Octasilsesquioxane Chemistry II. Hydrosilylation Reaction of Octa(hydrido)silsesquioxane with Unsaturated Substrates and Product Properties

The hydrosilylation reaction of octa(hydrido)silsesquioxane with ω‐halo‐1‐alkenes and other unsaturated substrates allows attachment of 8 long‐chain functionalized alkyls on the cubic Si₈O₁₂ skeleton. Pt/C and H₂PtCl₆ have been adopted as the catalysts, the yields being 74–98% for compounds 2–9 . For terminal alkenes, the hydrosilylation follows the anti‐Markonikov's rule. The morphological state of 2–9 ranges from viscous liquid to crystalline materials. The pyrolysis results indicate that 7 , a material of hard spherical core and soft flexible shell, may likely act as nanometer‐size ball bearings up to more than 400 °C. The X‐ray structure of 9 reveals that the molecule is required to possess a center of symmetry crystallographically. The linear arms on 9 , except for two of them, are virtually all‐trans in conformation, not counting the ω‐C‐Cl bond.     

NQR spectra of alloys of antimony-cadmium-zinc system

Conclusions A number of metal alloys in the Sb-Cd-Zn system was studied for the first time by the NQR method on the^121,123Sb nuclei. The constants of the quadrupole bond and the asymmetry parameter of the compounds ZnSb were determined.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No; 7. pp. 1638–1640, July, 1977.     

An analysis of the possible causes of apparent compensation effects when investigating a substance under varying experimental conditions

The major causes leading to the apparent compensation effect (lgA=aE+b) at the thermal decomposition of one and the same substance in a series of experimental conditions (varying of the mass of the sample, of the heating rate, of disperseness, and at different distances from the equilibrium) were discussed. It was found that the appearance of a compensation effect at the study of the thermal decomposition of one and the same substance demonstrates the incorrect setup of the experiment, resulting in erroneous values calculated for the kinetic parameters.

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Zusammenfassung Die Hauptursachen, welche zum scheinbaren Kompensationseffekt (lgA=aE+b) der thermischen Zersetzung ein und derselben Substanz führen, wurden unter verschiedenen Versuchsbedingungen untersucht: unter Änderung der Probenmasse, der Aufheizgeschwindigkeit, der Dispersität und der Entfernung vom Gleichgewicht. Es wurde festgestellt, daß das Auftreten eines Kompensationseffekts bei der Untersuchung der thermischen Zersetzung ein und derselben Substanz auf die unrichtige Durchführung des Experiments hinweist, die zur Berechnung falscher Werte der kinetischen Parameter führt.

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Résumé On a étudié les causes principales de l'effet de compensation apparent (lgA=aE+ +b) lors de la décomposition thermique de la même substance dans différentes conditions expérimentales, en faisant varier notamment la masse du prélèvement, la vitesse du chauffage, la dispersion et l'écart à l'équilibre. On a trouvé que l'apparition d'un effet de compensation lors de l'étude de la décomposition thermique de la même substance résultait de l'exécution incorrecte de l'expérience qui mène à des valeurs fausses lors du calcul des paramètres cinétiques.

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, (lg A=aE+b) : , , , . , , .

     

Reaction of gaseous hydrogen fluoride with aluminium and its compounds

The reaction of metallic aluminium surfaces, aluminium oxides, hydrated oxides and sulphate with gaseous anhydrous hydrogen fluoride was studied at 470°C and pressures between 10 and 100 torr. The complementary analytical techniques of X-ray induced photoelectron spectra, X-ray and electron diffraction, and electron microscopy were used for identifying the (frequently unexpected) products.     

Simple method for the preparation of 1-oxo-1-chlorophospholenes

Conclusions A new and simple method has been found for the synthesis of 1-oxo-1-chlorophospholenes by the reaction of phosphorus trichloride, a diene, and an oxygen-donor compound, the best of which is acetone.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 8, pp. 1847–1848, August, 1972.     

The application of chromatography to the analysis of pharmaceutical creams

Summary The application of GLC, HPLC and TLC to the analysis of pharmaceutical creams is discussed with special attention to sample clean-up. The results of the determination of hydrocortisone acetate, salicylic acid, benzoic acid, diethyl stilbestrol, chloramphenicol, diphenhydramine HCl, tretinoin and some cream base components by reversed phase HPLC are given.Presented at the 14th International Symposium on Chromatography London, September, 1982