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  • Analytical Chemistry and Spectroscopy  (29)
  • Atomic, Molecular and Optical Physics  (5)
  • 11.80.Et  (3)
  • 42.75
  • 2000-2004  (2)
  • 1990-1994  (35)
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Year
  • 11
    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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  • 12
    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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  • 13
    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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  • 14
    ISSN: 0935-6304
    Keywords: LC-GC ; Aqueous samples ; Solid phase extraction ; Thermal desorption ; PTV ; Tenax GC© ; Reversed phase adsorbent ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new approach to the introduction of large aqueous samples into a gas chromatograph, solid phase extraction - thermal desorption, is presented. Carrier gas pushes the sample through a packed liner mounted in a programmed temperature vaporizer; analytes retained by the packing material are thermally desorbed after drying of the adsorbent. The sorption properties and thermal stability of some packing materials have been studied off-line. Tenax GC®, and octyl-modified silica silylated with diphenyltetramethyldisilazane to improve its thermal stability, appeared to be suitable materials.The drying period and the desorption temperature are critical for satisfactory performance of the method. When Tenax GC® is used as packing material, thermal desorption at 250°C for 15 min gives quantitative recovery for methyl esters up to hexacosanoic acid methyl ester. With the silylated octyl-modified silica, the application range is limited to the methyl esters of decanoic to octadecanoic acids.
    Additional Material: 3 Ill.
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  • 15
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 459-463 
    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.
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  • 16
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 785-790 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Derivatization ; (Chloro)alkyl chloroformates ; Non-aqueous reaction media ; Aqueous reaction media ; Fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fatty acids can be conveniently derivatized in less than one minute with (chloro)alkyl chloroformates such as methyl chloroformate, 2-chloroethyl chloroformate and 2,2,2-trichloroethyl chloroformate. 2,2,2-Trichloroethyl chloroformate is the most reactive reagent, and yields a reaction product which can be sensitively detected by GC ECD (detection limit 50 ng/ml, i.e. 25 pg/injection, for C8, C10, and C12 acids).In non-aqueous media 3-picoline, N-methylpiperidine, and dimethylaminopyridine show catalytic activity comparable with that of pyridine and can, therefore, replace it. N-methylpiperidine is the best basic catalyst in aqueous media (i.e. media containing up to 40 % water).
    Additional Material: 7 Ill.
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  • 17
    ISSN: 1040-7685
    Keywords: supercritical fluid chromatography ; packed capillary columns ; thermionic detection ; organophosphorus pesticides ; vegetable extracts ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Packed capillary supercritical fluid chromatography coupled with thermionic detection was used for the selective determination of nineteen organophosphorus pesticides in vegetable extracts. The chromatographic behavior of some pesticides was studied using seven different stationary phases. Addition of an organic modifier to carbon dioxide was needed to improve peak shape and reduce retention. Quantitation of organophosphorus pesticides in vegetable extracts showed good linearity. Extraction was performed in a one-step extraction procedure using a water-miscible solvent (acetone) and an organic solvent with limited water capacity (dichloromethane). Under these conditions a wide range of both polar and apolar pesticides can be recovered from vegetable extracts down to the 3-25 μg kg-1 level. The recoveries found ranged from 35 to 95% depending on the polarity of the pesticides.
    Additional Material: 4 Ill.
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  • 18
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 5 (1993), S. 303-315 
    ISSN: 1040-7685
    Keywords: capillary GC ; solid phase extraction ; membrane disks ; water samples ; automation ; nitrogen-phosphorus detection ; mass selective detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated procedure for the analysis of aqueous samples by membrane disk extraction coupled on-line to capillary gas chromatography (GC) is presented. Organophosphorus pesticides are preconcentrated from aqueous samples on three 0.5 mm thick, 4.0 mm diameter XAD-2 membrane extraction disks which are mounted in a polymer holder for use in a PROSPEKT sample processor. The layers are dried by a stream of nitrogen (30 min at 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 vapor exit. The method is a fully software-controlled automated system, and includes sample preparation, sample transfer and GC analysis. The final analysis is carried out by GC with nitrogen-phosphorus (NPD) or mass-selective detection. The technique is applied to the determination of a series of organophosphorus pesticides in tap water and water from European rivers. With a sample volume of only 2.5 mL, the detection limits achieved with the NPD were 20-50 ng L-1 in tap water and 20-100 ng L-1 in river water.
    Additional Material: 9 Ill.
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  • 19
    ISSN: 1040-7685
    Keywords: micro-LC ; flame photometric detection ; thermionic detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Microcolumn liquid chromatography (micro-LC) with on-line flame photometric (FPD) or thermionic detection (TID) has been used for the determination of a series of organophosphoric and organophosphonic acids isolated from various sample matrices. Silica-based ion-exchange materials and polymer packings have been used as stationary phases. In order to improve the sensitivity (expressed in concentration units) of the technique, trace enrichment via a miniaturized precolumn (4 mm × 1 mm i.d.) and direct large-volume injections (1-10 μL) of aqueous samples have been studied. As an application, the verification of nonproduction of chemical warfare agents and their alleged use have been investigated by analyzing their hydrolysis products in spiked surface water and soil samples. The application of both the precolumn technique and large-volume injections permit the detection of organophosphorus acids in water and soil at the low ppm level.
    Additional Material: 8 Ill.
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  • 20
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A benzenesulphonic acid-type cation exchanger (pKa 〈 1) is used as trapping-column material in a phase-system switching for the on-line coupling of column liquid chromatography and thermospray mass spectrometry. Phase-system switching is used to remove non-volatile constituents from the mobile phase, so that eluents containing non-volatile buffers and ion-pairing agents can be used without contaminating the mass spectrometer. The total analytical system is optimized using four benzalkonium test compounds (quaternary ammonium compounds). The reversed-phase separation of the test compounds as well as the parameters involved in the sorption on and desorption from the trapping column are studied. Important parameters during sorption are the concentration of the phosphate buffer and the percentage of acetonitrile in the mobile phase. During desorption of the test compounds from the ion-exchanger the percentage of acetonitrile in the desorption eluent and the pH are the most important factors. As an example, the analysis of domiphen in nasal drops is shown.
    Additional Material: 10 Ill.
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