Substitution of calcium by strontium within selected calcium phosphates

Sr incorporation in the molecules of amorphous calcium phosphate, apatitic tricalcium phosphate, hydroxyapatite, octacalcium phosphate and dicalcium phosphate dihydrate was investigated. The concentration of Sr ranged from 225 to 1010 μ g / g, i.e. it overlapped with the physiological range of Sr concentrations in human bone. The leading experimental technique was extended X-ray absorption fine structure (EXAFS) at the Sr K edge. Results of these studies demonstrated the following: (1) Sr incorporation in the calcium phosphates is compound-dependent, (2) the coordination of incorporated Sr atoms in the Ca-P molecules is similar to that of Ca atoms, but interatomic distances are ≈0.015 nm larger, (3) in apatitic tricalcium phosphate, hydroxyapatite and octacalcium phosphate lattices Sr atoms may occupy selected Ca sites, which was not the case for dicalcium phosphate dihydrate, (4) in the apatite lattice Sr atoms are coordinated by 6 PO₄ tetrahedrals and (5) EXAFS spectra at the K edge of the incorporated Sr may be used to distinguish the structures of amorphous calcium phosphate, dicalcium phosphate dihydrate as well as apatite and its derivatives (apatitic tricalcium phosphate, octacalcium phosphate).     

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.     

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.     

Matrix effects in the determination of butyltin compounds in environmental samples by GC AA after hydride generation

Experiments for the determination of mono-, di and tri-butyltin (MBT, DBT and TBT) by hydride generation/gas chromatography/atomic absorption spectrometry in various matrices (sediment, suspended matter, mussel, algae and water) have revealed that poor butyltin recoveries are obtained in sediments displaying high sulphur and hydrocarbon contents; very poor recoveries were also observed for TBT in sediments with high chlorophyll pigment contents as well as in algal samples. It was however not clear whether the hydride generatin was inhibited by these infering compounds, as was previously assumed in the case of hydrocarbons, or whether interferences affected the atomization rate. Further studies were performed to solve this problem in order to validate this method in the case of analyses of, for example, oil-contaminated sediment and algae. This paper presents the results obtained. It is concluded here that the poor recoveries were due to an inhibition of hydride generation rather than to interference at the atomization stage.     

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.     

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.     

On the Causes and Effects of Contaminations during rf Diode Deposition of Cr-Si Alloys

Investigations to the causes and effects of contaminants at the rf diode deposition of CrSi films in a non-heated high vacuum apparatus were carried out comparing an oxygen-free fusion target with an oxygen-containing cermet target. The films of the fusion target contained considerable amounts of oxygen; analogously the oxygen concentration in the films was increased in the case of the cermet target. Moreover, hydrogen was found. The concentration of the contaminants decreased with the sputtering power, however the rate of incorporation increased. For high sputtering rates the contamination process was reproducible and independent of the plant conditioning; the deposited films were depth-homogeneous. The reasons for this behaviour lie in water sources which are activated first of all by the discharge itself. The electrical properties found are explained by the contaminants and the deposition conditions.