The purification of morin

Chemistry of Natural Compounds -     

Synthesis and Characterization of Microporous Titania Membranes

A procedure for the preparation of microporous titania membranes by the polymeric sol-gel technique is reported. The influence of acid/titanium ratio, water/titanium ratio, method of mixing components and refluxing time on particle size and sol stability was investigated. The thermal evolution, structural characteristics and liquid permeation properties of calcined materials were studied. Highly reproducible amorphous microporous titania layers with pore sizes ≤0.8 nm were obtained on both mesoporous γ-alumina and titania/zirconia coated substrates. The upper limit of thermal stability of the amorphous phase is ～300°C. Higher calcination temperatures led to phase transformation into anatase, which was accompanied by a collapse of the microstructure. The material was found to be chemically stable in a wide pH interval.     

Once again about determination and detection limits

The papers takes stock of different methods for evaluating the detection (c _min) and determination (c _lim) limits of components described in the literature and presents a comparative analysis of the results of such evaluations. It is shown that use of the data on the fluctuations of the blank experiment, in spite of their wide application for such evaluations, gives ambiguous estimates for c _min and c _lim. The most correct method for evaluating the specified parameters is the experimental determination of the actual analyte concentration (content) from the empirical concentration dependence of the relative standard deviation. In case when this estimation method cannot be used, it is recommended to evaluate c _lim by the lower boundary of the calibration graph. The article may be useful for inexperienced analysts experimenters in choosing a method for evaluating the results obtained.     

Investigation of Mercury(I) Dimedonate as a Reference Sample for Atomic-Absorption Spectrometry

It is shown that mercury(I) dimedonate meets the requirements imposed on the certified materials: it is homogenous and stable and the absolute value of the error of determination of mercury in a sample at P = 0.95 is 0.22%. A procedure is developed for the atomic-absorption determination of mercury in river water using the new reverence material.     

Synthesis of benzophenone-containing analogues of phosphatidylcholine

As part of a collaborative study of cellular efflux of cholesterol and phospholipids, photoactivable analogues 4-8 of phosphatidylcholine (PC) having benzophenone groups in the choline moiety and at the end of the C2 and C1 alkyl chains have been synthesized. The efficient preparation via Suzuki coupling of the appropriate long-chain benzophenone-containing carboxylic acid and alcohol and their incorporation by adaptation of known approaches into the acyl- and ether-linked PC analogues 6-8 are described. Development of a method for radiolabeling these PC analogues, via hydrogenation of a double bond in modified side chains, is also described.     

The molecular composition of non-modified and acac-modified propoxide and butoxide precursors of zirconium and hafnium dioxides

Long-term storage at 0 °C of a paraffin-sealed flask with commercial 70 wt% solution of zirconium n-propoxide in n-propanol resulted in crystallization of an individual oxoalkoxide complex Zr₄O(OⁿPr)₁₄(ⁿPrOH)₂ in over 20% yield. The structure of this molecule can be described as a triangular Zr₃(μ₃-O)(OR)₁₀(ROH) core of 3 edge-sharing octahedrons with an additional Zr(OR)₄(ROH) unit attached through a pair of (μ-OR) bridges. Mass spectrometric and ¹H NMR investigation of the commercial samples of the most broadly applied zirconium and hafnium n-propoxides and n-butoxides indicate the presence of analogous species in the commercial alkoxide precursors. The content of oxo-alkoxide species in the commercial precursors has been estimated to be ~20% for n-propoxide and ~35% for zirconium n-butoxide. A new route has been presented for synthesis of the individual crystalline mixed ligand precursor [Zr(OⁿPr)(OⁱPr)₃(ⁱPrOH)]₂, from zirconium n-propoxide. A high yield has been observed (~90%), indicative of an almost complete precursor transformation. Mass spectrometry has shown that the synthesized mixed ligand precursor is dimeric, which makes it an attractive alternative to zirconium n-propoxide. Addition of 1 eq of Acetylacetone to zirconium or hafnium alkoxide precursors results in formation of dimeric [M(OR)₃(acac)]₂ in high yields. These species have limited stability (much higher for Hf than for Zr) and transform in solution into hydrolysis-insensitive M(acac)₄ through very unstable M(acac)₃(OR) intermediates containing 7-coordinated metal centers. This transformation can be followed kinetically in hydrocarbon solvents by ¹H NMR and is noticeably accelerated by addition of parent alcohols. The obtained results clearly reveal limited applicability of EXAFS and XANES techniques for the study of such systems, especially in the context of structure prediction. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

First observation of 55, 56Zn

In an experiment at the SISSI/LISE3 facility of GANIL, the most proton-rich zinc isotopes ^55,56Zn have been observed for the first time. The experiment was performed using a high-intensity ⁵⁸Ni beam at 74.5 MeV/nucleon impinging on a nickel target. The identification of ^55,56Zn opens the way to ⁵⁴Zn, a good candidate for two-proton radioactivity according to theoretical predictions. Received: 31 October 2000 / Accepted: 9 November 2000