Beitr?ge zur Ultramikro-und Spurenanalyse organischer Stoffe

Zusammenfassung Zur Ultramikrobestimmung von Brom in schwerflüchtigen organischen Verbindungen werden 1–5 g Substanz (mit dieser Methode sind auch größere Substanzmengen analysierbar) durch Lösungsteilung abgemessen und nach Absaugen des Lösungsmittels im Wasserstoffstrom bei einer konstanten Temperatur von etwa 900°C pyrolysiert, wobei sich Brom quantitativ zu Bromwasserstoff umsetzt, der in einer Vorlage in Eisessig absorbiert und argentometrisch titriert wird. Die Endpunktsanzeige erfolgt bipotentiometrisch. Bei Abwesenheit von anderen Halogeniden und Sulfid werden Silberbromid-Elektroden benutzt, andernfalls SilberElektroden. Die relative Standardabweichung der Methode beträgt im ersten Fall ±1.4% und erhöht sich auf etwa ±3%, wenn gleichzeitig Chlor, Jod oder Schwefel vorliegen.

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Summary For the determination of bromine in ultramicro amounts of non-volatile organic compounds 1–5 g of the substance (this method can be used for larger amounts as well) are measured by taking an aliquot of a solution of known concentration. After evaporation of the solvent the sample is pyrolyzed in a hydrogen stream at a constant temperature of about 900°C. Hydrogen bromide obtained in a quantitative reaction, is absorbed in glacial acetic acid and titrated argentometrically. The endpoint of the titration is found by a bipotentiometric method. In the absence of other halogenides or sulphide silver bromide electrodes are used, otherwise silver electrodes. The relative standard deviation is ±1.4% in the first case and about ±3% in the latter.

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Herzlicher Dank gilt Herrn Prof. Dr. R. Bock für wertvolle Diskussionen. Der Deutschen Forschungsgemeinschaft, Bad Godesberg, sowie dem Verband der chemischen Industrie Düsseldorf, danken wir für ihre Unterstützung. Herrn cand. chem. H.-J. Anhuth sei vielmals für sorgfältig durchgeführte Messungen zur Bestimmung von Bromid neben anderen Halogeniden gedankt.

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Herrn Prof. Dr. F. Strassmann zum 65. Geburtstag gewidmet.

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VI. Mitteilung: Tölg, G., and K. Ballschmiter: Microchem. J. 9, 257 (1965).     

Modelling of rib waveguide bends for sensor applications

Wave propagation through curved bends in integrated optical waveguides is governed by the evanescent field and the radiation loss of the eigenmodes. Since these parameters are influenced by the refractive index of the surrounding medium, circular bends in rib waveguides have been successfully employed as chemical sensors for liquids and gases. In this paper the electromagnetic field, the refractive index and the radiation loss of the eigenmodes are precisely determined by a fully vectorial approach based on the method of lines. An axial discretization and Bessel functions of complex order are employed for the rigorous computation of the evanescent field. The intensity distributions of the first modes in a rib waveguide are presented. The influence of the rib height on the sensitivity of the modal index to the refractive index of the surrounding medium is investigated. The results are useful for the optimization of the sensor design.     

Converging algorithm for a class of BMI applied on state-dependent stabilization of switched systems

In this paper, a design of a stabilizing state-dependent switching law is presented. First, it is based on a new reformulation of this control problem into a class of BMI (Bilinear Matrix Inequality) problem. The originality of this reformulation is that it will be used, in a second part, by an algorithm dedicated to solve this class of BMI without loss of generality. The construction of this algorithm is then specified, and the proof of its convergence is given for the two-subsystem case. The last part of the work consists in presenting the problem for a polytopic switching system, and how the previous algorithm can be extended. The proposed scheme is illustrated by an academical example.     

Über eine Möglichkeit,geglühtes Chromoxyd oder Chromeisenstein bei Zimmertemperatur in Lösung zu bringen

Ohne Zusammenfassung     

Positrons in metals with voids,vacancies and surfaces

The behaviour of positrons near monovacancies and voids in a metal is discussed in terms of three contributions to the positron work function for the metal, namely the positron zero-point energy, the positron-electron correlation energy and the surface dipole barrier. The image potential when a positron comes near to a metal surface leads to a deep potential ‘trough’ just outside an exterior metal surface or just inside a void surface. Calculations indicate positron bound states localized at metal surfaces for most metals which should be manifested in a long lived positron lifetime component. The behaviour of positronium near metal surfaces is also discussed.     

Behavior of thin films of poly(oxyethylene)-poly(oxybutylene) copolymers studied by brewster angle microscopy and atomic force microscopy

Surface films of two copolymers of ethylene oxide (E) and butylene oxide (B), namely E23B8 and E87B18, have been examined by Brewster angle microscopy (BAM) and atomic force microscopy (AFM). Isotherms taken on unsupported films of these copolymers at the air-water interface showed a clear gas to liquid phase transition for E57B18 and a barely discernible phase transition for E23B8. The BAM studies showed a gradual brightening of the films as the surface pressure was increased, which was associated with a film thickening and/or a film densification. Several bright spots were also observed within the films, with the number of spots increasing gradually as the film surface pressure was increased. AFM studies of these films did not show any localized ordering, which fits in with the results from our previous X-ray study of these copolymers [Hodges, C. S.; Neville, F.; Konovalov, O.; Gidalevitz, D.; Hamley, I. W.; Langmuir 2006, 22 (21), 8821-8825], where no long-range ordering was observed. AFM imaging showed two sizes of particulates that were irregularly spaced across the film. The larger particulates were associated with silica contaminants from the copolymer synthesis, whereas the smaller particulates were assumed to be aggregated copolymer. An analysis of the semidilute region of the isotherm showed that while both copolymers had intermixed ethylene oxide and butylene oxide units, the lower molecular weight E23B8 copolymer manifested significantly more intermixing than E87B18.     

Mechanical properties of anodized coatings over molten aluminum alloy

A method to measure interfacial mechanical properties at high temperatures and in a controlled atmosphere has been developed to study anodized aluminum surface coatings at temperatures where the interior aluminum alloy is molten. This is the first time that the coating strength has been studied under these conditions. We have investigated the effects of ambient atmosphere, temperature, and surface finish on coating strength for samples of aluminum alloy 7075. Surprisingly, the effective Young's modulus or strength of the coating when tested in air was twice as high as when samples were tested in an inert nitrogen or argon atmosphere. Additionally, the effective Young's modulus of the anodized coating increased with temperature in an air atmosphere but was independent of temperature in an inert atmosphere. The effect of surface finish was also examined. Sandblasting the surface prior to anodization was found to increase the strength of the anodized coating with the greatest enhancement noted for a nitrogen atmosphere. Machining marks were not found to significantly affect the strength.