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  • 1
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 5 (1993), S. 141-147 
    ISSN: 1040-7685
    Keywords: light scattering detection ; supercritical fluid chromatography ; packed microcolumns ; argentation chromatography ; triacylglycerols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Packed capillary columns provide excellent separation of neutral lipids by supercritical fluid chromatography. For these separations, it is necessary to add a polar modifier to the mobile phase; hitherto, a detector suitable for quantitative analysis has been lacking. For this purpose, a miniaturized evaporative light scattering detector for combination with packed microcolumns in supercritical fluid chromatography has been developed. Since the detector response is dependent on the mobile phase flow rate, a drop in response was found at flow rates above 16 mL min-1 of expanded mobile phase. However, below this flow rate, there was a region of relatively constant response. In this region, quantitative analysis could also be successfully performed when the pressure and/or the temperature of the separation were programmed. The detection limit was lower than 6 ng. With pressure programming, the relative standard deviation in peak area was less then 4%. Minor peaks gave higher RSD values.Further, it is demonstrated that argentation SFC of triacylglycerols provides separation according to chain length as well as to the degree of unsaturation.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: In multi-component solution systems, the diffusion of one component can influence the diffusion of a second; in some instances, especially if the first component is an acid, the second component may diffuse against its own concentration gradient. The fundamental cause of this phenomenon is the local electrical field gradient established when particular ion species in mixtures of ionic components have different transport numbers. In ternary, quaternary and higher order systems, determination of the main and cross-term diffusion coefficients is difficult, and usually indirect.The Daresbury x-ray fluorescence (DXRF) microprobe was used to measure directly the concentrations of individual elements in an aqueous gel 1.45 mm from an interface with a solution of constant composition. The solutions contained known mixtures of cobalt, copper and zinc chlorides with and without hydrobromic acid. Similar measurements were made every 300 s over a period of 3 h. After this, measurements were made at 100 μm intervals from the interface of the gel to a depth of 6 mm to map the concentrations of Co, Cu and Zn.The diffusion coefficients were estimated by comparison of the concentration-time profiles for each metal with analytical or numerical simulations. The results show a significant coupling of the Cu, Co and Zn diffusive flows with the diffusive flow of the acid.This work has shown that the DXRF microprobe can be used to measure concentration-distance or concentration-time profiles of many elements simultaneously, thus enabling more direct measurements of multicomponent diffusion coefficients in solution to be made.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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