本书在介绍提纯相关技术(重结晶、干燥、色谱、蒸馏、萃取、衍生物的制备等)基础上，详细介绍了化学品的纯化方法，例如重结晶的溶剂选择，常压和减压蒸馏的沸点，纯化以前的处理手续等。从粗略纯化到高度纯化都有详细说明，并附参考文献。给出了几乎所有商品化有机化学品、无机化学品以及生化试剂的基本理化性质和纯化过程，包括名称、CAS登录号、分子量、熔点、沸点、相对密度、溶解性、离子化常数等。

本书是广大实验室工作人员必备的工具书。

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