Indian
Journal of Chemical Technology
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VOLUME 14 |
NUMBER 6 |
NOVEMBER 2007 |
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CODEN:ICHTEU |
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ISSN:0971-457X |
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CONTENTS
Papers |
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Optical
resolution of racemic tryptophan
through non-chiral membranes by ultrafiltration
using chiral selector in solution |
547 |
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IPC Code (s): C07B57/00, C12P41/00 |
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Improved
conversion to ethyl acetate through removal of water of esterification
by membrane pervaporation |
552 |
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IPC
Code (s):
B01D17/00, B01D61/36 |
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Swatilekha
Das, A K Banthia & Basudam
Adhikari |
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Electrochemical
reduction of ornidazole at a composite polymer
membrane electrode |
560 |
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IPC
Code (s):
C25C1/00, C25B11/00 |
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D C Tiwari,
Rajeev Jain & Gaurav Sahu |
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Electrochemical
reduction of 2-acetyl benzofuran and its
derivatives at glassy carbon electrode |
566 |
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IPC
Code (s):
C25B3/04, G01N |
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G P Mamatha, B |
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Preparation and characterization of an all solid supercapacitor based on polyaniline-Al2O3
layer
on aluminium alloy-Al-2024 |
572 |
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IPC
Code (s):
H01G9/025 |
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M Selva
Kumar & D |
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Some fatty
acid oxadiazoles for corrosion inhibition of mild
steel in HCl |
576 |
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IPC Code (s): C23F11/00 |
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M Z A Rafiquee,
Nidhi Saxena, Sadaf Khan & M A Quraishi |
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Inhibitory effects of some imines on the
corrosion of mild steel in hydrochloric acid solution |
584 |
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IPC
Code (s):
C23F11/00 |
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A V Shanbhag,
R A Prabhu, G M Kulkarni,
R G Kalkhambkar & T V Venkatesha |
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Recovery of
cephalosporin C from aqueous solution using polymeric adsorbent |
592 |
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IPC
Code (s):
B01D15/00 |
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Punita Mishra, Pradeep Srivastava, P K Mishra & Subir Kundu |
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Sorption of
water soluble dyes from aqueous solutions on zirconium phosphate |
597 |
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IPC
Code (s):
B01J39/02, C09B |
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Desilication of agro based black liquor and green liquor using jet loop reactor |
606 |
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IPC
Code (s):
D21C |
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Sachin A Mandavgane, G D Paradkar, J Varu, R Pamar & D
Subramanian |
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Sensitive
spectrophotometric methods for the determination of
pantoprazole sodium in pharmaceuticals using bromate-bromide, methyl orange and indigo carmine as
reagents |
611 |
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IPC
Code (s):
A61K, G01J3/00 |
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Flotability of barite particles with different shape and roughness |
616 |
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IPC
Code (s):
E21C50/00 |
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Studies on
effect of growth factor on morphological, chemical and pulp and paper making
characteristics and its impact on fluff generation |
626 |
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IPC
Code (s):
D21C3/00 |
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Dharm Dutt, C H Tyagi & R |
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Notes |
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Regeneration
of carbonyl compounds from their oxime using Ce (IV) based phase-transfer oxidants |
635 |
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IPC
Code (s):
C07C27/18, C07C251/32 |
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Anindita Dewan & Dilip Kumar Kakati |
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Estimation
of thermal conductivity of binary liquid mixtures employing new approach |
638 |
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IPC
Code (s):
G01N25/18 |
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J D Pandey,
R Dey, N K Soni, Prakash Chandra & M K Yadav |
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An
empirical correlation in predicting the viscosity of refined vegetable oils |
642 |
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IPC
Code (s):
A23D, G01N |
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Acknowledgement to referees |
647 |
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Annual
Author Index |
649 |
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Annual
Keyword Index |
652 |
Guidelines for Authors |
655 |
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 547-551
Optical resolution of racemic tryptophan through non-chiral membranes by ultrafiltration using chiral selector in solution
Kripal Singh
& H C Bajaj*
Optical resolution of racemic
mixture of tryptophan has been performed by ultrafiltration in solution containing bovine serum albumin
(BSA) as a chiral selector, using non chiral polysulfone (hydrophobic)
and polyamide (hydrophilic) membranes. The effectiveness of optical resolution
was characterized in terms of enantiomeric enrichment
(%ee) in permeate. Solute flux and enantiomeric enrichment of two different membranes were
compared. Effects of solute
and bovine albumin (chiral selector) concentration in feed solution, pH of the feed and operating pressure
were studied in detail to optimize the enantiomeric enrichment process. It has been observed that enantioselectivity
of ultrafiltration process is strongly pH-dependent and reaches a maxima at
feed pH 9.0–9.2. The solute flux (racemic tryptophan dissolved in
the liquid) as well as permeate flux (solution consisting racemic
tryptophan, BSA and buffer) decreases but %ee increases with
permeation time, which indicates that concentration polarization effects the enantioselectivity of
the process adversely. Enantioselectivity increases
with the BSA content in the feed solution. Optical resolution of tryptophan racemic mixture
upto 33 %ee in single pass, at a permeate flux of 9 l/m2-h was
obtained.
