Preface to the Fifth Edition Preface to the First Edition Preface to the Second Edition Preface to the Third Edition Preface to the Fourth Edition CHAPTER 1 COMMON PHYSICAL TECHNIQUES USED IN PURIFICATION INTRODUCTION THE QUESTION OF PURITY SOURCES OF IMPURITIES PRACTICES TO AVOID IMPURITIES Cleaning practices Silylation of glassware and plasticware SAFETY PRECAUTIONS ASSOCIATED WITH THE PURIFICATION OF LABORATORY CHEMICALS SOME HAZARDS OF CHEMICAL MANIPULATION IN PURIFICATION AND RECOVERY OF RESIDUES Perchlorates and perchloric acid Peroxides Heavy-metal-containing-explosives Strong acids Reactive halides and anhydrides Solvents Salts SAFETY DISCLAIMER METHODS OF PURIFICATION OF REAGENTS AND SOLVENTS SOLVENT EXTRACTION AND DISTRIBUTION Ionisation constants and pK pK and Temperature pK and solvent DISTILLATION Techniques Distillation of liquid mixtures Types of distillation The distilling flask Types of columns and packings Condensers Vacuum distillation Spinning-band distillation Steam distillation azeotropic distillation ii...iiii Kiigelrohr distillation lsopiestic or isothermal distillation RECRYSTALLISATION Techniques Filtration Choice of solvents Petroleum ethers Mixed Solvents RecrystaUisation from the melt Zone refining SUBLIMATION CHROMATOGRAPHY Vapour phase chromatography (GC or gas-liquid chromatography) Liquid chromatography Adsorption chromatography Thin layer chromatography (TLC) Paper chromatography Column Chromatography Graded Adsorbents and Solvents Preparation and Standardisation of Alumina Preparation of other adsorbents Silica Diatomaceous earth Charcoal Cellulose Flash Chromatography Paired-ion Chromatography Ion-exchange Chromatography Ion-exchange Resins Ion-exchange Celluloses and Sephadex Sephadex Sepharose CeUex CM Cellex D Crystalline Hydroxyiapatite Gel Filtration High Performance Liquid Chromatography (HPLC) Other Types of Liquid Chromatography DRYING Removal of Solvents Removal of Water Intensity and Capacity of Common Desiccants Suitability of Individual Desiccants Molecular sieves MISCELLANEOUS TECHNIQUES Freeze-pump-thaw and purging Vacuum-lines， Schlenk and glovebox techniques ABBREVIATIONS TABLES TABLE 1. SOME COMMON IMMISCIBLE OR SLIGHTLY MISCIBLE PAIRS OF SOLVENTS TABLE 2. AQUEOUS BUFFERS TABLE 3A. PREDICTED EFFECT OF PRESSURE ON BOILING POINT TABLE 3B. PREDICTED EFFECT OF PRESSURE ON BOILING POINT FIGURE 1： NOMOGRAM TABLE 4. HEATING BATHS TABLE 5. WHATMAN FILTER PAPERS TABLE 6. MICRO FILTERS TABLE 7. COMMON SOLVENTS USED IN RECRYSTALLISATION TABLE 8. PAIRS OF MISCIBLE SOLVENTS TABLE 9. MATERIALS FOR COOLING BATHS TABLE 10. LIQUIDS FOR STATIONARY PHASES IN GAS CHROMATOGRAPHY TABLE 11. METHODS OF VISUALISATION OF TLC SPOTS TABLE 12. GRADED ADSORBENTS AND SOLVENTS TABLE 13. REPRESENTATIVE ION-EXCHANGE RESINS TABLE 14. MODIFIED FIBROUS CELLULOSES FOR ION-EXCHANGE TABLE 15. BEAD FORM ION-EXCHANGE PACKAGINGS TABLE 16. LIQUIDS FOR DRYING