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  • 1
    Electronic Resource
    Electronic Resource
    On-line coupling of solid-phase extraction and gas chromatography with atomic emission detection for analysis of trace pollutants in aqueous samples (1995)
    Springer
    Chromatographia 40 (1995), S. 119-124 
    Details
    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
    URL: http://dx.doi.org/10.1007/BF02272157
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  • 2
    Electronic Resource
    Electronic Resource
    On-line solid-phase extraction-gas chromatography-ion trap tandem mass spectrometric detection for the nanogram per liter analysis of trace pollutants in aqueous samples (1997)
    Springer
    Chromatographia 44 (1997), S. 372-380 
    Details
    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
    URL: http://dx.doi.org/10.1007/BF02466313
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  • 3
    Electronic Resource
    Electronic Resource
    Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants (1998)
    Springer
    Chromatographia 48 (1998), S. 273-283 
    Details
    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
    URL: http://dx.doi.org/10.1007/BF02467683
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  • 4
    Electronic Resource
    Electronic Resource
    Determination of organophosphorus pesticides in aqueous samples by on-line membrane disk extraction and capillary gas chromatography (1992)
    Springer
    Chromatographia 34 (1992), S. 41-47 
    Details
    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
    URL: http://dx.doi.org/10.1007/BF02290457
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  • 5
    Electronic Resource
    Electronic Resource
    Drying agents for water-free introduction of desorption solvent into a GC after on-line SPE of aqueous samples (1994)
    Springer
    Chromatographia 38 (1994), S. 461-469 
    Details
    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
    URL: http://dx.doi.org/10.1007/BF02269837
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  • 6
    Electronic Resource
    Electronic Resource
    Automated derivatization for on-line solid-phase extraction-gas chromatography; phenolic compounds (1997)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 363-368 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solid-phase extraction ; Automation ; Water samples ; Acetylation ; Chlorophenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1-12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1-0.3 μg/1 range.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240200704
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  • 7
    Electronic Resource
    Electronic Resource
    Use of a temperature programmed injector with a packed liner for direct water analysis and on-line reversed phase LC-GC (1993)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 459-463 
    Details
    ISSN: 0935-6304
    Keywords: LC-GC ; Aqueous samples ; Large volume injection ; PTV injector ; Solid-phase extraction ; Thermal desorption ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A system is described that allows the introduction of large volumes of water samples in capillary GC. Water elimination is carried out in the solvent split mode in a PTV injector with a packed liner. Two ways of separating water and analytes, i.e. evaporative and non-evaporative (solid-phase extraction), are compared. Sampling in the solid-phase extraction mode is favorable both in terms of recovery as well as with regard to sampling time. Quantitative recovery is obtained for priority pollutants ranging in volatility from dimethyl-phenol to phenanthrene. Losses occur for more volatile compounds, but even for these compounds the repeatability of the recoveries remains acceptable. With the system described here, water samples up to at least 1 ml of water can be directly analyzed. The detection limits are in the sub-ppb range.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240160803
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