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–inorganic compound of {[NiL][Co(NCS) 4 ]} n , where L denotes 5,12-dimethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene. The compound belongs to a group of so-called molecular magnets, i.e. a modern material which can compete with the conventional inorganic magnets

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Abstract  

In situ leaching of uranium ores with sulfuric acid during active uranium mining activity on the Gessenheap has caused longstanding environmental problems of acid mine drainage and elevated concentrations of uranium. To study there remediation measures the test site Gessenwiese, a recultivated former uranium mining heap near Ronnenburg/East Thuringia/Germany, was installed as a part of a research program of the Friedrich-Schiller University Jena to study, among other techniques, the phytoremediation capacity of native and selected plants towards uranium. In the first step the uranium speciation in surface seepage and soil pore waters from Gessenwiese, ranging in pH from 3.2 to 4.0, were studied by time-resolved laser-induced fluorescence spectroscopy (TRLFS). Both types of water samples showed mono-exponential luminescence decay, indicating the presence of only one major species. The detected emission bands were found at 477.5, 491.8, 513.0, 537.2, 562.3, and 590.7 nm in case of the surface water samples, and were found at 477.2, 493.2, 513.8, 537.0, 562.4, and 590.0 nm in case of the soil water samples. These characteristic peak maxima together with the observed mono-exponential decay indicated that the uranium speciation in the seepage and soil pore waters is dominated by the uranium (VI) sulfate species UO2SO4(aq). Due to the presence of luminescence quenchers in the natural water samples the measured luminescence lifetimes of the UO2SO4(aq) species of 1.0–2.6 μs were reduced in comparison to pure uranium sulfate solutions, which show a luminescence lifetime of 4.7 μs. These results convincingly show that in the pH range of 3.2–4.0 TRLFS is a suitable and very useful technique to study the uranium speciation in naturally occurring water samples.

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Abstract

The non-isothermal kinetics of mullite formation from both non-activated and mechanically activated kaolinite have been studied by differential thermal analysis (DTA). Kaolinite was mechanically activated in a planetary mill, while amorphization in the structure was studied by X-ray diffraction analysis. It was established that the mechanical activation especially affected the loss of structural water. The activation energies depending on the conversion for mullite formation have been calculated from the DTA curves by using the non-isothermal method of Coats and Redfern at heating rates of 5, 10, 15, and 20 °C min−1. The mechanical activation and amorphization of the kaolinite brings to the formation of mullite at a lower heating temperature.

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Abstract

The non-isothermal kinetics of mullite formation from both non-activated and mechanically activated kaolinite + alumina ceramic system have been studied by differential thermal analysis (DTA). The mixture of kaolinite and alumina was activated mechanically in a planetary mill, while amorphization in the kaolinite and alumina structure was studied by X-ray diffraction analysis. The activation energies depending on the conversion for mullite formation have been calculated from the DTA curves by using the non-isothermal method of Coats and Redfern at heating rates of 5, 10, 15, and 20 °C min−1. The mechanical activation of the kaolinite and alumina mixture resulted in the decrease in activation energy values for mullite formation.

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Abstract

The reduction kinetics with CO of the 12-molybdophosphoric—HPMo, 1-vanado-11-molybdophosphoric—HPVMo acids and their salts with NH4 +, K+ and Cs+ cations were studied for reduction/reoxidation cycles with mixtures of CO:Ar and O2: Ar, by means of “in situ” UV–Vis–DRS measurements. The reflectivity versus time curves registered during the reduction/reoxidation processes for the HPMo and HPVMo and its salts with NH4 +, K+ and Cs+ cations, at the constant wavelength of 620 nm and different reaction temperatures between 523 and 623 K, were processed as the Kubelka–Munk function versus time. The linear shape of Kubelka–Munk function versus time curves for the reduction process suggests apparent zeroth order kinetics and it was used for the calculation of apparent activation energy. The kinetic compensation effect between the apparent activation energy and the pre-exponential factor was observed. The Kubelka–Munk function versus time curves for the reoxidation process consist of two steps, the first with a very fast reaction rate and the second with a slow reaction rate. An explanation for their shape is proposed. The heteropoly oxomolybdates reach a degree of reoxidation higher than heteropoly compounds containing vanadium together with molybdenum.

