Spectroscopic studies on some azo compounds and their cobalt, copper and nickel complexes

Synthesis and characterization of [o-carboxy phenylazo] moiety of barbituric acid, thiobarbituric acid, thiouracil, citrazinic acid, and disodium chromotropate and their complexes derived from cobalt (II), nickel (II), and copper (II) salts were done. The stereochemistry and the mode of bonding of the complexes were achieved based on elemental analysis, NMR, UV-Vis, IR and ESR. The dissociation constants of the free azo ligands are evaluated by spectrophotometric methods.     

Cloud-Point Extraction and Spectrophotometric Determination of Trace Quantities of Bismuth in Environmental Water and Biological Samples

ABSTRACT

A cloud-point extraction (CPE) process using the nonionic surfactant Triton X-114 to extract bismuth from aqueous solutions was investigated. The method is based on the complexation reaction of Bi(III) with 4-(2-benzothiazolylazo)2,2′-biphenyldiol (BTABD) and micelle-mediated extraction of the complex. The optimal extraction and reaction conditions (e.g., pH, reagent concentration, surfactant concentration, and effect of time) were studied. The analytical characteristics of the method (e.g., linear range, molar absorptivity, Sandell sensitivity, optimum Ringbom concentration ranges, limits of detection and quantification, preconcentration factor, and improvement factors) were obtained. Linearity was obeyed in the range of 2.50–85.0 ng mL^?1 of Bi(III) ion. The detection limit of the method was 0.75 ng mL^?1 of Bi(III) ion. The interference effect of some anions and cations was also tested. The method was applied to the determination of bismuth in environmental water, human hair, and urine samples.     

Quaternary n-Al0.08In0.08Ga0.84N/p-Si-based solar cell

Quaternary n-type Al_0.08In_0.08Ga_0.84N grown on p-Si using molecular beam epitaxy technique was fabricated as a pn-junction and an anti-reflection coating (ARC) of solar cells. The structural properties and surface morphology of the solar cells were investigated using scanning electron and atomic force microscopy. Optical reflectance was obtained using an optical reflectometery system (Filmetric F20-VIS). Current–voltage characteristics were examined under 100 mW cm^?2 illumination conditions. Quaternary n-type Al_0.08In_0.08Ga_0.84N coating was found to be an excellent ARC against incident light compared with other ARCs. This material also exhibited good light trapping over a wide wavelength spectrum, which produced highly efficient solar cells. The unique and strong polarization, as well as the piezoelectric effect, of the quaternary-nitrides was employed to reduce surface recombination velocities and enhance the solar cell performance. A solar cell with reasonable conversion efficiency of 9.74% was obtained when the n-Al_0.08In_0.08Ga_0.84N/p-Si was employed.     

Spectrophotometric microdetermination of phenylephrine hydrochloride in pure and in pharmaceutical formulations using haematoxylin

A simple, rapid, selective and sensitive method for the micro amount determination of phenylephrine hydrochloride either in pure form (raw material) or in pharmaceutical formulations is described. The method is based on the development of violet colour charge transfer complex with haematoxylin in alkaline medium with 10 min after heating at 65 °C. The wavelength and maximum absorption range was found in the range from 640 to 620 nm. Molar absorptivity and Sandell sensitivity were found to be 2.38 × 10⁴ L mol^− 1 cm^− 1 and 8.6 ng cm^− 2 respectively. A linear correlation was found between absorbance (at the λ_max) and concentration. The resulting colour is stable for more than 10 h. Results of the analyses of pure drug and dosage forms by the proposed method are in good agreement with those of the official BP 1998 procedure.     

Dielectric relaxation spectroscopy of heteronuclear cobalt(II)-copper(II) complex of 1-phenyl-3-methyl-5-pyrazolone

A bright green CoCu(PMP)(OH)2(H2O)2 complex was synthesized. Its structure was elucidated and characterized by different spectroscopic techniques. Both cobalt and copper atoms attain tetrahedral geometry. The complex was investigated by the dielectric relaxation spectroscopy. The dielectric parameters are discussed in terms of temperature and frequency changes. The conductivity of the complex decreased as the temperature increased in the temperature range 30-100 degrees C, while above this temperature range stepwise increase in the conductivity was observed.     

