Asian Journal of Chemistry

Print ISSN: 0970-7077
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Textile industry is one of the most water and chemical intensive industries worldwide. About 200-400 L of water are needed to produce 1 kg of textile fabric in textile factories. The water used in this industry is almost entirely discharged as waste. Moreover, the lost of dye in the effluents of textile industry can reach up to 50 %. The effluents are very complex, containing salt, surfactants, ionic metals and their metal complexes, toxic organic chemicals, biocides and toxic anions. Semiconductors are used to degrade pollutants in water to less harmful inorganic material. There have been numerous studies carried out across the globe focusing on the decolourization of textile wastewater. The importance of these types of research is being increasingly in the recent and has become a subject of major public health concern and scientific interest. Titanium dioxide and zinc oxide have good photocatalytic properties nominated both catalysts to be promising substrates for photodegradation of water pollutants and show the appropriate activity in the range of solar radiation. Recent studies focused on the most important photocatalytic applications of titanium dioxide and zinc oxide. These applications include the photodegradation of various pollutants killing bacteria and killing tumor cell in cancer treatments. In recent years there is a substantial interest in decolourization of industrial wastewater, especially textile wastewater. Textile industry generates large quantities of wastewater and also regarded as very toxic due to the difficulty of its disrobement by physical, chemical and microbiological methods. The overall benefits of the decolourization of textile industrial wastewater may include very interesting subjects, saving a huge amount of water and minimizing environmental pollutions. The treated water may be recycled in the same factory or reused in other applications such as other industries or agriculture that require a less quality water. This is considered to be very excellent means for saving huge amounts of water, especially, in the countries which are suffered with water deficiency. This work* 1 will describe some of the more common features of textile industrial wastewater and the evaluation of the treated wastewater by using titanium dioxide and zinc oxide to judge the validity of this type of water for using in different fields.
 
The paper describes the use of voltammetry in monitoring the reductive process of 2,4,6 Trinitrotoluene(TNT) to amine compounds by zero-valent Iron. This method let’s us determine simultaneously the reduction of TNT and the increase of Fe2+ concentrations in the samples. The method may be applied to determine quickly the efficiency of the conversion process of TNT, the role of zero-valent iron, and its efficiency in the reductive process. The factors such as pH, TNT concentration, reaction times and Fe(0) mass influencing on the conversion process into amine compounds have been studied.
 
Five transition metal(II) complexes, [ML2Cl2] 1~5, were synthesized from the reaction of MCl2·nH2O (M = Mn, Co, Ni, Cu, Cd) and the Schiff base ligand 2-[(4-methylphenylimino)methyl]-6-methoxyphenol (C15H15NO2, L), obtained by condensation of o-vanillin (2-hydroxy-3-methoxybenzaldehyde) with p-toluidine. They were characterized by elemental analysis, molar conductance, FT-IR spectra, thermal analysis. The structure of complex 1 was determined by single-crystal X-ray diffraction. Its crystal structure is of monoclinic system, space group P21/c with a = 9.0111(18) Å, b = 11.222(2) Å, c =28.130 (6) Å, α = 90 º, β = 92.29(3) º, γ = 90 º, V = 2867.6(10) Å3, Z = 4. The Mn atom is six-coordinate and displays distorted octahedral geometry.The Schiff base ligand and its complexes have been tested in vitro to evaluate their antibacterial activity against bacteria, viz., Escherichia coli, Staphylococcus aureus and Bacillus subtilis. It has been found that the complexes have higher activity than the corresponding free Schiff base ligand against the same bacteria.
 
The interaction between silver ion and adenine, guanine and guanosine monophosphate (GMP) has been followed by UV difference spectroscopy using the technique of continuous variation and high pressure liquid chromatography, combined with molecular modeling. Ag+ is found to combine with adenine to form three adducts with binding ratios (Ag+ : Adenine) of 2 : 1 and 1 : 1. It combines with guanine to form 1 : 1 adduct. It combines with GMP to form two adducts having the binding ratios (Ag+ : GMP) of 2: 1 and I : 1. The proposed structures of the complexes formed have been optimized based on molecular mechanics and semi-empirical calculations using HyperChem 7.
 
In this work, the quaternization reaction of some nitrogenous drugs in dichloromethane under stress condition and room temperature at different times are studied. Under these conditions, drug-chloromethochloride adducts or artifacts were found to be formed for clozapine, ofloxacin and olanzapine. The structures of the resultant adducts were elucidated using 1H NMR spectroscopy. In addition, the amount of intact drug was determined using in-house validated HPLC methods with UV detection.
 
Structural formulae for topiramate (MW = 339.4)
A stability-indicating high performance liquid chromatographic(HPLC) method was developed and validated for the quantitation and dissolution determination of topiramate in tablet dosage forms. An isocratic separation was achieved using a phenyl column with a flow rate of 1 mL/min using UV detection at 264 nm. Topiramate has low UV absorbtivity and was subjected to derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl). The mobile phase for the separation consisted of acetonitrile: 50 mM sodium dihydrogen phosphate(NaH2PO4) containing 3 % v/v triethylamine (pH 2.8) in a 48:52 v/v ratio. Topiramate was subjected to oxidation, hydrolysis, photolysis and heat for the purposes of stress testing. Separation was achieved for the parent compound and all the degradation products in an overall analytical run time of approximately 15 min with the parent compound topiramate eluting at approximately 9.2 min. The method was linear over the concentration range of 1-100 μg/mL (r = 0.9996) with limits of quantitation and detection of 1 and 0.3 μg/mL, respectively.
 
