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Indian Journal of Chemistry

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

 

VOLUME 43A

NUMBER 12

December 2004

 

CONTENTS

 

 

Papers

 

 

 

2497

 

 

A quantum chemical investigation of electrophilic addition reaction of bromine to
exo-tricyclo[3.2.1.02.4]oct-6-ene

 

   

 

 

Rıza Abbasoğlu* & Sevil Savaşkan Yılmaz

 

 

 

Full geometric optimization of exo-tricyclo[3.2.1.02,4]oct-6-ene(exoTCO) has been done by semiempirical methods. The exoTCO...Br2 system has been investigated by AM1 method and exoTCO...Br2(exo) molecular complex has been found to be relatively more stable than the exo...Br2(endo) complex.

 

 2503

 

23Na, 29Si, 27Al and 1H MAS NMR investigations of rare earth exchanged faujasite-Y zeolite and vapor phase alkylation of benzene with 1-octene

 

 

 

 

 

 

 

 

 

Bejoy Thomas & S Sugunan*

 

 

 

Rare earth exchanged NaFAU-Y zeolites have been prepared by simple ion exchange methods under moderate conditions. The effect of rare earth cations in the textural and structural properties of modified NaFAU-Y zeolite has been investigated. The prepared systems have been effectively employed for the alkylation of benzene with
1-octene in the vapor phase. Deactivation studies show that the as-exchanged rare earth zeolites possess better stability towards reaction conditions than the pure HFAU zeolite. The decrease in conversion of 1-octene with reaction time is due to the blocking of zeolite pores by heavy alkylation products.

 

2514

 

Synthesis and characterization of a novel lamellar type aluminosilicate molecular sieves, NCL-5

 

 

 

 

 

N Venkatathri*

 

 

 

A novel lamellar type aluminosilicate molecular sieve, NCL-5, has been synthesized and characterized by XRD, SEM, TG/DTA, FT-IR and MASNMR. Analyses show that NCL-5 is a novel short range ordered nanocrystalline aluminosilicate with phase purity. 27Al MASNMR shows the presence of maximum ocatahedral coordinated aluminium in NCL-5 sample while 29Si NMR shows the presence of three different types of silicon.

 

2518

 

Evaluation of excess thermodynamic properties in some binary mixtures of o-chlorophenol

  

 

 

G V Rama Rao, A Viswanatha Sarma & C Rambabu*

 

 

 

Ultrasonic velocity, density and viscosity measurements in binary mixtures of co-chlorophenol + ethyl benzoate + anisic aldehyde + acetonitrile are reported at 303.15, 308.15, 313.15, and 318.15K over the entire range of composition. The deviation from ideality of related thermodynamic parameters is explained on the basis of molecular interactions between the constituent components of the mixture.

 

2529

 

Synthetic, spectroscopic and toxicological aspects of novel eighteen to twenty two membered tetraazamacrocycles and their bivalent manganese complexes

 

 

 

 

 

 

 

 

 

 

Ashu Chaudhary & R V Singh*

 

 

 

 

2536

 

Preparation, characterization and antimicrobial properties of some palladium and platinum complexes with active Schiff base ligands

 

 

   

Mukesh Kumar Biyala, Nighat Fahmi & R V Singh*

 

 

 

Notes

 

2542

 

Preparation of small-sized particles of Eu2+-activated barium magnesium aluminate phosphors

 

 

 

 

 

 

 

 

 

 

Sang-Do Han*, Chi-Hwan Han, Ishwar Singh & Devender Singh

 

 

 

A new method for the preparation of europium activated barium magnesium aluminate phosphors by combustion method is reported.

 

 

2545

 

Effects of rare earths on activity and selectivity of hydrogenation of chloronitrobenzene over PtM/TiO2 (M=La, Ce, Pr, Nd and Sm) catalysts

 

 

 

 

 

 

 

 

G H Lai, X X Han, R X Zhou*, J X Zhang & X M Zheng

 

 

 

The effect of rare earths on the activity and selectivity of the hydrogenation of chloronitrobenzene to chloroaniline over PtM/TiO2 (M=La, Ce, Pr, Nd and Sm) catalysts has been studied in ethanol at 303K and atmospheric pressure. PtM/TiO2 catalysts show higher activity than Pt/TiO2 catalyst for the hydrogenation. The highest yield of p-, m- and o- chloroaniline is 95.7 mol% for PtLa/TiO2, 96.8 mol% for PtCe/TiO2 and 97.0 mol% for PtPr/ TiO2, respectively. The reaction rate is in the following order:
m-CNB > p-CNB > o-CNB.

