Intramolecular multiple scattering in electron diffraction from fluoro-methyl halides

Relative elastic differential cross sections for scattering of 1 keV electrons from CF₃H, CF₄, CF₃Cl, CH₃F and CH₃Cl molecules were measured for momentum transfer from 3 Å^?1 to 29 Å^?1. The oscillatory residuals remaining after substraction of the atomic scattering and the molecular interference contributions calculated in the independent atom model are ascribed to the influence of intramolecular multiple scattering. The data reflect the dominant contributions of the CF₃-group and show larger oscillations than obtained from triple scattering calculations according to the method of Liu and Bonham using the second Born approximation.     

Determination of thiopental in human serum and plasma by high-performance capillary electrophoresis-micellar electrokinetic chromatography.

The quantitation of thiopental in human serum and plasma was investigated using high-performance capillary electrophoresis (HPCE) in a micellar configuration and the results were compared with reversed-phase high-performance liquid chromatography (HPLC). Thiopental and an internal standard (carbamazepine for HPCE and thiamylal for HPLC) were extracted from serum or plasma using pentane and a phosphate buffer (pH 6.4). HPCE analysis took place in a phosphate-borate buffer with 50 mM sodium dodecyl sulphate using an automated instrument and HPLC was performed with a C8 column and a mobile phase of phosphate buffer-acetonitrile (65:35, v/v). HPCE and HPLC data from 66 patient samples compared well based on linear regression analysis. However, estimates obtained with the inclusion of the internal standard were lower than those based on the sample peak only. This example allows the elucidation of the advantages of using HPCE as an assay methodology for the therapeutic monitoring of thiopental and other drugs.     

A microcomputer-controlled titrator for automated individual analysis

A titration unit for automatic analysis systems is described. The titrator performs different titrations specified by strings of digital parameters. It has 4 independent titration stations with individual electrode systems. A multiburette with 20 cylinders provides all stations with the necessary reagents. End-point titrations, and incremental and equilibrium titrations are controlled by a microcomputer. In combination with a sample transport and a desk calculator, the titrator can be used to process automatically samples of different natures which require different treatment.     

Solvent release upon ion association from entropy data

The translational entropy loss on the association of two ions to form an ion pair or 11 complex is overcompensated by a rotational entropy gain, an electrostatic entropy gain, and an entropy gain due to solvent release from translational immobilization. The first three effects can be calculated, leaving the fourth as a difference from the experimental entropy change on association. The ratio of the solvent release entropy gain to the entropy change on melting of the solvent indicates the number of solvent molecules released on the association. A similar value is obtained from data for the volume change on association.Presented as a poster at the 10th International Conference on Non-Aqueous Solvents (ICNAS) at Leuven, Belgium, August 1986, and at the 24th International Congress on Coordination Chemistry (ICCC) at Athens, Greece, August 1986.     

Organic synthesis on the microgram scale. V

Summary This paper describes a method for theg synthesis of flavone acetates in a sealed capillary tube. The reaction products are separated and purified on a thin-layer plate. The esters are then hydrolyzed on the plate and the parent flavones regenerated. A simple heating device is used which allows for observation of the reaction.

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Zusammenfassung Beschreibung der Mikrogrammsynthese von Flavonacetaten in einem verschmolzenen Kapillarröhrchen. Die Reaktionsprodukte werden auf einer Dünnschichtplatte getrennt und gereinigt. Dann verseift man die Ester auf der Platte und stellt die freien Flavone dar. Ein einfaches Heizgerät ermöglicht die Beobachtung der Reaktion.

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For part IV of this series see Mikrochim. Acta [Wien]1969, 352.     

Characterization of SiC-platelets

Three fractions of SiC platelets were characterized using polarizing microscopy, X-ray diffraction, high resolution Auger electron spectroscopy (AES), electron spectroscopy for chemical analysis (ESCA) and scanning electron microscopy with energy dispersive analysis (SEM/EDX). The chemical analysis of the three fractions is given. The determination of the SiC polytypes (4H, 6H, 15R, 3C) was done and has been correlated with the chemical analysis. The results of the X-ray diffraction investigations confirm the polarizing microscopy observations. Using microanalytical techniques important conclusions about the impurity elements (e.g. B, Al, Fe) and their local distribution could be drawn. Most of them were found to be present on the outermost surfaces of the platelets. Some conclusions concerning the processing of the platelets are suggested.Dedicated to Professor Günther Tölg on the occasion of his 60th birthday     

Surface-enhanced Raman spectrometry with silver particles on stochastic-post substrates

A special type of substrate for surface-enhanced Raman scattering (s.e.r.s.) is evaluated. The substrates consist of silver particles deposited on stochastically arranged SiO₂ posts produced by plasma etching of a quartz surface using a silver island film as an etch mask. The optimization of various experimental parameters such as silver layer thickness, silver evaporation angle, and excitation energy are discussed in detail. Comparative studies with p-nitrobenzoic acid as the model compound indicate that this present substrate is at least one order of magnitude more effective than other common s.e.r.s. substrates, such as the silver island film and the crossed-grating surface, which were previously found to induce the strongest s.e.r.s. signals. The preparation of these silver-particle-post substrates avoids the elaborate lithographic procedures required for crossed-grating structures. The quantitation of species in a three-component mixture illustrates the selectivity of the s.e.r.s. technique.     

Relation of the Gibbs free energy of transfer of ions from water to polar solvents to the properties of the solvents and the ions

A statistical treatment of data for the standard molar Gibbs free energies of transfer of monovalent ions from water to polar solvents has been made in terms of properties of the solvents and the ions. A common multiple regression equation with seven fitting constants, for almost 200 data points, has been found to describe the data in terms of four solvent properties: their electron donor and acceptor abilities, dielectric constant, and cohesive energy density, and three ionic properties: charge, size, and softness. For the ions Na⁺, K⁺, Rb⁺, Cs⁺, Tl⁺, (Ph)₄As⁺, Cl^?, Br^? and N ₃ ^? the predictions of the equation are within acceptable error limits of the data, and encourage its application to solvents beyond the thirteen used for the data base. For other ions, e.g. H⁺, Ag⁺, and the larger anions, further interactions must be taken into account.