PISTOLS TABLE 17. VAPOUR PRESSURES (mm Hg) OF SATURATED AQUEOUS SOLUTIONS IN EQUILIBRIUM WITH SOLID SALTS TABLE 18. DRYING AGENTS FOR CLASSES OF COMPOUNDS TABLE 19. STATIC DRYING FOR SELECTED LIQUIDS (25~C) TABLE 20. BOILING POINTS OF SOME USEFUL GASES AT 760 mm TABLE 21. SOLUBILITIES OF HC1 AND NH3 AT 760mm (g/100g OF SOLUTION) TABLE 22. PREFIXES FOR QUANTITIES BIBLIOGRAPHY CHAPTER 2 CHEMICAL METHODS USED IN PURIFICATION GENERAL REMARKS REMOVAL OF TRACES OF METALS FROM REAGENTS METAL IMPURITIES DISTILLATION USE OF ION EXCHANGE RESINS PRECIPITATION Removal of lead contaminants Removal of iron contaminants Removal of other metal contaminants EXTRACTION COMPLEXATION USE OF METAL HYDRIDES LITHIUM ALUMINIUM HYDRIDE CALCIUM HYDRIDE SODIUM BOROHYDRIDE POTASSIUM BOROHYDRIDE PURIFICATION via DERIVATIVES ALCOHOLS ALDEHYDES AMINES Picrates Salts Double salts N-Acetyl derivatives N-Tosyl derivatives AROMATIC HYDROCARBONS Adducts Sulfonation CARBOXYLIC ACIDS 4-Bromophenacyl esters Alkyl esters Salts HYDROPEROXIDES KETONES Bisulfite adduct Semicarbazones PHENOLS Benzoates Acetates PHOSPHATE AND PHOSPHONATE ESTERS MISCELLANEOUS GENERAL METHODS FOR THE PURIFICATION OF CLASSES OF COMPOUNDS PROCEDURES CRITERIA OF PURITY GENERAL PROCEDURES FOR THE PURIFICATION OF SOME CLASSES OF ORGANIC COMPOUNDS ACETALS ACIDS Carboxylic acids Sulfonic acids Sulfinic acids ACID CHLORIDES ALCOHOLS Monohydric alcohols Polyhydric alcohols ALDEHYDES AMIDES AMINES AMINO ACIDS ANHYDRIDES CAROTENOIDS ESTERS ETHERS HALIDES HYDROCARBONS IMIDES IMINO COMPOUNDS KETONES MACROMOLECULES NITRILES NITRO COMPOUNDS NUCLEIC ACIDS PHENOLS POLYPEPTIDES AND PROTEINS QUINONES SALTS (ORGANIC) With metal ions With organic cations With sodium alkane sulfonates SULFUR COMPOUNDS Disulfides Sulfones Sulfoxides Thioethers Thiols Thiolsulfonates (disulfoxides) BIBLIOGRAPHY CHAPTER 3 THE FUTURE OF PURIFICATION INTRODUCTION SOLID PHASE SYNTHESIS SOLID PHASE PEPTIDE SYNTHESIS (SPPS) SOLID PHASE DEOXYRIBONUCLEOTIDE SYNTHESIS SOLID PHASE OLIGOSACCHARIDE SYNTHESIS SOLID PHASE ORGANIC SYNTHESIS (SPOS) POLYMER SUPPORTED REACTANTS SCAVENGER RESINS RESIN SUPPORT CHOICE OF RESIN FOR SPOS COMBINATORIAL CHEMISTRY MONITORING SOLID PHASE REACTIONS Infra red analysis of resin Qualitative and quantitative analyses DETECTION OF REACTIVE GROUPS ON RESINS Detection of hydroxy groups on resin Detection of aldehyde groups on resin Detection of carboxy groups on resin Detection of amino groups on resin Detection of thiol groups on resin Fmoc assay IONIC LIQUIDS FLUOROUS CHEMISTRY BIBLIOGRAPHY CHAPTER 4 PURIFICATION OF ORGANIC CHEMICALS CHAPTER 5 PURIFICATION OF INORGANIC AND METALORGANIC CHEMICALS(Including Organic compounds of B， Bi， P， Se， Si， and ammonium and metal salts of organic acids) CHAPTER 6 PURIFICATION OF BIOCHEMICALS AND RELATED PRODUCTS GENERAL SUBJECT INDEX CAS REGISTRY NUMBERS INDEX
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