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Journal of Radioanalytical and Nuclear Chemistry
Authors: Ian Hoffman, Kurt Ungar, Marc Bean, Jing Yi, René Servranckx, Calin Zaganescu, Nils Ek, Xavier Blanchard, Gilbert Le Petit, Guy Brachet, Pascal Achim, and Thomas Taffary

Abstract  

Radioxenon concentration data collected at International Noble Gas Experiment (INGE) monitoring sites in the Northern Hemisphere are demonstrably impacted by emissions from medical isotope (MI) production facilities at Chalk River (CRL), Ontario and Fleurus, Belgium [Saey, J Environ Radioact 100(5):396–406, 2009]. Temporary cessation at these European MI facilities in the latter half of 2008 allowed an opportunity to assess the relative impact of distant MI facilities at INGE monitoring stations. In particular, the concentration distributions at the measurement sites and calculated sensitivities to the putative emission locations through atmospheric transport modelling (ATM) of meteorological Source Receptor Sensitivity (SRS) computations were used to study MI impacts.

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Abstract  

[NiL3]X2 (where L=N-phenylethane-1,2-diamine and X=I and ClO4 ), [NiL2X2] (X is Cl, Br, NCS, 0.5SO4 2− or 0.5SeO4 2−) and [NiL2(H2O)2](NO3)2 have been synthesized from solution and their thermal study has been carried out in the solid phase. [NiL2Cl2] upon heating undergoes irreversible endothermic phase transition (142–152C, ΔH=0.35 kJ mol−1) without showing any visual colour change. This phase transition is assumed to be due to conformation changes of the diamine chelate rings. NiLCl2 and NiL2.5I2 have been prepared pyrolytically from [NiL2Cl2] and [NiL3]I2 respectively in the solid state. [NiL2(H2O)2](NO3)2 upon heating undergoes deaquation-anation reaction without showing any visual colour change. [NiL2X2] (X is Cl, Br, NCS), [NiL2(H2O)2](NO3)2 and [NiL2(NO3)2] possess trans-octahedral configuration, whereas, [NiL2X2] (X is 0.5SO4 2− or 0.5SeO4 2−) are having cis-octahedral configuration. Amongst the complexes, only NiLCl2 shows unusually high (5.1 BM at 27C) magnetic susceptibility value.

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Ni(II) Schiff base complexes of compositions NiL ROH (R=Me, Et, Pr, i-Pr) and NiL′·ROH (R=Me, Et, Pr, i-Pr, Bu) were prepared and investigated by methods of thermal analysis. The thermal decomposition of NiL·ROH led to NiL (plateau in TG curve), whereas NiL′·ROH underwent a similar decomposition only in an inert atmosphere (N2); thermal decomposition in air involved alcohol fragmentation, followed by a mass increase due to oxidation by atmospheric oxygen. The activation energy of alcohol fragmentation was calculated.

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Pyridine-type complexes of transition metal halides

IV. Preparation and thermal studies on some new complexes of nickel(II)-halides formed with 2-, 3-, and 4-methyl-pyridines

Journal of Thermal Analysis and Calorimetry
Authors: G. Liptay, G. Kenessey, and P. Bukovec

Abstract  

Formation of nitrogen ligated complexes of types NiL6X2, NiL4X2, NiL2X2 and NiL1X2 (whereL=pyridine, 2-, 3- and 4-methyl-pyridine andX=F, Cl, Br, I) have been studied by traditional preparative methods, i.e. from solutions and by solid-gas phase chemisorption. Quaternary mixed complexes were obtained by chemisorption from heated intermediates. The complexes thus formed were further analysed by simultaneous TG-DTG-DTA. Effects of the ligands on stoichiometry and thermal properties of the complexes are discussed.

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