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  • 1
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Journal of Chromatography A 477 (1989), S. 39-47 
    ISSN: 0021-9673
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 60-66 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Cold-trapping ; Drying ; Gas stripping ; Trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The design and features of an on-line purge and cold-trap pre-concentration device for rapid analysis of volatile organic compounds in aqueous samples are discussed. Excessive water is removed from the purge gas by a condenser or a water permeable membrane in order to avoid blocking of the capillary cold-trap. Synthetic mixtures covering concentrations ranging from tenths to tens of ppb's and different chemical classes are used to study the effect of various process factors on the efficiency and selectivity of water removal as well as on the purging recovery. The importance of the concentration of the solutes, the flow rate in conjunction with the volume of the purge gas, and the temperature of the condenser, the cold-trap and the sample is emphasized. Theoretical models describing the purge process and the blocking of the cold-trap agree fairly well with the highly reproducible experimental results (σ = 2-4%). Both the condenser and the Nafion membrane successfully remove water, although some compounds, dependent on volatility and polarity, are partly or completely lost. It is shown that non-polar volatile organic compounds are efficiently enriched so that recoveries between 80-100% and a detection limit of 1 ppt can be obtained. The applicability of the system is illustrated on some examples.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 273-279 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; High speed capillary GC ; Sample introduction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The speed of analysis in capillary gas chromatography can be substantially increased by reduction of the column inner diameter. However, special demands are then posed upon instrumental design. In particular, the sampling system is highly critical because it has to be capable of delivering extremely small injection band widths which must be compatible with the column inside diameter. This study focuses on the evaluation of two potentially suitable sample introduction systems with respect to input band width and detection limits and their compatibility with small bore (≦ 100 μm) columns in capillary gas chromatography. One of them allows liquid on-column injection, based on liquid splitting, of only a few nl onto small bore (≦ 100 ◂m) fused silica columns. For gases, input band widths as low as 1 ms are obtained with this system. The other one is part of a miniaturized gas chromatograph with extremely low dead volume interfaces and detector volumes. It allows input band widths for gases of a few ms. Without any preconcentration ppm concentrations are measured in gaseous samples with a 80 ◂m thick film capillary column. It will be shown that a further reduction of the minimum detectable amount and analysis time is possible with this equipment.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 852-857 
    ISSN: 0935-6304
    Keywords: High speed capillary GC ; Narrow bore columns ; Enrichment ; Cold trapping ; Flash thermodesorption ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reduction of the column diameter has proved to be a highly efficient tool to increase the speed of analysis. Unfortunately, the requirements for instrumental design with respect to sample input band width, low dead volume interfacing, and time constants of detection and registration systems are the more critical the smaller the inside diameter.Recently we reported input band widths as low as 1 ms [1] for gaseous samples at ppm concentration levels, without any preconcentration, in a study with narrow bore columns and thermal conductivity detection.In this study a simple versatile micro on-column cold trap/thermodesorption enrichment system for narrow bore columns is introduced and evaluated. The combination of considerable sample enrichment and preservation of the compatibility of the required input band width with column dimensions is critically examined. The process of thermodesorption (reinjection) which is the most critical step, is particularly emphasized.The system consists of a short aluminum coated fused silica or metal capillary with a low mass and a low cost electrical heating. Input band widths down to 1 ms are obtained without extreme demands on electrical power (300 watt). The potential of the system is illustrated with some extremely fast separations.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 862-869 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Column-detector systems ; Detectability ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Expressions for the minimum detectable amount Qo and the minimum analyte concentration Co as functions of the chromatographic parameters are derived for both mass and concentration sensitive detectors. The effects of pressure drop, column inner diameter, and film thickness are given.The minimum analyte concentration for mass flow sensitive detectors, Com, can be reduced considerably by selecting the carrier gas velocity well above its optimum value (related to Hmin), however, at the cost of long columns and long analysis times. For Qo the improvements can be neglected, and so the analysis can best be performed at uopt.When the flow rate in the detector, Fd, is equal to the column flow rate Fc, the maximum permissible detector volume of concentration sensitive detectors is proportional to dc2 up to dc3, and so narrow bore columns require detectors of extremely small volume. Make-up gas has to be added when the actual volume is too large, thus worsening the detectability. Another approach, vacuum operation of the detector cell, appears to be very attractive. On the other hand, when wide bore columns are used in combination with small volume concentration sensitive detectors, very small values of Qoc and Coc are obtainable when the abundant carrier gas can be removed before entering the detector cell.Digital noise filtering can further reduce the obtainable Qo and Co values, especially for broad peaks and thus for wide bore columns.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 12 (1989), S. 303-307 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Narrow bore columns ; Photoionization detection ; Thermal conductivity detection ; Detection limits ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Not only the required input band width and the availability of compatible instrumentation limit the reduction of column diameter but so do the column sample capacity and detector characteristics, such as volume and sensitivity. In this paper the scope and limitations of thermal conductivity and photoionization detection at atmospheric and reduced pressures for capillary gas chromatography are discussed at length.It is shown that the sensitivity of a thermal conductivity detector is inversely proportional to the pressure. Reduction of cell volume and decrease of pressure appear equivalent with respect to minimum detectable amount and peak broadening. This results in femtogram detection limits for column diameters as low as 10 μm.For photoionization detectors the sensitivity did not improve at reduced pressures, so that the effect of reduced pressure and addition of make-up gas on the detection limits is the same. Nevertheless, the applicability of a low volume photoionization detector (40 μl) for capillary columns with a diameter as low as 50 μm will be demonstrated by series coupled PID and FID detectors and illustrated with various applications.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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