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  • Analytical Chemistry and Spectroscopy  (29)
  • Atomic, Molecular and Optical Physics  (5)
  • 42.75
  • 2000-2004  (2)
  • 1990-1994  (32)
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  • 1
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Mass spectrometry ; Food analysis ; Polycyclic aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Twenty eight native vegetable oils were analyzed for polycyclic aromatic hydrocarbons. Generally PAH concentrations were low, but olive oils showed significantly higher contamination by light PAH ranging from 53 to 105.6 μg/kg. Muscle and liver samples of bream from the river Elbe contained little or no detectable amounts of PAH, whereas fresh and canned oysters and mussels showed higher contaminations. Highest PAH concentrations have been determined in “smoked oysters in oil” with 75.8 μg/kg benzo[a] pyrene for the oil and 12.2 μg/kg for the oyster meat.
    Additional Material: 7 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 447-450 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Atomic emission ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Tab.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 797-802 
    ISSN: 0935-6304
    Keywords: Capillary GC ; GPC and HPLC sample preparation ; Automation ; Planar chlorobiphenyls ; Horse fat ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The occurrence of the highly toxic non-ortho substituted (planar) chlorobiphenyls (CBs) at low levels in wildlife, (human) fat, and fish generates the need for a routine analytical procedure. The use of a fully automated system for the separation of planar and non-planar CBs, consisting of a gel permeation chromatography system, a sample preparation system employing extraction columns, and a porous graphitic carbon HPLC column is described, and tested with horse fat. Gas chromatography on capillary columns, with electron-capture or high resolution mass spectrometric detection, is used for quantitation of the CBs.
    Additional Material: 3 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 14 (1991), S. 475-480 
    ISSN: 0935-6304
    Keywords: Coupled RPLC-GC ; Partially concurrent solvent evaporation ; Trapping column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new technique for coupling reversed-phase liquid chromatography (RPLC) with gas chromatography is described. A fraction eluting from an RPLC column is trapped on a short column packed with polymeric adsorbent. After the mobile phase has been displaced with water, the analytes are desorbed with ethyl acetate. Following a delay time to enable the water to be flushed to waste, the ethyl acetate containing the analytes is introduced into the gas chromatograph under conditions suitable for partially concurrent solvent evaporation, i.e. below the solvent boiling point and at a rate just exceeding the evaporation rate. Post-column addition of water to the RPLC eluent helps to prevent breakthrough of compounds which are only modestly retained on the trapping column. The relationship between the capacity factors of the analytes on the trapping column and the required dilution factor is discussed. Polycyclic aromatic hydrocarbons are used as test compounds to study the system.
    Additional Material: 5 Ill.
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  • 5
    ISSN: 0935-6304
    Keywords: Coupled LC-GC-MS ; Aqueous sample ; s-Triazine Herbicides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Liquid chromatographic (LC) type trace enrichment is coupled online with capillary gas chromatography (GC) with mass spectrometric (MS) detection for the analysis of aqueous samples. A volume of 1-10 ml of an aqueous sample is preconcentrated on a trace-enrichment column packed with a polymeric stationary phase. After cleanup with HPLC-grade water the precolumn is dried with nitrogen and subsequently desorbed with ethyl acetate. A fraction of 60 μl is introduced on-line into a diphenyltetramethyldisilazane-deactivated retention gap under partially concurrent solvent evaporation conditions and using an early solvent vapor exit. The analytes are separated and detected by means of GC-MS. The potential of the LC-GC-MS system for monitoring organic pollutants in river and drinking water is studied. Target analysis is carried out with atrazine and simazine as model compounds; the detection limits achieved under full-scan and multiple ion detection conditions are 30 pg and 5 pg, respectively. Identification of unknown compounds (non-target analysis), is demonstrated using a river water sample spiked with 168 pollutants varying in polarity and volatility.
    Additional Material: 6 Ill.