Keywords: Enantioselectivity, Enantiomer enrichment, Ultrafiltration,
Bovine serum albumin, Chiral
selector
IPC Code (s): C07B57/00, C12P41/00
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 552-559
Improved conversion to ethyl acetate through removal of water of esterification by membrane pervaporation
Swatilekha Das, A K Banthia & Basudam Adhikari*
Crosslinked poly (vinyl alcohol) (PVA) membranes were prepared using maleic acid (MA) and citric acid (CA) as crosslinking agents. First the water separation ability of the crosslinked membranes from aqueous acetic acid (10-90% acetic acid) and ethanol (20-80% ethanol) solutions at 30 to 90°C was tested by pervaporation. The effects of temperature, feed concentration, crosslinker type on pervaporation characteristics were investigated. The PVAMA membrane showed separation factors of 1.9-16.2 and fluxes of 4.26-38.48 kg/m2 h and PVACA membrane showed separation factors of 3.8-33 and fluxes of 2.17-480.8 kg/m2 h for acetic acid-water separation. In case of ethanol-water separation, the PVAMA membrane showed separation factors of 0.7-17.9 and fluxes of 2.5-36.2 kg/m2 h and PVACA membrane showed separation factors of 1.4-41.9 and fluxes of 3.8-359.7 kg/m2 h. PVACA membrane has shown high separation efficiency of water than that of PVAMA membrane. Having high selectivity and good permeating ability for water both the membranes were then used to remove water of esterification from reaction of acetic acid with ethanol by a batch pervaporation. Compared to around 60% conversion in conventional esterification, up to 98% conversion to ethyl acetate was achieved from ethanol and acetic acid when water by product was removed by pervaporation using the prepared membranes at same temperature.
Keywords: Pervaporation, PVA membrane, Esterification, Flux
IPC Code (s): B01D17/00, B01D61/36
Indian Journal of Chemical Technology
Vol.
14, November 2007, pp. 560-565
Electrochemical reduction of ornidazole at a composite polymer
membrane electrode
D C Tiwari, Rajeev Jain* & Gaurav Sahu
Composite polymer membrane has been fabricated on platinum foil using electrochemical deposition of pyrrole and aniline as monomers. The composite has been used as an electrode to analyse ornidazole. The results were comparable with the glassy carbon electrode. The mechanism of biological action of ornidazole is dependent upon the nitro group reduction process. In aprotic medium the reduction of the ornidazole occurs in two steps, the first involving one electron to form the nitro radical and the second step involving three electrons, resulting in the formation of the hydroxylamine derivative.
Keywords: Composite polymer membrane, Pyrrole, Aniline, Ornidazole, Glassy carbon electrode
IPC Code (s): C25C1/00, C25B11/00
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 566-571
Electrochemical reduction of 2-acetyl benzofuran and its derivatives at glassy carbon electrode
G P Mamatha, B
Electrochemical reduction of 2-acetylbenzo[b]furan and its derivatives namely 2-acetylbromobenzo[-b]furan, 2-acetylbromo-5-bromobenzo[b]furan and 2-acetyl naphtha[2,1-b] furan has been carried out in four different aqueous solvents namely DMSO, DMF, acetonitrile, ethanol using Britton Robinson buffer as supporting electrolyte at glassy carbon electrode employing cyclic voltametric techinque. Single irreversible wave was observed due to the reduction of >C=O moiety to secondary alcohol derivatives of benzofuran. Formation of pinacol due to dimerization of the intermediate radical was ruled out on steric consideration. The other data viz. the effect of sweep rate, concentration of the electroactive species, effect of temperature, effect of surfactant, effect of dielectric constant on cathodic peak potential (Epc), and cathodic peak current (ipc) has been found out. Diffusion coefficent (D0) and heterogeneous rate constant (k0) have been evaluated. The electrode process was shown to be diffusion controlled and irreversible. The electrolytic products are characterised/identified by controlled potential electrolysis. The results of the electroreduction are compared with that of the chemical reduction method.
