Indian Journal of Chemistry

Sect. A: Inorganic, Bio-inorganic, Physical, Theoretical & Analytical

 

CODEN: ICACEC; ISSN: 0376-4710 (Print), 0975-0975 (Online)

 

http://www.niscair.res.in; http://nopr.niscair.res.in

Total visitors: 4399 since 30-11-2011

 

 

VOLUME 50A

NUMBER 12

DECEMBER 2011

CONTENTS

 

1689

 

Synthesis and characterization of Co(II)- and Zn(II)-8-hydroxyquinolate multilayer nanoparticles via successive ion layer adsorption and reaction technique

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Sawsan M S Haggag* & Mohamed E Mahmoud

 

 

 

Successive ion layer adsorption and reaction technique is used
to synthesize multilayer thin films of Co(II)- and
Zn(II)-8-hydroxyquinolate nanoparticles.

 

 

 

 

1697

 

Sol-gel derived nanostructured zinc oxide for
bright luminescence in ultraviolet and visible spectral regions

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Amita Verma* & A K Srivastava

 

 

 

The highest luminescence in the 950 °C sintered ZnO sample is due to the formation of nanowhiskers along with nanoparticles.

 

 

 

1703

 

Interaction of catechin with an iron(III) bis- benzimidazole diamide complex

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Nidhi Tyagi & Pavan Mathur*

 

 

 

The [Fe(L)Cl3] complex efficiently binds with catechin and the bound complex reduces the antioxidant activity of catechin considerably.

 

 

 

 

 

 

1709

 

Studies on volumetric properties of triethylamine in organic solvents with varying polarity

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

S P Ijardar, N I Malek & S L Oswal*

 

 

 

Values of limiting partial molar volumes and excess partial molar volumes decrease in the order: heptane > 2-butanone >
ethyl ethanoate >
1,4-dimethyl benzene > butyl ethanoate > ethylbenzene > chlorobenzene > nitrobenzene. The values of limiting partial molar volumes, partial volume of transfer and void volume have been rationalized in terms of solute-solvent and solute-solute interactions. The Flory theory/ERAS model has also been applied.

 

 

Notes

 

1719

 

Vapor phase fluorination of 1,1,1-trifluoro-2-chloroethane over CrOx-Y2O3 catalysts: Effects of calcination atmosphere and chromium content

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Zhi-Ying Pu*, Hong-Bo Yu, Wen-Zhi Jia,
Huan Zhou, Yue-Juan Wang & Meng-Fei Luo

 

 

 

The chromium oxide species of the catalysts calcined in nitrogen atmosphere are much easier to fluorinate to chromium fluoride and show higher catalytic activity than those calcined in air.

 

 


 

1725

 

Preparation, characterization and catalytic application of some polyoxometalates with Keggin, Wells-Dawson and Preyssler structures

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Shabnam Sheshmani*, Marzieh Arab Fashapoyeha, Masoud Mirzaei, Bita Abedi Rad,
Somayeh Nouri Ghortolmesh & Mohammad Yousefi

 

 

 

Catalytic activity of various POMs for esterification reaction of phthalic anhydride by 1-butanol has been investigated. Results show that the esterification yield of dibutylphthalatee depends on several factors such as reaction time, amount of catalyst and type of solvent. Amongst the various catalysts studied, K3[PMo6W6O40] shows the best reactivity and efficiency.

 

 

.

 

1730

 

Synthesis and application of cross-linked graft copolymer from poly(vinyl alcohol) and malic acid

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

P Chowdhury*, B Singha & A Mukherjee

 

 

 

A new polymer based on grafting and cross-linking of
poly(vinyl alcohol) has been synthesized for analytical purpose.

 

 

 

1735

 

Annual Index

 

 

 

 

Authors for correspondence are indicated by (*)

 

Indian Journal of Chemistry

Vol. 50A, December 2011, pp. 1689-1696

 

Synthesis and characterization of Co(II) and Zn(II)-8-hydroxyquinolate multilayer nanoparticles via successive ion layer adsorption and reaction technique

Sawsan M S Haggag* & Mohamed E Mahmoud

Faculty of Sciences, Chemistry Department, Alexandria University, PO Box 426, Alexandria 21321, Egypt

Email: smsh2006@hotmail.com

Received 29 November 2010; re-revised and accepted 27 October 2011

Successive ion layer adsorption and reaction (SILAR) technique was implemented to synthesize multilayer thin films of Co(II)- and Zn(II)-8-hydroxyquinolate nanoparticles. Two different approaches have been applied and compared for the formation of the thin films. The first approach is based on SILAR of Co(II)-(8HQ)2 (8HQ = 8-hydroxyquinoline) layer followed by Zn(II)-(8HQ)2, while the second is directed toward simultaneous SILAR of the two metal complexes. The two studied metal ions behave independently in their reaction with 8HQ with a molar stoichiometric ratio of 1:2 in the two metal complexes. Mixed metal complexes have not been identified under the experimental conditions. Under the same experimental conditions, Zn(II)-(8HQ)2 complex has been found to proceed four times faster than Co(II)-(8HQ)2 complex. The percentage compositions of the deposited thin film nanoparticles of Co(II)-(8HQ)2 and Zn(II)-(8HQ)2 complexes have also been tuned. Multilayer deposited and synthesized nanoparticles of Co(II)-(8HQ)2 and Zn(II)-(8HQ)2 complexes thin films have been monitored, and evaluated by using electron impact-mass spectra, scanning electron microscope, thermal analysis and elemental analysis.

