Bestimmung von Mikromengen Schwefel nach Aufspaltung des S8-Ringes in Indium-, Blei-, Antimonund Wismutsulfiden mit Hilfe einer induzierten Reaktion von Natriumazid mit Jod

Zusammenfassung Die Bestimmungsmethode für Mikromengen elementaren, in Sulfiden enthaltenen Schwefels mit Natriumazid und Jod wurde modifiziert. Der Analyse geht die Aufspaltung des S₈-Ringes voraus, die man dank der nukleophilen Wirkung von N₃ ^– in DMF-Lösung erreicht. Diese Methode wurde auf die Bestimmung des Schwefels in Indium-, Blei-, Antimon- und Wismutsulfid angewandt. Sie ist einfach und empfindlich. Ihre Fehlergrenze liegt bei ± 4%.

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Determination of microamounts of sulfur after cleavage of the S₈ king in indium, lead, antimony and bismuth sulfides by means of an induced reaction of sodium azide with iodine

Summary The determination of microamounts of elemental sulfur contained in sulfides using sodium azide and iodine was modified. The analysis was preceded by cleavage of the S₈ ring, which is achieved by virtue of the nucleophilic action of N₃ ^– in DMF solution. This method was applied to the determination of sulfur in indium, lead, antimony and bismuth sulfides. It is simple and sensitive. Its limit of error is ±4%.

     

Sticking probability for oxygen adsorption and readsorption on thin iron films

Sticking probability for oxygen adsorption on thin iron films and readsorption on surface sites liberated due to incorporation of the adsorbate adatoms below the surface during thermal treatment has been studied by means of the Wagener flow method. Sticking probability for oxygen adsorption on oxidized thin iron films has also been measured for comparison.

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Reprint of: Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological,pharmaceutical and environmental samples

The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds’ feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5–8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.     

The umpolung of substituent effect in nucleophilic aromatic substitution. A new approach to the synthesis of N,N-disubstituted melamines (triazine triskelions) under mild reaction conditions

By the umpolung of substituent effect 1,3,5-triazines substituted with three dialkylamino groups were prepared under mild reaction conditions by treatment of cyanuric chloride with tertiary amines. Quaternary N-triazinylammonium salts were identified as reactive intermediates activating the triazine ring and strongly promoting the persubstitution of all chlorine atoms. The final degradation of intermediate N-triazinylammonium chlorides proceeded at room temperature or in boiling dichloromethane spontaneously within irreversible evolution of appropriate chloroalkane.     

Nucleoside-boron cluster conjugates - Beyond pyrimidine nucleosides and carboranes

General methods for the synthesis of new purine and pyrimidine nucleosides modified with borane clusters and metallacarborane complexes are presented. They include: (1) attachment of carborane modification at 2′ position of nucleoside via formacetal linkage formation, (2) tethering of the metallacarborane group at nucleobase part of the nucleoside via dioxane ring opening in oxonium metallacarborane, carborane or dodecaborate derivatives, and (3) ‘‘click” chemistry approach based on Huisgen 1,3-dipolar cycloaddition. Proposed methodologies extend the range of nucleoside-boron cluster conjugates available and open new areas for their applications.     

Thermal degradation of copolymers based on selected alkyl methacrylates

The thermal stability and thermal degradation of copolymers based on selected alkyl methacrylates at temperatures between 250 and 400?°C have been studied using pyrolysis?Cgas chromatography. The type and composition of thermal degradation products gave useful information about the mechanism of pyrolysis of copolymers synthesized by using typical commercially available alkyl methacrylates. It was observed that the main thermal degradation products from alkyl methacrylate copolymers are monomers of alkyl methacrylates using by synthesis. Other pyrolysis by-products formed during thermal degradation were carbon dioxide, carbon monoxide, methane, ethane, methanol, ethanol, and propanol-1.     

Solid phase synthesis of two muramyl pentapeptide derivatives

Solid phase peptide synthesis (SPPS) of two selected muramyl pentapeptide derivatives is described. The simplicity of removing the protecting groups via one-step deprotection and cleavage from the resin is the biggest advantage of SPPS. Using this method, two muramyl pentapeptide derivatives, D-MurN₃-L-Ala-D-iGlu-L-Lys-D-Ala-D-Ser (5) and D-MurN₃-L-Ala-D-iGlu-L-Lys-D-Ala-D-Ala (6), were obtained. Their chemical structures were confirmed by high-resolution mass spectrometry (HRMS) and nuclear magnetic resonance (NMR) spectroscopy. To determine the absolute configuration of the carbon atom in the side chain of the muramic acid derivative, single-crystal X-ray diffraction measurements were recorded.     

Homo- and hetero-nuclear chromium(III) complexes with natural ligands. Part 2. Oxo- and hydroxo-bridged chromium(III)/vanadium(V) species

Six new heteropolynuclear chromium(III)/vanadium(V) complexes with natural ligands: glycine, glutaminic, nicotinic and asparginic acids, have been isolated and physicochemically characterised. The complexes have been analysed using spectroscopic (diffuse reflectance u.v.–vis., i.r.), magnetic methods and by FAB mass spectra. Spectral analyses with the digital filter and band deconvolution methods are presented. Additionally, preliminary toxicity studies have been performed.     

Dynamic Light Scattering and NMR Studies of Napin

We analyze the structure of napin (BngNAP1), a storage protein (m.w. 14.5 kDa) from Brassica napus. On the basis of the results of ¹H NMR spectroscopy and dynamic light scattering (DLS) studies, the overall shape and secondary structure of the molecule are estimated.