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  • 1
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Urea herbicides ; Catalytic hydrolysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method is described for the rapid catalytic hydrolysis of phenylurea herbicides on silica gel at elevated temperatures. After derivatisation of the anilines produced with heptafluorobutyric acid anhydride final analysis is done on a gas chromatograph equipped with an electroncapture detector. Detection limits are in the 1–5 picogram range. The method has successfully been applied to residue analysis of water samples at the 1 ppb level. The determination of free anilines present in water samples and the potential of various techniques to be used to discriminate between free anilines and parent herbicides are also discussed.
    Materialart: Digitale Medien
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  • 2
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Supercritical fluid extraction ; GC detectors ; Purity of gases
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The usefulness of several grades of carbon dioxide for online supercritical fluid extraction/capillary gas chromatography has been studied. If trace-level work has to be performed, no single grade can be recommended for all modes of detection studied. Good-quality carbon dioxide is available for use with flame ionization and thermionic detectors. With electron-capture detection, however, distinct problems still exist.
    Materialart: Digitale Medien
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  • 3
    ISSN: 1612-1112
    Schlagwort(e): Solid-phase extraction ; Gas chromatography ; Ion trap tandem mass spectrometry ; Water samples ; Environmental analysis ; Pesticides ; Bromide ; Nitrite
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Materialart: Digitale Medien
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  • 4
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 47 (1998), S. 313-345 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Sample pretreatment ; Coupling on-line to capillary GC ; Robotization
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Materialart: Digitale Medien
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  • 5
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Atomic emission and MS detection ; Solid-phase extraction ; Aqueous samples
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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).
    Materialart: Digitale Medien
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  • 6
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Atomic emission detection ; Aqueous samples ; Solid-phase extraction ; Organophosphorus pesticides
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 7
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Column liquid chromatography ; On-line coupling ; Ion-exchange membrane ; Ion-pair reagent
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant in the membrane was tetrabutylammonium hydroxide dissolved in acetonitrile/water, which effects an anion-exchange of methanesulphonate ions for regenerant hydroxide ions. The efficiency of the exchange process was found to be 99.9%. This enabled the direct introduction of the LC eluent, free of ions and with the proper acetonitrile/water ratio, into the GC. The applicability of the on-line LC-micromembrane-GC system has been illustrated for the potential drug eltoprazine, which is quantitatively recovered with a coefficient of variation for standard solutions of 3% at the 150 μg/ml analyte level.
    Materialart: Digitale Medien
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  • 8
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; ASPEC ; Trazodone in plasma ; Method automation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An automated sample preparation module, (the automated sample preparation with extraction columns, ASPEC), was interfaced with a capillary gas chromatograph (GC) by means of an on-column interface. The system was optimised for the determination of the antidepressant trazodone in plasma. The clean-up of untreated plasma was carried out with disposable C18 cartridges, using several washing steps. The analyte was desorbed with methanol, the extract was diluted on-line with buffer and preconcentrated on a PLRP-S trapping column. The trapping column was dried by purging with nitrogen gas. Desorption (phase switching) of the trapping column was carried out with ethyl acetate which was introduced into a retention gap using partially concurrent solvent evaporation conditions. Trazodone was determined by GC with flame ionisation detection (FID). With a 1 ml sample, this resulted in a detection limit for trazodone in plasma of 3 ng/ml. The system showed good linearity and repeatability in the range 0.01–1 μg/ml, thus covering the range of pharmacokinetic/dynamic-to-therapeutic concentrations of trazodone in plasma. Preliminary results for benzodiazepines are promising. They indicate that the use of a selective detector such as the nitrogen/phosphorus detector, is to be recommended.
    Materialart: Digitale Medien
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