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  • 1
    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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  • 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).
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  • 3
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chemiluminescence detection ; Phosphine derivatives ; Headspace analysis ; Fluorine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Phosphine, alkylated phosphines and monophosphinate esters are detected with high sensitivity in capillary gas chromatography (GC) by their chemiluminescent reactions with molecular fluorine. Detection limits are estimated to be 1.3 pg, 0.5 pg, 8 pg, and 17 pg for phosphine, trimethyl phosphine, trimethyl phosphinate ester, and triethyl phosphine, respectively. As found earlier with alkylated sulfur, selenium and tellurium compounds, the detector exhibits a linear response. For triethyl phosphine, a linear range of greater than three orders of magnitude was demonstrated. Emission spectra were obtained for the trimethyl phosphine and triethyl phosphine systems. Chemiluminescence emitters include electronically excited HCF, vibrationally excited HF, and an unknown species in the trimethyl phosphine system. Banded emission from vibrationally excited HF and a broad continuum were observed for both trimethyl phosphine and triethyl phosphine; however, HCF emission was observed only for TMP. Under the conditions employed, the principal emitter is HCF for trimethyl phosphine and HF and the unknown emitter for triethyl phosphine. This detector may have important applications in investigations of the biogeochemical cycling of phosphorus.
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  • 4
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; PTV-System ; Ethephon in drinking water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An indirect GC method is described for the determination of Ethephon in drinking water on the basis of the headspace analysis of the ethylene formed from Ethephon. In order to reach the necessary detection limit, the entire volume of the static headspace distribution is transferred into a cold injection system (CIS). There, the ethylene is adsorbed on Carbosieve SIII at 10°C and, subsequently, desorbed at 300 °C. The water vapour included in the headspace is completely eliminated through the splitting system. By means of this technique, a detection limit of 0.05 μg/l water was reached.
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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; On-line coupling ; Ion-exchange membrane ; Ion-pair reagent
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
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  • 6
    ISSN: 1612-1112
    Keywords: Gas chromatography ; ASPEC ; Trazodone in plasma ; Method automation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Urea herbicides ; Catalytic hydrolysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Supercritical fluid extraction ; GC detectors ; Purity of gases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Phosphine ; Flame photometric detection ; Anaerobic bacteria
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method is presented which distinguishes phosphine from hydrogen sulfide and other possible headspace gases of anaerobic microbial cultures. In anaerobic cultures spiked with phosphine, this gas is recovered in the liquid and gaseous phase down to 10 pg per ml of gas or liquid. No biogenically produced phosphine was found. Phosphine in amounts as small as 30 ng per 1 can be stored for several days in glass bottles covered with rubber septa, filled with nitrogen, in the presence or absence of water or of an anaerobic bacterial culture. Due to the selectivity of the detector and the retention characteristics of the porous layer open tubular polymer column alkanes, alkenes and organosulfur compounds routinely found in anaerobic bacterial headspaces do not interfere with the analytical quantification of phosphine.
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  • 10
    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.
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