 

2549

 

Volumetric properties of transfer of D(+)glucose and sucrose from water to mixed aqueous solutions at 298.15 K

 

 

 

 

 

 

T S Banipal*, Kultar Singh & P K Banipal

 

 

 

Apparent molar volumes and apparent molar compressibilities of D(+)-glucose and sucrose have been determined in aqueous solutions of potassium chloride, strontium chloride, barium chloride and guanidine hydrochloride at 298.15 K from their density and sound velocity data. Transfer parameters have been discussed in terms of solute-cosolute interactions on the basis of a cosphere overlap hydration model. Interaction coefficients have also been calculated from transfer parameters.

 

2555

 

Molar volume and viscosity of cupric chloride in aqueous mannitol

 

 

 

Shashi Kant*, Pankaj Dogra & Sushil Kumar

 

 

 

The apparent molar volume and viscosity of cupric chloride have been determined in 2, 4 and 6 wt/wt% aqueous mannitol solutions at 303, 308, 313 and 318 K. Cupric chloride has been found to be structure- maker in aqueous mannitol from molar volume as well as viscosity studies.

 

2558

 

Octameric molecular aggregates of cyclic tellurane (C5H10TeCl2) assisted by Te---Cl secondary bonds and long Cl---Cl contacts

 

 

   

 

 

Prakash Chandra Srivastava*, Smriti Bajpai, Sangeeta Bajpai, Rajesh Kumar & Ray J Butcher

 

 

 

 

2563

 

Thermal, magnetic and electrochemical properties  of  polymeric  copper  complexes of
2-hydroxy-1,4-naphthoquinone and its methyl derivative

  

Sunita Salunke Gawali, Sandhya Rane*, Kamel Boukheddaden, Ephiphane Codjovi, Jorge Linares, François Varret & Pramod Bakare

 

 

 

The reaction of 2-hydroxy-1, 4-naphthoquinone (Lw) and 3-methyl-2-hydroxy-1, 4-naphthoquinone (Phth) with anhydrous CuCl2 results in [Cu(Lw)2(NH3)2] and [Cu(Phth)2(NH3)].2H2O respectively. Thermal, magneto-structural and electrochemical studies point to the polymeric nature of both the complexes.

 

2568

 

Studies on benzoylhydrazone complexes derived from saturated six-membered heterocyclic ketones

 

  

 

 

A Manimekalai* & B Senthil Sivakumar

 

 

 

Ni(II) and Cu(II) complexes of the type [NiLOH.2H2O]2.nH2O and CuL2 [L=cis-2,6-diphenyltetra-hydrothiopyran-4-one benzoylhydrazone/ trans-3-methyl-cis-2,6-diphenylpiperidin-4-one benzoyl-hydrazone have been synthesized and characterized by elemental, electronic, IR, ESR, conductivity, magnetic and TGA/DTA studies.

 

2573

 

Cationic ruthenium complexes based on planar polypyridyl ligand 2,4,6-tris(2-pyridyl)-1,3,5-triazine

 

 

 

 

 

 

 

Sanjeev Sharma, Manoj Trivedi,  Manish Chandra & Daya Shankar Pandey*

 

 

 

New cationic complexes, [Ru(k3-tptz){(p-FC6H4)3P}2Cl]-BF4, [Ru(k3-tptz){(p-CH3C6H4)3P}2 Cl]BF4,[Ru(k3-tptz)
{(p-ClC6H4)3P}2 Cl]BF4, [Ru(
k3-tptz){(p-CH3OC6H4)3P}2-Cl]-BF4, and [Ru(k3-tptz){p-(CH3)2NC6H4)3P}2Cl]BF4 containing both group 15 donor and a planar polypyridyl ligand are prepared by reaction of RuCl3.xH2O with an excess amount of phosphines and 2,4,6-tris(2-pyridyl)-1,3,5-triazine (tptz) in methanol under refluxing conditions.