A representative chromatogram of a standard solution containing CPT-11, SN-38 and CPT 
A new simple, precise and accurate high performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of irinotecan (CPT-11) and two related compounds viz., 7-ethyl-10 hydroxycamptothecin (SN-38) and camptothecin (CPT) in pharmaceutical dosage forms. Chromatography was accomplished using a reversed-phase C18 column and ultraviolet (UV)detection and an isocratic mobile phase consisting of 3 % v/v triethylammonium acetate buffer (pH 3) and acetonitrile (70:30 v/v). The linear range of quantitation for all the compounds was 0.1-10 μg/mL. The limit of quantitation for all the compounds ranged between 0.01-0.05 μg/mL. The method has the requisite accuracy, selectivity, sensitivity and precision to assay of CPT-11 and related compounds in pharmaceutical dosage forms and bulk API.
 
A highly selective methacrylic based molecularly imprinted polymer (MIP) was synthesized and applied for the separation and the pre-concentration of salbutamol in urine samples. Spectrophotometric determination of salbutamol was achieved using 2,6-dichloroquinone chlorimide as colorimetric reagent. The detection limit of the method was ca. 13 ng/mL in urine after pre-concentration of the samples by MIP-SPE andanalysis with an optimized and sensitive spectrophotometric method. The linear dynamic range for salbutamol determination in urine was 0.04-0.75 μg mL-1. The recovery for the affinity based solid-phase extraction (SPE) with the MIP was more than 96 %.
 
The purpose of this study involves alternative ideas and misconceptions of the students play an important role in the studies of chemistry education in science. The basis of the chemistry education is constructed at schools through having the students understanding and the concepts of melting, dissolution, evaporation and chemical-physical change. The cross-age study was conducted with a total of 160 student (98 male, 62 female) aged 11, 12, 13 and 14 from 6th, 7th and 8th grades of Atakent elementary school in Adiyaman during 2008-2009 school year. Each group consists of 40 students. The questions related to melting, dissolution, the transformation of matter, chemical-physical changes and mixture topic were chosen from the science curriculum. The first test was the application test which assessed how to prepare the students for these subjects. The second test, named as the theoretical test, consisted of questions which seek the same answers related the same topics. In this cross-age study, the changes in the mental development and knowledge of the students were investigated. The 13 and 14 years-old students provided the best results among the age groups of 11, 12, 13, 14.
 
In this work, a double perovskite structured series was prepared by using simple citrate sol-gel method at 700 ºC for 5 h of sintering. The concentrated sample of x = 0.12 exhibits more intensity than all other concentration in their emission spectra for every series. Particle size, thickness of the particle, distance between particles and its surface morphology were identified by scanning electron microscopy. The size and distance between particles in each series lies in between the range of 1 μm-50 nm and 20-50 nm, respectively. Many voids with strong agglomerations were also observed. In addition, the absorption of light capacity for each series investigated through diffuse reflectance spectra method. All the samples of double perovskite structures exhibit a sharp cut-off of absorption light in the UV-visible regions of diffuse reflectance spectra. Predominantly, all the samples shows a very good charge transfer band in their excitation spectra that leads to more absorption of light correspondingly emits high intensity in emission spectra at 395, 464 and 545 nm. All the samples of every series emit main peaks in the range of 550-700 nm in their emission spectra. Out of all four main peaks, 614 nm peak represents the red phosphor with 5D0-7F2 transition in the emission spectra. The prepared double perovskite structure compound CRI coordinates were almost close to commercially available red phosphor i.e. Y2O2S(0.67,0.33) as per NTSC. Hence, the prepared red phosphors can be used in order to display devices, luminescent materials and WLEDs.
 
Temperature dependence of the real part of the permittivity (εr′) for BaTi1-xFexO3 for (a) x = 0.1, (b) x = 0.2, (c) x = 0.3 and (d) x = 0.6 
The BaTi1-xFexO3 ceramics (x = 0.0, 0.1, 0.2, 0.3, 0.4, 0.5 and 0.6) were prepared by the solid state reaction method. The effect of iron substitution on structural and dielectric properties of BaTiO3 ceramic was studied. These compounds are found to crystallize in the mixture of tetragonal and hexagonal phases for x ≤ 0.3 and only hexagonal phase for x > 0.3. Raman spectra indicate that when iron content increases, the intensity of Raman peaks of the tetragonal phase decreases and hexagonal phase grows, which confirm the X-ray results. The dielectric properties of BaTi1-xFexO3 ceramics as function of frequency are studied and showed a relaxation phenomena for pure barium and titanium (BT) (x = 0.0) which is displaced to the higher frequencies accompanied with a decrease in dielectric constant when x increase. The evolution of dielectric permittivity as function of temperature shows a phase transition temperature at Tc = 135 °C for BT and a clear shifting of this temperature to the higher temperature for BaTi1-xFexO3 ceramics.
 
