Neue Wege der Analytik durch Kombination der direkten quantitativen Dünnschicht-Chromatographie mit elektronischer Datenverarbeitung

A computer program for direct evaluation of thin-layer chromatograms, which already was described earlier [3] has been tested with a laboratory and some technical formulations of a pesticide. Results have been compared with those obtained by two conventional methods. Mean relative standard deviation calculated from results compiled by electronic data processing (method A) is about 6%, compared to 10% received by graphic method (method C) which is employed by most investigators. In addition, overall time of analysis is 34% higher if graphic method is used. Method A saves time and expense especially in routine analysis because working of the process is easier and may be performed even by assistent personal. The proposed method is suitable for the determination of different active ingredients and impurities even in difficult technical products.     

A study of thin surface layers by multilayer Mössbauer spectroscopy /MMS/

A stacking Mössbauer technique, MMS has been applied for studying thin surface layers. The surface layers formed on the⁵⁷Fe film in aqueous solutions of corrosion inhibitors, such as zinc phosphate and barium metaborate, and in distilled water was studied by this method. It has been found that the corrosion is much slower in the presence of zinc phosphate and barium metaborate. XPS analysis suggests the formation of a mixed iron zinc phosphate on the surface of the⁵⁷Fe film after corrosion in a zinc phosphate solution.     

Reactions de photoaddition de benzo[b]selenophenes avec l'acetylene dicarboxylate de methyle et avec le dichloro-1,2 ethylene

Photoirradiated in presence of acetophenone, benzo[b]selenophene and its 3-methyl derivative add to dimethyl acetylenedicarboxylate. In each ease, the primary reaction product is unstable and has not been isolated. Photoexeited in its triplet state (the energy of which is in the neighbourhood of 69 $\text{kcal}\text{mole}$) benzo[b]selenophene and its 2- and 3-methyl, 2,3 dimethyl, 3 acetoxy and 2-methyl-3-acetoxy derivatives add to 1,2 dichloroethylene leading to cyclobutanes. Neither cyclo-addition occurs in absence of photosensitiser. Single-crystal X-ray analysis gave the structures of the two adducts of 3-acetoxybenzo[b]selenophene with trans-1,2-dichloroethylene. In both compounds the chlorine atoms are trans.     

Mechanism of the decomposition of cumenyl hydroperoxide under the influence of complexes of divalent copper with o-phenanthroline

Russian Chemical Bulletin -     

Die quantitative Bestimmung von Vanadin mittels aktivierter Katalyse

Zusammenfassung Es wurden zwei Verfahren ausgearbeitet, um Vanadin mit Hilfe von aktivierter Katalyse zu bestimmen. Die Methodik ist geeignet, kleinste Spuren von Vanadin (bis herab zu 0,0006) mit ausreichender Genauigkeit zu ermitteln. Es werden Beleganalysen mitgeteilt.

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Summary Two procedures for the determination of vanadium have been worked out, based on activated catalysis, which allow minimal traces (down to 0,0006) of vanadium to be determined with adequate accuracy. Comparison analyses are given in the paper.

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Résumé On a élaboré deux procédés pour exécuter le dosage du vanadium à l'aide d'une catalyse activée. La méthode est apte à la détermination des plus petites traces de vanadium (jusqu'à 0,0006) avec une précision suffisante. On communique des analyses documentaires.

     

1,4 Addition to a perfluorinated cross-conjugated triene

Conclusions Perfluoro-(2-isobutenyl-1,1,4,4-tetramethyl-1,3-butadiene) yields 1,4 addition products both in nucleophilic addition and in radical chlorination.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 5, pp. 1061–1064, May, 1979.     

Zur Kenntnis von Natrium-hexafluoromanganat(III)

Sodium hexafluoromanganate(III) has been synthesized by heating equimolecular quantities of Na₂MnF₅ and NaF in argon atmosphere. The compound is monoclinic witha=5.56 (1) Å,b=5.84 (1) Å,c=8.10 (2) Å, =90.7 (2) andZ=2. It is a high spin complex with _eff and the deformation of the octahedra is evident from its IR-spectra. Two enantiotropic transitions (at 562 and 653°C) and the melting point at 800°C have been observed.

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8. Mitt.: Mh. Chem.106, 483 (1975).     

Thermal degradation of copolymers of styrene and methyl-vinyl-silane by pyrolysis gas chromatography

Pyrolysis gas chromatographic investigations have been carried out on copolymers of styrene with trimethyl-vinyl-silane and of styrene with dimethyl-phenyl-vinyl-silane, in order to study the mechansims of thermal degradation and the copolymer structures. We have identified the pyrolysis products and measured their relative amounts. The experiments show that the controlling factor in the mechanism of the degradation is the nature of the side-group attached to the carbon atom at which chain scission occurs. If this side-group is phenyl, the main degradation process is depropagation; if it is if it is trimethyl-silyl or dimethyl-phenyl-silyl, intramolecular hydrogen abstraction followed by β scission becomes more important than depropagation. From the point of view of degradation mechanism, the nature of the side-group attached to the carbon atom from which the hydrogen is abstracted is of minor importance.We estimated the average copolymer block length from the amounts of products containing both comonomers as well as from the amounts of trimer composed of the same monomer.