X-ray induced fluorescence spectrometry at grazing incidence for quantitative surface and layer analysis

Summary Single layers and layer systems on diverse substrates were measured by Total Reflection X-Ray Fluorescence (TXRF) spectrometry. The angular dependence of the fluorescence intensities at grazing incidence allows the elemental composition, density and thickness of the layers to be evaluated using model calculations.     

A note on dephasing and pair-breaking

It is shown that the dephasing which suppresses the weak localization correction to the conductivity has the same physical origin than pair-breaking in superconductors and thus-following de Gennes-may be expressed in terms of the correlation function of the operator for time reversal.     

Unoccupied electronic states of epitaxial iron layers on Cu(100)

Inverse photoemission spectra were taken for thin epitaxial iron films on Cu(100). For a film thickness of eight monolayers the observed electronic states are characteristic for a fcc(100) surface. Thed-bands of iron show a ferromagnetic exchange splitting of 1.1 eV, considerably smaller than the bulk value of 1.8 eV, which we observe for film thicknesses above 18 monolayers.     

A globally convergent multi-grid algorithm for moving boundary problems of two-phase Stefan type

In this paper we deal with the numerical solution of movingboundary problems of two-phase Stefan type. Based on an implicitdiscretization in time and the use of continuous, piecewiselinear finite elements in the space variables with respect tothe weak formulation of the problem, a globally convergent multi-gridalgorithm is developed. That algorithm strongly relies on thevariational characterization of the fully discretized problemas the unconstrained minimization of a subdifferentiable convexobjective functional. Numerical results indicate a significantimprovement in efficiency compared with previous multi-gridapproaches.     

Adaptation of an echelle spectrograph to a large CCD detector

A broad range echelle spectrograph with a CCD matrix detector is developed for different applications in atomic spectroscopy. The compact optical design in combination with a dispersive entrance slit illumination offers a low stray light level and high throughput in the UV spectral region comparable only with spectrographs of higher focal length. Ray tracing calculations for typical wavelengths and the multi-line spectrum of an iron arc show the excellent overall spectrum quality. The subtraction of two partial spectra of different steel alloys demonstrates the spectra evaluation possibilities of the CCD spectrograph.     

TLC-screening of important pharmaceutical substances using fluorescence detection

Summary Observation of fluorescence reactions on TLC plates is a valuable additional tool within the scope of screening procedures for many toxicologically relevant substances commonly encountered in clinical- and forensic-toxicological analysis. The reactions are based on native fluorescence without any treatment and on reactions obtained with an approved derivatization procedure. Due to the enormous sensitivity of the fluorescence detection, the method is also applicable to very low concentrations and small amounts of biological materials. The procedures described in this article have proven their high pragmatic usefulness in many practical cases.Dedicated to Professor Dr. Wilhelm Fresenius on the occasion of his 80th birthday     

Hybrid organosilazane/organosilylamine telechelic oligomers—I. Two-dimensional NMR spectroscopy characterization of dimethylsilylethylenediamine oligomers

The detailed characterization of multifunctional hybrid organosilazane/organosilylamine telechelic oligomers by IR and ¹H, ¹³C and ²⁹Si NMR spectroscopy in one and two dimenions has been undertaken. The specific multifunctional oligomers, comprising NH/NH₂ or SiCl functionalities depending on the monomer feed-ratio, were prepared from mono- and di-functionally reacted dichlorodimethylsilane (DDS) and mono-, di-, tri- and tetra-functionally reacted ethylenediamine (EDA). Varying the feed-ratio afforded control of the microstructures of the oligomers and the preparation of oligomers with, in some cases, conterminously located silicon–chlorine (SiCl) groups. The combination of the NMR methods with the IR technique has enabled the detailed microstructural characterization of the oligomers and the identification of the functionalities therein. This approach and the knowledge gained from the DDS/EDA system has been applied to the microstructural characterization of other hybrid organosilazane/silylamine preceramic telechelic oligomers.     

Liquid crystal properties of some substituted pyrazines

A number of biphenyl, terphenyl analogues and ethynes which contain a pyrazine ring have been made and their liquid crystal transition temperatures, together with examples of birefringence measurements, are reported. All the 2,5-disubstituted pyrazine systems are liquid crystalline showing high birefringence values for the biphenyl and terphenyl analogues, whereas the 1,5-disubstituted systems are not liquid crystalline. The pyrazine ethyne systems exhibit very high birefringence values. X-ray diffraction has been used to identify the liquid crystal phases of 2-n-nonyloxy-5-(4'-propylbiphenyl-4-yl)pyrazine.     

Branched chain discotics Phase structure and orientation behaviour

Studies show that branching the side chains of hexakis(acoyloxy)-benzenes (HAB) and -cyclohexanes (HAChx) does not modify the structure of the discotic mesophase formed. Shear fields appear to act on entire columns, not on individual discs, thereby causing alignment of columns in the shear direction. X-ray diffraction patterns of samples at temperatures between 30°C and 40°C above the clearing temperature provide evidence for the presence of mesophase order.