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  • 1
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; On-line LC-CE ; Sample pretreatment ; Matrix effects ; Benzoic acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Various methods are currently under investigation to improve concentration detection limits in capillary electrophoresis (CE). Stacking and isotachophoresis coupled in-line with free-solution electrophoresis are the techniques most frequently used. Samples containing a high and/or varying salt concentration, such as urine and serum, are difficult to handle: usually a significant loss in electrophoretic efficiency is observed compared with samples possessing a low electric conductivity. In the present paper an alternative approach is developed, i.e. a liquid chromatographic (LC)-type of sample pretreatment is coupled on-line with CE. To demonstrate the feasibility of this approach, the separation of three model compounds (benzoates) in water containing up to 400 mM of sodium chloride is studied using a 50 mM borate CE buffer of pH 9.5. The direct injection of samples with high salt concentrations in CE results in peak splitting and/or serious band broadening. These problems are not encountered when using the present LC-CE system. In addition, the detection limits are hardly influenced by the salt concentration of the sample; this underlines the robustness of the system.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 44 (1997), S. 129-134 
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; Temperature control ; Thermostating
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of high voltages across a electrophoresis capillary will increase the temperature of the buffer due to Joule heating. As a result temperature control in CE is rather important since variations in the buffer temperature will result in changes in the pH of the buffer, peak shape, migration time, reproducibility, efficiency, 3-D structure of macromolecular analytes, etc. Six different thermostating systems have been evaluated: (i) natural convection, (ii) fan, (iii) home-made and (iv and v) two commercially available high-speed air and a (vi) liquid thermostated device. In all cases the temperature of the buffer in the capillary is calculated according to the temperature-conductivity relationship. For this purpose two parameters are introduced describing temperature control: the temperature onset (δT) and the temperature rise factor (α). From these results, it can be concluded that high speed air thermostating can be as efficient as liquid thermostating.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 459-464 
    ISSN: 0935-6304
    Keywords: Fast gas chromatography ; gas chromatography ; resistive heating ; organophosphorus pesticides ; PAHs ; triazines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The features of a resistive-heated capillary column for fast temperature-programmed gas chromatography (GC) have been evaluated. Experiments were carried out using a commercial available EZ Flash GC, an assembly which can be used to upgrade existing gas chromatographs. The capillary column is placed inside a metal tube which can be heated, and cooled, much more rapidly than any conventional GC oven. The EZ Flash assembly can generate temperature ramps up to 1200°/min and can be cooled down from 300 to 50°C in 30 s. Samples were injected via a conventional split/splitless injector and transferred to the GC column. The combination of a short column (5 m×0.25 mm i. d.), a high gas flow rate (up to 10 mL/min), and fast temperature programmes typically decreased analysis times from 30 min to about 2.5 min. Both the split and splitless injection mode could be used. With n-alkanes as test analytes, the standard deviations of the retention times with respect to the peak width were less than 15% (n = 7). First results on RSDs of peak areas of less than 3% for all but one n-alkane indicate that the technique can also be used for quantification. The combined use of a short GC column and fast temperature gradients does cause some loss of separation efficiency, but the approach is ideally suited for fast screening as illustrated for polycyclic aromatic hydrocarbons, organophosphorus pesticides, and triazine herbicides as test compounds. Total analysis times - which included injection, separation, and equilibration to initial conditions - were typically less than 3 min.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 269-270 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 271-272 
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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