 

2578

 

Synthesis and characterization of tridentate Schiff’s base derived from 5-(2'-thiazolylazo) salicylaldehyde and p-methoxy aniline and their Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) complexes

 

P P Hankare*, L V Gavali , V M Bhuse, S D Deleka  & R S Rokade

 

 

 

 

2582

 

Spectrophotometric studies on the simultaneous determination of cadmium and lead using artificial neural network

 

 

M R Sohrabi, P Abdolmaleki, M Davallo*, M Rabbani & R Ebrahimi

 

 

 

Simultaneous spectrophotometric determination of cadmium(II) and lead(II) based on complexation with EDTA has been proposed using an artificial neural network (ANN) model to analyze the mixture spectra. An ANN consisting of three layers of nodes has been trained by applying a back-propagation learning rule.

 

2586

 

Synthesis, ion-exchange and physico-chemical studies on a polystyrene cerium(IV) phosphate hybrid fibrous ion exchanger

 

 

K G Varshney*, N Tayal, Puja Gupta, Arun Agrawal & M Drabik

 

 

 

Polystyrene based cerium(IV) phosphate (PStCeP) has been synthesized and characterized using IR, TGA, XRD and SEM studies. In addition, its ion-exchange capacity, elution, pH titration and distribution behaviour have also been studied. The Na+ ion exchange capacity is found to be 2.95 meq/dry g.

 

2590

 

Solid phase extraction and spectrophotometric determination of vanadium

 

 

Chengming Zhang, Qiufen Hu, Kun Gu,  Guangyu Yang* & Jiayuan Yin 

 

 

 

A sensitive, selective and rapid method has been developed for the determination mg/L level of vanadium based on the rapid reaction of V(V) with 2-(2-quinolylazo)-5-dimethylaminophenol and the solid phase extraction of the colored chelate with C18 cartridge.

2595

Annual Index

 

 

Authors for correspondence are indicated by (*)

 

 

Indian Journal of Chemistry

 Vol. 43A, December 2004, pp. 2497-2502

 

A quantum chemical investigation of electrophilic addition reaction of bromine to exo-tricyclo[3.2.1.02.4]oct-6-ene

Rıza Abbasoğlu* & Sevil Savaşkan Yılmaz

 

Full geometric optimization of exo-tricyclo[3.2.1.02,4]oct-6-ene(exoTCO) has been done by the semiempirical methods and the structure of the molecule investigated. The double bond of molecule is endo-pyramidalized and the two faces of double bond are no longer equivalent. Exo face of the double bond of the molecule has regions having high electron density(qi,HOMO) and bigger negative potential. The exoTCO...Br2 system has been investigated by AM1 method and exoTCO...Br2(exo) molecular complex has been found to be relatively more stable than the exo...Br2(endo) complex. The cationic intermediates of the reaction have been studied by semiempirical methods. Exo-bromonium cation is found to be more stable than endo bromonium cation. Exo-facial selectivity has been observed in the addition reaction to exoTCO of bromine which is caused by electronic and steric effects. Exo-classical bromocarbonium cation(III) is more stable than rearrangament cation(V) which is formed with Wagner-Meerwein rearrangament. Bromocarbonium cation(III) is the most stable ion among the cationic intermediates and the ionic addition occurs via the formation of this cation. The mechanism of the addition reaction has also been discussed.

 

IPC Code: Int.Cl.7 C07B 37/02
 

 

Indian Journal of Chemistry Vol

. 43A, December 2004, pp. 2503-2513

 

23Na, 29Si, 27Al and 1H MASNMR investigations of rare earth exchanged NaFAU-Y zeolite and vapour phase alkylation of benzene with 1-octene

Bejoy Thomas & S Sugunan*

 

Rare earth exchanged NaFAU-Y zeolites have been prepared by simple ion-exchange methods under moderate conditions. We have investigated the effect of rare earth cations in the textural and structural properties of modified NaFAU-Y zeolite. 23Na and 29Si MASNMR have been used to study the migration tendencies of the rare earth cations from the super cages to the small cages in the zeolite structure, which ultimately reduces the concentration of accessible Brönsted acid sites. 27Al and 29Si MASNMR techniques have been used to study the strain in the Si-O-T and Al-O-T framework tetrahedra induced by the bulky rare earth counter cations in the extra-framework cation positions. The prepared systems have been effectively employed for the alkylation of benzene with 1-octene in the vapour phase. We have tried to correlate the results from various MAS-NMR experiments with the activity of various rare earth exchanged zeolites for the alkylation of benzene with 1-octene. From the deactivation studies it is observed that the as-exchanged rare earth zeolites possess better stability towards reaction conditions compared the pure HFAU-Y zeolite. The decrease in the conversion of 1-octene with reaction time is due to the blocking of zeolite pores by heavy alkylation products.

