Girish Kumar,K; Saji John,Konnully(Department of Applied Chemistry, April 15, 2006)
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Abstract:
This paper reports the synthesis of a series of six new polystyrene anchored metal complexes of Co(II), Fe(III), Ni(II),
Cu(II), Zn(II), and dioxouanium(VI) using the polystyrene anchored Schiff base of 2-nitrobenzaldehyde and the corresponding
metal salts. The metal salts used were anhydrous FeCl3, CoCl2 Æ 6H2O, Ni(CH3COO)2 Æ 4H2O, Cu(CH3-
COO)2 Æ H2O, Zn(CH3COO)2 Æ 2H2O, and UO2(CH3COO) Æ 2H2O. Physico chemical characterizations have been made
from diffuse reflectance and vibrational spectra, elemental analysis, magnetic measurements, and TG studies. The elemental
analysis suggest a 1:2 metal:ligand ratio when the complexation has carried out at 70 C for about 12 h reflux. The
ligand is monodentate and coordinates through the azomethine nitrogen. The Fe(III), Co(II), Ni(II), and Cu(II) complexes
are all paramagnetic whereas Zn(II) and U(VI) are diamagnetic. Zn(II) is assigned a tetrahedral structure, Cu(II) and
Co(II) are assigned a square planar structure and Fe(III), Ni(II), and U(VI) are all assigned an octahedral structure.
The polystyrene anchored ligand has been developed as an excellent reagent for the removal of Cu(II). Optimum conditions
have been developed for the removal of metal ion from solutions by studying the effect of change of concentration of
metal ion, ligand, effect of pH, time of reflux, and interference effect of other ions. It was found that within a span of 20 min
it is possible to remove 90% of the metal ion from a 30 ppm metal ion solution in the pH range 4–5.5.
Sreekumar, K(Japaneese society of Applied physics, November 8, 2006)
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Abstract:
Copper doped methylene blue sensitized poly(vinyl alcohol) (MBPVA)–acrylamide films were fabricated to improve the
storage life of recorded gratings. The films were fabricated using gravity settling method and the copper chloride
concentration was optimized as 3:18 10 3 mol/l for a dye concentration of 6:2 10 4 mol/l. The gratings recorded on the
optimized film constitution could be stored for months with stable diffraction efficiency (24%) without any chemical or
thermal fixing techniques. The resolution of the material is found to be unaffected with the addition of copper chloride.
Prathapachandra Kurup, M R; Reena, T A(Elsevier, March 15, 2010)
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Abstract:
Five copper(II) complexes [CuLCl]2·CuCl2·4H2O (1), [CuLOAc] (2), [CuLNO3]2 (3), [CuLN3] (4) and
[CuLNCS]·3/2H2O (5) of di-2-pyridyl ketone-N4-phenyl-3-semicarbazone (HL) were synthesized and
characterized by elemental analyses and electronic, infrared and EPR spectral techniques. In all these
complexes the semicarbazone undergoes deprotonation and coordinates through enolate oxygen, azomethine
and pyridyl nitrogen atoms. All the complexes are EPR active due to the presence of an unpaired
electron. EPR spectra of all the complexes in DMF at 77K suggest axial symmetry and the presence of
half field signals for the complexes 1 and 3 indicates dimeric structures
Description:
Spectrochimica Acta Part A 76 (2010) 322–327 doi:10.1016/j.saa.2010.03.011
Mohammed Yusuff, K K; Rani, Abraham(Elsevier,Journal of Molecular Catalysis A: Chemical 198 (2003) 175–183, December 2, 2002)
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Abstract:
Copper(II) complexes of two biologically important ligands, viz., embelin (2,5-dihydroxy-3-undecyl-2,5-cyclohexadien
1,4-dione) and 2-aminobenzimidazole were entrapped in the cages of zeolite Y by the flexible ligand method. The capability
of these compounds in catalyzing the reduction of oxygen (industrially known as deoxo reaction) was explored and the
results indicate an enhancement of the catalytic properties from that of the simple copper ion exchanged zeolite. These
point to the ability of the ligands in enhancing the oxygen binding capability of the metal ion. Elemental analyses, Fourier
transform infrared (FTIR), diffuse reflectance and EPR spectral studies, magnetic susceptibility measurements, TG, surface
area analyses and powder X-ray diffraction studies were used in understanding the presence, composition and structure of
the complexes inside the cages. The study also reveals the increased thermal and mechanical stability of the complexes as a
result of encapsulation.