The compound of ?-Ca2SiO4 has been considered as one of the important portand cement components. The existence of metals in the cement raw materials causes ?-Ca2-xMxSiO4 formation possibility. The ?-Ca2-xZnxSiO4 (x = 0, 0.01 and 0.025) has been prepared and characterized, and aplied for degradation of Congo red. The samples were synthesized by heating stoichiometric amounts of Zn(NO3)2·6H2O, CaCO3 and SiO2 at 950 C for 4 h followed by air quenching. The samples were characterized by using XRD, SEM, EDA and UV-visible spectroscopic methods. The XRD patterns indicate that the samples are isomorphous with ?-Ca2SiO4. The SEM micrographs depicted the aggregated irregular shape particles having size about 0.2 ?m. The EDA measurements revealed that the bulk compositions of materials are as expected. The doping of zinc increases the Eg of the sample and decreases the photocatalytic power for degradation of Congo red under sunlight.
 
The CSDA range of electrons in some commonly used solvents
The extrapolated range of electrons in some commonly used solvents
The continuous slowing down approximation (CSDA) ranges of electrons have been determined in some selected solvents in the energy range of 0.01-100 MeV using an analytic formulation. The results have been compared with CSDA range values obtained through ESTAR program and are found to be in close agreement. The extrapolated ranges of electrons have also been obtained for these selected solvents through calculations of multiple scattering detours.
 
The synthesis of nano-sized Ce 0.8Y 0.18Ca 0.02O 1.89 (YCDC) powders by citrate gel route has been investigated. The details of gel's combustion were investigated by TG-DSC and the structure of as-synthesized powders from auto-combustion was characterized by XRD. The results show that single phase YCDC powders with average size of 50 nm can be synthesized by citrate gel route. The as-synthesized powders exhibited high sinter activity, it can be sintered to 95 % of its theoretical density at 1250 °C for 4 h. The YCDC composition exhibits a total conductivity of 0.02 S/cm at 700 °C.
 
CaZrO3 ceramics exhibits high chemical, thermal and structural stability. However, its application as a host for various luminophores/activators has not been clearly explored. In present study, CaZrO3 doped with Eu3+, as a potential orange-red phosphor and the effect of NH4Cl as flux during combustion synthesis is investigated. Ca1-xZrO3:Eux (x = 0.05) nanophosphor was prepared through a low temperature, one pot solution combustion synthesis approach using glycine as fuel. Various wt.% of NH4Cl (wt.% = 0, 1, 3, 5, 7) as flux added to the reaction mixture and combustion reaction was performed. X-ray diffraction results showed that the addition of flux has significant effect on the crystallite size and the crystallinity of Ca1-xZrO3:Eux (x = 0.05) phosphor. From SEM morphology, the particles were found to be significantly agglomerated. The extent of agglomeration varies with varying the wt.% of flux. The photoluminescence excitation and emission spectra were recorded under similar condition to evaluate the effect of flux on the optical properties. Interestingly, the amount of flux was found to have significant effect on the photoluminescence emission characteristics. The photoluminescence intensity was found to be the maximum when the flux used was 5 wt.% and further increase in flux amount the photoluminescence intensity decreases. The mechanistic aspects of effect of flux on the photoluminescence were also discussed.
 
In this paper, the sol-gel method is used to synthesize a series of double perovskite oxides Sr2FeMoO6and Sr1.9A0.1FeMoO6(A = Li, Na, K). The crystal structure was investigated by X-ray powder diffraction. The results show that all the as-synthesized samples have tetragonal crystal structure, small amount of substitution has little effect to the structure of Sr2FeMoO6and they can keep double perovskite structure. Their photocatalytic activities were evaluated by degradation of dye acid black 10 B. The effects of the dosage of photocatalyst, irradiation time, irradiation source, initial concentration of dye solutions and alkali metal ions doping on the photocatalytic activity of samples were investigated. The results show that all the samples present high photocatalytic activities. In the dye concentration range of 20-150 mg/L, the decolorizing rate of acid black 10 B can reach above 95 % when the dosage of photocatalyst Sr2FeMoO6is 100 mg under UV irradiation for 40 min. Moreover, the photocatalytic activity of Li-doped sample is lower than that of the un-doped sample, but the photocatalytic activity of the Na- or K-doped samples are much better than the un-doped sample and the decolorizing rate is nearly 100 %.
 
Synthesis of the xFe(2)O(3) (1-x)Bi2O3 (0.1 <= x <= 0.5) (A1-A5: x = 0.1, 0.2, 0.3, 0.4, 0.5) glasses was done via nitrate-citrate gel route. Glassy phase is ascertained by XRD studies. Magnetic susceptibility results in the range 4.2-400 K show ferromagnetic nature with exchange integrals similar to 60 mu eV in the glasses. The electron paramagnetic resonance in the range 4.2-363 K shows g = 2.0 and g = 4.3 which are due to octahedral symmetry with tetragonal distortion and tetrahedral [FeO4/2](2-) symmetry with rhombic distortion, respectively of Fe3+ (3d(5)) ions.
 
A series of catalysts Mx(M = Ni, Co, Cu)Oy/(MgO) 0.9(CeO2)0.1 have been prepared by a sol-gel method. The effect of the activity of Mx(M = Ni, Co, Cu)O y/(MgO)0.9(CeO2)0.1 on combustion of methane was investigated and characterized by BET, XRD and TEM techniques. In view of activity and stability of a catalyst, NiO/(CeO2) 0.1-(MgO)0.9 catalyst shows the highest catalytic activity and the best thermal stability for methane combustion. The structure of the catalyst calcined at 1000 °C does not have any change, only size increases slightly from TEM photos. It still has a specific surface area of 14.32 m 2 g-1 and high activity as well as good thermal stability.
 
