Purification of Laboratory Chemicals

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ISBN: 9780750675710 | 0750675713
Cover: Paperback
Copyright: 3/20/2003

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Now in its fifth edition, the book has been updated to include more detailed descriptions of new or more commonly used techniques since the last edition as well as remove those that are no longer used, procedures which have been developed recently, ionization constants (pKa values) and also more detail about the trivial names of compounds. In addition to having two general chapters on purification procedures, this book provides details of the physical properties and purification procedures, taken from literature, of a very extensive number of organic, inorganic and biochemical compounds which are commercially available. This is the only complete source that covers the purification of laboratory chemicals that are commercially available in this manner and format.

Preface to the Fifth Edition

Preface to the First Edition

xiii

Preface to the Second Edition

xiii

Preface to the Third Edition

xiv

Preface to the Fourth Edition

Common Physical Techniques Used in Purification

(52)

Introduction

(1)

The Question of Purity

(3)

Sources of Impurities

(1)

Practices to Avoid Impurities

(1)

Cleaning practices

(1)

Silylation of glassware and plasticware

(1)

Safety Precautions Associated with the Purification of Laboratory Chemicals

(2)

Some Hazards of Chemical Manipulation in Purification and Recovery of Residues

(1)

Perchlorates and perchloric acid

(1)

Peroxides

(1)

Heavy-metal-containing-explosives

(1)

Strong acids

(1)

Reactive halides and anhydrides

(1)

Solvents

(1)

Salts

(1)

Safety Disclaimer

(1)

Methods of Purification of Reagents and Solvents

(24)

Solvent Extraction and Distribution

(1)

Ionisation constants and pK

(1)

pK and Temperature

(1)

pK and solvent

(1)

Distillation

(1)

Techniques

(1)

Distillation of liquid mixtures

(1)

Types of distillation

(1)

The distilling flask

(1)

Types of columns and packings

(1)

Condensers

(1)

Vacuum distillation

(1)

Spinning-band distillation

(1)

Steam distillation

(1)

Azeotropic distillation

(1)

Kugelrohr distillation

(1)

Isopiestic or isothermal distillation

(1)

Recrystallisation

(1)

Techniques

(1)

Filtration

(1)

Choice of solvents

(1)

Petroleum ethers

(1)

Mixed Solvents

(1)

Recrystallisation from the melt

(1)

Zone refining

(1)

Sublimation

(1)

Chromatography

(1)

Vapour phase chromatography (GC or gas-liquid chromatography)

(1)

Liquid chromatography

(1)

Adsorption chromatography

(1)

Thin layer chromatography (TLC)

(1)

Paper chromatography

(1)

Column Chromatography

(1)

Graded Adsorbents and Solvents

(1)

Preparation and Standardisation of Alumina

(1)

Preparation of other adsorbents

(1)

Silica

(1)

Diatomaceous earth

(1)

Charcoal

(1)

Cellulose

(1)

Flash Chromatography

(1)

Paired-ion Chromatography

(1)

Ion-exchange Chromatography

(1)

Ion-exchange Resins

(1)

Ion-exchange Celluloses and Sephadex

(1)

Sephadex

(1)

Sepharose

(1)

Cellex CM

(1)

Cellex D

(1)

Crystalline Hydroxylapatite

(1)

Gel Filtration

(1)

High Performance Liquid Chromatography (HPLC)

(1)

Other Types of Liquid Chromatography

(1)

Drying

(1)

Removal of Solvents

(1)

Removal of Water

(1)

Intensity and Capacity of Common Desiccants

(1)

Suitability of Individual Desiccants

(1)

Molecular sieves

(1)

Miscellaneous Techniques

(1)

Freeze-pump-thaw and purging

(1)

Vacuum-lines, Schlenk and glovebox techniques

(1)

Abbreviations

(1)

Tables

(15)

Some Common Immiscible or Slightly Miscible Pairs of Solvents

(1)

Aqueous Buffers

(1)

Predicted Effect of Pressure on Boiling Point

(1)

Predicted Effect of Pressure on Boiling Point

(1)

Nomogram

(1)

Heating Baths

(1)

Whatman Filter Papers

(1)

Micro Filters

(1)

Common Solvents Used in Recrystallisation

(1)

Pairs of Miscible Solvents

(1)

Materials for Cooling Baths

(1)

Liquids for Stationary Phases in Gas Chromatography

(1)

Methods of Visualisation of TLC Spots

(1)

Graded Adsorbents and Solvents

(1)

Representative Ion-Exchange Resins

(1)

Modified Fibrous Celluloses for Ion-Exchange

(1)

Bead Form Ion-Exchange Packagings

(1)

