Structural,optical and photoelectron spectroscopic studies of nano/micro ZnO:Cd rods synthesized via sol-gel route

Thin films of cadmium doped zinc oxide rod like microstructure have been synthesized by a very simple sol-gel dip coating technique. Sols were prepared from hydrated zinc oxide precursor and 2-methoxyethanol solvent with monoethanolamine as a sol stabilizer. XRD pattern confirmed the hexagonal wurtzite structure of the deposited ZnO films. Surface morphologies of the films have been studied by a scanning electron microscope and an atomic force microscope, which confirmed that the films are composed of densely packed randomly oriented nano/submicron rods with diameter in the range 300–400 nm having various lengths. We proposed a possible growth mechanism for this rodlike structure. X-ray photoelectron spectroscopic study was used to determine the binding energies and the Zn 2p3/2, Cd 3d5 and O 1s peaks in the XPS spectra were located at 1021.08 eV, 404.6 eV and 529.8 eV respectively, which confirmed the Cd doping in ZnO. Cadmium content in the film was estimated both from energy dispersive X-ray analysis and XPS measurement. Band gap energy determined from optical transmittance spectra systematically varied from 3.28 eV to 3.15 eV for 0% to 5.6% of Cd doping. Urbach parameter determined from the band tail of the transmittance spectra showed that it increased with doping percentage and this parameter for a fixed cadmium doping level decreased with increase of temperature.     

Determination of 99Tc in bentonite clay samples using inductively coupled plasma mass spectrometry

A method was developed for the determination of ⁹⁹Tc at low concentrations in clay samples. The chemical treatment of the samples prior to chemical separation and analysis comprised leaching with sulphuric acid/ sodium bromate. After leaching, pertechnetate was extracted with Alamine-336/chloroform and then back-extracted into nitric acid. Detection was carried out using inductively coupled plasma mass spectrometry, ICP-MS. The instrumental detection limit was 0.45 pg/mL, which corresponds to 0.28 mBq/mL. With the use of a desolvating nebuliser, the detection limit was lowered by about a factor of five. The results were compared with a method using radiometric detection. Received: 16 April 1998 / Revised: 12 June 1998 / Accepted: 16 June 1998     

Voltammetric determination of 2-mercaptobenzothiazole in a mixture of ethylene glycol + water

Voltammetry employing rotating platinum and disc electrodes proves to be a suitable method for determining 2-mercaptobenzothiazole in the mixture ethylene glycol + water in the relatively large concentration range 0.005–1% (i.e. approximately 3 × 10^?4 ?6 × 10^?2 mol 1^?1).The shapes of the voltammetric curves of thiol on both electrodes are essentially identical. During the gradual anodic polarization of the electrodes thiol is oxidized to a disulphide and adsorbed on the electrode surface, which is not accompanied by a conspicuous peak. In the more positive regions of the potential the next anodic process takes place:

manifested by the formation of an anodic peak.The calibration graphs are based on the linear dependence of the current of anodic peak I_A on the thiol concentration.In all cases the use of the rotating platinum electrodes proves to be more advantageous. The results are time reproducible, the determination requires no treatment of samples and requires approximately 15 min.     

Neutron activation analysis of neonate and maternal hair sampled in areas with different levels of pollution

Instrumental neutron activation analysis has been performed on human head hair of newborns and mothers sampled in two areas with a different level of environmental exposure. The group of neonates from the exposed area (polluted by thermal power plants burning brown coal and by chemical industry) has exhibited higher levels of several trace elements in hair, e.g. Se, Zn, Hg and Sb in comparison with the control group. Moreover, the mean concentrations of Se, Hg, Zn and Br in neonate hair have been found to be higher than in mothers hair. Although the study revealed statistically significant differences in the composition of neonate hair sampled in areas with different levels of environmental exposure, the differences are relatively small. Only a thorough long-term study both with environmental and medical observations can prove a direct connection of the elevated levels of some trace elements in neonate hair with the higher frequency of mental diseases of children living in the exposed area.     

Eine indirekte polarographische Methode zur Bestimmung von β-Diäthylamino-äthyl-(o-benzyl-phenyl)äther-hydrochlorid (AH3)

Zusammenfassung Eine indirekte polarographische Methode zur Bestimmung von AH₃ wird beschrieben, das zu diesem Zweck mit rauchender Salpetersäure nitriert wird. Die optimalen Bedingungen für die Nitrierung und Reduktion an der Quecksilbertropfelektrode werden mitgeteilt. Zur Aufstellung einer Eichkurve wird ein scharfes Maximum der Derivativkurven beim Halbstufenpotential –0,60 V benutzt.