The formation constants of Zn(II)-glycinamide system were determined in buffer solution, pH = 4.0 (I = 0.1 mol L -1 in NaClO4 at 10, 15, 20, 25, 30 °C) using UV-Visible spectrophotometric method. The optical absorption spectra of Zn(II)-glycinamide system were analyzed in order to obtain formation constants and stoichiometries based on SQUAD software. Determining the formation constants at various temperatures enabled us to calculate some thermodynamic parameters as K, ΔG°, ΔH° and ΔS° related to the considered complexes.
 
In this communication, Ag 0.9Li 0.1(Nb 0.7Ta 0.3)O 3 (ALNT) mixed oxide powder was synthesized by citrate wet chemical method. TG-DTA, XRD and TEM analyses showed that the reaction temperature was 800 °C, the calcining time was 3 h and the product was pure Ag 0.9Li 0.1(Nb 0.7Ta 0.3)O 3 in well-dispersed grain structure (35 nm in average). The dielectric constant of ceramic sample prepared under traditional techniques is 516, dielectric loss tgδ is 4.7 × 10 -4.
 
Interfacial tension (γ) measurements were determined by using a modified drop volume technique at mixture of benzene and toluene - 0.1 M KC1 interfaces with varying concentration of dibutyl ester of sodium sulphosuccinic acid (BSS) using AGLA micrometer syringe. The value of interfacial tension regularly decreases with increase in concentration of BSS. The values of surface excess (Ts) at different concen- trations of BSS have been calculated from the gradients of γ - log C curves and appropriate form of Gibb's adsorption equation. From these data, number of surfactant ions adsorbed per cm2 of interface area occupied per surfactant ion have also been calculated. From π - A curves, it is clear that at low surfactant concentration, slight increase in surface pressure (π) reduces the area to a greater extent but at higher concentra- tions a large increase in surface pressure produces little decrease in surface area. At low surface pressure the film of surfactant ions is fully expanded and ions are stretched out in disorder manner. The surface area occupied per surfactant ion does not appreciably decrease when surfactant ions are tightly packed together which is seen from the vertical portion of π - A curves. It has been observed that as the mole fraction of benzene in hydrocarbon mixture increases, the area occupied per surfactant ion corresponding to closest packing of mono-molecular film increases.
 
In this paper, the sol-gel method is used to synthesize a series of double perovskite oxides Sr2FeMoO6 and Sr(1.9)A(0.1)FeMoO(6) (A = Li, Na, K). The crystal structure was investigated by X-ray powder diffraction. The results show that all the as-synthesized samples have tetragonal crystal structure, small amount of substitution has little effect to the structure of Sr2FeMoO6 and they can keep double perovskite structure. Their photocatalytic activities were evaluated by degradation of dye acid black 10 B. The effects of the dosage of photocatalyst, irradiation time, irradiation source, initial concentration of dye solutions and alkali metal ions doping on the photocatalytic activity of samples were investigated. The results show that all the samples present high photocatalytic activities. In the dye concentration range of 20-150 mg/L, the decolorizing rate of acid black 10 B can reach above 95 % when the dosage of photocatalyst Sr2FeMoO6 is 100 mg under UV irradiation for 40 min. Moreover, the photocatalytic activity of Li-doped sample is lower than that of the un-doped sample, but the photocatalytic activity of the Na- or K-doped samples are much better than the un-doped sample and the decolorizing rate is nearly 100 %.
 
Synthesis of the xFe203 (l-x)Bi2O 3 (0.1≤ x ≤ 0.5) (A1-A5: x = 0.1,0.2,0.3,0.4,0.5) glasses was done via nitrate-citrate gel route. Glassy phase is ascertained by XRD studies. Magnetic susceptibility results in the range 4.2-400 K show ferromagnetic nature with exchange integrals ̃60 μeV in the glasses. The electron paramagnetic resonance in the range 4.2-363 K shows g = 2.0 and g = 4.3 which are due to octahedral symmetry with tetragonal distortion and tetrahedral [FeO4/2]2- symmetry with rhombic distortion, respectively of Fe3+ (3d5) ions.
 
La1-xSrxMn0.50Fe0.50O3 {0.10 ≤ x ≤ 0.40} perovskite ceramics material is prepared by solid-state reaction method and samples are characterized to study their structural, thermal, electrical and dielectric properties. X-ray diffraction results show that as prepared samples are well crystallized in single phase and have rhombohedral crystal structure. Density is measured by Archimedes principle and with Sr substitution its value decreasing. Thermogravimetric analysis shows the weight gain in the material above 300 ºC. Thermal expansion coefficient value for x = 0.10 and 0.40 composition is found to be 12.9 × 10-6 ºC−1 and 11.3 × 10-6 ºC−1, respectively upto 800 ºC. Impedance analyzer is used to study dielectric and electrical properties which show that all the as prepared samples obey non-Debye relaxation behaviour. The maximum conductivity value is 121.09 S cm-1 for x = 0.10 and 155.96 S cm-1 for x = 0.40 at 600 ºC and 303.59 S cm-1 for x = 0.10 and 362.35 S cm-1 for x = 0.40 at 800 ºC which confirmed that in the experimental perovskite the conductivity increases after Sr doping. Activation energy also found to be decreases with Sr substitution. Therefore, studied properties confirmed that the as-prepared material is a suitable cathode material for intermediate temperature solid oxide fuel cells (SOFCs).
 
