Regional elemental signatures related to combustion of lignites

In ambient air, arsenic to selenium ratio (As/Se) is generally found to be less than 1, except in areas influenced by specific point sources, such as Cu smelters. However, the annual average of this ratio is found to be much higher than unity in Turkey. This finding is rather unique and may provide a marker for air masses influenced by the coal-related emissions in Turkey. This revised version was published online in August 2006 with corrections to the Cover Date.     

Synthesis of Functionalized (2-Thienylcarbonyl)thiazoles and 4-(2-Thienyl)pyridines by Reaction of (2-Thienylcarbonyl)thioacetanilides and their Enamine Derivatives

Summary. The condensation of two molecules of 2-(2-thienylcarbonyl)thioacetanilides catalyzed by piperidine yielded thiazole derivatives as confirmed by X-ray crystal structure analysis. The reaction of malononitrile with 3-morpholino-3-(2-thienyl)acrylic acid thioanilides furnished 6-amino-1-aryl-4-(2-thienyl)-1,2-dihydro-2-thioxopyridine-5-carbonitriles. A similar reaction of malononitrile with 3-morpholino-3-(2-thienyl)acrylic acid anilides provided 2-oxopyridine-5-carbonitriles.     

Radionuclides in a sediment trap and bottom sediment samples from the eastern Turkish coast of the Black Sea

Summary Radionuclide (¹³⁷Cs, ²³⁸U, ²³²Th and ⁴⁰K) concentrations were determined in a sediment trap and bottom sediment samples collected from a station at the eastern Turkish coast of the Black Sea. The specific activity of the ¹³⁷Cs radionuclide in the settling particles ranged from 0.04±0.01 to 0.10±0.02 Bq^. g^-1dry weight. The calculated flux rate of the ¹³⁷Cs was between 0.37 and 2.59 Bq^. m^-2. d^-1in the sampling periods of 2002 and 2003. The ¹³⁷Cs concentration in the bottom sediment profile were between 0.039±0.013-9.083±0.017 Bq^. g^-1dry weight in the same station. The vertical profile of the radionuclides suggests that they have little mobility during the 17 years after the Chernobyl accident.     

Elimination of bremsstrahlung in activation analysis by the deflection of β-particles in a magnetic field

The structureless background at X-ray and low energy -ray region, resulting from bremsstrahlung due to the stopping of -radiations, causes serious problems in nuclear spectroscopy. In this study, in order to reduce the background and therefore to increase the sensitivity of the nuclear analytical technique and the number of elements observable, a methodology is developed to deflect the -particles by a magnetic field. The experimental setup consists of a permanent magnet /1 kG/, Ge/Li/ solid-state detector, and multichannel analyzer.     

Leaching of uranium with the H2O2-Na2SO4-H2SO4 (HSS) system and the efficiency of Acigol Lake water

The applicability of a new leaching method, the HSS (H₂O₂-Na₂SO₄-H₂SO₄) system, in the extraction of uranium from Saricaolu-Bergama Region low grade ore, and the efficiency of Acigol Lake (Denizli)-Turkey water as a natural source of Na₂SO₄ has been investigated. The effect of H₂SO₄ concentration, temperature, leaching time, H₂O₂ and Na₂SO₄ concentrations and the amount of Acigol Lake water on the extraction of uranium was examined. HSS was found suitable for the extraction of uranium from Saricaolu-Bergama Region samples and it was observed that the acid consumption could be decreased by adding Na₂SO₄.     

Spectrothermal studies of 1,10-phenanthroline complexes of Co(II), NI(II), Cu(II) and Cd(II) orotates

The 1,10-phenanthroline (phen) complexes of Co(II), Ni(II), Cu(II) and Cd(II) orotates were synthesized and characterized by elemental analysis, magnetic susceptibility, spectral methods (UV-vis and FTIR) and thermal analysis techniques (TG, DTG and DTA). The Co(II), Ni(II), Cu(II) and Cd(II) ions in diaquabis(1,10-phenanthroline)metal(II) diorotate octahedral complexes [M(H₂O)₂(phen)₂](H₂Or)₂·nH₂O (M=Co(II), n=2.25; Ni(II), n=3; Cu(II) and Cd(II), n=2) are coordinated by two aqua ligands and two moles of phen molecules as chelating ligands through their two nitrogen atoms. The monoanionic orotate behaves as a counter ion in the complexes. On the basis of the first DTG_max, the thermal stability of the hydrated complexes follows the order: Cd(II), 68°C 68°C     