 

IPC code: Int. Cl.7 B01J 21/12

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2514-2517

 

Synthesis and characterization of a novel lamellar type aluminosilicate molecular sieves, NCL-5

N Venkatathri

 

A novel lamellar type aluminosilicate molecular sieve, NCL-5 has been synthesized and characterized using various physicochemical techniques such as XRD, SEM, TG/DTA, FT-IR and MAS NMR. The results have been compared with Si-MCM-41 sample synthesized using the same template (cetyltrimethyl ammonium bromide). XRD analysis shows that NCL-5 is a novel short range ordered aluminosilicate. SEM shows that it is nanocrystalline with phase purity. TG/DTA analysis shows that the NCL-5 sample oxidatively decomposes the occluded template in a single step while Si-MCM-41 oxidatively decomposes in two different steps. This may due to the nanocrystallinity of the former sample. Aluminium MAS NMR shows the presence of maximum octahedral co-ordinated aluminium in NCL-5 sample while silicon NMR shows the presence of three different types of silicon.

 

IPC Code: Int. Cl.7 B01J 29/06

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2518-2528

 

Evaluation of excess thermodynamic properties in some binary mixtures of o-chlorophenol

G V Rama Rao, A Viswanatha Sarma & C Rambabu*

 

 Ultrasonic velocity, density and viscosity measurements in binary mixtures of o-chlorophenol (1)+ethyl benzoate (2)+anisic aldehyde (2)+acetonitrile (2) are reported at 303.15, 308.15, 313.15, and 318.15K over the entire range of composition. From the experimental data, other related thermodynamic parameters viz, adiabatic compressibility, intermolecular free length, molar volume, excess adiabatic compressibility, excess viscosity, excess molar volume, Rao’s constant and Wada’s constant have been calculated. The deviation from ideality of these parameters is explained on the basis of molecular interactions between the constituent components of the mixture.

 

IPC Code: Int. Cl.7 G01N

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2529-2535

 

Synthetic, spectroscopic and toxicological aspects of novel eighteen to twenty two membered tetraazamacrocycles and their bivalent manganese complexes

Ashu Chaudhary & R V Singh*

 

The tetraamide macrocyclic ligands TTD1-TTD4 have been prepared by the condensation of 1,2-diaminoethane or 1,3-diaminopropane and glutaric acid or adipic acid in presence of condensing reagents dicyclohexylcarbodiimide and 4-dimethylaminopyridine. On reduction, these macrocyclic ligands give tetraazamacrocycles TTD5-TTD8, which form complexes with manganese(II) nitrate. The ligands and their complexes have been characterized by elemental analyses, molecular weight determinations, magnetic moment, infrared, electronic and X-ray spectral studies. On the basis of spectral studies, an octahedral geometry for these complexes has been proposed as the binding sites are the nitrogen sites of the macrocycles. The formulation of the complexes as [Mn(TTDn)(NO3)2] has been established on the basis of chemical composition. The ligands and their complexes have also been screened for their antimicrobial activities.

 

IPC Code: Int. Cl.7 C07F 13/00; C08

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2536-2541

 

Preparation, characterization and antimicrobial properties of some palladium and platinum complexes with active Schiff base ligands

Mukesh Kumar Biyala, Nighat Fahmi & R V Singh*

 

The synthetic, spectroscopic and biological studies of some palladium and platinum complexes derived from 5-methyl-1,3-dihydro-3-[2-(phenyl)ethylidene]-2H-indol-2-one-hydrazinecarbothioamide(L1H) and 5-methyl-1,3-dihydro-3-[2-(phenyl)ethylidene]-2H-indol-2-one-hydrazinecarboxamide(L2H) are reported here. These complexes have been characterized on the basis of elemental analysis, molecular weight determinations and spectral studies including IR, 1H NMR and electronic spectra. The resulting coloured products are monomeric in nature. On the basis of the above studies, square planar geometry has been proposed for the resulting complexes. Both the ligands and their complexes have been screened for their fungicidal and bactericidal activities and the results indicate that they exhibit significant antimicrobial properties.

