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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 19-27 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Large volume injection ; PTV injectors ; PTV splitless injection ; PTV solvent split injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Temperature programmable injectors with liner diameters ranging from 1 to 3.5 mm are evaluated and compared for solvent split injection of large volumes in capillary gas chromatography. The liner dimensions determine whether a large sample volume can be introduced rapidly or has to be introduced in a speed controlled manner. The effect of the injection technique used on the recovery of n-alkanes is evaluated. Furthermore the influence of the liner diameter on the occurrence of thermal degradation during splitless transfer to the analytical column is studied. Guidelines are given for the selection of the PTV liner internal diameter best suited for specific applications.
    Additional Material: 9 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 124-128 
    ISSN: 0935-6304
    Keywords: Large volume injection ; PTV injector ; PTV solvent split injection ; Packed inserts ; Thermal degradation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 69-79 
    ISSN: 0935-6304
    Keywords: Large volume injection ; PTV injector ; Water analysis ; River sediment ; Pesticides ; Polycyclic aromatic hydrocarbons (PAHs) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Temperature programmable (PTV) injectors with packed widebore (ca. 3.5 mm i.d.) liners are used for large volume injection in capillary gas chromatography with the aim to simplify and/or improve off-line sample pretreatment proecdures. A simple procedure for optimization of large volume PTV injection is described. The system performance, i.e. linearity and repeatability, is evaluated for polar nitrogen/phosphorus containing pesticides (PTV-GC-NPD) and organochlorine pesticides (PTV-GC-ECD) in river water extracts as well as for polycyclic aromatic hydrocarbons (PAHs) in river sediment (PTV-GC-MS).
    Additional Material: 8 Ill.
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  • 4
    ISSN: 0935-6304
    Keywords: On-line extraction ; Large volume introduction ; Capillary gas chromatography ; Atomic emission detection ; Solvent venting ; Pesticides ; Ground water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The on-line coupling of a liquid-liquid extraction system with capillary gas chromatography using atomic emission detection (GC-AED) has been studied. The required large volumes of about 100 μl of an iso-octane solution can be introduced into the GC-AED system by using the AED solvent vent and a solvent vapor exit in front of the capillary analytical column. Test solutions containing several pesticides were detected using the carbon, chlorine, nitrogen and sulfur channels. Analyte detectability (in concentration units) was improved significantly and low concentractions of the test compounds could be determined (1-5 ng/ml). Aqueous samples were on-line extracted and analyzed. The precision of the large-volume injection itself as well as the total extraction-GC-AED system was satisfactory (RSD of ca. 2 and 4%, respectively). As a real-life application, several ground water samples were screened.
    Additional Material: 6 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 7 (1995), S. 383-394 
    ISSN: 1040-7685
    Keywords: large-volume injection ; gas chromatography ; on-column injector ; environmental analysis ; organophosphorus pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Large-volume injection is an attractive means to improve detection limits when analyzing dilute sample extracts. There is now no need to achieve enrichment by means of solvent evaporation, which makes the total analytical procedure less reliable and less robust due to loss of volatile compounds. In this study on-column injection was applied for large-volume injection using an on-column injector in combination with a deactivated uncoated fused silica capillary (retention gap) and an early solvent vapor exit. Two strategies are described. The first one relies on the programmable speed of an infusion pump, which is adapted such that it lies just above the evaporation rate of the extraction solvent used. With the second procedure, which can be used for a commercially available autosampler, the evaporation speed is adjusted to the fixed speed of injection by varying the temperature during injection. During optimization the additional solvent evaporation time was determined. The optimum conditions for an injection volume of 100 μL of either n-hexane or ethyl acetate are reported. Large-volume injection was used for simplified and miniaturized solid-phase extraction procedures. The procedures were used to determine various organic micropollutants, such as organophosphorus pesticides and triazine herbicides, in tap and surface water extracts, using a flame photometric, and a mass spectrometric detector. For both methods good recovery for most of the analytes (70-87%), linear calibration curves (0.01-5 μg/L range), and relative standard deviations of less than 10% were obtained. Detection limits typically were in the range of 1-10 ng/L for GC-FPD and 10-150 ng/L for GC-MS. When working in the time-scheduled multiple ion detection mode detection limits in GC-MS were one order of magnitude lower. © 1995 John Wiley & Sons, Inc.
