Die Anwendung der “Neutronenhaubitze” zur Borbertimmung in Glas

Die bei der ¹⁰B (n, α) ⁷ Li-Reaktion entstehende prompte Strahlung von E_γ = 478 ke V bildet die Grundlage für zerstörungsfreie und quantitative Bestimmung von Bor in Glas. Es wird eine als “Neutronenhaubitze” bezeichnete Bestrahlungseinrichtung beschrieben, die mit einer ²¹¹ Am-Be-Neutronenquelle von 5 Ci ausgerüstet ist. Damit lassen sich bei 10 min Meβzeit im Konzentrationsbereich 5· · ·25 Masse-% Aanlysenfehler ∠2% relativ erreichen.     

Reduzierung des Störstrahlungseinflusses bei der Elementanalyse nach dem (n, γ)-Verfahren mit Neutronengenerator

Bei der Elementanaylse mittels Szintillalionsspektrometrie im Ausgangskanal der (n, γ)-Reaktion tritt ein hoher Linienuntergrund auf. Dieser Untergrund lafit läβt herabsetzen durch Puhung des Neutronengenerators (Plasyna-Pulsung), zweckmäβige Dimensionierung der Meβanordnung und Optimierung des Meβzeilintervalls.     

Orientational glasses

This review summarizes experimental evidence for the freezing of reorienting moments in solids. The moments may be of dipolar or quadrupolar nature, or both; they belong to one of the constituents of a mixed-crystal solid. Extensive results are reported for the following systems: KCl doped with hydroxyl, potassium tantalate doped with Li, Na and Nb, alkali halide cyanides and alkali-alkali cyanides, rubidium ammonium dihydrogen phosphate, solid ortho-para hydrogen and argon-nitrogen mixtures. These have clearly glass-like properties. In other systems, results are limited to one or two methods hinting at glass formation; some of those are also reported. Clustering phenomena and the slowdown of reorientations at the freezing temperature are observed in susceptibility measurements and by local probing on nuclear spins. The modulation of the structure by cluster formation is revealed by diffraction experiments. These phenomena are confronted with model predictions and numerical simulations.     

The kiel/berlin pressure cells for neutron powder diffraction

Abstract

Two piston/cylinder type pressure cells for neutron powder diffraction are presented. They provide a large sample volume and hence allow rapid data collection at moderate flux neutron sources. Structure refinements from the diffraction data are possible. The maximum attainable pressure is above 2 GPa for Ti/Zr zero-scattering pressure cylinders. Both cells may be equipped with a micro-furnace. This allows measurement up to 700 K, simultaneously to the application of pressure. The low temperature setup for the cell-I is presented which will allow experiments down to 1·5K.     

Melting and freezing of argon in a granular packing of linear mesopore arrays

Freezing and melting of Ar condensed in a granular packing of template-grown arrays of linear mesopores (SBA-15, mean pore diameter 8 nm) has been studied by specific heat measurements C as a function of fractional filling of the pores. While interfacial melting leads to a single melting peak in C, homogeneous and heterogeneous freezing along with a delayering transition for partial fillings of the pores result in a complex freezing mechanism explainable only by a consideration of regular adsorption sites (in the cylindrical mesopores) and irregular adsorption sites (in niches of the rough external surfaces of the grains and at points of mutual contact of the powder grains). The tensile pressure release upon reaching bulk-liquid-vapor coexistence quantitatively accounts for an upward shift of the melting and freezing temperature observed while overfilling the mesopores.     

Color and fastness of natural dyes encapsulated by a sol-gel process for dyeing natural and synthetic fibers

Natural dyes, namely, indigo carmine, cochineal carmine, curcumin and annatto, were encapsulated in silica by a sol-gel method and applied in the dyeing of different textile fibers by exhaustion. For comparative reasons, dyeing using the free (non-encapsulated) bare dyes was also carried out. The hybrid materials were analyzed by a set of techniques to investigate their elemental, structural, textural and morphological properties, and the results showed that it was possible to obtain stable natural dyes for applications in textile dyeing. The silica-structured dyes showed better affinities with the fibers (WO, PA, PAC and PET) in dyeing with cochineal carmine, while cotton (CO) showed better affinities with the encapsulated curcumin and annatto dyes. The performances of the encapsulated dyes were evaluated by color and washing fastness measurements and resulted in improved dye absorption and wash fastness properties. The color change and color transfer measurements of the encapsulated dyes were better (rated at 4–5 on a scale of 1–5) compared to the bare dyes.

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Why is cis/trans stereoinversion with Li+(THF)4 migration across the phenyl ring of α-lithiostyrene accelerated by two ortho-methyl groups?

Common wisdom might anticipate that two methyl groups placed on a molecular migration route should act as an impediment. However, the “conducted tour” migration of Li⁺(THF)₄ across the aryl ring (“π-route”) during the cis/trans stereoinversion of α-arylvinyllithiums had been found to occur with practically equal velocities in the presence of either one or two ortho-alkyl substituents. We now report that the omission of both ortho-methyl groups retards the stereoinversion process. In order to arrive at an answer to the title question, we investigate the aggregation equilibria and microsolvation states of ortho, ortho′-unsubstituted α-lithiostyrenes by means of approved secondary NMR criteria. Beyond such necessary knowledge about the ground-state properties, we provide kinetic evidence showing that the retarded cis/trans stereoinversion of α-lithiostyrene proceeds by the pseudomonomolecular, ionic mechanism with Li⁺(THF)₄ migration.     

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