Rapheal,P F; Manoj, E; Prathapachandra Kurup, M R(Elsevier, 2007)
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Abstract:
Ten copper(II) complexes {[CuL1Cl] (1), [CuL1NO3]2 (2), [CuL1N3]2 · 2/3H2O (3), [CuL1]2(ClO4)2 · 2H2O (4), [CuL2Cl]2 (5), [CuL2N3] (6), [Cu(HL2)SO4]2 · 4H2O (7), [Cu(HL2)2] (ClO4)2 · 1/2EtOH (8), [CuL3Cl]2 (9), [CuL3NCS] · 1/2H2O (10)} of three NNS donor thiosemicarbazone ligands {pyridine-2-carbaldehyde-N(4)-p-methoxyphenyl thiosemicarbazone [HL1], pyridine-2-carbaldehyde-N(4)-2-phenethyl thiosemicarbazone [HL2] and pyridine-2-carbaldehyde N(4)-(methyl), N(4)-(phenyl) thiosemicarbazone [HL3]} were synthesized and physico-chemically characterized. The crystal structure of compound 9 has been determined by X-ray diffraction studies and is found that the dimer consists of two square pyramidal Cu(II) centers linked by two chlorine atoms.
Rare earth exchanged Na–Y zeolites,
H-mordenite, K-10 montmorillonite clay and amorphous
silica-alumina were effectively employed for the
continuous synthesis of nitriles. Dehydration of benzaldoxime
and 4-methoxybenzaldoxime were carried
out on these catalysts at 473 K. Benzonitrile (dehydration
product) was obtained in near quantitative yield
with benzaldoxime whereas; 4-methoxybenzaldoxime
produces both Beckmann rearrangement (4-methoxyphenylformamide)
as well as dehydration products
(4-methoxy benzonitrile) in quantitative yields. The
production of benzonitrile was near quantitative under
heterogeneous reaction conditions. The optimal protocol
allows nitriles to be synthesized in good yields
through the dehydration of aldoximes. Time on stream
(TOS) studies show decline in the activity of the catalysts
due to neutralization of acid sites by the basic reactant
and product molecules and water formed during the
dehydration of aldoximes.
Mohammed Yusuff, K K; Sridevi, Nadimpall; Jelaja, Padmavathy(Kluwer Academic Publishers, July 20, 2000)
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Abstract:
The nature of the diperiodatocuprate(III) (DPC) species present in aqueous alkaline medium has been investigated
by a kinetic and mechanistic study on the oxidation of iodide by DPC. The reaction kinetics were studied over the
1.0 ´ 10)3±0.1 mol dm)3 alkali range. The reaction order with respect to DPC, as well as iodide, was found to be
unity when [DPC] [I)]. In the 1.0 ´ 10)3±1.0 ´ 10)2 mol dm)3 alkali region, the rate decreased with increase in
the alkali concentration and a plot of the pseudo-®rst order rate constant, k versus 1/[OH)] was linear. Above
5.0 ´ 10)2 mol dm)3, a plot of k versus [OH)] was also linear with a non-zero intercept. An increase in ionic
strength of the reaction mixtures showed no e ect on k at low alkali concentrations, whereas at high concentrations
an increase in ionic strength leads to an increase in k. A plot of 1/k versus [periodate] was linear with an intercept in
both alkali ranges. Iodine was found to accelerate the reaction at the three di erent alkali concentrations employed.
The observed results indicated the following equilibria for DPC.
Prathapachandra Kurup, M R; Nisha, K; Sithambaresan, M(November 21, 2011)
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Abstract:
The title compound, C21H19N3O2S, exists in the thione form.