Keywords: Multilayer films, Thin films, Nanoparticles, SILAR technique, Hydroxyquinolates, Cobalt, Zinc

 

Indian Journal of Chemistry

Vol. 50A, December 2011, pp. 1697-1702

 

Sol-gel derived nanostructured zinc oxide for bright luminescence in
ultraviolet and visible spectral regions

Amita Verma* & A K Srivastava

CSIR-National Physical Laboratory, Dr K S Krishnan Road, New Delhi 110 012, India

Email: amitaverma75@gmail.com

Received 24 June 2011; revised and accepted 1 November 2011

Nanostructured pure zinc oxide powder with granular and rod shaped morphologies has been synthesized employing a sol-gel process using zinc acetate as the precursor material and diethanolamine as the sol stabilizer. The effect of sintering temperature (750, 850, 950, 1050 and 1150 °C) on different properties of ZnO has been examined. The present work describes the structural, morphological and photoluminescence characteristics of zinc oxide. X-ray diffraction study has elucidated the formation of wurtzite hexagonal crystalline structure with the crystallite size varying in the nano-scale range between 20-30 nm. The scanning electron micrographs have shown the surface structure to be highly porous. The samples have demonstrated the presence of round clusters (200-500 nm) of uniformly distributed polycrystalline grains. The excellent luminescence in these samples in the UV and visible regions (green emission) is attributed to their nanocrystalline characteristics. The best photoluminescence response is found in the 950 °C sintered sample due to the presence of optimum size nanoparticles (dia.: 40 nm) and nano-whiskers (length: 500 nm).

Keywords: Nanomaterials, Nanocrystals, Nanowhiskers, Sol-gel process, Luminescence, Zinc oxide

 

Indian Journal of Chemistry

Vol. 50A, December 2011, pp. 1703-1708

 

Interaction of catechin with an iron(III) bis-benzimidazole diamide complex

Nidhi Tyagi & Pavan Mathur*­

Department of Chemistry, University of Delhi, Delhi 110 007, India

Email: pavanmat@yahoo.co.in

Received 16 May 2011; revised and accepted 4 November 2011

Bis-benzimidazole diamide ligand, 3,3'-thiobis-(N-((1H-benzo[d]imidazol-2-yl)methyl) propanamide [GBTPA = L] has been synthesized and utilized to prepare new Fe(III) complexes with exogenous anionic ligands, Cl¯and NO¯. The complexes have been characterized by IR, UV-visible, cyclic voltammetry, EPR and mass spectrometry. Low temperature EPR spectra are characteristic of a rhombic complex undergoing an axial distortion. Redox chemistry of catechin and iron(III) chloride complex in dimethyl sulfoxide, shows that catechin binds with Fe(III) complex leading to a considerable loss of antioxidant activity.

Keywords: Coordination chemistry, Iron, Benzimidazole diamides, Catechin, Electrochemical studies

 

Indian Journal of Chemistry

Vol. 50A, December 2011, pp. 1709-1718

 

Studies on volumetric properties of triethylamine in organic solvents with varying polarity

 

S P Ijardara, N I Maleka & S L Oswalb*

aApplied Chemistry Department, SV National Institute of Technology, Surat 395 007, India

bBiochemistry Division, R&D Span Diagnostic Ltd., 173-B, New Industrial Estate, Udhna, Surat 394 210, India

Received 21 July 2011; revised and accepted 8 November 2011

Apparent molar volumes () of dilute solutions of triethylamine in heptane, 2-butanone, ethyl ethanoate, butyl ethanoate, 1,4-dimethylbenzene, ethylbenzene, chlorobenzene, and nitrobenzene, at 303.15 K have been calculated from the densities determined. The limiting partial molar volumes (), limiting excess partial molar volumes () and volumes of transference () from heptane to the other investigated solvents of varying polarity have been analysed in terms of solute-solute-solvent interactions and structural effects of the molecules. Using the Terasawa model, an attempt has been made to find a measure of the contribution of specific interactions in terms of void volumes of triethylamine in the investigated solvents over a range of polarity. The Flory theory/ERAS model has also been applied to estimate the apparent molar volumes, excess apparent molar volumes and limiting excess partial molar volumes of triethylamine in investigated systems.

