Prathapachandra Kurup, M R; Neema, Ani Mangalam(Elsevier, July 27, 2008)
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Abstract:
Four oxovanadium and one dioxovanadium complex with 2-hydroxyacetophenone N(4)-
phenylthiosemicarbazone (H2L) which are represented as [VOLphen]·2H2O (1), [VOLbipy] (2),
[VOLdmbipy] (3), [VOL]2 (4) and [VO2HL]·CH3OH (5) have been synthesized and characterized by
elemental analyses, electronic, infrared and EPR spectral techniques. In all the complexes 1–4 the
ligand coordinates through phenolic oxygen, azomethine nitrogen and thiolate sulfur. But in complex
[VO2HL]·CH3OH, coordination takes place in thione form instead of thiolate sulfur. All the complexes
except [VO2HL]·CH3OH are EPR active due to the presence of an unpaired electron. In frozen DMF at 77 K,
all the oxovanadium(IV) complexes show axial anisotropy with two sets of eight line patterns
Iron pillared Montmorillonite has been synthesised and it is then wet impregnated with vanadia with different vanadia
composition. These catalysts are characterised using conventional techniques such as XRD analysis,FTIR analysis and
surface area and pore volume measurements. Acidity is measured using spectrophotometric monitoring of adsorption of
perylene, thermogravimetric desorption of 2.6 dimethylpyridine and temperature programmed desorption of ammonia.
Activity studies are done in the liquid phase. It has been concluded that Lewis acidic sites are responsible for the benzylation
of toluene when the benzylating agent is benzyl chloride while Bronsted acidic sites are responsible when the reagent is
benzyl alcohol.
The (Ba1-x Srx) (Nd1/2, Nb1/2) O3 ceramics have been prepared by the conventional
ceramic route for different values of x. Addition of a small amount of
CeO2(1 wt%) as a sintering aid increased the density of the samples. The structure
and microstructure of the sintered samples are studied by X-ray diffraction
and SEM methods. The dielectric properties of the samples are measured in the
microwave frequency region as a function of composition. The dielectric constant
decreases as x increases. The coefficient of thermal variation of resonant
frequency decreases as the Sr content increases and goes to the negative side.
The dielectric properties of (Ba1-x Srx) (Nd1/2, Nb1/2) O3 are in the range suitable
for application as dielectric resonators in microwave circuits
Sunajadevi, K R; Sugunan, S(Elsevier, October , 2004)
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Abstract:
Chromia loaded sulfated titania has been synthesized via sol–gel route with different chromia loadings. These catalysts are characterized using conventional techniques such as XRD analysis, FTIR analysis, surface area and pore volume measurements, EDX, SEM and UV–Vis diffuse reflectance spectral analysis. Acidity is measured using spectrophotometric monitoring of adsorption of perylene, thermogravimetric desorption of 2,6-dimethylpyridine and temperature programmed desorption of ammonia. Activity studies are done in the liquid phase. It has been concluded that Lewis acid sites are responsible for the benzylation of arenes with benzyl chloride.
A series of rare-earth neodymia supported vanadium oxide catalysts with various V205 loadings ranging from 3 to 15 wt.% were prepared
by the wet impregnation method using ammonium metavanadate as the vanadium precursor. The nature of vanadia species formed on the
support surface is characterized hy a series of different physicochemical techniques like X-ray diffraction (XRD). Fourier transform infrared
spectroscopy (FTIR). BET surface area, diffuse reflectance UV-vis spectroscopy (DR UV-vis), thermal analysis (TG-DTG/DTA) and SEM.
The acidity of the prepared systems were verified by the stepwise temperature programmed desorprion of ammonia (NH3-TPD) and found that
the total acidity gets increased with the percentage of vanadia loading. XRD and FT1R results shows the presence of surface dispersed vanadyl
species at lower loadings and the formation of higher vanadate species as the percentage composition of vanadia is increased above 9 wt.%.
The low surface area of the support. calcination temperature and the percentage of vanadia loading are found to influence the formation of
higher vanadia species. The catalytic activity of the V205-Nd203 catalysts was probed in the liquid phase hydroxylation of phenol and the
result show that the present catalysts are active at lower vanadia concentrations.
