Peroxides of higher aliphatic ethers

The oxidation of higher aliphatic ethers with oxygen at 50° yields two peroxides as the main oxidation products for each ether, namely a dihydroperoxy-dialkyl ether and a dihydroperoxy-dialkyl peroxide. The mass spectra of these compounds are recorded and the main fragmentation pattern is discussed.     

Exchange of halogen bonded on aromatic core. Heterogeneous catalysis—I : Reaction mechanism of iodine exchange in o-iodobenzoic acid

Reaction mechanism of halogen exchange between arylhalogenide and halogenide anion is studied in a case when the aromatic core is inactivated with respect to the S_NAr substitution by other substituents. The exchange of iodine between o-iodobenzoic acid and ¹³¹I labelled NaI serves as a modelling reaction. The reaction was found to proceed heterogeneously on a glass surface. In the case of a rapid course of the surface reaction the reaction mechanism is more complicated and the equation derived by McKay cannot be applied for expressing the time dependence of the degree of isotopic exchange. Reaction mechanism was proposed for this reaction and compared with experimental data.     

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.     

The study of degradable polystyrene: Photolysis in solution and photo-oxidation in films

Radical copolymerization of styrene with benzalacetophenone or benzalacetone in bulk or in suspension yielded copolymers with as much as 10 wt% of carbonyl monomer. They were characterized by GPC, viscometry and spectroscopy. Photolysis of copolymers was investigated in benzene at 313 nm. Quantum yields for main chain scissions were about 0.005 and the life-time of the triplet state was 5 nsec. Photo-oxidation in films was followed by monitoring the decrease in molecular weight and by i.r. and emission spectra. Quantum yield for main chain scission in films was about 0.0002. During photooxidation in film, the molecular weight distribution widened. A new i.r.-band appeared at 3580 cm^?1 and the carbonyl band was spread between 1700 and 1800 cm^?1. In the emission spectra, the vibrational resolved emission (typical of the carbonyl chromophore) disappeared.     

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.     

Large deviations for martingales with some applications

Let(X _i ) be a martingale difference sequence. LetY be a standard normal random variable. We investigate the rate of uniform convergence

Kneser-type oscillation criteria for self-adjoint two-term differential equations

It is proved that the even-order equationy ⁽²ⁿ⁾ +p(t)y=0 is (n,n) oscillatory at if

q-Sigma-algebra generated by balls

The q--algebra, i.e., the system of sets closed under complementation, countable disjoint unions, and containing the empty set, generated by the system of open balls coincides with the -field of Borel sets inR sun forn=1,2, and 3. A first step to extend the proof forn=4, 5, 6, and 7 is indicated.     

Encapsulation of magnetite in vesicles

The encapsulation of fine magnetite particles of 10 nm size and marker ANS within asolectin vesicles has been made by sonication of the mixture in water. For the proof of encapsulation of magnetite in vesicles the electron microscope and spectrofluoriphotometer technique were used. The theory for the calculation of the magnetic force acting on the system consisted of non-capsulated magnetic particles dispersed in water and magnetic vesicles was developed.This work was supported by the Slovak Academy of Sciences within the framework of Project GAV No. 1361.     

On the critical regimes in the theory of randomly forced magnetohydrodynamic turbulence

In this paper large-scale properties of developed magnetohydrodynamic turbulence have been investigated by using double expansion method in the frame of quantum field renormalization group. It has been shown that universal kinetic scaling regime exists, but the double expansion in general leads to qualitatively different results than those provided by the usual -expansion treatment.This work was supported by Slovak Grant Agency for Science.