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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' journal of analytical chemistry 364 (1999), S. 106-112 
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An automated at-line SPE–GC–MS system for the determination of micropollutants in aqueous samples, which is based on the PrepStation and uses large-volume on-column injections, has been redesigned. A cartridge made from stainless steel and polychlorotrifluoroethylene and a 2-needle system was constructed which allow the determination of micropollutants at the low ng/L level without interferences from impurities extracted from the septa of the vials or the commercial cartridges. No time-consuming pre-cleaning of the cartridges or septa is required. The SPE sample extract (300 μL) is transferred from the sample preparation module to the autosampler of the GC–MS and 50 or 100 μL are injected. The analytical characteristics of the integrated procedure such as analyte recovery (typically 80–105%) and repeatability (RSDs, 2–9%), were satisfactory. Several micropollutants were detected in (unfiltered) river water at the 0.2–400 ng/L level using full-scan MS acquisition. The system proved to be robust during the analysis of more than 100 tap and river water samples.
    Type of Medium: Electronic Resource
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  • 2
    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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  • 3
    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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