Two novel long-chain alkanoic acid esters of lupeol from alecrim-propolis

Two new long-chain alkanoic acid esters of lupeol were isolated together with known triterpenoids, alpha-amyrin, beta-amyrin, cycloartenol, lanosta-7,24-diene-3beta-ol and lupeol from Alecrim-propolis collected in Brazil. The structures were characterized by spectroscopic means.     

Statistical analysis of HDPE fatigue lifetime

Fatigue lifetime of HDPE structures such as pipes is recognized to show a large scatter. This study aims to compare different statistical methods and distributions, in order to give convenient modeling of tensile and fatigue test results of commercially available polyethylene compression molded sheets. The median rank, the maximum likelihood and the Kolmogorov-Smirnov fitting are compared for the estimation of Weibull parameters. The choice of the best distribution to fit fatigue lifetime is discussed on the basis of the goodness-of-fit results. It is found that whether the three-parameter distributions of Weibull and lognormal types are suitable for lifetime prediction, the two-parameter Weibull is more conservative for probabilistic fatigue design.     

Colorimetric Estimation of Melatonin in Pharmaceutical Formulations

 Three simple and sensitive colorimetric methods (A–C) for the determination of melatonin in bulk samples and in pharmaceutical formulations are described. They are based on the formation of coloured species by reaction of ninhydrin with the drug (method A, λ_max 397 nm) by oxidation of the indol moiety in melatonin with potassium persulphate (method B, λ_max 450 nm) or by reduction of osmium (VIII) (method C, λ_max 516 nm). Regression analysis of Beer-Lambert plots showed good correlations in concentration ranges between 0.8–14.2, 70.0–140.0 and 2.0–40.0 μg/mL for methods A, B and C, respectively. The molar absorptivity, Sandell sensitivity and detection limit were calculated. For more accurate analysis, Ringbom optimum concentration ranges were calculated. The validity of the proposed methods was tested by analysing pharmaceutical formulations containing melatonin. The relative standard deviations were ≤ 0.95% with recoveries 99.0–101.33%. Received October 20, 1999. Revision February 10, 1999.     

Characterization of modified styrene-co-2-acrylamido-2-methylpropane sulfonic acid magnetite nanoparticles

This work provides an insight into the effect of incorporating of magnetite nanoparticles on the rheology of fluids. In this respect, polymer-stabilized magnetite nanoparticles were obtained using sodium salt of poly (2-acrylamido-2-methylpropanesulfonate (PAMPS-Na). Monodisperse polymer coated magnetite nanoparticles Fe₃O₄/poly(styrene-AMPS) copolymer nanoparticles with diameters of 50–300 nm were prepared by radical polymerization in the presence of a ferrofluid coated with PAMPS-Na. The magnetic nanoparticles were easily separated in a magnetic field. The structure of the obtained magnetic nanoparticles was characterized by Fourier transform infrared spectroscopy (FTIR). The morphology and size of the magnetic nanoparticles were determined by transmission electron microscopy (TEM). FTIR and TEM revealed that the Fe₃O₄ nanoparticles were incorporated into the shells of poly(styrene-AMPS). Aqueous dispersed solutions of a charged hydrophobically modified Fe₃O₄/poly(styrene-AMPS) copolymer nanoparticles exhibit high viscosities even at low polymer concentrations (0.1 wt %), which is an interesting feature in connection with enhanced oil recovery. Effects of temperature and addition of sodium chloride on the viscosity properties of a semidilute dispersed solution of Fe₃O₄/poly(styrene-AMPS) copolymer nanoparticles are examined. The results indicated that Fe₃O₄/poly(styrene-AMPS) copolymer nanoparticles disclose strong interactions between magnetite and coated polymers of both PAMPS-Na and styrene-AMPS copolymers.     

Recent Heterocyclic Compounds from (1,3‐Dioxo‐2,3‐dihydro‐1H‐inden‐2‐ylidene)propanedinitrile

This review summarizes the literatures dealing with the synthesis of some important nitrogen or nitrogen/sulfur heterocyclic, spiroheterocyclic, and fused heterocyclic compounds.