Automatisches Verfahren zur Bestimmung des Bleioxidgehalts von Grauoxid durch Messung der L?sungsw?rme

Zusammenfassung Für das zur Herstellung von Bleibatterien verwendete Grauoxid (bestehend aus einem feinteiligen Gemisch von ca. 60 bis 90% Bleioxid, PbO, und einem Rest metallischem Blei) wurde ein Verfahren zur kontinuierlichen bzw. quasikontinuierlichen, automatischen Bestimmung des PbO-Gehaltes an den Fertigungsanlagen benötigt. Eine schnelle Analyse mit vergleichsweise geringem Aufwand war durch Messung der Lösungswärme bei Behandlung einer abgewogenen Menge Grauoxid mit verd. Essigsäure möglich. Unter technisch bequem realisierbaren Bedingungen wurden Temperaturerhöhungen von einigen Grad erhalten. Der Einfluß verschiedener Arbeitsbedingungen, der verschiedenen PbO-Modifikationen und der Teilchengröße und -form wurde untersucht. Zur Zeit wird eine für die Fertigung bestimmte, automatische Apparatur aufgebaut, die bei einer Analysenfolge von 1 min die Bestimmung mit einer Standardabweichung unter ±1% durchzuführen gestattet.

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Automatic procedure for the determination of the lead oxide content of gray oxides by measurement of the heat of solution

A continuous or semicontinuous automatic method for the determination of the lead oxide content was needed in the manufacturing process of gray oxides (a fine particle mixture of about 60 to 90% lead oxide, PbO, and metallic lead, used in manufacturing lead batteries).A rapid determination with comparatively small effort was possible by measuring the heat of solution of a weighed amount of gray oxides treated with acetic acid. Temperature rise of a few degrees could be reached under technically realisable conditions. The influence of different working conditions, of the particle size and shape and of the PbO modifications were investigated. An automatic apparatus for the determination is at present being built and will give one determination per minute with a standard deviation of less than ±1%.

     

Molecular Structure of 1,3,5-Tris (Trimethylstannyl) Benzene: An Electron Diffraction Study

The molecular structure of 1,3,5-tris (trimethylstannyl) benzene has been determined by gas-phase electron diffraction. The C — C bond length is in good agreement with that in benzene. In agreement with the somewhat electron-releasing character of the substituents, the endocyclic bond angles at the substituents are somewhat smaller than 120°. The mean value of Sn — C bond lengths is greater than that in tetraphenyltin and tetramethyltin. The SnMe₃ groups appear freely rotating around the C_aryl — Sn bonds. The following bond lengths (r _g) and bond angles were determined: (Sn — C)_mean 2.150 ± 0.007 Å, C — C 1.399 ± 0.005 Å, (C — H)_mean 1.105 ± 0.006 Å, < C — C(Sn) — C 117.7 ± 1.7º, < C_aryl — Sn — C_methyl 106.7 ± 0.7º < Sn — C — H 111.5 ± 0.9º.     

Infrared intensities of the external modes of crystalline nitrous oxide

The absorption intensities of two infrared active lattice modes of crystalline N₂O have been measured. Both the frequencies and intensities of the external modes of N₂O have been found to be very similar to those of CO₂, and most of the differences between the spectra of CO₂ and N₂O can be explained by the differences in the quadrupole moments.     

Heterogeneity of cardiac rat and human elongation factor 2

Elongation factor 2 (EF-2) catalyses the last step of the elongation cycle, translocation, in the course of protein biosynthesis. A system for analyzing post-translational modifications of EF-2, which is a single polypeptide of 857 amino acids, is reported and its application to cytosolic extracts of cultured neonatal rat heart myocytes, neonatal and adult rat cardiac tissue, and extracts of human left ventricular myocardium is described. Comparing different pH ranges in immobilized pH gradient-isoelectric focusing (IPG-IEF), a range of pH 3 - 10 and 4 - 9 resulted in a highly defined and reproducible resolution of six different EF-2 variants of all extracts in the first dimension. These six variants were detected by the "imaging plate" (phosphor radiation image sensor) after specific labeling with Pseudomonas exotoxin A catalyzed [32P]ADP-ribosylation. This finding could be confirmed in Western blot analysis with a specific polyclonal rabbit antibody. Using two-dimensional polyacrylamide gel electrophoresis (2-D-PAGE), five to six EF-2 variants could be demonstrated in all extracts. By application of a second IPG indicator strip to the 2-D gel, they could be aligned with corresponding spots in a silver-stained 2-D separation of human myocardial tissue, revealing that the EF-2 variants belong to the group of low-abundance proteins.     

Conformations and base-catalyzed equilibrations of N-nitroso-decahydroquinolines and N-nitroso-2-methyldecahydroquinolines

Conformations of six title compounds were determined by¹³C-NMR spectroscopy. Equilibration of the 2-methyl-compounds gives as main products the derivatives of the amines least abundant in the product mixture of the catalytic hydrogenation.

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Konformation und Base-katalysierte Äquilibrierungen von N-Nitroso-decahydrochinolinen und N-Nitroso-2-methyl-decakydrochinolinen (Kurze Mitt.)

Zusammenfassung Die Konformationen der sechs Titelverbindungen wurden mittels¹³C-NMR Spektroskopie bestimmt. Äquilibrierung der 2-Methyl-verbindungen ergab als Hauptprodukte die Derivate der bei katalytischer Hydrierung in geringster Menge entstandenen Amine.

     

Formation and Crystal Structure of Stable Five‐coordinate Diorgano Cobalt(III) Complexes

The mer‐octahedral complexes(2‐carbonyl)(4‐Me)(6‐tBu)phenolato[C,O]hydridotris(trimethylphosphine)cobalt(III) ( 1 ) or ‐(1‐carbonyl)(2‐oxo)(1,2‐diphenylethene)[C,O]hydridotris(trimethylphosphine)cobalt(III) ( 2 ) via formal insertion of propynoic acid ethyl ester into Co‐H functions afford pentacoordinate vinylcobalt(III) 3 and 4 , respectively, that are diamagnetic and attain a square pyramidal structure as exemplified by an X‐ray diffraction analysis of 3 .     

New minimal geodesics in the group of symplectic diffeomorphisms

We compute the Hofer distance for a certain class of compactly supported symplectic diffeomorphisms of ²ⁿ. They are mainly characterized by the condition that they can be generated by a Hamiltonian flow _H ^t which possesses only constantT-periodic solutions for 0 <T 1. In addition, we show that on this class Hofer's and Viterbo's distances coincide.