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  • Analytical Chemistry and Spectroscopy  (3)
  • Liquid chromatography  (3)
  • Sample pretreatment  (2)
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 47 (1998), S. 313-345 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Sample pretreatment ; Coupling on-line to capillary GC ; Robotization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Sample pretreatment is often the bottleneck of a tracelevel analytical procedure. In order to increase performance, increasing attention is therefore being devoted to combining sample pretreatment on-line with the separation technique that has to be used. In the present review, a variety of procedures in use today for sample treatment coupled on-line to capillary gas chromatography (GC) is briefly discussed. Special attention is devoted to coupled-column techniques such as SPE-GC and LC-GC (SPE, solid-phase extraction; LC, column liquid chromatography) which are topics of much current interest, also because of their frequent use in so-called hyphenated systems.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Liquid chromatography ; Chlorophenols in water ; Preconcentration ; Post-column photochemical dechlorination ; Electrochemical, UV and fluorescence detection ; Column switching
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A specific HPLC method has been developed for the trace analysis of lower chlorinated aromatic compounds. The method consists of an on-line preconcentration and a post-column reaction step. On-line preconcentration of mono- and dichlorophenols from aqueous samples has been performed using PRP1, a divinylbenzene-styrene copolymeric sorbent as packing material for both pre-and analytical column. Enrichment factors of over 300 were obtained compared to regular (100 μl) loop injections, even for the highly polar monochlorophenols. After reversed-phase separation, post-column photochemical dechlorination is carried out directly in the eluent stream, using a photochemical reactor. Upon dechlorination, fluorescent products are formed, which can be detected selectively. The resulting fluorescence signal shows a linear response to the quantity of solute present over 2 to 3 orders of magnitude (correlation coefficients: 0.990–0.98). For the mono- and dichlorophenols, the detection limit of the photoconversion method is in the lower nanogram range. The method is especially suitable for the analysis of complex matrices such as effluent water samples or biological fluids containing traces of the polar chloroaromatic compounds together with large amounts of other constituents, which interfere when using more general methods of detection like UV absorption. The potential of this technique for automation has been demonstrated by using a microprocessor-controlled column switching unit.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1612-1112
    Keywords: Liquid chromatography ; Photochemical reaction detection ; Chemical post-column reduction ; Fluorimetric detection ; Air segmented flow systems ; Non-aqueous reversed-phase chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new photochemical reaction method for the on-line fluorimetric detection of natural vitamin K homologs was developed. In addition to its high sensitivity, the method features an interesting selectivity for the determination of these compounds in a complex matrix such as human serum. The formation of different photolysis products as a function of reaction conditions, and the optimalisation of a segmented flow reaction system will be discussed. The results indicate that the method is 4 times more sensitive than UV detection, and at least as selective as fluorescence detection after post-column chemical reduction.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 16 (1982), S. 237-241 
    ISSN: 1612-1112
    Keywords: Liquid chromatography ; Electron capture detection ; Improved interface
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An improved interface for the coupling of a liquid chromatograph (LC) and an electron-capture detector (ECD) allows the use of the LC-ECD combination for the determination of various types of chlorinated aromatic compounds. The addition of up to 6% of dioxan to the hexane used as mobile phase can be tolerated without serious deterioration of detector performance. Derivatization of polar compounds such as anilines, phenylurea herbicides, chlorophenols and hydroxylated polychlorobiphenyls with fluorine-and non-fluorine-containing acid anhydrides is a useful tool to extend the application range of LC-ECD. As an example, the analysis of a spiked soil sample is discussed.
    Type of Medium: Electronic Resource
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  • 5
    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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  • 6
    ISSN: 0935-6304
    Keywords: Coupling LC/GC ; Retention gap ; Polychlorinated biphenyls ; Sediment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Narrow-bore column liquid chromatography coupled on-line with capillary gas chromatography (LC/GC) is used for the determination of polychlorinated biphenyls (PCBs) in sediment via a heart-cutting technique. This method is compared with a method in which two off-line column clean-up steps are used with subsequent analysis by capillary gas chromatography. For the LC/GC analysis the recovery of PCBs was 90-100%. For two sediment samples from the river Meuse the LC/GC and the other, more laborious method showed good agreement.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 12 (1989), S. 793-796 
    ISSN: 0935-6304
    Keywords: Microcolumn liquid chromatography ; Flame photometric detection ; Organophosphorus compounds ; On-line preconcentration ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The potential of an interface for the on-line coupling of microcolumn liquid chromatography (LC)and a flame photometric detector (FPD) has been further investigated. With the micro-LC/FPD system, relatively high-molecular-weight polar compounds such as cyclic adenosine monophosphate, guanosine monophos- phate, glucose monophosphate, fructose monophosphate, and phytic acid were separated and selectively detected. In order to increase the sensitivity, on-line preconcentration with a microprecolumn inserted in the rotorof a Valcovalve has been applied. Preliminary results have shown that an injection volume of at least 500 1-11 water containing organophosphorus acids at a 5-50 ng/rnl concentration level is possible.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 0935-6304
    Keywords: Polar solvents ; Coupled LC-GC ; Partially concurrent solvent evaporation ; Trace enrichment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Coupling column liquid chromatography and gas chromatography on-line is becoming more important in analytical chemistry. Especially when large amounts of polar solvents can be introduced into the gas chromatograph without any problem, the technique will offer new possibilities. With a DPTMDS retention gap, evaporation rates and flooded zones of some solvents have been determined. Two modes of operation using partially concurrent solvent evaporation conditions are discussed: (1) injecting a sample via a loop of an LC valve followed by introduction into the gas chromatograph with an LC pump; (2) trace enrichment on a precolumn followed by on-line desorption with n-propanol into the gas chromatograph. Preliminary results for a splitter system, inserted between the retention gap and the analytical column which allows a considerable increase of the evaporation rate are also presented.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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