Liquids for Drying Pistols

(1)

Vapour Pressures (mm Hg) of Saturated Aqueous Solutions in Equilibrium With Solid Salts

(1)

Drying Agents for Classes of Compounds

(1)

Static Drying for Selected Liquids (25°C)

(1)

Boiling Points of Some Useful Gases at 760 mm

(1)

Solubilities of HCl and NH3 at 760mm (g/100g of Solution)

(1)

Prefixes for Quantities

(1)

Bibliography

(8)

Chemical Methods Used in Purification

(19)

General Remarks

(1)

Removal of Traces of Metals From Reagents

(2)

Metal Impurities

(1)

Distillation

(1)

Use of Ion Exchange Resins

(1)

Precipitation

(1)

Removal of lead contaminants

(1)

Removal of iron contaminants

(1)

Removal of other metal contaminants

(1)

Extraction

(1)

Complexation

(1)

Use of Metal Hydrides

(1)

Lithium Aluminium Hydride

(1)

Calcium Hydride

(1)

Sodium Borohydride

(1)

Potassium Borohydride

(1)

Purification via Derivatives

(4)

Alcohols

(1)

Aldehydes

(1)

Amines

(1)

Picrates

(1)

Salts

(1)

Double salts

(1)

N-Acetyl derivatives

(1)

N-Tosyl derivatives

(1)

Aromatic Hydrocarbons

(1)

Adducts

(1)

Sulfonation

(1)

Carboxylic Acids

(1)

4-Bromophenacyl esters

(1)

Alkyl esters

(1)

Salts

(1)

Hydroperoxides

(1)

Ketones

(1)

Bisulfite adduct

(1)

Semicarbazones

(1)

Phenols

(1)

Benzoates

(1)

Acetates

(1)

Phosphate and Phosphonate Esters

(1)

Miscellaneous

(1)

General Methods for the Purification of Classes of Compounds

(1)

Procedures

(1)

Criteria of Purity

(1)

General Procedures for the Purification of Some Classes of Organic Compounds

(9)

Acetals

(1)

Acids

(1)

Carboxylic acids

(1)

Sulfonic acids

(1)

Sulfinic acids

(1)

Acid Chlorides

(1)

Alcohols

(1)

Monohydric alcohols

(1)

Polyhydric alcohols

(1)

Aldehydes

(1)

Amides

(1)

Amines

(1)

Amino Acids

(1)

Anhydrides

(1)

Carotenoids

(1)

Esters

(1)

Ethers

(1)

Halides

(1)

Hydrocarbons

(1)

Imides

(1)

Imino Compounds

(1)

Ketones

(1)

Macromolecules

(1)

Nitriles

(1)

Nitro Compounds

(1)

Nucleic Acids

(1)

Phenols

(1)

Polypeptides and Proteins

(1)

Quinones

(1)

Salts (Organic)

(1)

With metal ions

(1)

With organic cations

(1)

With sodium alkane sulfonates

(1)

Sulfur Compounds

(1)

Disulfides

(1)

Sulfones

(1)

Sulfoxides

(1)

Thioethers

(1)

Thiols

(1)

Thiolsulfonates (disulfoxides)

(1)

Bibliography

(2)

The Future of Purification

(8)

Introduction

(1)

Solid Phase Synthesis

(5)

Solid Phase Peptide Synthesis (Spps)

(1)

Solid Phase Deoxyribonucleotide Synthesis

(1)

Solid Phase Oligosaccharide Synthesis

(1)

Solid Phase Organic Synthesis (Spos)

(1)

Polymer Supported Reactants

(1)

Scavenger Resins

(1)

Resin Support

(1)

Choice of Resin for Spos

(1)

Combinatorial Chemistry

(1)

Monitoring Solid Phase Reactions

(1)

Infra red analysis of resin

(1)

Qualitative and quantitative analyses

(1)

Detection of Reactive Groups on Resins

(1)

Detection of hydroxy groups on resin

(1)

Detection of aldehyde groups on resin

(1)

Detection of carboxy groups on resin

(1)

Detection of amino groups on resin

(1)

Detection of thiol groups on resin

(1)

Fmoc assay

(1)

Ionic Liquids

(1)

Fluorous Chemistry

(1)

Bibliography

(2)

Purification of Organic Chemicals

(309)

Purification of Inorganic and Metalorganic Chemicals (Including Organic compounds of B, Bi, P, Se, Si, and ammonium and metal salts of organic acids)

389

(111)

Purification of Biochemicals and Related Products

500

(78)

General Subject Index

578

(7)

Cas Registry Numbers Index

585

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Purification of Laboratory Chemicals

Summary

Table of Contents

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