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A method for semi-automatic background estimation in energy-dispersive x-ray fluorescence spectra is outlined. Two cubic splines were investigated and the spline called the Butland interpolant was chosen for further investigation. Prior to the calculation of the spline, peak regions are set up, and suitable knots are defined outside the peak regions. To set up the peak regions, an automatic peak-search routine and a calibration equation are used. For a given peak, the latter relates the full width at half maximum (FWHM) to the peak centre. In turn, the size of the peak regions are defined by the FWHM multiplied by a constant given by the user. The method was tested on several types of spectra. It was found that the optimal size of the peak region decreased with increasing peak density. Reproducibility tests showed that the standard deviation of the summation of counts within a peak region and after background subtraction was less than would be expected from the counting statistics. 相似文献
56.
[reaction: see text] The combination of catalytic palladium(0) and Trost ligand provides an effective catalyst for the rearrangement of allyl beta-ketoesters. The mechanism of the transformation involves formation of pi-allyl palladium intermediates which undergo enantioselective attack by ketone enolates. Decarboxylation of beta-ketocarboxylates allows regiospecific generation of enolates under extremely mild conditions. 相似文献
57.
H. Flyger J. Fenger E. Lund Thomsen E. Lewin S. E. Gryning E. Lyck 《Fresenius' Journal of Analytical Chemistry》1976,282(4):297-300
Summary Pertinent, previous studies of the oxidation of SO2 in the atmosphere are briefly reviewed. A project dealing with the conversion in the plume from an oil-fired power station is described in greater detail. Measurements were performed from an aircraft and included continuous registration of NOx, SO2 and ozone concentrations. The possibility of using NOx as an internal tracer is discussed; also the use of the inert tracer SF6 is treated and a special detector for the continuous registration of SF6 in relative concentrations down to 10–6 ppm is described. Preliminary results indicate a half-life for SO2 in the plume of about half an hour.
Umsetzung von Schwefeldioxid in der Atmosphäre
Zusammenfassung Einschlägige frühere Studien über die Oxidation von SO2 in der Atmosphäre werden kurz diskutiert. Ein Projekt zum Studium der Umwandlung im Abrauch eines ölbefeuerten Kraftwerkes wird im Detail beschrieben. Die Messungen wurden mit Hilfe eines Flugzeuges vorgenommen und schließen die kontinuierliche Aufzeichnung von NOx-, SO2- und Ozon-Konzentrationen ein. Die Möglichkeit der Verwendung von NOx als interner Indicator wird diskutiert. Außerdem wird der Gebrauch des inerten Indicators SF6 behandelt und ein spezieller Detektor für die kontinuierliche Aufzeichnung von SF6 mit relativen Konzentrationen bis herunter auf 10–6 ppm beschrieben. Vorläufige Ergebnisse deuten auf eine Halbwertszeit von SO2 im Abrauch von etwa 30 min hin.
Presented at the 6th Annual Symposium on Recent Advances in the Analytical Chemistry of Pollutants, April 21–23, 1976; Vienna, Austria 相似文献
58.
Jon Volden Yngvar Thomassen Tyge Greibrokk Syvert Thorud Paal Molander 《Analytica chimica acta》2005,530(2):263-271
The storage stability of the occupationally frequently occurring compounds, methylethylketone, methylisobutylketone, benzene, toluene, tetrachloroethylene, n-butylacetate, -pinene, β-pinene, limonene and n-decane, has been investigated on the adsorbents Tenax TA, Chromosorb 106 and Carbotrap using thermally desorbable tube type samplers, commonly utilized in ambient and workroom atmospheric measurements. Fifty and 500 ng of each compound were loaded on the various adsorbents tubes, stored at both ambient (20 °C) and refrigerated (4 °C) temperatures and analysed by means of thermal gas chromatography with mass spectrometric detection on days 0, 7, 14 and 28 after exposure. A 90% storage recovery was chosen as acceptance criteria for storage stability, and statistical testing by Student's t-test, analysis of variance and Bonferroni post hoc tests were employed to investigate the effect of the categorical variables storage time, storage temperature and analyte loading on the different adsorbents. Chromosorb 106 showed the overall best behaviour with recoveries of 90% or better for all analytes during the 28-day test period. Tenax TA and Carbotrap yielded lower recoveries and were more influenced by variations in storage time, storage temperature and analyte loading. Refrigerated temperatures were best avoided for storage on Tenax TA, but may increase the recovery of some compounds on Carbotrap (e.g. n-butylacetate). The blank build-up on the adsorbents was also investigated, and Carbotrap and Tenax TA showed no signs of artefact development over time. Chromosorb 106, however, contained inherently more artefacts that build up over time, which in spite of the excellent storage capability, may limit its use in field studies where long storage times are normal. 相似文献
59.
The structure and configuration of gilmaniellin, a metabolite of Gilmaniella humicola BARRON , has been shown to be 2 by X-ray analysis. By comparison of spectral data structure 1 has been assigned to dechlorogilmaniellin. 相似文献
60.
[Reaction: see text] Various substituted conjugated dienes have been made by olefin cross-metathesis. Using either electronic or steric "protection," one of the olefins of the conjugated diene was deactivated relative to the other for cross-metathesis. The reactions proceed with very high chemoselectivity and, when steric deactivation is used, very high diastereoselectivity. 相似文献