on steel

 

S Shivakumara, Y Arthoba Naik*, Ganesha Achary, H P Sachin & T V Venkatesha

 

Electrodeposition of zinc-manganese alloy was attempted from sulphate bath containing condensation product (CP) of furfuraldehyde (FRL) and L-lysine monohydrochloride (LL). The effect of bath constituents, pH, current density and temperature on nature of deposit was studied through Hull cell experiments. The throwing power was measured using Haring and Blum cell. The bath constituents and operating parameters were optimized. Deposit properties and corrosion resistance were discussed. Current efficiency and polarization studies were carried out. SEM photomicrographs of the deposit obtained from optimum bath revealed that the condensation product modifies the morphology of zinc-manganese alloy deposit. IR spectrum of the scrapped deposit showed inclusion of addition agent.

Keywords: Brightener, Condensation product, Electrodeposition, Sulphate solution

 

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 36-40

 

Acetylation of anisole on TPA/ZrO2

 

R Sakthivel*& E Kemnitz

 

Zirconia loaded with 5 - 20wt% of tungstophosphoric acid (TPA) were prepared by suspending solid hydrous zirconia in methanolic TPA solution followed by evaporation of methanol and calcination at 400°C for 4 h. The products were characterized by X-ray diffraction, photoacoustic FTIR spectroscopy, and NH3-TPD. XRD results show the formation of single tetragonal phase of ZrO2 only for the sample loaded with 5wt% of TPA (5-TPA/ZrO2), whereas the samples loaded with 10, 15 and 20wt% of TPA show two separate phases; cubic phase of hydrogen tungsten phosphate hydrate and tetragonal phase of ZrO2. The photoacoustic FTIR-spectra of pyridine chemisorbed catalysts show the existence of both BrØnsted (BC) and Lewis (LC) acid sites. The intensity of BrØnsted acid sites band (at 1535 cm-1) and the intensity ratios of BrØnsted to Lewis acid site bands increase with increased loading of TPA from 5 to 15wt% and decrease with 20wt% loading of TPA. This is correlating with catalytic yields (4- and 2- methoxy acetophenone) obtained for catalysts loaded with 5 to 20wt% of TPA for the acetylation of anisole reaction with acetic anhydride. The results suggest that only the BrØnsted acid sites of catalyst take part in the acetylation of anisole reaction. The NH3-TPD curves of above catalysts show that the ‘strong’ acid sites which are in the >450°C region participate in the reaction.

Keywords: TPA: 12-tungstophosphoric acid, B/L ratio, BrØnsted acid sites

 

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 41-44

 

Combustion synthesis of LiMn2O4 by thermal decomposition of oxalate precursors

 

Arunkumar Lagashetty*, Vijayanand Havanoor, S Basavaraja & A Venkataraman

 

Self-propagating low temperature combustion method for the synthesis of LiMn2O4 is reported. Synthesis of LiMn2O4 was carried out by thermal decomposition of lithium oxalate and manganese oxalate precursors employing poly(ethylene glycol) (PEG) as a fuel. The prepared LiMn2O4 was then characterized for structure by employing X-ray diffraction (XRD), morphology by scanning electron microscopy (SEM), particle size and shape by transmission electron microscopy (TEM) and bonding by Fourier transform infrared (FT-IR) spectral studies. The powders resulting from this method are pure, spinel-structure LiMn2O4 particles of regular shapes.

Keywords: Combustion, Synthesis, Morphology, Bonding

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 45-52

 

Preparation of semi-refined k-carrageenan:
Recycling of alkali solution and recovery of alkali from spent liquor

 

A S Mehta*, K H Mody, Anita Iyer & P K Ghosh

The data on the preparation of semi-refined carrageenan (SRC) from Hypnea musciformis and Eucheuma cottonii from the Indian sea coast are presented in the article. Improvements in the process of preparation of SRC such as: reduction in usage of water, reduction in soaking time of seaweed, increase in throughput, reuse of alkali, minimization of waste and regeneration of good quality KOH from spent liquor are achieved. Results obtained on lab scale (50 g seaweed) and bench scales (2.5 and 15 kg seaweed) are presented in the article and requirements of alkali, water and steam for a commercial unit are projected.

