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1.
Julia K Pruns Jens-Peter Vietzke Manfred Strassner Claudius Rapp Ulrich Hintze Wilfried A K?nig 《Rapid communications in mass spectrometry : RCM》2002,16(3):208-211
A new solvent-free sample preparation method using silver trifluoroacetate (AgTFA) was developed for the analysis of low molecular weight paraffins and microcrystalline waxes by laser desorption/ionization time-of-flight mass spectrometry (LDI-TOFMS). Experiments show that spectral quality can be enhanced by dispersing AgTFA directly in liquid paraffins without the use of additional solvents. This preparation mixture is applied directly to the MALDI probe. Solid waxes could be examined by melting prior to analysis. The method also provides sufficiently reproducible spectra that peak area ratios between mono- and bicyclic alkane peaks indicated variations in the cycloalkane content of paraffin samples. Dehydrogenation of hydrocarbons observed during the desorption/ionization process was studied by analysis of alkane standards. 相似文献
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A high-performance thin-layer chromatographic (HPTLC) method is described for the determination of tributyltin compounds (bis(tri-n-butyltin) oxide, TBTO, and tri-n-butyltin naphthenate, TBTN) and their degradation products (dibutyltin and monobutyltin compounds). The organotin compounds are extracted from wood with ethanol containing 0.5% (v/v) of hydrochloric acid and the separation of the defferent kinds of organotin compounds is achieved by thin-layer chromatography. The sample spots are measured using a scanning densitometer after decomposing the organotin compounds to inorganic tin by ultraviolet irradiation and visualization of the spots with pyrocatechol violet. Applications of the method to detection and quantification of organotin compounds in preservative solutions, in recently impregnated wood, and in wood samples from five-year-old window frames are described. 相似文献
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Ternary Halides of the A3MX6 Type. II. The System Ag3?xNaxYCl6: Synthesis, Structures, Ionic Conductivity . The influence of the substitution of Ag+ by Na+ ions on the crystal structure and the ionic conductivity of Ag3YCl6 (stuffed LiSbF6-type structure) has been investigated. The system Ag3?xNaxYCl6 forms a complete solid solution. The stuffed LiSbF6-type structure is stable for all compositions. For compounds with Na+ contents of x > 1.67, the cryolite-type structure is observed as the high-temperature form. The transition temperature decreases steadily with increasing Na+ content. The “end member” phase Na3YCl6 transforms at 243 K from the monoclinic cryolite-type structure to the stuffed LiSbF6-type structure (trigonal, R3 ; a = 697.3(1), c = 1 868.4(14) pm, Z = 3; R = 0.094; Rw = 0.069). The crystal structures of Ag1.3Na1.7YCl6 (trigonal, R3 ; a = 691.5(2), c = 1 853.7(6) pm, Z = 3; R = 0.099, Rw = 0.081) and AgNa2YCl6 (trigonal, R3 ; a = 691.7(1), c = 1 853.9(5) pm, Z = 3; R = 0.099, Rw = 0.064) have also been determined. Both chlorides crystallize like Ag3YCl6 and Na3YCl6-I in the stuffed LiSbF6-type structure. The monovalent cations, Ag+ and Na+, are distributed over the five octahedral voids that are occupied by the Ag+ ions alone in Ag3YCl6. The ionic conductivity for compounds within the solid solution Ag3?xNaxYCl6 decreases with increasing Na+ content. The values for Na3YCl6 (σ = 1 · 10?6 Ω?1 cm?1 at T = 500 K) are by 2.5 to 3.5 orders of magnitude smaller than those for Ag3YCl6 (σ = 6 · 10?4 Ω?1 cm?1 at T = 500 K). 相似文献
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Let k be a field and let Λ be an indecomposable finite dimensional k-algebra such that there is a stable equivalence of Morita type between Λ and a self-injective split basic Nakayama algebra over k. We show that every indecomposable finitely generated Λ-module V has a universal deformation ring and we describe explicitly as a quotient ring of a power series ring over k in finitely many variables. This result applies in particular to Brauer tree algebras, and hence to p-modular blocks of finite groups with cyclic defect groups. 相似文献
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Freia Ruegenberg Dr. Markus Seibald Dr. Dominik Baumann Dr. Simon Peschke Dr. Frauke Philipp Prof. Dr. Hubert Huppertz 《Chemistry (Weinheim an der Bergstrasse, Germany)》2021,27(45):11701-11706
In order to expand the field of alkali lithosilicates, a new representative of the substance class with a previously unknown structure type was found based on solid-state synthesis. The novel compound with the sum formula Rb[Li5Si2O7] crystallizes in the orthorhombic space group Pbcm (no. 57) with a=7.6269(3), b=9.5415(4), and c=9.4095(3) Å by means of single-crystal X-ray diffraction. The structure consists of a highly condensed lithosilicate framework, built up of corner- and edge-linked [LiO4]-tetrahedra and [Si2O7]-units, and the rubidium ions aligned in channels. Suitable crystals of the material were obtained using sealed tantalum ampoules as reaction tube at a temperature of 750 °C. The new compound was further characterized via powder diffraction, Rietveld analysis, and EDX measurements. At first glance, Eu2+-doped Rb[Li5Si2O7] reveals an intense green luminescence. In-depth crystal analysis shows that a core-shell formation is present even for apparently high quality single-crystals. As a minority phase, the known green phosphor RbLi[Li3SiO4]2:Eu2+ is the origin of the luminescence, representing a tiny core inside of the particles surrounded by a large matrix of transparent Rb[Li5Si2O7] dominating the single-crystal diffraction pattern. 相似文献
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