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1.
On‐line coupling of LC and ICP‐MS has been used for fractionation and detection of species of Cu, Fe, I, Se and Zn in human serum. It has been shown that anion exchange chromatography provided better separation capability (both intra‐ and inter‐element) than size‐exclusion chromatography. The mobile phases for ion exchange chromatography consisted of Tris–HNO3 buffer and ammonium salt (nitrate, acetate or formate). Formate was found to be the best mobile phase counter ion, enabling good chromatographic separation, and is acceptable for mass spectrometry too. The quantitative evaluation of element concentrations adhering to individual fractions was performed by the peak area normalization method. The repeatability of results ranged from 3 to 15% (depending on the element concentration level) and represented the main part of the result uncertainty. The accuracy of Cu and Zn fraction determinations was confirmed by comparison with the isotope dilution technique. Copyright © 2006 John Wiley & Sons, Ltd.  相似文献   
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The stoichiometric reactions of trimethylaluminum with 2,6‐(MeOCH2)2C6H3OH (LH) revealed compounds L3Al ( 1 ) and L2AlMe ( 2 ). On the other hand reaction of 1 equiv. of LH with trimethylaluminum did not lead to the formation of complex LAlMe2 ( 3 ), rather 2 together with Me3Al were observed as a result of a disproportionation of 3 . Compounds 1 and 2 were characterized by elemental analysis, 1H and 13C NMR spectroscopy and in the case of 1 by X‐ray diffraction. Derivative 2 underwent transmetalation with Ph3SnOH, giving LSnPh3 ( 4 ) as the result of a migration of ligand L from the aluminum to the tin atom. The identity of 4 was established by elemental analysis, 1H, 13C and 119Sn NMR spectroscopy and 1H, 119Sn HMBC experiments. The system 2 and B(C6F5)3 in a 1:1 molar ratio was shown to be active in the polymerization of propylene oxide and ε‐caprolactone. Copyright © 2007 John Wiley & Sons, Ltd.  相似文献   
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Zusammenfassung Durch spektrophotometrische Messungen in Dimethylformamid (DMF) werden die Koordinationsformen [CuCl]+ und [CuCl3] sowie [NiCl]+, [NiCl3] und [NiCl4]2– nachgewiesen. Bei Nickel(II)-chlorid und Kupfer(II)-chlorid wird Autokomplexbildung diskutiert. Die Solvate [Cu(DMF)4] (ClO4)2 und [Ni(DMF)6] (ClO4)2 werden isoliert.Im Zuge der Untersuchungen über Chlorokomplexe von Ionen der Übergangsmetalle1, 2 in nichtwäßrigen Lösungsmitteln wurden die Spektren der Lösungen von Kupfer(II)- und Nikkel(II)-perchlorat inDMF in Gegenwart verschiedener Mengen Tetraäthylammoniumchlorid aufgenommen.Mit 5 Abbildungen  相似文献   
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The formation of slip bands is the main mechanism of cyclic deformation in pure Al. Their density, orientation and heights in polycrystalline Al were investigated during cycling. Types, sizes and densities of precipitates are responsible for the mode of cyclic deformation in AlCu4 pure alloy. In technical Al alloys intermetallic phases have detrimental effects on deformation homogeneity and largely govern the fatigue mechanism of the material and especially microcrack initiation.  相似文献   
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Amorphous precursors for PbZrO3 and PbTiO3 ceramics were prepared from lead acetate and the transition metaln-propoxide inn-propanol orn-butoxide inn-butanol and hydrolysed with an excess of water. According to GLC and TGA/EGA analyses, the type of alkoxide group influences distinctly the structure of heterometallic precursors, i.e., oxo or acetate bridging, and the amounts of hydroxyl and organic groups bound to the metal network. The local environments of metal atoms in the amorphous precursors were also studied by EXAFS. The analysis reveals that in Pb−Zr precursors alkoxide groups modify the coordination spheres of the zirconium atoms. Conversely, local environments of both lead and titanium atoms within the analysed range of 3.4 A depend weakly on the type of alkoxide used.  相似文献   
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The paper describes the results of investigations of the solar wind ions, carried out on board the high apogee Prognoz 7 and Prognoz 8 Earth's satellites with the aid of an SKS instrument (USSR) and a Monitor instrument (USSR-SSR). Behaviour of proton and that of components on the front of Earth's bow and interplanetary shock waves were compared by means of the energoanalysis and energy-mass analysis techniques. In several long-term periods of observation the solar wind heavy ions — oxygen, silicon and iron were determined. It enabled us to estimate the solar corona chemical composition and electron temperature.Presented at the 5th General Assembly IAGA/IAMAP August 5–17, 1985, Prague, Czechoslovakia.  相似文献   
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