Keywords: Semi-refined carrageenan, Hypnea musciformis, Eucheuma cottonii, Polysaccharide, BOD and COD

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 53-58

 

Application of ANN for prediction of cellulase and xylanase production by Trichoderma reesei under SSF condition

Aruna Singh, Divya Tatewar, P N Shastri* & S L Pandharipande

 

Solid state fermentation is a bioconversion process that involves treatment of biodegradable solid substrate with microorganisms. This technique is widely applied for biotransformation of agricultural waste into industrial enzymes, organic solvents and other biochemicals. It is characterized by the presence of moisture, sufficient to solubilize the nutrients, but avoids leaching and operates at water activity (aw) of 0.85. On account of difference in water binding capacity of different substrates, optimum moisture level needs to be established for various combination of substrates, which involves extensive laborious experimental work. Present investigations were carried out to study the application of Artificial Neural Network as a tool for predicting cellulase and xylanase production by Trichoderma reesei as a function of bagasse content and moisture level in comparison to wheat bran medium. A correlation coefficient > 0.8 and root mean square error < 0.4 indicates ANN as a good prediction tool for such complex biological process.

Keywords: Solid state fermentation, Artificial neural network, Enzyme activity, Water binding capacity, Optimization

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 59-62

 

Spectrophotometric determination of artemisinin and dihydroartemisinin

 

T V Sreevidya & B Narayana*

 

A simple and rapid spectrophotometric method for the determination of artemisinin (ART) and dihydroartemisinin (DHA) is described. The method is based on the reaction of hydrogen peroxide (H2O2), generated by the cleavage of endoperoxide linkage of ART/DHA and its reaction with potassium iodide to liberate iodine. The liberated iodine bleaches the red coloured safranin O to colourless species and is measured at 521 nm. Beer’s law is obeyed in the range of 16-112 µg mL-1 for both ART and DHA. The molar absorptivity, Sandell’s sensitivity, detection limit and quantitation limit for ART were found to be 0.3401´104 Lmol-1cm-1, 1.43 ´ 10-2 µg cm-2, 0.0685 µg mL-1 and 0.2075 µg mL-1 respectively; while that for DHA were found to be 0.2891 ´ 104 L mol-1cm-1, 1.33 ´ 10-2 µg cm-2, 0.0491 µg mL-1 and 0.1488 µg mL-1 respectively. The optimum reaction conditions and other analytical parameters were evaluated. The statistical evaluation of the method was examined by determining intra-day and inter-day precision.

Keywords: Spectrophotometry, Artemisinin (ART), Dihydroartemisinin (DHA), Safranin O

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 63-67

 

Radiation effects on MHD flow past an impulsively started infinite isothermal vertical plate

P Chandrakala*  &  S Antony Raj

 

MHD (Magneto hydrodynamics) flow past an impulsively started infinite vertical isothermal plate in the presence of thermal radiation is studied here. The fluid considered is a gray, absorbing-emitting radiation but a non-scattering medium. It is observed that for an increase in radiation parameter N, there is a fall in the velocity or temperature.

Keywords:  Impulsively started vertical plate,  Radiation, Magnetic field

 

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 68-71

 

Influence of formic acid addition on the electrochemical behaviour of mild steel in glacial acetic acid

 

S K Singh, A K Mukherjee & M M Singh*

 

Electrochemical behaviour of mild steel in pure glacial acetic acid and contaminated with formic acid at different temperatures has been investigated and discussed in the present communication. Anodic and cathodic polarization behaviour have been studied using potentiostatic technique. Anodic polarization behaviour of mild steel in glacial acetic acid and in presence of different amounts of formic acid showed active behaviour in the whole range of the applied potential. On the addition of 0.5 M sodium salts to the acetic acid, active-passive-transpassive behaviour for most of the mixture compositions was observed. The cathodic polarization behaviour observed both in the absence and presence of the salt shows a shift of the curves towards higher current density with increasing concentration of formic acid.

Keywords: Mild steel, Acetic acid, Formic acid, Passivity, Corrosion

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 72-74

 

Synthesis of physiologically important quinoxaline derivatives using conventional method and microwave irradiation

 

G Bhattacharjee*, S M Sondhi, Monica Dinodia & Sushanta K Mishra

 

Quinoxaline derivatives are pharmacologically active and are very useful. A number of quinoxaline derivatives have been synthesized by the reaction of 2-chloroquinoxaline with various substituted amines in the presence of pyridine. The reactions have been carried out following conventional procedure and also under microwave irradiation.