 

IPC Code: Int. Cl.7 C07F 15/00; C07C 251/02

 

 

 

Indian Journal of Chemistry

 Vol. 43A, December 2004, pp. 2542-2544

 

Preparation of small-sized particles of Eu2+-activated barium magnesium aluminate phosphors

 Sang-Do Han* & Chi-Hwan Han, Ishwar Singh & Devender Singh

 

A new method for the preparation of europium activated barium magnesium aluminate phosphors by combustion method has been proposed. The corresponding metal nitrates have been decomposed with diformylhydrazine to give very fine sized particles, which were then fired at 1300ºC for 1 h in a slightly reducing atmosphere. This method gives better brightness to the phosphor than that made by the conventional method.

 

IPC Code: Int Cl7 C09K 11/00

 

 

 

Indian Journal of Chemistry

 Vol. 43A, December 2004, pp. 2545-2548

 

Effects of rare earths on activity and selectivity of hydrogenation of chloronitrobenzene over PtM/TiO2 (M=La, Ce, Pr, Nd and Sm) catalysts

G H Lai, X X Han, R X Zhou*, J X Zhang & X M Zheng

 

The effect of rare earths on the activity and selectivity of the hydrogenation of chloronitrobenzene to chloroaniline over PtM/TiO2 (M=La, Ce, Pr, Nd and Sm) catalysts has been studied in ethanol at 303 K and atmospheric pressure. PtM/TiO2 catalysts show higher activity than Pt/TiO2 catalyst for the hydrogenation. Some PtM/TiO2 catalysts increase the selectivity for chloroaniline. The conversion of chloronitrobenzene is >99%. The highest yield of p-, m- and o- chloroaniline is 95.7mol% for PtLa/TiO2, 96.8mol% for PtCe/TiO2 and 97.0mol% for PtPr/ TiO2, respectively. The reaction rate is in the following order: m-CNB > p-CNB > o-CNB.

 

IPC Code: Int. Cl.7 B01J; C07B 35/02

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2549-2554

 

Volumetric properties of transfer of D(+)-glucose and sucrose from water to mixed aqueous solutions at 298.15 K

T S Banipal*, Kultar Singh & P K Banipal

 

Apparent molar volumes (fv) and apparent molar compressibilities (KS,2,f) of D(+)-glucose and sucrose have been determined in aqueous solutions of potassium chloride (0.5, 1.0, 2.0 and 4.0 mol kg-1), strontium chloride (0.25, 0.5 and 2.0 mol kg-1), barium chloride (0.25, 0.5 and 1.0 mol kg-1) and guanidine hydrochloride (0.25, 0.5 and 2.0 mol kg-1) at 298.15 K from their density and sound velocity data. Partial molar volumes (Vo2) and adiabatic compressibilities (KoS,2) at infinite dilution have been determined from the respective apparent molar properties and used to calculate partial molar volumes (Vo2,tr) and adiabatic compressibilities (KoS,2,tr) of transfer for saccharides from water to aqueous potassium chloride, strontium chloride, barium chloride and guanidine hydrochloride solutions. Transfer parameters have been discussed in terms of solute-cosolute interactions on the basis of a cosphere overlap hydration model. Interaction coefficients have also been calculated from transfer parameters.

 

IPC Code: Int. Cl.7 G01N

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2555-2557

 

Molar volume and viscosity of cupric chloride in aqueous mannitol

Shashi Kant*, Pankaj Dogra & Sushil Kumar

 

The apparent molar volume, (fv) and viscosity of cupric chloride have been determined in 2, 4 and 6 wt/wt percent aqueous mannitol solutions at 303, 308, 313 and 318K. The fv values vary linearly with square root of concentration of cupric chloride. The limiting apparent molar volume has been interpreted in terms of solute-solvent interaction. The fv0 values vary with temperature and can be represented in the power series of temperature. Structure making/breaking capacity of electrolyte is inferred from the sign of ( 2fv0/ T2) and dB/dT values. The apparent molar expansibility has also been determined. Cupric chloride has been found to be structure- maker in aqueous mannitol from molar volume as well as viscosity studies.

