Gas Phase Chromatography - Kaiser, Rudolf

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Sommaire:
Survey of the four fundamental chromatographic methods-Limits of application, definitions and methods of gas chromatography-Nomenclature-History of gas chromatography.- 1. Theory of Gas Chromatography.- Definition and derivation of the characteristic values for gas chromatography-Retention volume and partition coefficient-Retention values and the liquid phase in isothermal gas chromatography-Height equivalent to a theoretical plate-Separation formula for gas chromatographic methods-Selectivity, column performance and resolution-Retention values and temperature of separation; retention temperature-Number of theoretical plates and peak form-Gas chromathermography by the circulation technique.- 2. Apparatus.- 2.1. The column.- The column packing-Evaluation of packed columns-Calculation of the number of theoretical plates, column performance and separation factor-Resolution-Calculation of the number of theoretical plates or column length necessary for a given separation-Load capacity-Performance index-Time of analysis and resolution-Column material-Column diameter-The solid support-Removal of residual adsorption activity-Particle diameter-The liquid phase-Quantity of liquid phase-Impregnation of the support-Testing the column packing-Peak form-Control of the quantity of liquid phase -Temperature load capacity-Filling the column-Testing the column-Ageing of the column packing-Summary of the factors governing the preparation and operation of efficient columns.- 2.2. The carrier gas.- Gas purification-Control and measurement of the carrier gas flow rate-Disturbances of constant flow rate-Production of a constant gas flow rate-Gas tightness-Flow rate meters.- 2.3. The sample injector.- Sample injectors for gases-Sample injectors for liquids.- 2.4. Detectors.- Desirable and necessary properties of detectors-Principles of measurement-The thermal conductivity cell-The flame ionization detector-Testing of detectors-Comparison of sensitivity.- 2.5. Recorders.- 2.6. Temperature.- The optimum operating temperature-Constant temperature-Temperature control-Heat insulation-Variable temperatures.- 2.7. Industrial gas chromatographs and other special apparatus.- High temperature instruments-Multi-column instruments-Apparatus for preparative work-Sample collection systems- Fully automatic instruments-Trace analysis instruments-Low pressure instruments.- 3. The Analytical Result.- 3.1. The qualitative analytical result.- Preparation of the sample-Choice of the most suitable column and operating conditions-Qualitative evaluation-Qualitative testing of columns.- 3.2. The quantitative result.- Requirements for the quantitative evaluation of gas chromatographic results-Measurement of peak area-Evaluation from peak area measurements-Direct surface area method-Evaluation by peak area measurements using specific calibration factors-Evaluation of the analysis by a calibration method-External calibration of the peak heights-External calibration of the peak areas-Internal calibration with addition of extraneous substance-Internal calibration with component already present-Evaluation by the height and area methods for constant sample quantity-Evaluation methods using integral detectors.- 3.3. Application of gas chromatography to the determination of thermodynamic values.