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Summary An indirect polarographic method for determining AH₃ is described, that for this purpose is nitrated with fuming nitric acid. The optimal conditions for the nitration and reduction on the mercury dropping electrode are stated. A sharp maximum of the derivative curves at the half-potential –0.60 V was used to set up a calibration curve.

     

Kinetic Spectrophotometric Determination of Metoprolol Tartrate in Commercial Dosage Forms

A kinetic spectrophotometric method has been described for the determination of metoprolol tartrate in commercial dosage forms. The procedure is based on the reaction of the drug with 1‐chloro‐2, 4‐dinitrobenzene (CDNB) in dimethylsulfoxide (DMSO) at 100 ± 1 °C. The reaction is investigated by measuring the change in absorbance with time at 420 nm. Fixed‐time (ΔA) and equilibrium methods are chosen for obtaining the calibration curves. Both calibration curves were found to be linear over the concentration range of 5‐60 μg mL^?1. The regression analysis of calibration data resulted in the linear regression equations of ΔA = ?1.608 × 10^?4 + 3.96 × 10^?3 C and A = 7.31 × 10^?4 + 1.90 × 10^?2 C for fixed time (ΔA) and equilibrium methods, respectively. The limit of detection (LOD) for fixed time and equilibrium methods are 1.16 and 0.415 μg mL^?1, respectively. The method has been successfully applied to the quantitation of metoprolol tartrate in commercial dosage forms. Statistical comparison of the results shows that there is no significant difference between the proposed methods and El‐Ries's spectrophotometric method.     

The stability of some metal EDTA, DTPA and DOTA complexes: Application as tracers in groundwater studies

Studies of the stability of various metal EDTA, DTPA and DOTA complexes in order to evaluate their applicability as non-sorbing tracers have been performed. In laboratory tests, the stability generally increases for the individual metal ions in the EDTA<DTPA<DOTA order. For most metal ions, the same trend can be observed for the thermodynamic stability constants. In the in situ experiment, various metal EDTA tracers were used in very low concentrations; YbEDTA⁻, for example had a breakthrough and recovery which were very similar to the non-sorbing tracers used. According to the extremely low tracers concentrations used, thermodynamic data indicate that all metal EDTA tracers should have been decomplexed as a result of the competition with the naturally occurring cations in the groundwater. This was not found, which indicates that the decomplexation rate and sorption mechanism are important in estimating the applicability of the metal complexes as tracers. The DOTA complexes of elements in the middle of the lanthanide series have indicated high stability in the laboratory tests and therefore appear to be good candidates as non-sorbing tracers. However, in contrary to the metal EDTA, tracers, the DOTA complexes of La³⁺ and Lu³⁺ seemed to be slightly delayed in the in situ experiment.     

Symmetric anti-eigenvalue and symmetric anti-eigenvector

The idea of symmetric anti-eigenvalue and symmetric anti-eigenvector of a bounded linear operator T on a Hilbert space H is introduced. The structure of symmetric anti-eigenvectors of a self-adjoint and certain classes of normal operators is found in terms of eigenvectors. The Kantorovich inequality for self-adjoint operators and bounds for symmetric anti-eigenvalues for certain classes of normal operators are also discussed.     

Electrical properties of transparent carbon nanotube networks prepared through different techniques

Ultra‐thin, optically transparent and electrically conducting films of pure carbon nanotubes (CNTs) are widely studied thanks to their promise for broad applications. In the present work, we study and compare different deposition techniques for the production of these networks: dip‐coating, spray‐coating, vacuum filtration and electrophoretic deposition on a quartz glass using single‐walled carbon nanotubes (SWCNTs) produced by the HiPCo method. In order to optimize the networks, besides the various deposition techniques we also investigate how the optical and electrical properties vary if the networks are fabricated from different CNTs, all synthesized by the CVD method: SWCNTs, DWCNTs and MWCNTs. As the main criteria for evaluating the quality of these CNT networks we measure the electrical surface resistance at a certain optical transmittance and correlate it to the morphology (homogeneity and roughness) of the networks. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)