Indian Journal of Chemical Technology

http://www.niscair.res.in

Total visitors:2,350 since 19-01-08

 

 

VOLUME 16

NUMBER 1

JANUARY 2009

CODEN:ICHTEU

 

ISSN:0971-457X

 

CONTENTS

 

Papers

 

 

Stability and response analyses of phenol degrading biochemical systems

7

Susmita Dutta, Ranjana Chowdhury & Pinaki Bhattacharya

 

 

 

Effect of column diameter on dynamics of gas-solid fluidized bed: A statistical approach

17

Y K Mohanty, G K Roy & K C Biswal

 

 

 

Corrosion protection of copper by self assembled monolayers

25

B V Appa Rao, K Chaitanya Kumar, Md Yakub Iqbal & B Sreedhar

 

 

 

Fatty acid triazoles derived from Neem, Rice bran and Karanja oils as corrosion

inhibitors for mild steel

32

S D Toliwal & Kalpesh Jadav

 

 

 

Rhodamine B adsorption by activated carbon: Kinetic and equilibrium studies

38

M Hema & S Arivoli

 

 

 

Kinetics of tween-80 micellar catalysed chloramine-T oxidation of vitamins in HClO4 medium

46

Varuna Shukla & Santosh K Upadhyay

 

 

 

Effects of alkaline additives on conversion of 2,4,5-trichlorophenol over Pd-Rh/C

catalysts

52

Gulin Selda Pozan

 

 

 

Anaerobic biogas generation from sugar industry wastewaters in three-phase fluidized-bed bioreactor

58

Sk Masud Hossain, N Anantharaman & Manas Das

 

 

 

Thin layer chromatographic study of Indian bauxites

65

P A Mohamed Najar, K R Janbandhu, P G Bhukte & R S Mishra

 

 

 

Simple and facile methods for the determination of carvedilol in pharmaceuticals

74

T V Sreevidya & B Narayana

 

 

 

Notes

 

 

 

Performance evaluation of an effluent treatment plant for a pulp & paper mill

79

Deepti Mishra, Mohd Akram Khan, Manish Mudgal, Prabha Padmakaran &
B Chakradhar

 

Removal of Cu and Pb ions from aqueous solutions by electric furnace slag: Kinetic and
thermodynamic aspects

84

Lidija Curkovic, Marina Trgo, Alenka Rastovcan Mioc &
Nediljka Vukojevic Medvidovic

 

 

 

Spectrophotometric determination of nitrite using new coupling agents

89

K Veena & B Narayana

 

 

 

Author Index

93

 

 

Keyword Index

94

 

 

Guidelines for Authors

95

 

 

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 7-16

 

 

Stability and response analyses of phenol degrading biochemical systems

 

Susmita Dutta1, Ranjana Chowdhury2 & Pinaki Bhattacharya2*

1Chemical Engineering Department, National Institute of Technology, Durgapur 713 209, India

2Chemical Engineering Department, Jadavpur University, Kolkata 700 032, India

Email: pinaki_che@yahoo.com

 

Chemical systems having non-linear dynamic state equation exhibit unusual behaviour like multiplicity, sustained oscillations etc., when perturbation in any forcing function is somehow introduced to an existing steady state. Under this situation a reacting system may exhibit one or more ambiguous steady states. Biochemical systems using microorganisms following either substrate- or product-inhibited growth kinetics are usually characterized with this type of behaviour. In the present investigation biodegradation of phenol using Pseudomonas putida following substrate inhibited growth kinetics has been taken as model system. The system has been studied in a 2 dm3 B. Braun fermenter in batch and continuous modes of operation separately. Using the experimental data obtained in batch mode of operation the kinetic parameters of the systems have been determined considering substrate inhibited Haldane type kinetics for biodegradation of phenol. Two separate techniques, viz., linear stability analysis and phase plane analysis have been performed to study the characteristics of steady states from local and global points of view respectively. Response analysis of the system has been performed using step-type perturbations in inlet substrate concentrations of different amplitudes. The experimental findings show good agreement with the simulated results.