In the title TiIIIdoped ZnIIcomplex, Ti0.15Zn0.85(C6H2N2O4)2[(H3O)1.85.(H2O)0.15] (1), obtained during exploring new photochromic materials based on TiIII/IV ion, the coordination polyanion ribbons constructed by pyrazine-2,3-dicarboxylato (2,3-PZDC) ligands is balanced with the close-by hydronium cations. The asymmetric unit consists of a half metal center (composed of 15 % TiIIIand 85 % ZnII) on the symmetry axis, a 2,3-PZDC ligand and one hydronium cation (2.91 H atoms disordered at three sites). The TiIII/ZnIIion is coordinated by four 2,3-PZDC ligands, giving a distorted Ti(Zn)N2O4octahedral coordination geometry. The 2,3-PZDC ligand adopts a bridged 3- coordinated mode with one N and 2-carboxyl O atoms biting one metal center and the other 3-carboxyl O atom coordinating a adjacent metal. In addition, the connected mode of 2,3-PZDC ligand could append a π-π stacking interaction of two pyrazine within the doubly ribbons and especially append three strong hydrogen bonding interactions with hydronium cations. These hydrogen bonding interactions play a key role not only in the formation of the three-dimensional supramolecular network but also to the good thermal stability of the molecular structure. The optical absorption properties of powder samples of the title compound have also been studied and the colored profile of the sample also confirms the presence of the TiIIIion, just like a sapphire.
 
(a) XRD patterns and (b) Zoom of the peak (110) in the 2θ range of 29-33° of PCxZT samples calcined at 700 °C for 4 h
In present work, the structural and dielectric properties of Pb1-xCuxZr0.52Ti0.48O3 (PCxZT) ceramics where x = 0. 0.025, 0.05, 0.075, 0.10, 0.15 and 0.20 were studied. Powder of the compositions (PCxZT) was obtained by sol-gel route, the powders were calcined at 700 ºC for 4 h and sintered at 1100 ºC for 4 h. X-ray diffraction analysis and Raman spectroscopy suggest the formation of mixed-phase of tetragonal and rhombohedral structure which was confirmed by Rietveld refinement. Dielectric measurements of the compounds were studied as a function of temperature (from room temperature to 420 ºC at different frequencies) and as a function of frequency (from 100 Hz to 2 MHz at different temperatures). The temperature variation of the real permittivity gives evidence of the ferroelectric phase transition as well as of the resonance behaviour also observed in the dielectric permittivity frequency-dependent variation.
 
A double perovskite structured series Bi2–xEuxWO6 (x = 0.03-0.24) was prepared by using simple citrate sol-gel method at 700 ºC for 5 h of sintering. The double perovskite structure and its lattice parameters were analyzed by the XRD technique and found to be pure orthorhombic phase. The concentrated sample of x = 0.12 exhibits more intensity than all other concentration in their emission spectra. Particle size, thickness of the particle, distance between particles and its surface morphology were identified by scanning electron microscopy. The size and distance between particles lies in between the range of 1-50 nm and 20-50 nm, respectively. In addition to this the absorption of light capacity for every sample was investigated through diffuse reflectance spectra method. All the samples of double perovskite structures exhibit a sharp cut-off of absorption light in the UV and visible regions of diffuse reflectance spectra. Predominantly, sample x = 0.12 shows very good charge transfer band in their excitation spectra that leads to more absorption of light correspondingly emits high intensity in emission spectra. All the samples of series emit main peaks in the range of 550-700 nm in their emission spectra. Out of all four main peaks, 614 nm peak represents the red phosphor with 5D0−7F2 transition in the emission spectra. The prepared double perovskite structure compound CRI co-ordinates (0.6254, 0. 3739) are almost close to commercially available red phosphor i.e. Y2O2S (0.67, 0.33) as per NTSC. Hence, the prepared red phosphors can be used in order to display devices, luminescent materials and WLEDs.
 
Cd-Cr ferrospinels prepared by co-precipitation method were impregnated with cerium as promoter. Ce-impregnated ferrospinels were tested for the vapor phase alkylation of m-cresol with methanol. It has been observed that with increase in value of 'x' in Ce-impregnated Cd1-xCrxFe2O4 ferrospinels, the selectivity of 2,5-dimethyl phenol increases considerably. The reason for the improved catalytic selectivity may be due to the preferential adsorption, the strong synergistic effects among the different metal components and the relative changes in the redox nature of catalysts.
 
Vapor phase methylation of indole has been carried out over nanocrystalline Cd1-xCrxFe2O4 (x = 0, 0.25, 0.5, 0.75 and 1.0) ferrospinels in a fixed bed down-flow reactor. Catalyst characterization was performed by Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy with EDX, BET surface area and temperature programmed ammonia-desorption method. Product selectivity is shown to be strongly influenced by acidic properties of the catalyst. A maximum yield of 64.29 % of 3-methyl indole with 91.46 % selectivity at 70.3 % indole conversion was obtained under optimized reaction conditions.
 
The MgMn0.75Ti0.25O3 was synthesized by a solid state reaction crystallization method. using MgO, MnO2 and TiO2 as raw materials. The optimum conditions were obtained by thermal experiment, calcination temperature was at 900 °C, calcination time was 4.5 h. The characterization results showed that the exchange capacity of Li+ was 8.9 mmol g-1 for Li+ in the solution.
 