    Additional Material: 6 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 7 (1995), S. 365-374 
    ISSN: 1040-7685
    Keywords: capillary electrophoresis ; temperature control ; heat transfer ; helium gas cooling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A comparative study on the properties of helium and air as thermostatting fluids in Capillary Electrophoresis (CE) has been carried out. Equations that relate the properties of fluids to their control of the temperature of the capillary are shown. Results from theory and experiments are compared under different cooling conditions, i.e., natural and forced gas convection, using air and helium. Experimental results are qualitatively in good agreement with those predicted by theory. The better thermostatting capability of helium compared to air is demonstrated by an improved efficiency in real separations and a lower degree of denaturation of a thermolabile protein during its purification by CE. © 1995 John Wiley & Sons, Inc.
    Additional Material: 10 Ill.
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  • 7
    ISSN: 1040-7685
    Keywords: on-line extraction-GC ; open-tubular traps ; coiled tubes ; secondary flow ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effect of geometrical deformation of open-tubular extraction columns on peak dispersion of retained solutes is evaluated. By coiling or stitching of the columns peak dispersion is decreased, with a factor of two and more than five, respectively, due to secondary flow enhanced radial dispersion. This enables the increase of sampling flow rates in on-line extraction-GC using open-tubular extraction columns up to 4 mL/min while still obtaining quantitative trapping of the analytes. © 1995 John Wiley & Sons, Inc.
    Additional Material: 9 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 30 (1995), S. 324-332 
    ISSN: 1076-5174
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Early in the development of electrohydrodynamic mass spectrometry (EH-MS), it was realized that ion source performance improved when the sample liquid was supplied discontinuously to the capillary emitter. Based on this realization, an ion source was designed that operates without an external sample supply system. Its essential part is a metal capillary that serves both as the liquid reservoir and the field anode and is mounted exchangeably on a pushrod. As the liquid flow is field induced, the flow rates are extremely low, in the range of 0.2 nl min-1. Thus, in spite of high analyte concentrations needed, sample consumption is only a few picomoles per mass scan. Moreover, the emission of larger droplets is avoided, which contributes to the stability of the ion signal. As the capillary emitter is mounted on a standard emitter carrier known from field desorption (FD) MS, the new ion source is compatible with conventional FD ion sources. EH mass spectra of analytes could be obtained from substances whose solubility in glycerol was〉0.5 mol l-1. The substances investigated with the new ion source include sugars, amino acids, peptides and an antibiotic. The general characteristics of the mass spectra are essentially the same as those known from other EH ion sources. Besides abundant solvent cluster ions, only cationated or protonated molecules of the analytes could be detected, frequently with one or more solvent molecules attached to the ions. Fragment ions were not observed.
    Additional Material: 9 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 99-104 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Micellear electrokinetic chromatography ; Organic modifiers ; Naphthalene sulfonates ; Surface water ; Thermostatting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The production and use of naphthalene sulfonates can easily cause pollution of surface and other types of waters. In the present study, capillary electrophoresis in combination with UV absorption detection was used to separate 21 amino- and hydroxy-substituted naphthalene sulfonates which included multiple isomeric compounds. The influence of various parameters such as pH (which turned out to be extremely important), temperature of the surrounding air flow, and the use of buffer additives (micelles, cyclodextrins, organic modifiers) was studied. Complete separation of all analytes including the isomers, was achieved in two runs with a 50 mM boric acid/borate buffer, containing either 100 mM sodium dodecylsulfonate or 15% acetonitrile. The limits of detection obtained for the individual compounds typically were 20μgI-1. River water samples spiked at this concentration level could be analysed using a simple three-step sample clean-up procedure.
    Additional Material: 6 Ill.
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  • 10
    ISSN: 0935-6304
    Keywords: Solid-phase extraction-thermal desorption ; Gas chromatography ; Ion trap detection ; Tandem mass spectrometry ; Water samples ; Microcontaminants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An improved set-up for solid-phase extraction with thermal desorption coupled on-line to gas chromatography (SPETD-GC) is presented. It includes a newly designed liner for a programmable temperature vaporizer (PTV) and an improved water elimination system. The SPETD procedure now includes a washing step with HPLC-grade water to prevent degradation of analytes due to interaction with remaining sample constituents. The system was used to analyze surface and tap water samples over a 4-month period. No decrease of chromatographic or trace-enrichment performance was observed, and a liner packed with Tenax GR could be used for at least 150 analyses. The SPETD module was coupled to GC with ion-trap detection for mass spectrometric (MS) and MS/MS detection. The linearity and repeatability of the procedure for several pesticides which were tested in the 0.5-10 μg/1 range were fully satisfactory (1 μg/1, RSD range 5-11%; n = 5). When using sample volumes of 0.1 ml only, detection limits were as low as 0. 1-0.2 μg/1. As an example, the confirmation and quantification of a suspected pesticide in a real-life sample using electron impact and positive chemical ionization in both the MS and MS/MS mode is shown.
    Additional Material: 7 Ill.
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