Keywords: Phenol biodegradation, Bioreactors, Stability analysis, Dynamic simulation, Mathematical modeling

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 17-24

 

 

Effect of column diameter on dynamics of gas-solid fluidized bed:
A statistical approach

 

Y K Mohanty*, G K Roy & K C Biswal

Department of Chemical Engineering, NIT, Rourkela 769 008, India

Email: yashobantkumar@yahoo.com

 

Experiments have been carried out to study the effect of column internal diameters on fluctuation and expansion ratios. Three cylindrical columns with internal diameters as 0.099, 0.127 and 0.1524 m have been used to predict the effect of column diameters on fluctuation and expansion ratios. Factorial design (statistical approach) has been developed to predict fluctuation and expansion ratios in a gas-solid fluidized bed with varying gas-flow rates, internal column diameters and static bed heights. The values of fluctuation and expansion ratios predicted using the developed model have been found to agree well with the corresponding experimental ones. Columns with larger internal diameters give less fluctuation in the lower mass velocity range (Gf < 2.5 Gmf ) and vice-versa. The expansion ratio bears an inverse relation with the column internal diameter.

Keywords: Gassolid fluidized beds, Fluctuation ratio, Expansion ratio, Factorial design, Column diameter

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 25-31

 

 

Corrosion protection of copper by self assembled monolayers

 

B V Appa Raoa*, K Chaitanya Kumara, Md Yakub Iqbala & B Sreedharb

aDepartment of Chemistry, National Institute of Technology, Warangal 506 004, India

bInorganic & Physical Chemistry Division, Indian Institute of Chemical Technology, Hyderabad 500 007, India

Email: boyapativapparao@rediffmail.com

 

Self assembled monolayer (SAM) of 3-methyl-5-octadecylsulfanyl-[1,2,4]triazole-4-ylamine (MOSTY) was formed on the copper surface and the optimum conditions of formation of SAM were established. Corrosion behaviour of copper with the SAM was investigated in 0.02 M aq. HCl (acidic) and 0.02 M aq. NaCl (neutral) solutions. Weight-loss measurements, potentiodynamic polarization studies and electrochemical impedance studies were carried out in order to investigate the effect of MOSTY SAM on the corrosion protection of copper. Appropriate equivalent circuit models were used for impedance measurements of bare copper and the SAM covered copper in the chosen aggressive environments. These studies revealed the corrosion inhibition efficiency of SAM to an extent of 98% in 0.02 M aq. NaCl and 86% in 0.02 M aq. HCl environments. Potentiodynamic polarization studies revealed that this SAM controls both the anodic and cathodic reactions and thus protects copper from corrosion. The X-ray photoelectron spectroscopy (XPS) was used to characterize the SAM. The XPS revealed the presence of various elements viz. carbon, nitrogen and sulphur in the SAM. Shifts in binding energies of nitrogen and sulphur were interpreted. The inhibition of copper dissolution was interpreted due to the chelating effect of Cu (I) ions with the chemisorbed ligand molecules forming a complex of SAM on copper surface.

Keywords:Self assembled monolayer, 3-Methyl-5-octadecylsulfanyl-[1,2,4]triazole-4-ylamine, Copper, Corrosion inhibition

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 32-37

 

 

Fatty acid triazoles derived from Neem, Rice bran and Karanja oils as corrosion inhibitors for mild steel

 

S D Toliwal* & Kalpesh Jadav

Department of Industrial Chemistry, Institute of Science and Technology for Advanced Studies and Research (ISTAR),
Vallabh Vidyanagar 388 120, India

Email: toliwalsd@yahoo.co.in

 

5-Alkyl-4 phenyl-4H-[1,2,4]triazole-3-thiol of phenyl hydrazides of fatty acids from Neem, Rice bran and Karanja oils have been synthesized and evaluated as corrosion inhibitors of mild steel (MS) in hydrochloric acid solutions by weight loss method. The adsorption of all the phenyl hydrazides derivatives on mild steel surface in the acid solution has been found to obey Langmuirs adsorption isotherm. Inhibition efficiency of these compounds has been found to vary with concentration of the compound, solution temperature, immersion time and concentration of acid solution. The activation energies (Ea) have been calculated to investigate the mechanism of the corrosion inhibition. The inhibition efficiency increases with the increase in concentration of the inhibitors.