Keywords: Synthesis, Quinoxaline, Microwave irradiation

 

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 75-78

 

Esterification of carboxylic acids by acid activated Kaolinite clay

 

Dilip Konwar*, Pradip K Gogoi, Pranjal Gogoi, Geetika Borah, Ruby Baruah, Neelakshi Hazarika &
Rituraj Borgohain

 

Esterification of carboxylic acid was carried out by using acid activated kaolinite clay. This heterogeneous catalyst, activated Kaolinite clay has been found to be a mild solid catalyst for the esterification of carboxylic acid in good yields. The catalyst is recoverable and can be recycled after activation.

           Keywords: Carboxylic acid, Alcohols, Kaolinite, Esterification

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 79-81

 

Solvent extraction and spectrophotometric determination of copper(II) with
2-hydroxy-5-methylacetophenoneisonicotinoylhydrazone (HMAINH)

 

A S Aswar* & M D Joshi

 

A new simple and sensitive extractive spectrophotometric method for the determination of copper (II) with reagent 2-hydroxy-5-methylacetophenoneisonicotinoylhydrazone (HMAINH) has been presented in this paper. The reagent HMAINH reacts with Cu (II) to give a yellow coloured complex, which can be quantitatively extracted into chloroform at 3.4 pH. The complex shows absorption maximum at 440 nm, where absorption due to reagent is negligible. The Beer’s law is obeyed in the concentration range of 0.5 - 4.0 ppm of Cu (II). The molar absorpitivity and Sandell’s sensitivity of extracted species are 9.340 ´ 103 dm3 mol-1cm-1 and 6.8 hg cm-2 respectively. The stoichiometry of the extracted species is found to be 1:1. The standard deviation is 0.0566. The effect of various diverse ions on the estimation of Cu (II) has been studied.

Keywords: HMAINH, Extraction, Copper determination, Spectrophotometry

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 82-84

 

Electrodeposition of nickel from dimethyl sulphoxide bath: Effect of nucleoside

 

Ashutosh K Gupta*, H K Srivastava, Jyotsna Singh, Priyanka Srivastava & Rahul Kashyap

 

        Dimethylsulphoxide (DMSO) may act as a potent medium for electrodeposition of Ni in presence of nucleosides. Totally bright electroplate may result from NiAc+NiSO4+NiSMT/DMSO bath in presence of trace amount of nucleoside (ribocytine/deoxycitidine). Too many coordinating centers of nucleoside facilitate the release of Ni from [Ni(DMSO)6]3+ complex in the vicinity of catholite causing outwardly growth more dominant than lateral growth, resulting in bright, adherent, Ni electrodeposite.

Keywords: Nickel electrodeposits, Nucleosides, Additive, DMSO bath

 

Indian Journal of Chemical Technology

Vol. 15, January 2008, pp. 85-89

 

Prediction of minimum slugging velocity, bubbling bed index and range of bubbling fluidization in cylindrical and non-cylindrical gas-solid fluidized beds

 

R K Singh* & G K Roy

 

A bubbling fluidization regime exists between the minimum bubbling velocity and the minimum slugging velocity. Experimental investigations have been carried out for the determination of the minimum slugging velocity and the range of bubbling fluidization for non-spherical particles in cylindrical and non-cylindrical beds. In the present paper, correlations have been developed for the prediction of minimum slugging velocity for gas-solid fluidization in cylindrical and non-cylindrical (viz. semi-cylindrical, hexagonal and square) beds for non-spherical particles fluidized by air at ambient conditions. The bed materials used have varied diameter (324 to 925 micron) and density (1500 to 4800 kg/m3). Experimental values of the minimum slugging velocity have been compared with the values calculated by the developed equations and also with the values calculated by Geldart’s equation. A fairly good agreement has been obtained between the calculated and the experimental values. Based on the experimental data, it is concluded that, under similar operating conditions minimum slugging velocity and minimum bubbling velocity are maximum in case of a semi-cylindrical conduit and minimum in case of a square one. It is further observed that the range of bubbling fluidization is maximum in case of a semi-cylindrical bed for the identical operating conditions.

Keywords: Minimum slugging velocity, Bubbling bed index, Range of bubbling fluidization, Non-cylindrical beds