Gadolinium-doped barium cerate (BaCe 0.8Gd 0.2O 3, BCG) powders were prepared by the sol-gel auto-combustion process. According to the X-ray diffraction analysis, the formed BaCe 0.8Gd 0.2O 3 powders with perovskite structure are orthorhombic phase. When doped with larger sized Gd3+ ions and higher dopant concentration, the orthorhombic barium cerate lattice expanded. Results revealed that BaCe 0.8Gd 0.2O 3 proton-conducting solid electrolyte showed higher sinterability, its conductivity increased with the increase of the sintering temperature and a total conductivity 7.49 × 10 -3 S/cm at 800 °C could be obtained.
 
La 0.7Sr 0.3MnO 3 powders were prepared by liquid-solid reaction method using humidified (3 % H 2O) hydrogen as fuel and ambient air as oxidant. These powders were evaluated in terms of phase structure, morphology and fuel cell performances. An electrolyte-supported solid oxide fuel cell was prepared in a conventional manner. The results showed that the formation of La 0.7Sr 0.3MnO 3 perovskite phase was acquired at 1100 °C for 5 h. The particles of the powders were uniform and were about 0.1-0.3 μm. At 750 °C, the maximum power density of a single cell with La 0.7Sr 0.3MnO 3 powder were 135 mW cm -2.
 
Temperature-programmed reactions of mixtures of NO, CO, C3H6 and O2 were investigated over rhodium supported on microporous AlPO4-5 catalyst. Same reactions were studied after treating the catalyst in a stream of H2 to evaluate the catalytic performance after reduction treatment. Microporous AlPO4-5 was synthesized hydrothermally using triethylamine as structure directing agent and then been used as a support for rhodium metal. A lower amount of rhodium (0.4 wt %) supported on microporous AlPO4-5 catalyst exhibited satisfactory light-off at temperature (T50 % = 300 °C) with a steep rise in conversion efficiency after aging the catalyst at 900 °C for 25 h in a stream of 10 % H2O/air. Outstanding result was observed after reduction treatment of the catalyst, where light-off shifted to a lower temperature 200 °C maintaining steep rise in conversion efficiency. Rhodium nanoparticles were well dispersed on the high surface area microporous AlPO4-5 material, which is believed to be the key factor for exhibiting excellent catalytic activity both in the oxidizing as well as reducing environment. This newly developed rhodium supported microporous AlPO4-5 catalyst with minimum rhodium loading having excellent catalytic performance after reduction treatment, has the potential to serve as a new generation there-way catalyst.
 
The corrosion inhibition of steel in 0.5 M HCl by lemon leaves extracts with saffron, almonds, guava leaves and Origanum majorana extracts was studied using electrochemical polarization and EIS methods. The result indicate that the corrosion current density (Icorr) of steel increases on increasing the concentration of lemon leaves extracts while adding of each saffron, almonds, guava leaves and Origanum majorana extracts to solution of lemon leaves extracts in 0.5 M HCl increasing the inhibition efficiency of steel by decreasing corrosion current density and increasing charge-transfer resistance (Rct) with increasing the concentration of saffron, almonds, guava leaves and Origanum majorana extracts in the following order: Origanum majorana > Guava leaves ≈ Almonds > Saffron. The effect of temperature on the corrosion behaviour of steel indicates that inhibition efficiency of the lemon leaves with saffron, almonds, guava leaves and Origanum majorana extracts decreases with the rise of temperature. The adsorption isotherm of inhibitors extracts on the steel has been determined and found to follow Langmuir adsorption isotherm where the negative value of free energy of adsorption indicates that the adsorption of the inhibitors components on the steel surface occurs spontaneously.
 
A perovskite oxide BixSr1-xCo0.2Fe0.8O3 (BSCF, x = 0.5, 0.6, 0.7) is investigated as a cathode material for solid oxide fuel cells. The BSCF is prepared using solid state reaction method. The XRD shows the perovskite phase is formed at x = 0.5 and impurity phases are detected with x increasing. The area specific resistance value for the BSCF cathode is as low as 0.07 W cm2 at 750 °C as x = 0.5. The electrolytesupported fuel cell generates good performance with the peak power densities of 0.078, 0.057, 0.032 Wcm-2 at 750 °C as x = 0.5, 0.6, 0.7, respectively.
 
The present study reports on performance of acid extracts of Abutilon indicum as mild steel corrosion inhibitor in 1 M HCl and 0.5 M H 2SO4 solutions studied by electrochemical techniques. The inhibition efficiency was found to be greater than 95 % in acid media and potentiodynamic polarization study revealed that inhibitor as a mixed type of inhibitor in both HCl and H2SO4 acid media controlling anodic and cathodic reactions. Linear polarization study showed increase in resistance and the electrochemical impedance study showed a decrease in double layer capacitance as the adsorption of inhibitor caused structural changes at electrode-solution interface.
 
A bio-nondegradable functional glycoside derivative, viz. ortho-N-glycoside, was extracted from natural cabbage plants and its corrosion inhibition behavior was evaluated in relation to tin in a 0.5 M citric solution. An electrochemical study, using potentiodynamic polarization and scanning electrochemical microscopy (SEM), was conducted to determine corrosion inhibition. The results indicate that ortho-Nglycoside possesses a corrosion inhibition efficiency of 75.83% at a concentration of 0.5 mol L-1. The results of adsorption over the tin surface obeys Langmuir isotherm. The surface and the electrochemical reactivity of the tin samples in the citric acid solutions were examined using the SEM technique. This enable the corrosion type to be demonstrated. The results of the surface analysis be obtained using scanning electron microscopy (SEM).
 