Keywords: Neem oil, Rice bran oil, Karanja oil, Corrosion inhibition, 5-Alkyl-4 phenyl-4H-[1,2,4]triazole-3-thiol, Mild steel

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 38-45

 

 

Rhodamine B adsorption by activated carbon: Kinetic and equilibrium studies

M Hema & S Arivoli*

Department of Chemistry, H H The Rajahs Government College, Pudukkottai 622 001, India

Email: arivu3636@yahoo.com

 

A carbonaceous adsorbent (TPC) prepared from Thespusia populinia bark by acid treatment was tested for its efficiency in removing Rhodamine B (RDB). The parameters studied include agitation time, initial dye concentration, carbon dose, pH and temperature. The adsorption followed first order reaction equation and the rate is mainly controlled by intra-particle diffusion. Freundlich and Langmuir isotherm models were applied to the equilibrium data. The adsorption capacity (Qm) obtained from the Langmuir isotherm plots were 60.836, 64.239, 68.695 and 77.178 mg/g respectively at an initial pH of 7.0 at 30, 40, 50 and 60oC. The temperature variation study showed that the RDB adsorption is endothermic and spontaneous with increased randomness at the solid solution interface. Significant effect on adsorption was observed on varying the pH of the RDB solutions. Almost 79% removal of RDB was observed at 60oC. The Langmuir and Freundlich isotherms obtained, positive H0 value, pH dependent results and desorption of dye in mineral acid suggest that the adsorption of RDB on TPC involves physisorption mechanism.

Keywords: Thespusia populinia bark carbon (TPC), Rhodamine B (RDB), Adsorption isotherm, Equilibrium, Kinetic andThermodynamic parameters, Intraparticle diffusion

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 46-51

 

 

Kinetics of tween-80 micellar catalysed chloramine-T oxidation of vitamins in HClO4 medium

 

Varuna Shukla & Santosh K Upadhyay*

Department of Chemistry, H B Technological Institute, Kanpur 208 002, India

Email: upadhyay_s_k@ rediffmail.com

 

A catalytic effect of non-ionic (tween-80) micelles on the rate of oxidation of thiaminehydrochloride (vitamin B1) and pyridoxine hydrochloride (vitamin B6) by sodium salt of p-toluene sulphonamide (chloramine-T) in acidic medium has been observed and rate has been found to be proportional to {k' + k" [Tween-80]}, where k' and k" are the rate constants in absence and in presence of surfactant, respectively. The rate showed a first order, a fractional order and a zero order dependence on [Chloramine-T]0, [Vitamin]0 and [H+]0, respectively. The association/binding between the oxidant and the surfactant micelle is supported by the spectrophotometric evidence. A mechanism has been proposed and binding parameters have been evaluated.

Keywords: Kinetics of tween-80, Micellar catalyzed, Oxidation of vitamins, Chloramine-T

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 52-57

 

 

Effects of alkaline additives on conversion of 2,4,5-trichlorophenol over Pd-Rh/C catalysts

Glin Selda Pozan

Istanbul University, Faculty of Engineering, Chemical Engineering Department, Avcilar, 34320, Istanbul, Turkey

Email: gpozan@istanbul.edu.tr

 

Effects of alkaline additives on conversion of 2,4,5-trichlorophenol (TCP) over Pd-Rh/C catalysts were studied at 80C and 1 Atm. The catalysts were prepared by incipient wetness impregnation of carbon support and characterized by BET surface area, temperature programmed reduction (TPR) and X-ray diffraction (XRD) methods. The dechlorination of TCP occurs mainly via two pathways: hydrodechlorination and hydrolysis. The dechlorination of TCP can be accelerated significantly by alkalis. The addition of alkali had increasing effect on the initial reaction rate, conversion and crystallite size of Pd. The initial TCP dechlorination activity without alkali was found to be in the following order: 0.97%Pd/C>0.8%Pd/0.19%Rh/C>0.98%Rh/C. The selectivities of mono and di-chlorophenol were also improved with Pd/C catalyst.

Keywords: Hydrodechlorination, 2,4,5-Trichlorophenol, Pd/Rh/C catalyst, Alkaline additives

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 58-64

 

 

Anaerobic biogas generation from sugar industry wastewaters in three-phase fluidized-bed bioreactor

 

Sk Masud Hossaina*, N Anantharamanb & Manas Dasc

aCentre of Advanced Studies and Research, C Abdul Hakeem College of Engineering & Technology,

Melvisharam 632 509, India

bDepartment of Chemical Engineering, National Institute of Technology, Tiruchirapalli 620 015, India

cDepartment of Chemical Engineering, University of Calcutta, Kolkata 700 009, India

Email: skmhossain@yahoo.co.in; naraman@nitt.edu; manas_das1948@yahoo.com

 

