Development and evaluation of an interface for coupled capillary supercritical fluid chromatography/magnetic sector mass spectrometry. Application to thermally unstable and high molecular mass compounds

An interface for coupling supercritical fluid chromatography to a magnetic sector mass spectrometer was developed and evaluated. The interface is based on direct introduction of the mobile phase, carbon dioxide, into the ion-source of the mass spectrometer. The SFC-MS system was optimized with respect to the signal-to-noise ratio. Under optimized conditions, the estimated detection limit for n-pentadecane is approximately 30 ppm. Spectra obtained in the electron-impact ionization mode show a very good similarity with library spectra. The performance of the SFC-MS system was evaluated by the analysis of a number of test mixtures. A sample containing several low molecular mass, thermally unstable compounds, which could neither be analyzed by GC-MS nor by LC-MS, was analyzed. Also for the analysis of high molecular mass compounds, the coupled system showed a good performance.     

Synthesis and Controlled Polymerisation of a Novel Gramicidin S Analogue

Summary: The controlled polymerisation of a bulky, peptide‐based monomer was investigated. The cyclic β‐sheet forming decapeptide gramicidin S was modified with a methacrylate handle and subsequently polymerised via atom transfer radical polymerisation (ATRP), to yield a well‐defined gramicidin‐S‐containing polymer. The secondary structure of the peptide moiety was retained within the resulting polymer, as indicated by IR spectroscopy. This is the first example of the use of ATRP to create a synthetic polymer with a cyclic peptide as a side chain.

The gramicidin S based monomers synthesised here were then polymerised by ATRP.     

Experimental visualization of temperature fields and study of heat transfer enhancement in oscillatory flow in a grooved channel

An experimental study was conducted of incompressible, moderate Reynolds number flow of air over heated rectangular blocks in a two-dimensional, horizontal channel. Holographic interferometry combined with high-speed cinematography was used to visualize the unsteady temperature fields in self- sustained oscillatory flow. Experiments were conducted in the laminar, transitional and turbulent flow regimes for Reynolds numbers in the range from Re = 520 to Re = 6600. Interferometric measurements were obtained in the thermally and fluiddynamically periodically fully developed flow region on the ninth heated block. Flow oscillations were first observed between Re = 1054 and Re = 1318. The period of oscillations, wavelength and propagation speed of the Tollmien–Schlichting waves in the main channel were measured at two characteristic flow velocities, Re = 1580 and Re = 2370. For these Reynolds numbers it was observed that two to three waves span one geometric periodicity length. At Re = 1580 the dominant oscillation frequency was found to be around 26 Hz and at Re = 2370 the frequency distribution formed a band around 125 Hz. Results regarding heat transfer and pressure drop are presented as a function of the Reynolds number, in terms of the block-average Nusselt number and the local Nusselt number as well as the friction factor. Measurements of the local Nusselt number together with visual observations indicate that the lateral mixing caused by flow instabilities is most pronounced along the upstream vertical wall of the heated block in the groove region, and it is accompanied by high heat transfer coefficients. At Reynolds numbers beyond the onset of oscillations the heat transfer in the grooved channel exceeds the performance of the reference geometry, the asymmetrically heated parallel plate channel. Received on 26 April 2000     

Preparation and Fungitoxicity of Some Trichloro-, Tribromo-, Tetrachloro-, and Tetrabromo-8-Quinolinols

 3,5,6-, 3,5,7-, 4,5,7-, and 5,6,7-trichloro- and -tribromo-8-quinolinols as well as 3,5,6,7-tetrachloro- and -tetrabromo-8-quinolinols were prepared and tested against six fungi (Aspergillus niger, Aspergillus oryzae, Myrothecium verrucaria, Trichoderma viride, Mucor cirinelloides, and Trichophyton mentagrophytes) in Sabouraud dextrose broth. The compounds strongly inhibit five fungi but not M. cirinelloides. They are less active than the related dichloro-8-quinolinols which is attributed to steric hindrance.     

Determination of phosphine in biogas and sludge at ppt-levels with gas chromatography-thermionic specific detection

A gas chromatographic (GC) system to measure free phosphine in biogas and matrix bound phosphine in manure and sludge is presented. The system consists of a sample preconcentration trap filled with glass beads, connected with a capillary GC equipped with a thermionic specific detector. With a trap temperature as low as -155 degrees C, a sampling flow of 20 ml/min and a typical total sample volume of 100 ml, free phosphine concentrations in the low ng/m3 range and matrix bound phosphine in the low ng/kg dry matter range, can be accurately and reproducibly determined.