(a) FTIR spectra of pure dipropyl sulphide (b) film formed on the carbon steel surface after immersion in 0.5N H2SO4 solution containing 100 mM dipropyl sulphide
In aqueous solution of 0.5M H2SO4, the Annona Squamosa extract was systematically analyzed to ensure its inhibition mechanism by using potentiodynamics polarization, the weight loss method, and electrochemical impedance spectroscopy (EIS) and its inhibitory effect on mild steel corrosion. For mild steel corrosion in 0.5 M H2SO4 solution, its inhibition efficiency increases and decreases with an increase in its concentration and temperature, respectively. Potentiodynamic polarization analyses revealed that the Annona Squamosa behaves as a cathodic inhibitor. In presence of Annona Squamosa extract in 0.5 M H2SO4 solution, an increase in the activation energy of corrosion leads to a decrease in the rate of mild steel corrosion. On mild steel surfaces, the adsorption behaviour of the extract conformed to the Temkin isotherm, Langmuir isotherm and Arrhenius equation. The EIS results were correlated with the polarization findings. According to atomic force microscopy (AFM) and scanning electron microscopy (SEM), the inhibition of mild steel corrosion proceeds through the adsorption of the extract on the mild steel surface.
 
The effect of two synthesized salicylaldiminato Schiff base bis-(2-hydroxy-3-methoxy)-1,6-diaminohexane salicylaldimine (A) and bis-(2-hydroxy)-1,6-diaminohexane salicylaldimine (B) compounds on the corrosion inhibition of mild steel in 0.5 M H2SO4 has been studied by using electrochemical Tafel polarization technique at 25°C. The results show that these compounds revealed a good corrosion inhibition in 0.5 M H 2SO4 media. The inhibition efficiency changes with the type of Schiff base and the inhibition efficiency for compound A is higher than for compound B. The adsorption of compounds A and B on the mild steel surface in 0.5 M H2SO4 obeys the Langmuir isotherm. The correlation between the molecular structures and corrosion inhibition efficiencies of compounds A and B has also been investigated using AMI semi-empirical calculations. The theoretical results have been compared with the experimental data and the relations between the inhibition efficiency and quantum parameters have been discussed. A good agreement between the inhibition efficiency of compounds A and B on mild steel in 0.5 M H2SO4 and theoretical data with some quantum chemical calculations on the structures of compounds A and B are found.
 
The search for low cost, biodegradable and easily available green corrosion inhibitors against metal corrosion has incited the study of the inhibition potentiality and adsorption behaviour of Bombax ceiba flowers extract for mild steel in 0.5 M H2SO4 medium. Weight loss, potentiodynamic polarization and scanning electron microscopy techniques were employed for the analysis. Inhibition efficiency and various thermodynamic parameters such as activation energy (Ea), adsorptive equilibrium constant (Kads) and free energy of adsorption (∆Gads) were obtained using weight loss measurements data. Bombax ceiba flower extract constituents inhibited the mild steel corrosion process by formation of protective layer on surface follows the Langmuir adsorption isotherm. The results of electro-chemical analysis directed the mixed-type behaviour of investigated inhibitor. Weight loss measurements showed the 90.84 % inhibition efficiency of Bombax ceiba flower extract at optimum concentration of inhibitor at 298 K. SEM analysis shows the remarkable upgraded surface of the mild steel strips with the inhibitor in 0.5 M H2SO4 medium.
 
A new self-assembled Schiff base of nickel(II) complex with the molecular formula [NiL]4(ClO4)8(H2O)8(CH3OH)0.5 {L = (6Z,15Z)-N1',N2'-bis(amino(pyridin-2-yl)methylene)oxalohydrazide} has been synthesized and characterized by IR spectra, elemental analysis and TG measurement. The magnetic properties investigation shows that there is weak antiferromagnetic interactions between the Ni(II) ions of the complex.
 
The cadmium complex {[Cd(adi)0.5Cl(bimt)]·H2O}n (H2adi = adipic acid, bimt = 2-((benzoimidazol-yl)methyl)-1H-tetrazole) was prepared by reaction of CdCl2·2.5H2O, bimt and H2adip in methanol/water solution and its structure was determined by single crystal X-ray diffraction analysis. The crystals are triclinic, space group P-1 with a = 8.4863(17) Å, b = 8.5551(17) Å, c = 11.422(2) Å, α = 100.08(3)°, β = 106.33(3)°, γ = 98.37(3)°, V = 766.7(3) Å3, Z = 2, F(000) = 434, Dc = 1.898 g/cm3, μ = 1.623 cm-1, the final R = 0.0252 and wR = 0.0566. A total of 8672 reflections were collected, of which 3584 were independent (Rint = 0.0216).
 