The studies are undertaken to develop an effective anaerobic continuous digestion process for biogas generation from sugar industry wastewaters using actively digested sludge from a sewage plant, in three-phase fluidized bed bioreactor. Attempts are made to optimize hydraulic retention time (HRT), initial feed pH, feed temperature and flow rate of feed (organic loading rate) for maximum production of methane gas and maximum removal of chemical oxygen demand (COD) and biological oxygen demand (BOD) of sugar industry wastewaters. The optimum conditions for the system are: digestion time, 8 h; initial pH of feed, 7.5; feed temperature, 40C; feed flow rate, 14 L/ min with maximum organic loading rate (OLR), 39.513 kg COD m−3 h−1. The organic loading rates (OLR) are calculated on the basis of COD inlet in the bioreactor at different flow rates. The maximum expansion of the bed is observed as 23.67 m at optimum feed flow rate of 14 L/ min. The maximum methane gas concentration is 63.56% (v/v) of the total biogas generation at optimum process parameters. The maximum biogas yield rate is 0.835 m3 /kg COD m−3 h−1 with maximum methane gas yield rate of 0.530 m3 /kg COD m−3 h−1 (63.56% v/v) at optimum process parameters. The values for maximum reduction of COD and BOD are 76.82% (w/w) and 81.65% (w/w) with maximum OLR of 39.513 kg COD m−3 h−1 at optimum conditions.

Keywords: Activated bacteria, Anaerobic, Biogas, Biomethanation, Fluidized- bed, Methane

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 65-73

 

 

Thin layer chromatographic study of Indian bauxites

P A Mohamed Najar1*, K R Janbandhu1, P G Bhukte2 & R S Mishra1

Analytical1 and Bauxite Alumina2 Divisions, Jawaharlal Nehru Aluminium Research Development and Design Centre
Amaravati Road
, Nagpur
, 440 023, India

Email: najarp@hotmail.com

 

Thin layer chromatography (TLC) has been used for the detection and separation of Al3+, Fe2+, Si4+ and Ti4+ in bauxite. Thirty bauxite samples of different geological origin have been studied to identify the optimized chromatographic systems capable of selective separations of the constituents. Binary and ternary separations of Al3+, Fe2+, Ti4+ and Si4+ in bauxite were realized with chromatographic systems comprising various combinations of silica gel G, silica gel H and microcrystalline cellulose coated plates and aqueous mobile phases consisting alkali salt solutions, formic acid and hydrochloric acid etc. The chromatographic system consisting of silica gel H and mixture of 10% aqueous solutions of sodium chloride and formic acid in 8:2 (v/v) ratio was found to be the ideal combination for the analogous separation of Al3+, Fe2+ and Ti4+ in bauxites. The efficacy of optimized chromatographic system has been investigated by monitoring reproducibility of RF values and spot compactness with respect to change in bauxite geology, sample concentration and change of mobile phase composition. Chromatograms of the cations were quantitatively evaluated by scanning densitometry in comparison with wet analysis method.

Keywords: Bauxite, TLC, Separation of Al3+, Fe2+, Si4+ and Ti4+

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 74-78

 

 

Simple and facile methods for the determination of carvedilol in pharmaceuticals

 

T V Sreevidya & B Narayana*

Department of Post Graduate Studies and Research in Chemistry, Mangalore University,

Mangalagangothri 574 199, India

Email: n_badiadka@yahoo.co.uk 

 

Simple and sensitive methods for the determination of carvedilol (CAR) are described. The methods are based on the reaction of CAR with ninhydrin (NIN) in basic medium to form coloured iminium salt having absorption maximum at 402 nm and also with acetaldehyde (AA) in presence of sodium nitroprusside in basic medium to form coloured product having absorption maximum at 558 nm. The calibration graphs are found to be linear over 0.2 - 1.2 and 0.6 - 2.0 g mL-1 with molar absorptivity values of 2.571 104 and 1.617 104 L mol-1 cm-1 for CAR-NIN and CAR-AA respectively. The optimum reaction condition and other analytical parameters were evaluated. The statistical evaluations of the methods were examined by determining intra-day and inter-day precision. The methods were successfully applied to the assay of CAR in tablet formulations. The accuracy and reliability of the methods were further ascertained by parallel determination by a reference method and by calculating the Students t-test and F-test values at 95% confidence level.