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  • 6
    ISSN: 0935-6304
    Keywords: Capillary GC ; On-line extractive alkylation ; On-line acylation ; Carboxylic acids ; Amines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatographic procedures are described for the determination of carboxylic acids and chlorinated anilines in water samples.Propionic acid and 2,6-difluorobenzoic acid in aqueous solution have been simultaneously alkylated and extracted by means of a continuous two-phase reaction system, and then quantitated by on-line coupled capillary gas chromatography; tetrahexyl-ammonium hydrogen sulfate was used as phase transfer catalyst and pentafluorobenzyl bromide as reagent.A factorial design approach was used to optimize on-line derivatization of aqueous propionic acid with regard to pH and concentration of phase transfer catalyst. Alkylation and extraction, under optimized conditions, followed by quantitation of the pentafluorobenzyl ester by flame ionization detection furnished a linear calibration for concentrations between 0.1 and 10 μg/ml. The relative standard deviation was 9-15 %.The continuous two-phase reaction system was also used to determine (chlorinated) anilines present in water at concentrations of 0.1-1 μg/ml; pentafluorobenzoyl chloride was used as reagent and analysis was performed by capillary gas chromatography with flame ionization or electron capture detection. The on-line acylation of p-chloroaniline was optimized with regard to pH, reagent concentration, and reaction time.The on-line reaction system worked satisfactorily for both applications, although excess reagent caused some problems with the chromatography.
    Additional Material: 6 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 95-97 
    ISSN: 0935-6304
    Keywords: Chemical warfare agents ; Microcolumn liquid chromatography ; Enantiomeric separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An improved interface for the on-line coupling of microcolumn liquid chromatography (micro-LC) with thermionic detection (TID) is described. Modifications have been made to enable separate adjustment of the eluent introduction and the detector flame temperature in order to improve the sensitivity and ease of use of the system.The micro-LC-TID was used for the chiral separation of the nerve agent O-ethyl S-2-diisopropylaminoethyl methylphosphonothioate (VX). Baseline separation for the enantiomers of VX was obtained on Chiralcel OD using 1% isopropanol in hexane as the eluent. The detection limit of VX using 60 nl injections is ca. 5 μg/ml (ppm range). However, when using large-volume injections (10 μl) the detection limit is ca. 25 ng/ml (ppb range).
    Additional Material: 2 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 157-161 
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Partially concurrent solvent evaporation ; Trace enrichment ; Surface water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The feasibility of using ethyl acetate for the desorption of trace pollutants from a liquid chromatographic precolumn on-line into a diphenyltetramethyldisilazane-deactivated retention gap and, subsequently analysis by means of capillary gas chromatography has been demonstrated. First 5% of methanol are added to the water sample to prevent sorption of analytes onto parts of the preconcentration system. About 1 ml of this aqueous sample is injected onto a precolumn containing a polymeric stationary phase, using water-methanol (95:5, v/v) for transport and clean-up. The precolumn is desorbed with ethyl acetate and a fraction of 75 μl is injected on-line into the retention gap; separation is then achieved on a capillary CP Sil 19 column. No breakthrough of the test compounds was observed in the preconcentration step. The recovery was quantitative and the response obtained with flame ionization detection was linear in the range 0.1-100 ng/ml. The effect of varying the sorption flow rate on the recovery was studied. The system was applied to the analysis of river water.
    Additional Material: 6 Ill.
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  • 9
    ISSN: 0935-6304
    Keywords: Micropacked liquid chromatography ; Enantiomer separation ; HPLC-TID ; Organophosphorus pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Microcolumn liquid chromatography (micro-LC) of some chiral organophosphorus pesticides has been studied using Chiralcel OD columns and simultaneous ultraviolet (UV) and phosphorus selective detection, the latter by means of a micro-UV cell coupled on-line to a thermionic detector (TID). Micro-LC showed a ca. 5-fold improved separation impedance, a ca. 1.8-fold increased column permeability, and greater inertness compared with conventional LC.By using the TID, organophosphorus pesticides could be satisfactorily determined at trace levels, the detection limit being 4 pg/s of phosphorus. The response of the micro-LC-TID system is linear in the range of 0.05-20 ng (r = 0.9994).
    Additional Material: 4 Ill.
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  • 10
    ISSN: 0935-6304
    Keywords: HR-GC ; Organochlorine pesticides ; Pyrethroids ; Water analysis ; Sample clean-up ; Solid-phase extraction cartridges ; LC-GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The ASPEC (Automatic Sample Preparation with Extraction Columns) system has been coupled on-line to capillary GC-ECD by means of a loop-type interface equipped with a solvent vapour exit. Both ASPEC and GC conditions have been optimized leading to an effective clean-up of the extracts analyzed.By means of solid-phase extraction cartridges filled with silica, it has been possible to analyze concentrated surface water extracts for a group of 18 electron-capturing compounds present in the water at ppt levels. ASPEC-GC has also been applied to the determination of synthetic pyrethroids at ppt levels in surface water.The complete analytical procedure is greatly facilitated by automation and miniaturization. Miniaturization results in a considerable decrease in the sample volume required. The potential of the method for the analysis of other pesticides is estimated.
    Additional Material: 6 Ill.
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