Keywords:   Solution chemistry, Volumetric properties, Alkylamines, Triethylamine, Partial molar volume, Void volume, Flory theory, ERAS model

 

Indian Journal of Chemistry

Vol. 50A, December 2011, pp. 1719-1724

 

Vapor phase fluorination of 1,1,1-trifluoro-2-chloroethane over
CrOx-Y2O3 catalysts: Effects of calcination atmosphere
and chromium content

Zhi-Ying Pua*, Hong-Bo Yub, Wen-Zhi Jiab, Huan Zhoua, Yue-Juan Wangb & Meng-Fei Luob

aResearch Center of Analysis and Measurement, Zhejiang University of Technology, Hangzhou 310014, China

Email: zhiyingpu@zjut.edu.cn

bZhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces, Institute of Physical Chemistry,
Zhejiang Normal University, Jinhua 321004, China

Received 25 May 2011; revised and accepted 14 November 2011

CrOx-Y2O3 catalysts (CrYO) prepared by a coprecipitation method transformed to Cr2O3-YF3 (CrYF) catalysts after being fluorinated with HF. The effects of calcination atmosphere and chromium content on its catalytic activity for the vapor phase fluorination of 1,1,1-trifluoro-2-chloroethane have been investigated. The CrYF catalysts calcined in nitrogen atmosphere show higher catalytic activity than those calcined in air. In addition, the CrYF-20 and CrF catalysts (calcined in nitrogen or air) show higher catalytic activity than CrYF-50 and CrYF-80 catalysts. Characterization results indicate that the CrYO and CrYF catalysts calcined in nitrogen atmosphere are amorphous and much easier to fluorinate with HF than those calcined in air, while CrO-N and CrF-N exist mainly as crystalline phase and difficult to be fluorinated. It is also observed that the surface acidity plays an important role in the catalyst activity for the vapor phase fluorination of HCFC-133a.

Keywords: Catalysts, Oxides, Chromium oxide, Yttrium oxide, Fluorination, Vapor phase fluorination

 

Indian Journal of Chemistry

Vol. 50A, December 2011, pp. 1725-1729

 

Preparation, characterization and catalytic application of some polyoxometalates with Keggin, Wells-Dawson, and Preyssler structures

Shabnam Sheshmania*, Marzieh Arab Fashapoyeha, Masoud Mirzaeib, Bita Abedi Rada, Somayeh Nouri Ghortolmesha & Mohammad Yousefia

aDepartment of Chemistry, Shahr-e Rey Branch, Islamic Azad University,
Shahr-e Rey Branch, PO Box
18155-144, Tehran, Iran

Email: shabnam_sheshmani@yahoo.com

bDepartment of Chemistry, Ferdowsi University of Mashhad, PO Box 917791436, Mashhad, Iran

Received 16 May 2011; revised and accepted 3 November 2011

Dibutylphthalate has been prepared via esterification reaction in the presence of some solid acidic catalysts. Transition metal polyoxometalates with Keggin (K3[PMo6W6O40], K3[PMo12O40], K4[SiMo12O40], K4[SiW12O40], Na7[PW11O39]), Wells-Dawson (K6[P2W18O62]), and Preyssler structures (K14[NaP5W30O110]) have been synthesized and characterized. The reactivity of these catalysts has been studied for the preparation of dibutylphtalate by esterification reaction of phthalic anhydride and 1-butanol. Among the various acidic catalyst used, K3[PMo6W6O40] showed the best reactivity and efficiency compared to other catalysts.

Keywords:   Catalysts, Solid catalysts, Polyoxometalates, Keggin structure, Wells-Dawson structure, Preyssler structure, Esterification, Dibutylphthalate

 

Indian Journal of Chemistry

Vol. 50A, December 2011, pp.1730-1734

 

Synthesis and application of cross-linked graft copolymer from
poly (vinyl alcohol) and malic acid

P Chowdhury*, B Singha & A Mukherjee

Department of Chemistry, Visva-Bharati, Santiniketan 731 235, India

Email: pranesh_02@yahoo.co.in/ biswajit04011976@gmail.com

Received 15 July 2011; revised and accepted 4 November 2011

A novel polymeric sorbent has been synthesized by graft copolymerization of crosslinked polyvinyl alcohol with malic acid, and characterized by FTIR, TGA and swelling studies. A suitable and interesting method has been developed for the extraction and separation of lead ion with the graft copolymer. The lead ion uptake capacity of the polymer has been evaluated vis-a-vis varying pH and metal ion concentration. Pb(II) ion has been isolated quantitatively from various synthetic mixture containing metal ions (Cd(II), Zn(II), Ni(II), Hg(II)) commonly found in battery and electroplating waste. The synthesized material has also been tested for analyzing real samples such as solder, lead concentrate and electroplating waste.

Keywords: Analytical chemistry, Cross-linked copolymers, Polymers, Graft copolymers, Solid phase extraction, Lead