Mohammed Yusuff, K K; Anas, K(Elsevier, Applied Catalysis A :General 264 (2004) 213–217, December 25, 2003)
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Abstract:
CoMo/gama-Al2O3 catalysts for hydrodesulphurisation activity were prepared by making use of the molecular designed dispersion (MDD)
method. Molybdenum and cobalt pyrrolidine-N-carbodithioate (Pydtc) complexes were used for the incorporation of metals on the support.
The catalysts were characterized by elemental analysis, low temperature oxygen chemisorption, temperature programmed reduction (TPR)
and laser Raman spectroscopy. The hydrodesulphurisation activity of all the catalysts were carried out and results were compared with those
of the catalysts prepared through the conventional method. Higher molybdenum dispersion, smaller molybdenum clusters, lower reduction
temperature of catalyst and better hydrodesulphurisation activity were observed for the catalysts prepared through the MDD method
The title reaction was undertaken to establish the interaction between amantadine and molybdate at physiological pH. Identical FTIR spectra, TG-DTA curves and CHN data of the complexes formed from three solutions at pH 1.5, 7.4 and 8.0 indicate that the same complex was formed at all the three pHs. The FTIR spectrum shows shift in peaks corresponding to primary amino group of the drug due to coordination to molybdate. An octahedral geometry is assigned to the complex. The kinetics of the complexation has been studied at low concentrations of the reactants using UV-visible spectrophotometry. At pH 7.4, the initial rate varies linearly with [molybdate]. A plot of initial rate versus [drug] is linear passing through origin. These results indicate that the drug and molybdate react at pH 7.4 even at low concentrations. At pH 1.5, the rate increases linearly with increase in [drug] but decreases with [molybdate]. The effect of pH and ionic strength on the rate of the reaction has also been studied. A suitable mechanism has been proposed for the reaction. Reaction between the drug and molybdate even at low concentrations and the fact that the amino group of amantadine required to be free for its function as antiviral, is bound to molybdate in the complex suggests that simultaneous administration of the drug and molybdate supplements should be avoided.
Prathapachandra Kurup, M R; Suma, S; Sudarsana Kumar, M R; Siji, V L(Elsevier, February 26, 2010)
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Eight new transition metal complexes of benzaldehyde-N(4)–phenylsemicarbazone have been synthesized
and characterized by elemental analyses, molar conductance, electronic and infrared spectral
studies. In all the complexes, the semicarbazone is coordinated as neutral bidentate ligand. 1H NMR
spectrum of [Zn(HL)2(OAc)2] shows that there is no enolisation of the ligand in the complex. The magnetic
susceptibility measurements indicate that Cr(III), Mn(II), Fe(III), Co(II) and Cu(II) complexes are
paramagnetic and Ni(II) is diamagnetic. The EPR spectrum of [Mn(HL)2(OAc)2] in DMF solution at 77K
shows hyperfine sextet with low intensity forbidden lines lying between each of the two main hyperfine
lines. The g values calculated for the [Cu(HL)2SO4] complex in frozen DMF, indicate the presence of
unpaired electron in the dx2−y2 orbital. The metal ligand bonding parameters evaluated showed strong
in-plane bonding and in-plane bonding. The ligand and complexes were screened for their possible
antimicrobial activities.