The nickel(II) compound of a tetraazamacrocycle ligand (L) (5,5,7,12, 12,14-hexamethyl-1,4,8,1 1-tetraazamacrocyclic crown ethers) has been synthesized and characterized by IR spectra and elemental analysis. The crystal structure of the NiL was determined by single-crystal X-ray. The possessing parameters: a = 21.075(4)angstrom, b = 7.7038(13)angstrom, c = 16.366 (3)angstrom, alpha = 90 degrees, beta = 104.870(2)degrees, gamma = 90 degrees, V = 2568.3(8)angstrom(3), Z = 2, Mr = 1174.41, Dc = 1.519 Mg/m(3), mu = 1.330 mm(-1), F(000) = 1226, T = 293(2) K, R = 0.0356. wR = 0.0969 for 5834 reflections with I > 2 sigma(I)
 
A novel complex Ni[phen(DTC)2H2O]·0.5H 2O, where phen = 1,10-phenanthroline and DTC is biphthalate, was synthesized and characterized by IR spectra, elemental analysis and single-crystal X-ray. The crystal is orthorhombic, space group Pbcm with unit cell parameters: a = 11.6669(6) Å, b = 11.1701 (6) Å, c = 14.0370(6) Å, α = 90°, β = 90°, γ = 90°, V = 1829.31(16) Å3, Z = 4, Mr = 430.05, Dc = 1.561 Mg/cm 3, μ = 1.099 mm-1, F(000) = 884, T = 293(2) K, R = 0.0351, wR = 0.0930 with I > 2σ(I). The crystal structure analysis shows that the nickel(II) is a five-coordinated in a slightly distorted tetragonal pyramid.
 
The objective of the study is to determine the effect of extract of Ocimum basilicum on corrosion of mild steel in aqueous 0.5M H 2SO 4. The systematic study was done by using weight loss method, potentiodynamics polarization technique and electrochemical impedance spectroscopy. The corrosion inhibition is found to occur on mild steel in presence of the extract and the inhibition efficiency of the extract increases with increase in concentration. Polarization measurement indicates that Ocimum basilicum acts as a mixed-type inhibitor and the inhibition efficiency decreases with rise in temperature. The corrosion inhibition on mild steel is found to occur due to the adsorption of inhibitor molecules on metal surface, which obeys Langmuir adsorption isotherm. The increasing values of activation energies (Ea) in presence of the extract indicate the retardation in rate of corrosion on metal surface. Scanning electron microscopic study confirmed the inhibition of corrosion on metal surface.
 
The effect of a mall amount MnO2 doping on the piezoelectric and ferroelectric properties of (Bi0.5Na0.5)(0.9)Ba0.07Sr0.03TiO3 (BNBST) lead-free ceramics prepared by the conventional mixed oxide method was systematically investigated. At x = 0.25, the MnO2-modified BNBST ceramics exhibit optimal piezoelectric and dielectric properties (d(33) = 157pC/N, k(p) = 33 %, Q(m) = 364, tan delta = 2 %, epsilon(r) = 843) and excellent ferroelectric properties composed by a higher remanent polarization P-r (P-r = 25.9 mu C/cm(2)) and lower coercive field E-c (E-c = 2.54 kV/mm) at room temperature. Moreover, the two characteristic dielectric peaks can be observed in this ceramics.
 
(Na0.5K0.5)0.94Li0.00.NbO 3-x (mol %) CuO ceramics were prepared by a solid state reaction approach and their dielectric and ferroelectric properties were evaluated by conventional methods. The high piezoelectric properties of d33 = 115Pc/N, kp = 0.259, er = 697, tan d = 2.9 % were obtained for the (Na0.5K 0.5)0.94Li0.00.NbO3 ceramics containing 1 mol % CuO sintered at 1035 °C for 2 h. Therefore, the (Na 0.5K0.5)0.94Li0.00.NbO3 ceramics containing a small amount of CuO are a good candidate material for lead-free piezoelectric ceramics.
 
The effect of a small amount of MnO2 doping on the structure and ferroelectric properties of (Bi0.5Na0.5)(0.9)Ba0.07Sr0.03TiO3 (BNBST)ceramics prepared by the conventional mixed oxide method was systematically investigated. X-Ray diffraction shows that all ceramics samples have a pure perovskite structure and a morphotropic phase boundary between tetragonal and rhombohedral phase locates in the range of 0.20 < x < 0.75. At x = 0.25, the MnO2-modified BNBST ceramics exhibit excellent ferroelectric properties composed by a higher remanent polarization P-r (P-r=25.9 mu C/cm(2)) and lower coercive field E-C (E-C=2.54 kV/mm) at room temperature. Moreover, the two characteristic dielectric peaks can be observed in this ceramics.
 
The formation process and electronic structure of a pyrazine(1) 1D molecular chain formed on the Si(001)-(2x1) surface have been studied by density functional theory calculations and angle-resolved photoemission spectroscopy. It was found by the density functional theory cluster simulation with two pyrazine molecules adsorbed on the Si substrate that the most stable structure is obtained with linearly arranged inter-dimer-bridging pyrazine adsorbates. The angle-resolved photoemission spectroscopy measurements and the density functional theory calculations reveal that the pyrazine-saturated surface is semiconducting.
 
The formation process and electronic structure of a pyrazine 1D molecular chain formed on the Si(001)-(2×1) surface have been studied by density functional theory calculations and angle-resolved photoemission spectroscopy. It was found by the density functional theory cluster simulation with two pyrazine molecules adsorbed on the Si substrate that the most stable structure is obtained with linearly arranged inter-dimer-bridging pyrazine adsorbates. The angle-resolved photoemission spectroscopy measurements and the density functional theory calculations reveal that the pyrazine-saturated surface is semiconducting.
 
Top-cited authors
Falah H Hussein
  • University of Babylon
Shahid Adeel
  • Government College University Faisalabad
Rd Kaushik
  • Gurukula Kangri Vishwavidyalaya
Shaukat Ali
  • University of Agriculture Faisalabad
Haq Bhatti
  • University of Agriculture Faisalabad