Keywords: Voltammetry, 2-Acetyl benzo [-b] furan, Reduction, Glassy carbon electrode
IPC
Code (s): C25B3/04, G01N
Indian Journal of Chemical Technology
Vol.
14, November 2007, pp. 572-575
Preparation and characterization of an all solid supercapacitor based on polyaniline-Al2O3 layer on aluminium alloy-Al-2024
M Selva Kumar &
D
The characteristics of an all solid state supercapacitor based on polyaniline (Pani)-Al2O3 coating on aluminium alloy 2024 (Al-2024) surface prepared by the constant current method have been investigated. Three stages are observed in the potential- electrolysis time relation for the simultaneous preparation of the dielectric layer and the conducting polymer on the aluminium foil. The deposition of polyaniline film has been confirmed by cyclic voltammetry. The solid state capacitor has been studied by AC impedance spectroscopy and the capacitive behaviour of the cell is discussed in terms of Nyquist plots, complex capacitance and complex power. The study revealed that the capacitor has comparatively good capacitance, ranging from 450 to 600nF/cm2, a low time constant and also very low resistance. The normalized reactive power, |Q|/|S| and active power |P|/|S| versus frequency plot for the solid state capacitor allow an overview of the whole frequency behaviour of the supercapcitors, ranging from a pure resistance at high frequency to a pure capacitance at low frequency. When a capacitor is used as a source stiffening capacitor and is buffering the supply by delivering initial current, a lower RC time constant allows delivering significantly more current. So this type of solid-state capacitor can be used for the DC-DC converter modules.
Keywords: Supercapacitors, Electrochemical deposition, Polyaniline, Aluminium Alloy Al-2024, Solid electrolyte
IPC Code (s): H01G9/025
Indian Journal of
Chemical Technology
Vol.
14, November 2007, pp. 576-583
Some fatty acid oxadiazoles for corrosion inhibition of mild steel in HCl
M Z A Rafiquee, Nidhi Saxena*, Sadaf Khan & M A Quraishi
inhibition effect of some fatty acid oxadiazoles on the corrosion of mild steel (MS) in aqueous solution containing 1 N HCl was investigated by weight loss, potentiodynamic polarization technique, electrochemical impedance spectroscopy and scanning electron microscopy. The adsorption of these compounds was found to obey Langmuir adsorption isotherm. Various thermodynamic parameters were calculated to investigate the mechanism of corrosion inhibition. The effect of inhibitor concentration, solution temperature, immersion time and acid concentration on the corrosion of mild steel has also been investigated by weight loss technique. Scanning electron microscopy (SEM) is used to examine the surface morphology of the mild steel samples both in absence and presence of inhibitor at optimum concentration. Potentiodynamic polarization data showed that the compounds studied are cathodic type inhibitors in the acid solution. Electrochemical impedance spectroscopy was also used to investigate the mechanism of the corrosion inhibition.
Keywords: Mild steel, Oxadiazoles, Potentiodynamic polarization, Electrochemical impedance spectroscopy (EIS), Scanning electron microscopy (SEM)
IPC Code (s): C23F11/00
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 584-591
Inhibitiory effects of some imines on the corrosion of mild steel in hydrochloric acid solution
A V Shanbhag, R A Prabhu, G M Kulkarni, R G Kalkhambkar & T V Venkatesha*
The inhibition effect of 4-[(E)-(phenylimino)methyl]phenol (PIP), 4-[(E)-(4-fluorophenylimino)methyl]phenol (FIP), 4-[(E)-(4-chlorophenylimino)methyl]phenol (CIP), 4-[(E)-(4-bromophenylimino)methyl]phenol(BIP) and 4-[(E)-(4-nitro-phenylimino) methyl]phenol (NIP) on the corrosion of mild steel in hydrochloric acid was investigated. The corrosion inhibiting action was studied through weight loss and electrochemical techniques. The corrosion parameters such as anodic and cathodic Tafel slopes (ba and bc), corrosion potential (Ecorr), corrosion current densities (Icorr), surface coverage (q) and corrosion inhibition efficiencies %IE were determined. The polarization measurements indicated that the inhibitors are of mixed type. The adsorption obeyed Langmuir adsorption isotherm. The inhibition efficiencies increased with increase in inhibitor concentration but decreased with increase in temperature and also with increase in acid concentration. The activation and thermodynamic parameters were calculated for different temperatures.