Description:
Spectrochimica Acta Part A 76 (2010) 22–28 doi:10.1016/j.saa.2010.02.035
Pazhoor Bijumon, Varghese; Mohanan, P; Mailadil, Thomas Sebastian(The Japan Society of Applied Physics, 2002)
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Abstract:
Microwave ceramic dielectric materials Ca5Nb2TiO12 and Ca5Ta2TiO12 have been prepared by a conventional solid-state
ceramic process. The structure was studied by X-ray diffraction and the dielectric properties were characterized at microwave
frequencies. The ceramics posses a relatively high dielectric constant, very low dielectric loss (Q5 x f > 30000GHz) and
small temperature variation of resonant frequency. These materials are potential candidates for dielectric resonator
applications in microwave integrated circuits. [DOI: 10. 1 143/JJAP.41.3834]
Dielectric ceramics based on solid solution phases of [RE1_x= REr]TiNb06, where REI_s = Nd, Pr, Sm and RE' = Dy, Gd and Y, were prepared by the conventional solid-state ceramic route for values of x. The ceramic samples are characterized by X-ray diffraction and microwave methods. Ceramics based on RE (Pr, Nd and Sm) belonging to aeschynite group shows positive value of Tf and those based on RE (Gd, Dy and Y) belonging to euxenite group show negative value of r f. The solid solution phases between the aeschynite and the euxenite group shows intermediate dielectric constant and r f values. The results indicate the possibility of tailoring the dielectric properties by varying the composition of the solid solution phases. The range of solid solubility of euxenite in aeschenite and aeschenite
in euxenite are different for different rare earth ions
Mohammed Yusuff, K K; Manju, Sebastian; Arun, Vasudevan; Robinson, P P; Leeju, Pally; Digna, Varghese; Varsha, Gopalakrishnan(Taylor & Francis, Journal of Coordination Chemistry, October 15, 2009)
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Abstract:
The mononuclear cobalt(II) complex [CoL2] H2O (where HL is quinoxaline-2-carboxalidine-
2-amino-5-methylphenol) has been prepared and characterized by elemental analysis, conductivity
measurement, IR, UV-Vis spectroscopy, TG-DTA, and X-ray structure determination.
The crystallographic study shows that cobalt(II) is distorted octahedral with each tridentate
NNO Schiff base in a cis arrangement. The crystal exhibits a 2-D polymeric structure parallel to
[010] plane, formed by O-H...N and O-H... O intermolecular hydrogen bonds and pye
stacking interactions, as a racemic mixture of optical enantiomers. The ligand is a Schiff base
derived from quinoxaline-2-carboxaldehyde
Reena Mary, A P; Narayanan, T N; Vijutha, Sunny; Sakthi Kumar, D; Yasuhiko, Yoshida; Joy, P A; Anantharaman, M R(Springer, 2010)
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Abstract:
Bio-compatible magnetic fluids having high
saturation magnetization find immense applications in
various biomedical fields. Aqueous ferrofluids of superparamagnetic
iron oxide nanoparticles with narrow size
distribution, high shelf life and good stability is realized by
controlled chemical co-precipitation process. The crystal
structure is verified by X-ray diffraction technique. Particle
sizes are evaluated by employing Transmission electron
microscopy. Room temperature and low-temperature magnetic
measurements were carried out with Superconducting
Quantum Interference Device. The fluid exhibits good
magnetic response even at very high dilution (6.28 mg/cc).
This is an advantage for biomedical applications, since only
a small amount of iron is to be metabolised by body organs.
Magnetic field induced transmission measurements carried
out at photon energy of diode laser (670 nm) exhibited
excellent linear dichroism. Based on the structural and
magnetic measurements, the power loss for the magnetic nanoparticles under study is evaluated over a range of
radiofrequencies.
Bejoy, Thomas; Prathapan, Sreedharan; Sugunan, Sankaran(Elsevier, May , 2005)
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Abstract:
The synthesis of dimethyl acetals of carbonyl compounds such as cyclohexanone, acetophenone, and benzophenone has successfully been carried out by the reaction between ketones and methanol using different solid acid catalysts. The strong influence of the textural properties of the catalysts such as acid amount and adsorption properties (surface area and pore volume) determine the catalytic activity. The molecular size of the reactants and products determine the acetalization ability of a particular ketone. The hydrophobicity of the various rare earth exchanged Mg–Y zeolites, K-10 montmorillonite clay, and cerium exchanged montmorillonite (which shows maximum activity) is more determinant than the number of active sites present on the catalyst. The optimum number of acidic sites as well as dehydrating ability of Ce3+-montmorillonite and K-10 montmorillonite clays and various rare earth exchanged Mg–Y zeolites seem to work well in shifting the equilibrium to the product side.
