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  • 1
    ISSN: 0935-6304
    Keywords: On-line SFE-GC ; Split/splitless interface ; Quantitative aspects ; Discrimination ; Reproducibility ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The quantitative aspects of on-line supercritical fluid extractioncapillary gas chromatography (SFE-GC) with a split/splitless injector as interface were investigated. Special attention was paid to the discrimination behavior and the reproducibility of the split/splitless interface. A simple experimental set-up is proposed that allows accurate quantitation in on-line SFE-split GC. The results obtained in on-line SFE-GC compare favorably with those from conventional GC with split injection. Discrimination was found to be absent when working at sufficiently high interface temperatures. Finally, the effects of the carbon dioxide flow rate, interface temperature and split ratio on both discrimination and reproducibility were studied.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0935-6304
    Keywords: Fused silica model substrates ; Adsorption characteristics ; Surface OH distribution ; Inverse gas-solid chromatography ; 29Si CP MAS NMR ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The possibilities of inverse gas-solid chromatography (IGC) in obtaining chromatographic data on fumed silica were examined. Aerosil A-200, a fused silica model substrate in 29Si nuclear magnetic resonance analysis, was trimethylsilylated to different degrees. IGC was used to very reproducibly determine the free specific energies of adsorption of several functionalized probe solutes. Hydrogen bonding solutes have a free specific energy of adsorption that is at least about 50% higher than that of non-hydrogen bonding probe solutes. NMR was used in combination with elemental analysis to calculate surface concentrations of the different chemical surface structures. IGC data and surface concentrations were combined in order to determine the contribution of each type of surface structure to the total free specific adsorption energy. It could be concluded that residual silanols from the reaction of dihydroxydi-siloxysiloxane (Q2 groups) with trimethylchlorosilane possess a higher adsorption activity than the silanols initially present.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction (SFE) ; On-line SFE-GC ; Programmed temperature vaporizer (PTV) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative transfer of solutes to the seperation column. The problems caused by impurities in the extraction fluid in on-line SFE-GC are discussed. Simple methods are described for the purification of commercially available carbon dioxide. The trapping efficiency of the PTV injector is studied. Applications of the SFE-PTV-GC system are given for the analysis of polymer anti-degradants, polar compounds, and samples with environmental relevance.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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