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  • 1
    ISSN: 1520-6882
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    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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  • 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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  • 4
    ISSN: 1612-1112
    Keywords: Coupled LC-GC-MS ; Polycyclic aromatic hydrocarbons ; Vegetable oil samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An on-line combination of liquid chromatography, gas chromatography and mass spectrometry has been realized by coupling a quadrupole mass spectrometer to an LC-GC apparatus. Liquid chromatography was used for sample pretreatment of oil samples of different origin. The appropriate LC fraction, containing polycyclic aromatic hydrocarbons, was transferred to the gas chromatograph using a loop-type interface. After solvent evaporation through the solvent vapour exit and subsequent GC separation, the compounds were introduced into the mass spectrometer for detection and identification. The GC column was connected to a short piece of deactivated fused silica that protruded into the ion source. The total analytical set-up allowed the direct analysis of oil samples after dilution in n-pentane without any sample clean-up. Detection limits are about 40 pg in the full scan mode and about 1 pg with selective ion monitoring, i.e. 20 ppb and 0.5 ppb respectively.
    Type of Medium: Electronic Resource
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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography/liquid chromatography ; Solid-phase extraction ; Water analysis ; Drying agents ; Organic contaminants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A small cartridge containing a drying agent is inserted between a solid phase extraction (SPE) column and a gas chromatograph (GC) to enable the introduction of water-free desorption solvent into the GC in on-line liquid chromatography (LC)-type enrichment of trace-level analytes from water samples. Some characteristics of the drying agents, such as their capacity to retain water and their re-usability after heating, have been tested. Possible interactions of the drying agent with the analytes, e.g., irreversible adsorption or catalyzed degradation, have been checked for a wide range of alkanes, alkylbenzenes chlorobenzenes, chlorophenols and phthalate esters. Using the on-line SPE-GC system with flame ionization detection (FID) and spiked samples containing different levels of the test compounds, the repeatability was shown to be satisfactory (6–17%). For 10 mL samples, the detection limits were lower than 0.1 μg/L. The on-line SPE-GC-FID system here presented can be used for the repeated analysis of water samples without exchange of the dyring cartridge. The technique is applied to the analysis of tap water.
    Type of Medium: Electronic Resource
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  • 6
    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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  • 7
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A liquid chromatographic method using gradient elution and diode array UV detection for the trace level determination of seven synthetic pyrethroids is described. The procedure involves automated on-line preconcentration on precolumns containing octadecylbonded silica using a Prospekt. Although the analytes display a “mixed” hydrophobic/hydrophilic behaviour, both breakthrough on the precolumn and adsorption to inner walls and surfaces can be prevented by adding Brij-35, a neutral surfactant, to the aqueous sample. The procedure has been tested for the analysis of surface water; detection limits typically are at the sub-μg/l level and repeatability is excellent. The automated system is robust and there are no maintenance problems.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1612-1112
    Keywords: Column liquid chromatography/gas chromatography ; Solid-phase extraction ; Empore® extraction disks ; Organophosphorus pesticides ; Nitrogen-phosphorus detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A fast and simple procedure for the analysis of aqueous samples by on-line membrane disk extraction and capillary gas chromatography (GC) is presented. As an example, organophosphorus pesticides are preconcentrated from aqueous samples on three 0.5 mm thick, 4.2 mm diameter extraction disks. The layers are dried by a stream of nitrogen (10–15 min; ambient temperature). Desorption of the analytes is carried out with ethyl acetate which is directly introduced into a retention gap under partially concurrent solvent evaporation conditions, using an early solvent vapour exit. The final analysis is carried out by GC with thermionic detection. The technique is applied to the determination of a series of organophosphorus pesticides in tap water and water from two European rivers. With a sample volume of only 2.5 ml, detection limits of 10–30 ppt are achieved in tap water and of 50–100 ppt in river water.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 1612-1112
    Keywords: Solid-phase extraction ; Gas chromatography ; Ion trap tandem mass spectrometry ; Water samples ; Environmental analysis ; Pesticides ; Bromide ; Nitrite
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary On-line solid-phase extraction-gas chromatographyion-trap tandem mass spectrometry (SPE-GC-MS/MS) has been used for the trace-level determination of polar and apolar pesticides. The SPE-GC interface, an Autoloop 2000, was operated at an injection temperature of 90°C which permitted the determination of thermolabile pesticides such as carbofuran and carbaryl. Rectilinear calibration curves were obtained for the analytes tested over a range of 0.1–500 ng L−1, using a sample volume of 10–100 mL for enrichment on an SPE cartridge packed with styrene-divinylbenzene copolymer. The detection limits for the pesticides were in the 0.01–4 ng L−1 range. For a number of pesticides acceptable tandem mass spectra were obtained at levels as low as 0.1 ng L−1 level in real-life water samples. As a demonstration of the applicability of this technique for inorganic anions, bromide and nitrite were converted into 4-bromoacetanilide and 2-phenylphenol, respectively. The reaction products were pooled and subjected to simultaneous analysis by the present method using full-scan mass spectrometric detection. The detection limits were 0.3 and 2 ng L−1, respectively.
    Type of Medium: Electronic Resource
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  • 10
    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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