 

IPC Code: Int. Cl.7 G01N

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2558-2562

 

Octameric molecular aggregates of cyclic tellurane (C5H10TeCl2) assisted by Te---Cl secondary bonds and long Cl---Cl contacts

Prakash Chandra Srivastava*, Smriti Bajpai, Sangeeta Bajpai, Rajesh Kumar & Ray J Butcher

 

The supramolecular association in the cyclic tellurane [1,1,2,3,4,5,6-heptahydro-1,1-dichloro tellurane] (C5H10TeCl2) is described. It exists as tetrameric molecular aggregates assisted by Te---Cl secondary bonds. The tetramers are further associated through long Cl---Cl contacts to yield octameric molecular aggregates. The supramolecular association in C5H10TeCl2 is compared with the supramolecular associations (trimeric molecular aggregates) present in C5H10TeBr2 and C5H10TeI2..

 

IPC Code: Int. Cl.7: C 07 C 395/00

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2563-2567

 

Thermal, magnetic and electrochemical properties of polymeric copper complexes of 2-hydroxy-1,4-naphthoquinone and its methyl derivative

Sunita Salunke-Gawalib, Sandhya Rane*, Kamel Boukheddaden,

Ephiphane Codjovi, Jorge Linares, François Varret & Pramod Bakare

 

The reaction of 2-hydroxy-1, 4-naphthoquinone (Lawsone; Lw) and 3-methyl-2-hydroxy-1, 4-naphthoquinone (Phthiocol; Phth) with anhydrous CuCl2 results in [Cu(Lw)2(NH3)2] (M-1) and [Cu(Phth)2(NH3)].2H2O (M-2) complexes respectively. Thermal, magnetostructural and electrochemical studies indicate the polymeric nature of both the complexes. The energy of activations calculated from the thermogramms is found to be 65 kJ/Lw, 23.75 kJ/NH3 in M-1 and 178.90 kJ/H2O, 221.5 kJ/NH3, 566.2 kJ/Phth and 28.19 kJ/ Phth in M-2. The increasing and decreasing nature of cm.T with decrease in temperature in M-1 and M-2 reveals the ferro and antiferromagnetic interactions in M-1 and M-2 respectively. The cyclic voltammetry studies indicate occurrence of effective metal ligand interactions in solution for both the complexes.

 

IPC Code: Int.Cl.7 C07F 1/08

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2568-2572

 

Studies on benzoylhydrazone complexes derived from saturated six-membered heterocyclic ketones

A Manimekalai* & B Senthil Sivakumar

 

Ni(II) and Cu(II) complexes of the type [NiLOH.2H2O]2.nH2O and CuL2 [L=cis-2,6-diphenyltetrahydrothiopyran-4-one benzoyl-hydrazone (DTTBH)/trans-3-methyl-cis-2,6-diphenylpiperidin-4-one benzoylhydrazone (MDPBH)] have been synthesized and characterized by elemental, electronic, IR, ESR, conductivity, magnetic and TGA/DTA studies. Both the ligands react in the enol form with the metal ions and hence act as uninegative bidentate/tridentate ligands. Enolic oxide bridged dimeric structure has been proposed for the nickel complexes on the basis of spectral and magnetic data.

 

IPC Code: Int.Cl.7 C07F 15/04; C07F 1/08

 

 

 

 

Indian Journal of Chemistry Vol. 43A, December 2004, pp. 2573-2577

 

Cationic ruthenium complexes based on planar polypyridyl ligand 2,4,6-tris (2-pyridyl)-1,3,5-triazine

Sanjeev Sharma, Manoj Trivedi, Manish Chandra and Daya Shankar Pandey*

 

New cationic complexes [Ru(k3-tptz){(p-FC6H4)3P}2Cl]BF4, [Ru(k3-tptz){(p-CH3C6H4)3P}2Cl]BF4,[Ru(k3-tptz){(p-ClC6H4)3P}2 Cl]BF4, [Ru(k3-tptz){(p-CH3OC6H4)3P}2Cl]BF4, and [Ru(k3-tptz){p-(CH3)2NC6H4)3P}2Cl]BF4 containing both group 15 donor and a planar polypyridyl ligand are prepared by reaction of RuCl3.xH2O with an excess amount of phosphines and 2,4,6-tris(2-pyridyl)-1,3,5-triazine (tptz) in methanol under refluxing conditions. The complexes have been characterized by elemental analyses and spectral techniques, viz., IR, 1H NMR, 31P NMR, FAB-MS and electronic spectral studies.