Determination of the complex formation constants for some water-soluble polymers with trivalent metal ions by differential pulse polarography

The formation of metal complexes between water-soluble polymers, poly(vinyl alcohol) [PVA], poly(N-vinylpyrrolidone) [PVP], poly(acrylamide) [PAAm] and poly(ethylene oxide) [PEO] with trivalent metal ions, Fe³⁺, Cr³⁺, and V³⁺ were studied by using differential pulse polarography (DPP). The general experimental observation is the shift of totally reversible reduction peaks (M³⁺+Hg+e^–M²⁺+Hg) towards more negative potentials when the complexing water-soluble polymers are added to the solution of trivalent metal ions. The negative shift in potential permitted the determination of complex formation constants (K_f) between trivalent metal ions and water soluble polymers. The complex formation constants for Fe³⁺, Cr³⁺, and V³⁺ ions with these polymers increased in the order of V³⁺>Cr³⁺>Fe³⁺.     

Sampling procedure and a radio-indicator study of mercury determination in whole blood by using an AMA 254 atomic absorption spectrometer

A sampling procedure appropriate for the determination of mercury in whole blood was tested by using both inactive controls and a ¹⁹⁷Hg mercury radio-indicator. To exclude the influence of the instrumental device (an AMA 254 single-purpose mercury atomic absorption spectrometer) on the determination of mercury in whole blood, the function of the instrument was checked by using rat blood with metabolised ¹⁹⁷Hg. The measurement procedure was found to be free of errors. However, the study showed that the material used for the sampling vessels is a crucial parameter for obtaining accurate analytical results. The stability of solutions and samples was tested towards polyethylene (PE) and polypropylene (PP) vessels. PE displayed a time-dependent increase in the mercury content both in the samples and in the blood control material. The probable cause of this increase was direct contamination from the material of the vessel and/or diffusion of mercury from the environment through the vessel walls related to a strong complexing affinity of the sample matrix. This assumption was confirmed by supplying the vessels with the complexing agent Na₂EDTA (0.05 mol L^–1). Commercial PP vessels for blood sampling (Sarstedt S-Monovette Metall Analytik) did not give rise to statistically significant variations in mercury content in the samples and blood control material over a 30-day period.     

Electrochemical studies and square-wave voltammetric determination of fenofibrate in pharmaceutical formulations

The electrochemical reduction of fenofibrate at a hanging mercury drop electrode (HMDE) was investigated by cyclic voltammetry, square-wave voltammetry, and chronoamperometry. Different buffer solutions were used over a wide pH range (3.0–10.0). The best definition of the analytical signals was found in borate buffer (pH 9.0)–tetrabutylammonium iodide mixture containing 12.5% (v/v) methanol at –1.2 V (versus Ag/AgCl). According to cyclic voltammetric studies, the reduction was irreversible and diffusion controlled. The diffusion coefficient was 2.38×10^–6 cm² s^–1 as determined by chronoamperometry. Under optimized conditions of square-wave voltammetry, a linear relationship was obtained between 0.146–4.96 g mL^–1 of fenofibrate with a limit of detection of 0.025 g mL^–1. Validation parameters such as sensitivity, accuracy, precision, and recovery were evaluated. The proposed method was applied to the determination of fenofibrate in pharmaceutical formulations. The results were compared with those obtained by a published high-performance liquid chromatography method. No difference was found statistically.     

Evaluation of the redox properties and anti/pro-oxidant effects of selected flavonoids by means of a DNA-based electrochemical biosensor

Quercetin and rutin as well as catechin and epigallocatechin gallate were investigated, as widely distributed representatives of flavonols and flavanols, respectively, regarding their anti/pro-oxidant properties. The flavonoids are irreversibly oxidized at a dsDNA-modified screen-printed electrode within 0.368 to 0.449 V vs. SHE without binding to DNA. Using the DNA biosensor the detection scheme of a DNA prevention/degradation exploits the [Co(phen)(3)](3+) complex as an electrochemical DNA marker. Antioxidant activity of flavonoids was tested in a model cleavage mixture composed of 5 x 10(-7) mol L(-1) [Cu(phen)(2)](2+) as the catalyst, 1 x 10(-3) mol L(-1) ascorbic acid as the chemical reductant and atmospheric oxygen as the natural oxidant where reactive oxygen radicals are generated. The antioxidant activity increases with the concentration of flavonoids reaching a maximum where pro-oxidative behaviour becomes of importance. The pro-oxidant potency of flavonoids depends on the presence of atmospheric oxygen and follows the order quercetin>rutin>epigallocatechin gallate>catechin.