The configuration about the C N bond is E. The
hydrazinecarbothioamide unit adopts an almost planar
arrangement, with maximum deviations of 0.016 (3) and
0.016 (2) A ° for the two thiourea N atoms. An intramolecular
O—H N hydrogen bond occurs. Weak intermolecular N—
H S, C—H O and C—H interactions are observed in
the crystal structure
The effect of chromium doping on methylene
blue sensitized Poly (vinyl alcohol)/Acrylamide was carried
out by varying the ratios of Ammonium dichromate
and methylene blue. In the case of films without ammonium
dichromate, the diffraction efficiency was found to
decrease on storage. On chromium doping the storage life
was improved. Interestingly, a self-enhancement in efficiency
was observed for a particular ratio of methylene
blue and ammonium dichromate.
One-pot acetalizations of cyclohexanone. acetophenone and benzophenone were carried out using methanol over H-montmorillonite clay
(a mesoporous material). silica, alumina, and different zeolites such as HFAU-Y.HBeta, H-ZSM-5, and H-mordenite. In all the cases a single
product-the corresponding dimethylacetal-was obtained in high yields. Hemiacetal formation was not observed with any catalyst. A
comparison of catalytic activity indicated that montmorillonite K-10 is the most active catalyst for the reaction. As evidenced by the reaction
time studies, the catalyst decay is greater over the zeolite catalyst than over the clay.
Sugunan, S; Renuka, N K(Indian Journal of Chemistry, April , 2002)
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Abstract:
Physico-chemical characterization of DY203/V2O5 systems prepared through wet impregnation method has been carried
out using various techniques like EDX, XRD, FTIR. thermal studies, BET surface area, pore volume and pore size
distribution analysis. The amount of vanadia incorporated has been found to influence the surface properties of dysprosia.
The spectroscopic results combining with X-ray analysis reveal that vanadia species exist predominantly as isolated
amorphous vanadyl units along with crystalline dysprosium orthovanadate. Basicity studies have been conducted by
adsorption of electron acceptors and acidity and acid strength distribution by temperature programmed desorption of
ammonia. Cyclohexanol decomposition has been employed as a chemical probe reaction to examine the effect of vanadia on
the acid base property of Dy2O3. Incorporation of vanadia titrates thc Lewis acid and base sites of Dy2O3, while an
enhancement of Bronsted acid sites has been noticed. Data have been correlated with the catalytic activity of these oxides
towards the vapour phase methylation of phenol
Dipyrromethene-Cu(II) derivatives possessing two dodecane alkyl chains have been used for the modification of gold
electrodes. Electroactive host molecules have been incorporated into a lipophilic dodecanethiol SAM deposited onto
gold electrodes through hydrophobic and van der Waals interactions (embedment technique). The presence of
dipyrromethene-Cu(II) redox centers on the electrode surface was proved by cyclic voltammetry and Osteryoung
square-wave voltammetry. The Au electrodes incorporating redox active Cu(II)-dipyrromethene SAMs were used for
the direct voltammetric determination of paracetamol in human plasma.
Girish Kumar,K; Joseph, Renjini(Taylor & Francis, June 1, 2009)
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Abstract:
A metalloporphyrin incorporated carbon paste sensor has been developed
for the determination of metronidazole benzoate (MTZB). Zn(II) complex
of 5,10,15,20-tetrakis (3-methoxy-4-hydroxy phenyl) porphyrin (TMHPP) was
used as the active material. The MTZB gave a well-defined reduction peak at
- 0.713V in 0.1 mol l -1 phosphate buffer solution of pH around 7. Compared
with bare carbon paste electrode (CPE), the TMHPP Zn(II) modified electrode
significantly enhanced the reduction peak current of MTZB as well as lowered
its reduction potential. Under optimum conditions the reduction peak current
was proportional to MTZB concentration over the range 1×10-3 mol1-1 to 1×10-5mol1-1. The detection limit was found to be 4.36×10-6mol1-1
. This
sensor has been successfully applied for the determination of MTZB in pharmaceutical
formulations and urine samples.
