A rapid and sensitive extractive spectrophotometric determination of copper(II) in pharmaceutical and environmental samples using benzildithiosemicarbazone.

Benzildithiosemicarbazone (BDTSC) is proposed as a sensitive and selective analytical reagent for the extractive spectrophotometric determination of copper(II). BDTSC reacts with copper(II) in the pH range 1.0-7.0 to form a yellowish complex. Beer's law is obeyed in the concentration range 0.5-0.4 microg cm(-3). The yellowish Cu(II)-BDTSC complex in chloroform shows a maximum absorbance at 380 nm, with molar absorptivity and Sandell's sensitivity values of 1.63 x 10(4) dm3 mol(-1) cm(-1) and 0.00389 microg cm(-2), respectively. A repetition of the method is checked by finding the relative standard deviation (RSD) (n = 10), which is 0.6%. The composition of the Cu(II)-BDTSC complex is established as 1:1 by slope analysis, molar ratio and Asmus' methods. An excellent linearity with a correlation coefficient value of 0.98 is obtained for the Cu(II)-BDTSC complex. The instability constant of the complex calculated from Edmond and Birnbaum's method is 7.70 x 10(-4) and that of Asmus' method is 7.66 x 10(-4), at room temperature. The method is successfully employed for the determination copper(II) in pharmaceutical and environmental samples. The reliability of the method is assured by analyzing the standard alloys (BCS 5g, 10g, 19e, 78, 32a, 207 and 179) and by inter-comparison of experimental values, using an atomic absorption spectrometer.     

Effective thermal conductivity of water-saturated sintered powder-metal plates

An experimental apparatus and related procedures for the determination of the effective thermal conductivity of sintered powder-metal plates saturated with distilled water at temperatures in the range 20–150°C are discussed. The apparatus and procedures are applied to two samples of sintered powder-metal plates, one made of nickel 200 and the other of stainless steel 316, with porosities of 28.10 and 46.45%, respectively, and each of nominal dimensions 127 mm × 127 mm × 6.35 mm. The experimental results are compared with corresponding predictions yielded by several correlations available in the literature. The correlations based on experimental data for packed beds of spherical particles and also porous plates made of cold-pressed (but not sintered) particles of angular shapes do not apply well to sintered powder-metal plates. A new correlation, which is based on extensions of ideas contained in earlier works and provides improved predictions, is proposed.     

Physicochemical studies on hydrophobic PEO‐PPO‐PEO triblock copolymer micelles in SDS micellar environment

The shape, size, aggregation, hydration, and correlation times of water insoluble PEO‐PPO‐PEO triblock copolymer micelles with sodium dodecylsulfate (SDS) micelles were investigated using transport studies and dynamic light scattering technique. From the conductance of micellar solutions of the polymer in 25 mM SDS and 5 mM NaCl, the hydration of polymer micelles were determined using the principle of obstruction of electrolyte migration by the polymer. The asymmetry of the micellar particles of polymer and polymer‐SDS mixed micellar systems in 5 mM NaCl and their average axial ratios were calculated using intrinsic viscosity and hydration data obeying Simha–Einstein equation. Hydration number and micellar sizes were variable with temperature. The shape of the polymer micelles has been ellipsoidal rather than spherical. The micellar volume, hydrodynamic radius, radius of gyration, diffusional coefficients as well as translational, rotational and effective correlation times have been calculated from the absolute values of the axes. The partial molal volume of polymer micelles has also been determined and its comparison with the molar volume of pure polymer suggested a volume contraction due to immobilization of the water phase by the hydrophilic head groups of the polymer. The thermodynamic activation parameters for viscous flow favor a more ordered water structure around polymer micelles at higher temperatures. © 2007 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 2410–2420, 2007     

Inverse problems for a mathematical model of redox sorption

We consider a mathematical model of sorption that allows for external diffusion kinetics and a redox reaction. Two inverse problems are considered for this model, uniqueness is proved, and numerical solution methods are proposed. The efficiency of the numerical methods is investigated by computer experiments. __________ Translated from Prikladnaya Matematika i Informatika, No. 23, pp. 15–23, 2006.     

X-ray induced fluorescence spectrometry at grazing incidence for quantitative surface and layer analysis

Summary Single layers and layer systems on diverse substrates were measured by Total Reflection X-Ray Fluorescence (TXRF) spectrometry. The angular dependence of the fluorescence intensities at grazing incidence allows the elemental composition, density and thickness of the layers to be evaluated using model calculations.     

Unoccupied electronic states of epitaxial iron layers on Cu(100)

Inverse photoemission spectra were taken for thin epitaxial iron films on Cu(100). For a film thickness of eight monolayers the observed electronic states are characteristic for a fcc(100) surface. Thed-bands of iron show a ferromagnetic exchange splitting of 1.1 eV, considerably smaller than the bulk value of 1.8 eV, which we observe for film thicknesses above 18 monolayers.     

Thermoplastic polymers quality control

A technique is proposed for improving the accuracy of the heat of fusion of semicrystalline polymers by DSC. The results of three commercially available instruments are compared.