Gas chromatographic-mass spectrometric analysis of acids and phenols in distilled alcohol beverages. Application of anion-exchange disk extraction combined with in-vial elution and silylation

A GC-MS protocol for profiling spirits, based on 19 acids and phenolic compounds, has been proposed and evaluated. The method combined a simple preconcentration procedure based on solid-phase (anion-exchange) disk extraction, and in-vial elution and silylation of the analytes. The derivatized extract was directly injected into the GC-MS system. These analytes were: C6, C8, C10, C12 acids, pyruvic acid, 2-furoic acid, succinic acid, fumaric acid, glutaric acid, lactic acid, glycolic acid, malic acid, tartaric acid, citric acid, vanillin, syringaldehyde, coniferaldehyde, vanillic acid and gallic acid. The profiles of six different spirits were found reproducible from day-to-day with <20% RSD for measurements of most of the analytes at different concentrations. Recoveries of individual analytes appear to be affected by the level of tannins in the spirits, and they varied from sample to sample. The method of standard addition was used to quantify age-related analytes. Good linearity of response with correlation coefficients in the range of 0.992-0.999 was obtained. The results of the study indicate that for spirits of the same brand but of different ages, the amounts of these analytes appear to increase with the ageing period.     

Visualization of enantiomers in cholesteric solvents through deuterium NMR

Abstract

Proton decoupled deuterium NMR of mixtures of enantiomers in homogeneously oriented cholesteric solvents produces simple spectra with linewidths of 10 to 50 Hz in cases where the proton spectra would give second order patterns so complicated as to defy analysis. The chiral solvent orders each of a pair of enantiomers differently which results in a difference in the residual quadrupolar coupling constant yielding well resolved spectra for each enantiomer. That the technique constitutes a new tool for measurement of enantiomeric ratios is illustrated using several chiral benzylic alcohols.     

Effect of Addition of MTES on the Structure of Siloxane-PPG Nanocomposites

Hybrid transparent and flexible siloxane-polypropyleneglycol (PPG) materials with covalent bonds between the inorganic (siloxane) and organic (polymeric) phases were prepared by sol-gel process. In order to improve the quality of the mechanical properties of these materials, different amounts of methyltriethoxysilane (MTES) were added to the initial sol. The effect of MTES addition on the structure of the composites was studied by Small-Angle X-Ray Scattering (SAXS) and ²⁹Si Nuclear Magnetic Resonance (²⁹Si NMR). In absence of MTES, SAXS spectra exhibit a peak that is assigned to spatial correlation due to short range order between the siloxane clusters embedded in the polymeric phase. The experimental results indicate that, for low MTES concentrations ([MTES]/[O] 0.8, O: ether-type oxygen of PPG), the silicon species resulting from hydrolysis and condensation of MTES fill the open spaces between polymeric chains, interacting with the ether-type oxygens. For larger MTES content ([MTES]/[O] 0.8), the number of free ether-type oxygen sites avalaible for reaction with such silicon species is not large enough. Consequently, a fraction of silicon species resulting from MTES addition graft to siloxane clusters formed by hydrolysis and condensation of the hybrid precursor. For all MTES concentrations the condensation degree of the siloxane phase, determined from ²⁹Si NMR spectroscopy, is high (>69%), as expected under neutral pH synthesis conditions.     

NMR study of the magnetic properties of the polymerized phase of Cs1C60

\chem{Cs_{1}C_{60}} . The NMR spectrum allows, when the Magic Angle Spinning (MAS) technique is used, to get information about the electronic structure of this phase, which points out that the spin density is not uniformly distributed on the ball. An estimation of the strength of the quadrupolar effects on is then given, which shows that it is possible to analyse the spin-lattice relaxation time in terms of magnetic effects. A comparison with the of is then justified and allows us to point out the importance of low dimensional antiferromagnetic fluctuations in this compound. We also investigate the nature of the magnetic ground state in : the broadening of the spectra states unambiguously its magnetic nature and a detailed analysis of their shape gives further indications on the antiferromagnetic nature of the magnetic order, which seems characterized by a large amount of disorder. Received: 19 November 1996/Accepted: 19 December 1996     

Remarques sur les variétés conformément plates

Sans résumé     

How does imposing a step-by-step solution method impact students’ approach to mathematical word problem solving?

This paper presents the second phase of a larger research program with the purpose of exploring the possible consequences of a gap between what is done in the classroom regarding mathematical word problem solving and what research shows to be effective in this particular field of study. Data from the first phase of our study on teachers’ self-proclaimed practices showed that one-third of elementary teachers from the region of Quebec require their students to follow a specific sequential problem-solving method, known as the ‘what I know, what I look for’ method. These results led us to hypothesize that the observed gap may have an impact on students’ comprehension of mathematical word problems. The use of this particular method was the foundation for us to study, in the second phase, the effect of the imposition of this sequential method on students’ literal and inferential understanding of word problems. A total of 278 fourth graders (9–10 years old) solved mathematical word problems followed by a test to assess their understanding of the word problems they had just solved. The results suggest that the use of this problem solving method does not seem to improve or impair students’ understanding. From a more fundamental point of view, our study led us to the conclusion that the way word problem solving is addressed in the mathematics classroom, through sequential and inflexible methods, does not help students develop their word problem solving competence.     

Inner membrane lipids of Escherichia coli form domains

In prokaryotic cells, the hypothesis of the existence of lipid domains was considered. In order to test this hypothesis and study the organization of lipids in the inner membrane of Escherichia coli, we elaborated Langmuir films mimicking the inner leaflet of this membrane by considering lipids extracted from the inner membrane of E coli by Folch protocol.

Lipid monolayers were elaborated by using these extracts (Langmuir technique); the organization of the resulting films was studied at the air–water interface by Brewster angle microscopy and after transfer onto muscovite by atomic force microscopy. The existence of domains was demonstrated for different interfacial pressures of biological interest, and their stability was studied.     

Transimination: An efficacious reaction for the synthesis of macrocycles

A new family of main-chain liquid crystal polymers containing azomethine units have been synthesized and characterized. Our attention has been focused on their strong tendency to generate macrocyclic dimers (AB)² constituted with two mesogenic rods and siloxane spacers. In favourable conditions (diluted solution, acid catalysis) macrocycles may be rapidly formed and purely obtained by fractionation. Synthetic aspects and main thermotropic properties are discussed. In spite of their large size some macrocycles have been obtained as single crystals and then characterized by X-ray diffraction.     

A remark about static space times

We discuss a differential equation, whose unknowns are a function and a Riemannian metric. This equation occurs both in general relativity (static space times) and in the study of the space of Riemannian metrics on a manifold (singularities of the map from the space of metrics into the space of functions, which assigns to any metric its scalar curvature).     

Demonstration of fiber-laser-produced plasma source and application to efficient extreme UV light generation

Efficient generation of extreme UV (EUV) light at lambda = 13.5 nm from a bulk Sn target has been demonstrated by using a fiber laser. The conversion efficiency from the 1064 nm IR to the EUV was measured to be around 0.9% into 2pi steradians within a 2% bandwidth. To the best of our knowledge, this is the first time an all-fiber system was used to generate EUV or soft x rays.