Non-destructive analysis of archeological samples by energy-dispersive X-ray fluorescence

Summary A non-destructive method is described for the determination of major and minor constituents in archeological specimens by energy-dispersive X-ray fluorescence. Homogeneity tests are made by measuring at various sites of the specimen. In the same way, mean values are obtained for inhomogeneous specimen without taking samples. For calibration, powder standards are used. In case of the determination of elements with numbers up to 14 (Si) a vacuum chamber is used and the dimensions of the specimens are limited by the dimensions of that vacuum chamber, whereas for the determination of elements from K up to U specimens of any size, form or weight are suitable.

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Zerstörungsfreie Analyse von archäologischen Proben mit Hilfe der Energie-dispersiven Röntgenfluorescenzanalyse

Zusammenfassung Eine zerstörungsfreie Methode für die Bestimmung von Haupt- und Nebenbestandteilen in archäologischen Proben mit Hilfe der Energie-dispersiven Röntgenfluorescenzanalyse wird beschrieben. Für Homogenitätstests wird an mehreren Stellen der Probe gemessen. In der gleichen Weise werden für inhomogene Proben Mittelwerte erhalten ohne Probenahme. Für die Eichung werden Pulverstandards verwendet. Im Falle der Bestimmung von Elementen mit Ordnungszahlen bis 14 (Si) wird eine Vakuumkammer eingesetzt, und die Dimensionen der Proben sind durch die Dimensionen dieser Vakuumkammer begrenzt, während für die Bestimmung der Elemente K bis U Proben jeder Größe, jeder Form oder jeden Gewichts verwendbar sind.

     

Determination of residual solvents in a transdermal system by means of headspace gas chromatography

Summary Pharmaceutical products have to be tested for impurities including residual solvents. This is also required in production control. The simplest solution to this problem is headspace gas chromatography. This paper describes the determination of residual volatile hydrocarbons in the transdermal system DEPONIT by only one headspace measurement. Accuracy is ensured by the multiple headspace extraction technique.

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Bestimmung von Restlösungsmittelgehalten in einem transdermalen System durch Headspace-Gas-Chromatographie

Zusammenfassung Pharmazeutische Produkte müssen auf Verunreinigungen geprüft werden, auch auf Restlösungsmittelgehalte. Ein zusätzlicher Grund ist die fortlaufende Kontrolle der Herstellung. Die einfachste Möglichkeit für dieses Problem ist die Bestimmung durch Headspace-Gas-Chromatographie. Dieser Artikel beschreibt die Bestimmung von noch vorhandenen flüchtigen Kohlenwasserstoffen in dem transdermalen System DEPONIT durch nur eine Headspace-Messung. Die Richtigkeit ist durch die Anwendung der Mehrfach-Gasextraktionstechnik sichergestellt.

     

A new group of fluorescent pH-indicators for an extended pH-range

Summary The pH versus fluorescence intensity profiles of a series of new pH-indicators are reported. They are characterized by two pK_a-values in the 3.7–4.9 and 6.9–7.9 range, respectively. The strong change in fluorescence intensity with pH allows the determination of pH's over a much wider range (typically 2–9) than with one-step indicators. They are therefore considered to be of potential utility for measurement of pH over the neutral and slightly acidity range which occurs, for instance, in bioliquids such as urine.

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Eine neue Gruppe fluorescierender pH-Indicatoren für einen erweiterten pH-Bereich

Zusammenfassung Die Fluorescenzintensitätsprofile als Funktion des pH-Wertes einer Reihe von neuen pH-Indicatoren werden untersucht. Sie sind charakterisiert durch zwei pK_a-Werte im Bereich 3,7–4,9 bzw. 6,9–7,9. Die gefundene starke Änderung der Fluorescenzintensität mit dem pH-Wert erlaubt eine pH-Bestimmung über einen viel weiteren Bereich (typischerweise 2 – 9) als mit einstufigen Indicatoren. Aus diesem Grund werden sie als potentiell nützlich angesehen zur Messung von pH-Werten im neutralen und schwach sauren Bereich, wie er z.B. in biologischen Flüssigkeiten, etwa im Urin, gegeben ist.

     

Surface analytical characterization of oxide-free Si(100) wafer surfaces

Summary Wet-chemical cleaning procedures of Si(100) wafers are surface analytically characterized and compared. Hydrophobic surfaces show considerably less native oxides in comparison to hydrophilic surfaces.The growth of the oxide is determined as a function of exposure to air by means of XPS measurements. The chemically shifted Si2p XPS signal is utilized for the quantification of the growth kinetics.One hour after cleaning no chemically shifted Si2p XPS peak is discernible on the hydrophobic surfaces. Assuming homogeneous oxide growth, the detection limit of native oxides is estimated to be below 0.05 nm using an emission angle of 18° with respect to the wafer surface. The calculation of the oxide thickness from the chemically shifted and nonchemically shifted Si2p XPS peak intensities is carried out according to Finster and Schulze [1]. For more than a day after cleaning no surface oxides can be identified on the hydrophobic surfaces. The oxide growth kinetics is logarithmic. The very slow oxidation rate cannot be attributed to fluorine residues since no fluorine is seen by XPS. We explain the slow oxidation rate by a homogeneous hydrogen saturated Si(100) wafer surface.

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Oberflächenanalytische Charakterisierung oxidfreier Si(100)-Waferoberflächen

     

Anchoring Properties of Nematic Liquid Crystals Studied Using the Attenuated Total Reflection Method

By using the attenuated total reflection method associated with the excitation of surface plasmons, the tilt angle of the liquid crystal director and its gradient at the surface are measured in a planar nematic cell as a function of the applied voltage. The surface anchoring anisotropy δπ of the liquid crystal and the surface elastic constant k_s, are found to be δπ = 0.288 erg/cm and k_s, = 9·12 × 10^-11 erg, respectively, when the boundary condition suggested by Barbero et al is used. The theoretical and experimental values obtained with this boundary condition and that of Mada are discussed. The results show that the boundary condition proposed by Barbero et al is in better agreement with the experiment.     

Observation of hydrogen induced intermediate borides in PrFeB based alloys by Mössbauer effect spectroscopy

In the present work, a quantitative analysis of the phase compositions by Mössbauer effect spectroscopy of solid and conventional hydrogen disproportionated Pr_13.7Fe_80.3B_6.0 and Pr_13.7Fe_63.5Co_16.7Zr_0.1B_6.0 alloys was carried out. Significant amounts of intermediate borides t-Fe₃B and Pr(Fe, Co)₁₂B₆ were detected after solid hydrogen disproportionation treatment in Pr_13.7Fe_80.3B_6.0 and Pr_13.7Fe_63.5Co_16.7Zr_0.1B_6.0 alloys, respectively. After conventional hydrogenation–disproportionation–desorption–recombination treatment these phases were not detected and in no case residual Pr₂Fe₁₄B-phase was found. It was observed that the amount of intermediate borides after disproportionation can be correlated with the degree of texture after recombination at various temperatures.