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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