Thermal decomposition of N2H6GeF6 · H2O,isolation and characterization of intermediates

The thermal behaviour of N₂H₆GeF₆ · H₂O was investigated by TG, DTG and DTA measurements. The decomposition proceeded in three steps, in which anhydrous N₂H₆GeF₆ and N₂H₅GeF₅; were isolated and characterized by chemical analysis and vibrational spectroscopy. The X-ray powder photographs of the intermediates were indexed, namely, for N₂H₆GeF₆ on the basis of a monoclinic cell with a = 8.86(9), b = 9.29(2), c =7.40(0) Å, β = 85° and for N₂H₅GeF₅ on the basis of an ortrhorhombic cell with a = 8.43(5),b = 9.19(9), c = 7.43(6) Å.     

Delphinidin–Aluminum(III) Complexes in Aqueous and Non-Aqueous Media: Spectroscopic Characterization and Theoretical Study

Summary. The study of delphinidin complexation with trivalent aluminum in acidic aqueous buffered (pH 3.0 and 3.8) and methanolic solutions was performed utilizing electronic absorption spectroscopy and quantum chemical calculations. In its structure delphinidin possesses several chelating sites in competition towards aluminum(III). Molar ratio plots denoted the formation of only one aluminum(III):delphinidin complex of stoichiometry of 1:1 in both investigated media. Semiempirical calculations, performed at the restricted HF AM1 level, enabled the determination of the structural features of free delphinidin and structural modifications caused by chelation of aluminum(III). Considering the pigment molecular structure and the results of the theoretical calculations it is possible to equally implicate C3′–C4′ and C4′–C5′ hydroxyl groups as those with the predominant chelating power.     

Neighbouring group participation in formation of condensed azines. Formation of pyrazolo(3,4-b)pyrazines,isoxazolo(4,5-b)pyrazines and isothiazolo(5,4-b)pyridine

Pyrazine- and pyridinecarboxamidoximes with an amino, potentially tautomeric hydroxy or mercapto group inortho position could be transformed in the appropriate condensed azines. In this manner, representatives of pyrazolo(3,4-b)pyrazine, isoxazolo(4,5-b)pyrazine and isothiazolo(5,4-b)pyridine ring system were synthesized and some transformations investigated.Presented in part at the 8th International Congress of Heterocyclic Chemistry, Graz, 1981.     

Strukturanalyse organischer Sulfide mit Hilfe der Gras-Chromatographie

Zusammenfassung Eine Methode der Identifizierung von Alkyl- und Arylgruppen organischer Sulfide wurde ausgearbeitet, die die Spaltung dieser Stoffe mit Raney-Nickel zur gaschromatographischen Bestimmung der dabei entstandenen Kohlenwasserstoffe ausnützt.

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Summary A method was developed for identifying alkyl- and aryl groups of organic sulfides. The method employs the cleavage of these materials with Raney nickel for the gas chromatographic determination of the resulting hydrocarbons.

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Résumé On a mis au point une méthode d'identification des groupes alkylés et arylés des sulfures organiques exploitant la dissociation de ceux-ci par le nickel Raney pour le dosage par chromatographic en phase gazeuse des carbures d'hydrogène qui se forment.

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Die Autoren danken den Kollegen Dr.M. Veea, Ing.J. Petránek und Ing.J. Gaspari für die Überlassung von Proben organischer Sulfide.     

Collisional population of the 23 ∏ g state inK 2

We have measured the effect of potassium vapour pressure within the heat-pipe oven on the shape of the 2³ ∏ _g ?1³∑ _u ⁺ fluorescence induced by collision energy transfer from theC ¹∏ _u state which was optically excited by the 457.9 nm argon-ion laser line. The estimated cross section of that process is 300 Ų. The simulation of the diffuse band shape indicates a non-thermalised vibrational distribution in the 2³ ∏ _g state.     

Thermal properties of cyanatocopper(II) complexes with pyridine,bipyridine and phenanthroline

The thermal properties of cyanatocopper complexes with pyridine, bipyridine and phenanthroline are described in this paper. It was found that the thermal stabilities of the complexes were found to increase in the order pybipy2(NCS)₂ (L=pyridine and its methyl derivates) which are composed of the liberation of ligandsL and redox reactions of thiocyanate ligands with the central Cu(II) atom [1, 2]. The decomposition temperature of thiocyanate ligands depends on the properties of the ligandsL present in the coordination sphere. An analogous course of thermal decomposition was also observed for [Cu(bipy)₂(NCX)](NCX) (X=S or Se) [3]. For the phenanthroline complexes [Cu(phen)₂(NCX)₂] (X=S or Se) the thermal stability was found to increase significantly (by about 140C) and the decomposition stoichiometry was also changed [3].The present paper contains the results of thermoanalytical studies on bipyridine and phenanthroline cyanatocopper complexes, and a comparison of the thermal properties of pyridine cyanato and isothiocyanatocopper complexes.     