Anantharaman, M R; Suchand Sandeep, C S; Narayanan, T N; Shaijumon, M M; Ajayan, P M; Reji, Philip(IOP Publishing LTD, June 24, 2009)
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Abstract:
Magnetic heterostructures with carbon nanotubes having multiple functionalities are fascinating
materials which can be manipulated by means of an external magnetic field. In this paper we
report our investigations on the synthesis and optical limiting properties of pristine cobalt
nanotubes and high coercivity cobalt-in-carbon nanotubes (a new nanosystem where carbon
nanotubes are filled with cobalt nanotubes). A general mobility assisted growth mechanism for
the formation of one-dimensional nanostructures inside nanopores is verified in the case of
carbon nanotubes. The open-aperture z-scan technique is employed for the optical limiting
measurements in which nanosecond laser pulses at 532 nm have been used for optical
excitation. Compared to the benchmark pristine carbon nanotubes these materials show an
enhanced nonlinear optical absorption, and the nonlinear optical parameters calculated from the
data show that these materials are efficient optical limiters. To the best of our knowledge this is
the first report where the optical limiting properties of metal nanotubes are compared to those of
carbon nanotubes
Anantharaman, M R; Narayanan, T N; Shaijumon, M M; Ajayan, P M(American Chemical Society, July 3, 2008)
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Abstract:
Cobalt nanotubes (CoNTs) with very high longitudinal coercivity were prepared by electrodeposition of cobalt
acetate for the first time by using anodized alumina (AAO) template. They were then characterized with
X-ray diffraction (XRD), a field emission scanning electron microscope (FESEM), and a transmission electron
microscope (TEM). Formation of a highly ordered hexagonal cobalt phase is observed. Room temperature
SQUID (superconducting quantum interference device) magnetometer measurements indicate that the easy
axis of magnetization is parallel to the nanotube axis. These CoNTs exhibit very high longitudinal coercivity
of ∼820 Oe. A very high intertubular interaction resulting from magnetostatic dipolar interaction between
nanotubes is observed. Thick-walled nanotubes were also fabricated by using cobalt acetate tetrahydrate
precursors. A plausible mechanism for the formation of CoNTs based on mobility assisted growth is proposed.
The role of the hydration layer and the mobility of metal ions are elucidated in the case of the growth mechanism
of one-dimensional geometry
Anantharaman, M R; Shaijumon, M M; Ajayan, P M; Narayanan, T N(Springer, October 21, 2009)
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Abstract:
Hybrid magnetic nanostructures with high
coercivity have immense application potential in various
fields. Nickel (Ni) electrodeposited inside Cobalt (Co)
nanotubes (a new system named Ni @ Co nanorods) were
fabricated using a two-step potentiostatic electrodeposition
method. Ni @ Co nanorods were crystalline, and they have
an average diameter of 150 nm and length of *15 lm.
The X-ray diffraction studies revealed the existence of two
separate phases corresponding to Ni and Co. Ni @ Co
nanorods exhibited a very high longitudinal coercivity. The
general mobility-assisted growth mechanism proposed for
the growth of one-dimensional nanostructures inside nano
porous alumina during potentiostatic electrodeposition is
found to be valid in this case too
Muhammad, Abdul Jamal E; Joy, P A; Anantharaman, M R; Philip, Kurian(Elsevier, January , 2009)
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Abstract:
Nanocomposites based on natural rubber and nano-sized nickelwere synthesized by incorporating nickel
nanoparticles in a natural rubber matrix for various loadings of the filler. Structural, morphological, magnetic
and mechanical properties of the compositeswere evaluated along with a detailed study of dielectric
properties. Itwas found that nickel particleswere uniformly distributed in the matrix without agglomeration
resulting in a magnetic nanocomposite. The elastic properties showed an improvement with increase
in filler content but breaking stress and breaking strain were found to decrease. Dielectric permittivity
was found to decrease with increase in frequency, and found to increase with increase in nickel loading.
The decrease in permittivity with temperature is attributed to the high volume expansivity of rubber at
elevated temperatures. Dielectric loss of blank rubber as well as the composites was found to increase
with temperature.