Practical Liquid Chromatography

1: Liquid Chromatography-The Background.- 1.1. Perspective.- 1.2. Plan of the Book.- 1.3. Chromatography and Its Basic Variants.- 1.3.1. Adsorption Chromatography.- 1.3.2. Ion-Exchange Chromatography.- 1.3.3. Partition Chromatography.- 1.3.4. Exclusion Chromatography.- 1.4. Development Methods in Chromatography.- 1.4.1. Elution.- 1.4.2. Frontal Analysis.- 1.4.3. Displacement.- 1.5. Basic Experimental Arrangements.- 1.5.1. Column Chromatography.- 1.5.2. Layer Chromatography.- 1.6. Measures of the Effectiveness of Chromatographic Separations.- 1.6.1. HETP.- 1.6.2. Resolution.- 1.7. Retention Parameters.- 1.7.1. Measures of Retention.- 1.7.2. Retention and Identification.- References.- Further Reading.- 2: Band Spreading in Chromatography.- 2.1. Introduction.- 2.2. Factors Leading to Band Spreading.- 2.3. The "Random-Walk" Concept.- 2.4. Simple Mathematics of the Random Walk.- 2.5. Molecular Diffusion.- 2.6. Mass Transfer.- 2.7. Eddy Diffusion.- 2.8. Final Expression for Plate Height.- 2.9. Extrabed Contributions to Band Spreading.- 2.10. Columns versus Plates.- 2.11. Summary-Important Practical Consequences of Theory.- 2.11.1. Choice of Stationary Phase.- 2.11.2. Stationary Phase Particle Size.- 2.11.3. Dimensions of the Stationary Phase Bed.- 2.11.4. Choice of Mobile Phase.- 2.11.5. Mobile Phase Velocity.- 2.11.6. Operating Temperature.- 2.11.7. Availability of Appropriate Instrumentation.- References.- Further Reading.- 3: Adsorption Chromatography: Mechanism and Materials.- 3.1. Introduction.- 3.2. Adsorption Isotherms.- 3.3. Nature of Adsorption Forces.- 3.3.1. Van der Waals Forces (London Dispersion Forces).- 3.3.2. Inductive Forces.- 3.3.3. Hydrogen Bonding.- 3.3.4. Charge Transfer.- 3.3.5. Covalent Bonding (Chemisorption).- 3.4. Choice of Chromatographie System in LSAC.- 3.4.1. Choice of Adsorbent.- 3.4.2. Sample Size and Linear Capacity.- 3.4.3. Adsorbent Standardization.- 3.4.4. Choice of Mobile Phase.- 3.5. Variation of Adsorption Coefficient Kº with Solute Structure.- 3.6. Individual Adsorbents.- 3.6.1. Silica Gel.- 3.6.2. Alumina.- 3.6.3. Magnesium Silicates.- 3.6.4. Magnesia.- 3.6.5. Modified Adsorbents.- 3.6.6. Porous Layer Beads.- 3.6.7. Carbon.- 3.6.8. Ion Exchangers.- References.- Further Reading.- 4: Liquid Partition Chromatography-Mechanism and Materials.- 4.1. Introduction.- 4.2. Thermodynamics of Liquid-Liquid Partition.- 4.2.1. Relation between Partition Coefficient and Solution Properties.- 4.3. Selection of Phase Pairs.- 4.3.1. Selectivity.- 4.3.2. Stability of Phase Pairs.- 4.3.3. Relation of Dynamics to Phase Pair Choice.- 4.4. Support Materials.- 4.5. Further Practical Considerations.- 4.5.1. Preparation of Stationary Phases.- 4.5.2. Liquid Phase "Loading" and Sample Capacity.- References.- Further Reading.- 5: Exclusion Chromatography-Mechanism and Materials.- 5.1. Introduction.- 5.2. Peak Broadening in Exclusion Chromatography.- 5.3. Theories of Exclusion Chromatography.- 5.4. Stationary Phases for Exclusion Chromatography.- 5.4.1. Inorganic Stationary Phases.- 5.4.2. Alkylated Cross-Linked Dextrans.- 5.4.3. Polyvinyl Acetate Gels.- 5.4.4. Polystyrene-Divinyl Benzene Gels.- Appendix: Applications of Exclusion Chromatography.- References.- Further Reading.- 6: The Technique of Thin-Layer Chromatography.- 6.1. Introduction.- 6.2. Outline of Technique.- 6.3. The Stationary Phase.- 6.4. Preparation of TLC Plates.- 6.4.1. Choice of Support.- 6.4.2. Preparation of Slurry.- 6.4.3. Coating the Plate.- 6.4.4. Drying and Storage of Plates.- 6.4.5. Precoated Plates.- 6.4.6. Conclusions.- 6.5. Application of the Sample.- 6.5.1. Analytical Scale.- 6.5.2. Preparative Scale.- 6.6. Choice of Mobile Phase.- 6.7. Development of Chromatogram.- 6.7.1. Tank Development.- 6.7.2. Sandwich Chambers.- 6.7.3. Other Methods of Development.- 6.8. Reproducibility of RF Values.- 6.8.1. Introduction.- 6.8.2. Factors Affecting Reproducibility.- 6.8.3. Conclusions.- 6.9. Detection of Solutes.- 6.9.1. Inspection under Ultraviolet