Photokilling Squamous Carcinoma Cells SCCVII with Ultrafine Particles of Selected Metal Oxides

The ability of ultrafine particles of TiO₂, WO₃ and iron-doped TiO₂ to kill cancer cells in the presence of UV irradiation was investigated. The best photokilling effect on carcinoma cells SCVII cultured in vitro showed iron-doped TiO₂ ultrafine particles synthesized by the sol-gel procedure with starting chemicals Ti(IV)-isopropoxide and anhydrous Fe(II)-acetate. It was found that a small particle size and high dispersity influenced citotoxicity and photocatalytic efficiency. The remarkable photokiling effect of highly iron-doped TiO₂ ultrafine particles (the molar ratio Fe/Ti = 0.136) in the presence of UV irradiation was observed. The influence of ultrafine metal oxide particles on the inhibition of cancer cell proliferation was measured using a ³H-thymidine incorporation test. The possible mechanism involved in the photokilling of carcinoma cells with ultrafine particles of selected metal oxides was discussed.     

Asymptotic and exponential decay in mean square for delay geometric Brownian motion

Applications of Mathematics - We derive sufficient conditions for asymptotic and monotone exponential decay in mean square of solutions of the geometric Brownian motion with delay. The conditions...     

Polarographische Bestimmung des Pyridoxols in pharmazeutischen Präparaten

Zusammenfassung Es wird eine neue polarographische Methode zur direkten Bestimmung des Pyridoxols in Injektionspräparaten und Tabletten beschrieben. Die ausgearbeitete Methode beruht auf der polarographischen Reduktion des Pyridoxolmoleküls im Milieu von Ammoniak-Ammoniumchlorid-Puffern und weiter auf der Bildung einer katalytischen Stufe des Pyridoxols in Veronalpuffern. Die polarographische Methode ist rascher und in manchen Fällen genauer und empfindlicher als die bisher in Gebrauch stehenden Methoden. Die Anwesenheit der in den Präparaten laufend vorkommenden Begleitstoffe des Pyridoxols stört nicht die polarographische Bestimmung. Die Methode kann auch zur Bestimmung des 3-Hydroxy-4-methoxymethyl-5-oxymethyl-2-methylpyridins benutzt werden, das ein Zwischenprodukt bei der Pyridoxolerzeugung ist.

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Summary A new polarographic method is described for the direct determination of pyridoxol in injection preparations and tablets. This method is based on the polarographic reduction of the pyridoxol in ammonia-ammonium chloride buffer medium and also on the formation of a catalytic stage of the pyridoxol in veronal buffers. The polarographic method is faster and in many cases more accurate and more sensitive than the methods now in use. The presence of the materials which always accompany the pyridoxol in the preparations does not interfere with the polarographic determination. The method can likewise be used for determining 3-hydroxy-4-methoxymethyl-5-oxymethyl-2-methylpyridine, which is an intermediate product in the manufacture of pyridoxol.

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Résumé On décrit une nouvelle méthode polarographique pour le dosage direct du pyridoxol dans les préparations pour injections et dans les comprimés. La méthode élaborée repose sur la réduction polarographique de la molécule de pyridoxol dans le milieu tampon ammoniaque-chlorure d'ammonium, et, en outre, sur la formation d'une phase catalytique du pyridoxol dans les tampons au véronal. La méthode polarographique est plus rapide et dans de nombreux cas plus exacte et plus sensible que les méthodes utilisées jusqu'ici. La présence d'impuretés existant couramment dans les préparations à côté du pyridoxol ne gêne pas le dosage polarographique. On peut aussi utiliser la méthode pour le dosage de l'hydroxy-3 méthoxyméthyl-4 oxyméthyl-5 méthyl-2 pyridine, substance intermédiaire dans la préparation du pyridoxol.

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Herrn Dr.P. Zuman danken wit für Ratsehläge bei der Abfassung dieser Arbeit.