 

IPC Code: Int.Cl7. C07F 15/00

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2578-2581

 

Synthesis and characterization of tridentate Schiff’s base derived from 5-(2'-thiazolylazo)salicylaldehyde and p-methoxy aniline and their Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) complexes

P P Hankare*, L V Gavali , V M Bhuse, S D Delekar & R S Rokade

 

A series of new complexes involving Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) ions and Schiff’s base ligand obtained by condensation of 5-(2'-thiazolylazo) salicylaldehyde and p-methoxy aniline have been synthesized. The complexes are characterized by elemental analysis, magnetic susceptibility, molar conductance, IR, electronic spectra, ESR and thermal analysis (TGA). The ONN environment of the metal ion is realized in the complexes by involvement of the –N=N- group in coordination. The analysis of magnetic moment and electronic spectral data indicate tetrahedral geometry for the Mn(II), Co(II), Ni(II), Zn(II), Cd(II) and Hg(II) complexes, while distorted tetrahedral geometry for the Cu(II) complex.

 

IPC Code: Int. Cl.7 C07F 15/06 C07F 15/04; C07F 1/08; C07F 3/06; C07F 3/08; C07F 3/10; C07F13/00; C07C 251/02

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2582-2585

 

Spectrophotometric studies on the simultaneous determination of cadmium and lead by using artificial neural network

M R Sohrabi, P Abdolmaleki, M Davallo*, M Rabbani & R Ebrahimi

 

Simultaneous spectrophotometric determination of cadmium(II) and lead(II) based on formation of their complexes with ethylendiaminetetraacetic acid (EDTA) has been proposed. An artificial neural network (ANN) model has been used to analyze the mixture spectra. Absorption spectra of various concentrations of Cd-EDTA and Pb-EDTA solutions in the wavelength between 190-290 nm have been recorded, and the spectral data and concentration used as input and output for the ANN, respectively. In this study, an ANN consisting of three layers of nodes has been trained by applying a back-propagation learning rule. Sigmoid transfer functions have been used in the hidden and the output layers to facilitate non-linear calibration. The root mean square error for cadmium and lead are 0.048 and 0.023, respectively.

 

IPC Code: Int. Cl.7 G01N; C07F 3/08; C07F 7/24

 

 

 

Indian Journal of Chemistry

Vol. 43A, December 2004, pp. 2586-2589

 

Synthesis, ion-exchange and physico-chemical studies on a polystyrene cerium(IV) phosphate hybrid fibrous ion exchanger

K G Varshney*, N Tayal, Puja Gupta, Arun Agrawal & M Drabik

 

Polystyrene based cerium(IV) phosphate (PStCeP) has been synthesized as a new phase of fibrous ion exchanger. It has been characterized using IR, TGA, XRD and SEM studies in addition to its ion-exchange capacity, elution, pH titration and distribution behaviour. The Na+ ion exchange capacity is found to be 2.95 meq/dry g. A comparison of PStCeP with other materials of this class such as acrylonitrile cerium(IV) phosphate (ANCeP), acrylamide cerium(IV) phosphate (AACeP) and polystyrene thorium(IV) phosphate (PStThP), have also been discussed.

 

IPC Code: Int. Cl.7 B01J 39/02

 

 

 

Indian Journal of Chemistry

 Vol. 43A, December 2004, pp. 2590-2594

 

Solid phase extraction and spectrophotometric determination of vanadium

Chengming Zhang, Qiufen Hu, Kun Gu, Guangyu Yang* & Jiayuan Yin

 

A sensitive, selective and rapid method has been developed for the determination mg/L level of vanadium based on the rapid reaction of V(V) with 2-(2-quinolylazo)-5-dimethylaminophenol (QADMAP) and the solid phase extraction of the colored chelate with C18 cartridge. QADMAP reacts with V(V) in the presence of citric acid-sodium hydroxide buffer solution (pH=3.5) and cetyl trimethylammonium bromide (CTMAB) medium to form a violet chelate of a molar ratio 1:2 (V:QADMAP). This chelate is enriched by solid phase extraction with C18 cartridge and the enrichment factor of 50 was obtained by elution of the chelate from the cartridge with ethanol. Molar absorptivity of the chelate has been found to be 1.22´105 L.mol–1.cm–1 at 585 nm. Beer’s law is obeyed in the range of 0.01-0.6 mg/mL. The detection limit is 0.04 mg/L in original samples. This method has also been applied to the determination of V(V) in water and biological samples. The relative standard deviations are 1.8-2.5%, and the recoveries are 96-103%.

 

IPC Code: Int. Cl.7 G01N; C07F 9/00