THE present volume, which is the first of a three-volume work on gas phase chromatography, deals with the problems of gas chromatography in packed columns. Gas chromatography, like any other analytical method, is mainly a matter of practical skill, and therefore emphasis has been given to the apparatus at the expense of a more detailed presentation of the theory. The aim of this book is to make lecturers and students, chemists, works engineers and laboratory workers familiar with this highly effective branch of analytical physical chemistry. I hope too that the experienced worker may find references which will be of value to him in his work and which will spare him part of the now almost impossible task of keeping up to date with the literature. The nomenclature used here is the result of a number of discussions with Professor E. Cremer and Dr. E. Bayer, and I should like to take this opportunity of expressing my grateful thanks to them. The present book is based partly on my book Gas Chromatography which appeared at the end of 1959. Numerous discussions with Professor E. Leibnitz and his colleagues H. P. Angele, M. Hofmann, H. Holzhauser, M. Kuhl and H. G. Struppe and the experimental work carried out with them have all influenced this revision. I should also like to thank Dr. H. Kienitz and his colleagues Dr. K. Dorfner, Dr. H. D. Ermshaus and Dr. H. Runge for valuable suggestions.
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Table of ContentsSurvey of the four fundamental chromatographic methodsLimits of application, definitions and methods of gas chromatographyNomenclatureHistory of gas chromatography.- 1. Theory of Gas Chromatography.- Definition and derivation of the characteristic values for gas chromatographyRetention volume and partition coefficientRetention values and the liquid phase in isothermal gas chromatographyHeight equivalent to a theoretical plateSeparation formula for gas chromatographic methodsSelectivity, column performance and resolutionRetention values and temperature of separation; retention temperatureNumber of theoretical plates and peak formGas chromathermography by the circulation technique.- 2. Apparatus.- 2.1. The column.- The column packingEvaluation of packed columnsCalculation of the number of theoretical plates, column performance and separation factorResolutionCalculation of the number of theoretical plates or column length necessary for a given separationLoad capacityPerformance indexTime of analysis and resolutionColumn materialColumn diameterThe solid supportRemoval of residual adsorption activityParticle diameterThe liquid phaseQuantity of liquid phaseImpregnation of the supportTesting the column packingPeak formControl of the quantity of liquid phase Temperature load capacityFilling the columnTesting the columnAgeing of the column packingSummary of the factors governing the preparation and operation of efficient columns.- 2.2. The carrier gas.- Gas purificationControl and measurement of the carrier gas flow rateDisturbances of constant flow rateProduction of a constant gas flow rateGas tightnessFlow rate meters.- 2.3. The sample injector.- Sample injectors for gasesSample injectors for liquids.- 2.4. Detectors.- Desirable and necessary properties of detectorsPrinciples of measurementThe thermal conductivity cellThe flame ionization detectorTesting of detectorsComparison of sensitivity.- 2.5. Recorders.- 2.6. Temperature.- The optimum operating temperatureConstant temperatureTemperature controlHeat insulationVariable temperatures.- 2.7. Industrial gas chromatographs and other special apparatus.- High temperature instrumentsMulti-column instrumentsApparatus for preparative workSample collection systems Fully automatic instrumentsTrace analysis instrumentsLow pressure instruments.- 3. The Analytical Result.- 3.1. The qualitative analytical result.- Preparation of the sampleChoice of the most suitable column and operating conditionsQualitative evaluationQualitative testing of columns.- 3.2. The quantitative result.- Requirements for the quantitative evaluation of gas chromatographic resultsMeasurement of peak areaEvaluation from peak area measurementsDirect surface area methodEvaluation by peak area measurements using specific calibration factorsEvaluation of the analysis by a calibration methodExternal calibration of the peak heightsExternal calibration of the peak areasInternal calibration with addition of extraneous substanceInternal calibration with component already presentEvaluation by the height and area methods for constant sample quantityEvaluation methods using integral detectors.- 3.3. Application of gas chromatography to the determination of thermodynamic values.