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  • 1
    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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  • 2
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Atomic emission and MS detection ; Solid-phase extraction ; Aqueous samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC systems to enable the determination of microcontaminants at the 0.02–1 μg L−1 level in 7–50 mL of aqueous sample. The screening was limited to compounds present in at least one heteroatom-selective GC-AED trace above a predetermined concentration level. These compounds were identified by their partial formulae (AED) and the corresponding mass spectra, which were obtained from the GC-MS chromatogram via the retention index concept. The potential of the approach was demonstrated by the identification of target compounds as well as all unknowns present in tap and waste water above the predetermined threshold of 0.05 μg L−1 (tap water) or 0.5 μg L−1 (waste water).
    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
    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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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Atomic emission detection ; Aqueous samples ; Solid-phase extraction ; Organophosphorus pesticides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An on-line, solid-phase extraction gas chromatography atomic-emission detection (SPE-GC-AED) system has been set up using an on-column interface to transfer 100 μl of desorbing solvent to the GC part of the system. Analytical characteristics such as recovery, precision and linearity of calibration plots were comparable with those of the off-line combination of SPE-GC-AED using organophosphorus pesticides as test compounds. The fully on-line set-up causes a marked improvement in detection because of the quantitative transfer of the analytes from the SPE module to the GC: detection limits are as low as 5–20 ng l−1 for the analysis of 10 ml raw and spiked surface water samples using the phosphorus channel. Detection levels can be further enhanced by processing up to 100 ml samples. The integrated analytical system is robust. The potential of the on-line set up has been demonstrated for the analysis of surface water and waste water.
    Type of Medium: Electronic Resource
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