Keywords: Corrosion, Mild steel, Langmuir’s isotherm, Imines, Thermodynamic parameters
IPC Code(s): C23F11/00
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 592-596
Recovery of cephalosporin C from aqueous solution using polymeric adsorbent
Punita Mishra, Pradeep Srivastava*, P K Mishra & Subir Kundu
Commercially
available neutral polymeric sorbents are used for
recovery of beta lactam antibiotic cephalosporin C
(CPC), from aqueous solution. The objective of this work is to evaluate the
separation of CPC from fermentation broth during purification process. The
neutral forms of CPC are preferentially adsorbed onto the neutral sorbents. Adsorption of CPC was higher onto the aromatic
(XAD 4) as compared to aliphatic ester sorbent (XAD
8). The kinetics of CPC adsorption on aromatic polymeric adsorbent has been
investigated. Isopropyl alcohol solution was used to desorb
CPC.
Keywords: Adsorption, Desorption, Cephalosporin C, Polymeric adsorbents
IPC Code (s): B01D15/00
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 597-605
Sorption of water soluble dyes from aqueous solutions on zirconium phosphate
Amit Jayswal & Uma Chudasama*
Amorphous zirconium phosphate (ZP) an inorganic ion exchange material of the class of tetravalent metal acid (tma) salt has been synthesized by sol-gel method. The material has been characterized for elemental analysis (ICP-AES), thermal analysis (TGA, DSC), FT-IR and X-ray diffraction studies. Chemical resistivity of the material in various media has been assessed. The sorption behaviour of dyes methylene blue (MB), crystal violet (CV), methyl violet (MV) and janus green B (JGB) towards ZP has been studied at 313, 323 and 333 K and kinetic and thermodynamic parameters evaluated. Adsorption isotherms (Langmuir and Fruendlich), breakthrough capacity and elution behaviour of dyes have also been studied. Sorption affinity of dyes towards ZP is found to be MB > CV ≈ MV > JGB.
Keywords: Zr (IV) phosphate, Inorganic ion exchanger, Tetravalent metal acid salt, Waste treatment containing dyes
IPC Code (s): B01J39/02, C09B
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 606-610
Desilication of agro based black liquor and green liquor using jet loop reactor
Sachin A Mandavgane*, G D Paradkar, J Varu, R Pamar & D Subramanian
Non-wood fibers
represent the largest resource of fibrous materials for many developing
countries in the world. Attention is now being focused on cellulose bearing
agricultural residues, which can be used as raw materials for production of
paper. Though chemical pulping of
these raw materials poses no problem, major difficulty arises in the recovery
of heat and chemicals from the spent cooking chemical (black liquor). The
presence of silica in black liquor obtained from agro based pulp and paper mill
causes serious problems at filtration, washing, evaporation, burning, recausticizing and clarification
levels of chemical recovery. It is, therefore, necessary to remove silica
before the black liquor is concentrated to
high solid content. The success of the desilication
process by carbonation lies in accurate pH
control otherwise lignin
co-precipitation occurs during desilication. In the
present work, a high mass transfer efficient, compact Jet Loop Reactors (JLR)
or some times called as Highly Compact Reactor (HCR) is used for desilication to obtain exact pH control. The experiments were carried out in a
Keywords: Black liquor, Green liquor, Desilication,
Delignification, JLR, BCR, Carbonation
IPC Code (s): D21C
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 611-615
Sensitive spectrophotometric methods for the determination of pantoprazole sodium in pharmaceuticals using bromate-bromide, methyl orange and indigo carmine as reagents
K Basavaiah*
& U R Anil kumar
Two new sensitive spectrophotometric methods are described for the determination of pantoprazole sodium sesqui hydrate (PNT) using bromate-bromide mixture and two dyes, methyl orange and indigocarmine, as reagents. The methods entail the addition of a known excess of bromate-bromide mixture to PNT in hydrochloric acid medium followed by determination of residual bromine by reacting 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 both methods, the amount of bromine reacted corresponds to the amount of PNT. The absorbance is found to increase linearly with concentration of PNT. Under the optimum conditions, PNT could be assayed in the concentration ranges 0.12-1.50 and 0.5-6.0 mg mL-1 by method A and method B, respectively. The apparent molar absorptivities are calculated to be 1.8x105 and 4.1x104 L mol-1cm-1 for method A and method B, respectively, and the corresponding Sandell sensitivity values are 0.002 and 0.011 µg cm-2. The limits of detection and quantification are also reported for both methods. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The methods were successfully applied to the assay of PNT in its tablet formulation and the results were compared with those of a reference method by calculating the Student’s t-value and F-value. No interference was observed from common tablet adjuvants. The accuracy and reliability of the methods were further ascertained by recovery experiments via standard-addition procedure.
