Capacitance-conductance detector for high-pressure liquid chromatography. Application to alkaloids and fatty acids

Summary A new type of detector for high-pressure liquid chromatography has been designed. This detector is equipped with a RC resonance circuit, and is similar to the capacitance detector previously reported. It is operated as a capacitance detector with nonpolar eluents; while with polar solvents, it behaves as a conductance detector. Electrolytes such as salts, acids and bases are sensitively detected. The detector was successfully used for the detection of fatty acids and alkaloids.

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Zusammenfassung Ein neuartiger Detektor für die Hochdruck-Flüssigchromatographie wurde entwickelt. Dieser ist mit einem Resonanzstromkreis ausgestattet und ähnelt dem kürzlich beschriebenen Kapazitanz-Detektor. Als solcher funktioniert er mit nichtpolaren Eluenten, während er sich mit polaren Lösungsmitteln wie ein Leitfähigkeitsdetektor verhält. Salze, Säuren und Basen werden empfindlich nachgewiesen. Das Gerät wurde zum Nachweis von Fettsäuren und Alkaloiden verwendet.

     

Electric-field oriented polymer blend film for proton conduction

A novel proton conductor has been realized by employing a ternary polymer blend system in combination with an electric-field orientation technique. A polymer film recast from a solution containing poly(acrylic acid), poly(vinyl butyral), and fluoroalkyl graft polymer under 2 kV.cm(-1) exhibited 10 times higher proton conductivity than that prepared without the external electric field. However, when the film was prepared under a field higher than 4 kV.cm(-1), proton conductivity decreased. The membranous character has been investigated by SEM and AFM observations. As a result, it has been proven that an electric-field treatment of 2 kV.cm(-1) forms the largest hydrophilic domains for proton conduction in the film. The alteration of the phase separation morphology induced by the electric field well explains the proton conductivity change.     

The formation of clathrate-like hydrates of tetrabutylammonium halogenated carboxylates

The solid-liquid phase diagrams of binary mixtures of tetrabutylammonium halogenated carboxylates with water were examined in order to confirm the formation of clathrate-like hydrates. It was found that, among thirteen carboxylates examined, four carboxylates having CH₂FCOO^–, CHF₂COO^–, CF₃COO^–, and CH₂ClCOO^–, formed a hydrate with hydration numbers around 30 and seven carboxylates having CHCl₂COO^–, CCl₃COO^–, CH₂BrCOO^–, CHBr₂COO^–, CBr₃COO^–, CH₃CHClCOO^–, and CH₃CHBrCOO^– formed a hydrate with hydration numbers around 23. The latter hydrate has not been reported earlier. The melting points of these newly found hydrates were fairly high: they lie between 10 and 16°C. The effect of Cl and Br atoms attached to the carbon atom of the-position of a carboxylate anion both on the type of hydrate formed and on its stability was greatly different from that of a CH₃ group attached to the same position of the carboxylate anion.Dedicated to Dr D. W. Davidson in honor of his great contributions to the sciences of inclusion phenomena.     

Subincanadines A-C,novel quaternary indole alkaloids from Aspidosperma subincanum

Three novel quaternary indole alkaloids with an unprecedented 1-azoniatricyclo[4.3.3.0(1,5)]undecane moiety, subincanadines A-C (1-3), as well as two new indole alkaloids with a 1-azabicyclo[5.2.2]undecane moiety, subincanadines D (4) and E (5), and a new indole alkaloid with a 1-azabicyclo[4.3.1]decane moiety, subincanadine F (6), have been isolated from the barks of Aspidosperma subincanum Mart, and the structures of 1-6 and the stereochemistry of 1-3 were elucidated by spectroscopic data and chemical means.     

Stereochemistry of reduction of the C-24,25 double bond in the conversion of desmosterol into cholesterol

Feeding of the chemically prepared [24-¹³C, 24-²H]desmosterol to cell-free systems derived from rat liver and silkworm gut and to cultured cells of Oryza sativa followed by deuterium-decoupled ¹H, ¹³C shift correlation NMR analysis of the biosynthesized cholesterol revealed the stereospecific incorporation of hydrogen atoms from the re-face of the C-24 position of desmosterol.     

Formation and characterization of high-density Fe cluster-assembled films with soft magnetic behaviors

High-density, magnetically soft Fe cluster-assembled films were obtained at room temperature by an energetic cluster deposition. Size-monodispersed Fe clusters with the mean cluster size d = 9, 13 and 16 nm were produced using a plasma-gas-condensation technique. Ionized clusters in cluster beam were accelerated electrically and deposited onto the substrate together with neutral clusters from the same cluster source. The morphology, microstructure and magnetic properties of the cluster-assembled films have been studied by an atomic force microscopy, scanning electron microscopy, transmission electron microscopy, and superconducting quantum interference device magnetometer. By increasing the impact energy of the ionized clusters up to 0.6 eV/atom, the Fe cluster-assembled film has a packing fraction of 0.86±0.03, and reveals a soft magnetic behavior. In addition, it is found that oxidization of the cluster-assembled films is remarkably suppressed with the increase in the density of the films.     

Thin-layer chromatographic behaviour and separation of rare earths in silica gel-aqueous alkali metal chloride systems

Summary The thin-layer chromatographic behaviour of all the rare earths except Pm on silica gel in aqueous solutions of five alkali metal chlorides has been surveyed. The Rf-values and the logarithms of the separation factors relative to Gd vary in a regular and peculiar way with increasing atomic number, through a reflection of the strong tetrad effect. A discussion concerning the effects on the Rf-values of the solvent cations and the solvent anions, and typical chromatograms for the separations of multi-component mixtures containing adjacent lanthanoids are also presented.     

Structure comparison between Th2Zn17-type and TbCu7-type Sm–Fe intermetallic compounds and their nitrides by means of 57Fe-Mössbauer spectroscopy

Samarium–iron intermetallic compounds were prepared by a melt spinning method with low and high wheel speeds, which resulted in a Th₂Zn₁₇-type and a TbCu₇-type structure, respectively. Structure comparison between these types was investigated for Sm–Fe intermetallic compounds and their nitrides by ⁵⁷Fe-Mössbauer spectroscopy.