Girish Kumar,K; Thomas, D; Joseph, R; Issac, S; Lonappan, L(The Institution of Engineering and Technology, October 10, 2011)
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Abstract:
A differential pulse voltammetric sensor for the determination of tamsulosin hydrochloride (TAM) using multiwalled carbon nanotubes
(MWNTs)–Nafion-modified glassy carbon electrode (GCE) has been developed. MWNTs were dispersed in water with the help of Nafion
and were used to modify the surface of GCE via solvent evaporation. At MWNT-modified electrode, TAM gave a well-defined oxidation
peak at a potential of 1084 mV in 0.1 M acetate buffer solution of pH 5. Compared to the bare electrode, the peak current of TAM
showed a marked increase and the peak potential showed a negative deviation. The determination conditions, such as the amount of
MWNT–Nafion suspension, pH of the supporting electrolyte and scan rate, were optimised. Under optimum conditions, the oxidation
peak current was proportional to the concentration of TAM in the range 1 × 1023 M–3 × 1027 M with a detection limit of
9.8 × 1028 M. The developed sensor showed good stability, selectivity and was successfully used for the determination of TAM in pharmaceutical
formulations and urine samples
The electron-donor properties of Sm2O3 activated at 300, 500, and 800°C are reported from studies on the adsorption of electron acceptors of various electron affinities (electron affinity values in eV are given in parentheses): 7,7,8,8-tetracyanoquino-dimethane (2.84), 2,3,5,6-tetrachloro-1,4-benzoquinone (2.40), p-dinitrobenzene (1.77), and m-dinitrobenzene (1.26) in acetonitrile and 1,4-dioxane. The extent of electron transfer during the adsorption was determined from magnetic measurements. The acid-base properties of Sm2O3 at different activation temperatures are reported using a set of Hammett indicators. Electron donor-acceptor interactions at interfaces are important in elucidating the adhesion forces.
Sugunan, S; Jalaja, J M(Indian Journal of Chemistry, March , 1995)
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Abstract:
The electron donating properties of Ce02 and its mixed
oxides with alumina have been determined from the studies
of adsorption of electron acceptors of various electron
affinities on the surface of these oxides. The catalytic
activity of these oxides towards some reactions such as
oxidation of alcohols and reduction of ketones have been
Correlated with their surface electrondonor properties. The
surface acidity/basicity of these oxides have also been
determined by titration method using a set of Hammett
indicators.
The catalytic activity of Perovskite-type mixed oxides (LaCo03 . PrCo03 and SmCo03 ) for the
reduction of cyclohexanone to cyclohexanol with 2-propanol (Meerwein-Ponndorf-Verley reduction)
has been studied. The data have been correlated with the surface electron donor properties
of these mixed oxides.
Sugunan, S; Devika Rani, G(Indian Journal of Chemistry, November , 1993)
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Abstract:
The adsorption of electron acceptors, viz.,7,7,8,8-tetracyanoquinodimethane(TCNQ), 2,3,5,6-tetrachloro-p-
benzoquinone (chloranil) and p-dinitrobenzene
(PDNB) on the surface of three rare earth oxides Y2O3,
Nd203 and Pr6O11 has been studied in acetonitrile and
dioxan. From the radical concentration on the surface
determined using ESR spectral data, the electron donor
strength of the rare earth oxides are reported.
Invertase was adsorbed onto micro-porous acid-activated montmorillonite clay (K-10) by two procedures, namely adsorption and covalent binding. The immobilized enzymes were characterized by XRD, surface area measurements and 27Al NMR. XRD measurements revealed an expansion of clay layers due to immobilization which suggests that intercalation had taken place. Surface area measurements also support this observation. 27Al NMR showed that interaction of enzyme with tetrahedral and octahedral Al changes with the immobilization procedure. Sucrose hydrolysis was performed in a batch reactor. The immobilized enzymes showed enhanced pH and thermal stabilities. Optimum pH and temperature were found to increase upon immobilization. The effectiveness factor (η) and Michaelis constant (Km) suggest that diffusional resistances play a major role in the reaction. The immobilized invertase could be stored in buffer of pH 5 and 6 at 5 °C without any significant loss in activity for 20 days.