Keywords: Carvedilol (CAR), Ninhydrin, Sodium nitroprusside, Spectrophotometry

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 79-83

 

 

Performance evaluation of an effluent treatment plant for a pulp & paper mill

 

Deepti Mishra1*, Mohd Akram Khan1, Manish Mudgal1, Prabha Padmakaran1 & B Chakradhar2

1Advanced Materials and Processes Research Institute, (CSIR)

Hoshangabad Road, Bhopal 462 064, India

2National Environmental Engineering Research Institute Zonal Laboratory, (CSIR), IICT Campus, Uppal Road,
Hyderabad
500 007, India

Email: aditi_mishra@sify.com

 

Monitoring and performance evaluation studies were carried out for an effluent treatment plant of a pulp and paper mill located in central part of India. The paper presents the characteristics of wastewater from different units of effluent treatment plant (ETP). Effluent samples from different locations of ETP area including combined treated effluent and river water samples were collected at monthly interval and analyzed for detailed physico-chemical and biological parameters for a period of ten months. The pH of raw as well as treated effluent indicates its neutral nature. The BOD, COD and suspended solids in treated effluents were reduced significantly, whereas very small reduction was observed in dissolved solids and chlorides in treated effluents in comparison to raw effluents. Most of the parameters of combined effluent were well within the permissible limits of Central Pollution Control Board, India. Recommendations were given to increase the efficiency of ETP.

Keywords: Pulp & Paper mill, Treated effluent, Raw effluent, Monitoring, Performance evaluation


 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 84-88

 

 

Removal of Cu and Pb ions from aqueous solutions by electric furnace slag: Kinetic and thermodynamic aspects

Lidija Ćurkovića*, Marina Trgob, Alenka Rastovčan Miočc & Nediljka Vukojević Medvidovićb

aFaculty of Mechanical Engineering and Naval Architecture, University of Zagreb, Ivana Lučića 5,

1000 Zagreb, Croatia

bFaculty of Chemical Technology, University of Split, Teslina 10/V, 21000 Split, Croatia

cFaculty of Metallurgy, University of Zagreb, Aleja narodnih heroja 3, Sisak, Croatia

Email: lidija.curkovic@fsb.hr; mtrgo@ktf-split.hr; nvukojev@ktf-split.hr

 

Electric furnace slag, instead of deposition as a non-toxic metallurgical waste material, can be used as a valuable secondary raw material in many industrial processes. In this paper, removal of copper and lead ions from aqueous solutions by sorption on electric furnace slag (EFS) has been investigated. Experiments were performed at three temperatures of 23, 40 and 55C. The results of sorption kinetics are tested by kinetic model that describes intraparticle diffusion, and diffusion coefficients have been calculated. Diffusion rate of both systems increases with temperature, in dependence of time is constant for copper ions, while for lead decreases. The energy of activation (Ea), activation enthalpy (DH*), activation entropy (DS*) and free energy of activation (DG*) have been calculated based on kinetic data. Values of Ea characterize binding of lead and copper ions on EFS as activated chemisorption, whereas positive values of DH*, DG* and negative values of DS* describe process as endothermic, nonspontaneous and without changes in the structure of the solid particle. The studies showed that this low cost waste material could be used as an efficient sorbent material for the removal of lead and copper from aqueous solutions.

Keywords: Copper, Lead, Electric furnace slag, Diffusion, Thermodynamic parameters

 

 

Indian Journal of Chemical Technology

Vol. 16, January 2009, pp. 89-92

 

 

Spectrophotometric determination of nitrite using new coupling agents

K Veena & B Narayana*

Department of P.G. Studies and Research in Chemistry,

Mangalore University, Mangalagangotri 574 199, India

Email: n_badiadka@yahoo.co.uk

 

A method is described for the spectrophotometric determination of nitrite. It is based on the reaction of nitrite with p-nitroaniline (PNA) in acid medium to form diazonium ion, which is coupled with frusemide (FRU) or 5-methyl-4-{[(1E)-phenylmethylene]amino}-2,4-dihydro-3H-1,2,4-triazole-3-thione (MPAT) in basic medium to form azo dyes, showing absorption maxima at 680 or 395 nm respectively. The range of linearity for PNA-MPAT and PNA-FRU system are 0.4-2.0 g/mL, 0.02-0.6 g/mL of nitrite respectively. Molar absorptivity, Sandell sensitivity, Detection limit, Quantitation limit for PNA-MPAT and PNA-FRU system were found to be 3.314 103 Lmol-1cm-1, 0.014 g cm-2, 0.559 g mL-1, 1.695 g mL-1and 1.46 103 Lmol-1cm-1, 0.032 g cm-2, 0.485 g mL-1, 1.470 g mL-1 respectively. The method has been applied to various water samples, soil samples and tablets.

Keywords: Spectrophotometry, Diazotization, Nitrite, Frusemide, 5-methyl-4-{[(1E)-phenylmethylene] amino}-2, 4-dihydro-3H-1,2, 4-triazole-3-thione