Keywords: Pantoprazole sodium, Assay, Spectrophotometry,
Bromate-bromide
IPC Code (s): A61K, G01J3/00
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 616-625
Floatability of barite particles with different shape and roughness
U Ulusoy & M Yekeler*
In this article, different mill (ball, rod and autogenous) products of barite mineral were characterized in terms of their shape, roughness and wettability. 2D shape parameters were measured by the particle projections using SEM and expressed by elongation and roundness. Surface roughness values were determined and stated as the parameters of Ra value on the surface of the compressed discs. The wettability characteristics (gc) of barite were determined by microflotation and contact angle measurement techniques. Finally, some correlations were established between the shape parameters, surface roughness values and the wettability characteristics. In conclusion, the degree of hydrophobicity was favoured with elongation, while it was not favoured with roundness and roughness regardless of the type of the mill used.
Keywords: Floatability, Shape, Roughness, Grinding, Barite
IPC Code (s): E21C50/00
Indian Journal of Chemical Technology
Vol.
14, November 2007, pp. 626-634
Studies on effect of growth factor on morphological, chemical and pulp and paper making characteristics and its impact on fluff generation
Dharm Dutt*, C H Tyagi
& R
The dearth of cellulosic fibers has compelled the paper technocrats to search for high yielding and fast growing trees. Leucaena leucocephala has solved the manifold purposes of both farmers as well as paper manufacturers. However, paper manufacturers face the serious problem of fluff in the drying section of paper machine with this furnish. L. leucocephala of the same species was cut after 2, 3 and 4 years and was analyzed for, morphological, chemical and pulp evaluation characteristics. The fibers of 2 and 3 years old of L. leucocephala are immature and consist of more non-fibrous elements i.e. vessels and parenchymatous cells. When such type of fibers are subjected to mechanical attrition for removal of primary wall, cause more fiber cuttings instead of fibrillation. The primary wall is permeable to water but does not participate in bond formation. These non-fibrous elements have larger surface area than fibers and their presence affects fiber bonding adversely. The loosely bonded fibers from the paper sheet adhere on press rolls or dryers during sheet making and contribute to fluff problem. L. leucocephala cut after 4 years of cultivation does not show fluff problem because of complete cellulose formation of fibers.
Keywords: Ageing effect, Proximate chemical analysis, Pulping, Black liquor, Fluff
IPC Code (s): D21C3/00
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 635-637
Regeneration of carbonyl compounds from their oximes using Ce(IV) based phase-transfer oxidants
Anindita Dewan & Dilip Kumar Kakati*
Regeneration of ketone and aldehyde from their oximes is an important reaction in synthetic organic chemistry. In the oxidative deoximation processes the use of inorganic reagents is restricted by the insolubility of inorganic reagents in organic solvents. However this problem can be alleviated by the use of oxidants, like tetra-alkyl ammonium salts in the form of phase-transfer reagents. In the present case two phase transfer oxidants cetyldimethyl benzyl ammonium cerium nitrate (CDBACN) and cetyltrimethyl ammonium cerium nitrate (CTACN) were used for oxidative deoximation of oximes of carbonyl compounds. The regenerated carbonyl compounds were characterized from their melting points and spectroscopic analysis.
Keywords: Phase-transfer oxidant, Cetyldimethyl benzyl
ammonium cerium nitrate (CDBACN), Cetyltrimethyl
ammonium cerium nitrate (CTACN)
IPC Code (s): C07C27/18, C07C251/32
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 638-641
Estimation of thermal conductivity of binary liquid mixtures employing new approach
J D Pandey*, R Dey, N K Soni, Prakash Chandra & M K Yadav
Thermal conductivity of four binary liquid mixtures of polyethers with n-dodecane have been computed using a new approach. Decent agreement has been found between the experimental and estimated values of thermal conductivity for all systems.
Keywords: Thermal conductivity, Binary
liquid mixtures, Polyethers, New approach
IPC Code (s): G01N25/18
Indian
Journal of Chemical Technology
Vol.
14, November 2007, pp. 642-645
An empirical correlation in predicting the viscosity
of refined vegetable oils
Anupama Gupta, S K Sharma & Amrit Pal Toor*
Accurate knowledge of
transport properties of oil is essential for mass and heat flow. Viscosity is
one of the important properties of an oil which needs
to be determined as it influences the ease of handling, transport and nature of
storage. The effect of temperature on viscosity of six refined vegetable oils viz. palm oil, rice bran oil, cottonseed
oil, mustard oil, sunflower oil and soybean oil has been studied. An empirical
correlation between reduced viscosity and reduced temperature has been derived
for the determination of viscosities of refined vegetable oils showing Arrhenius behaviour above
Keywords: Refined vegetable oils, Temperature, Viscosity
IPC Code (s): A23D, G01N