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Preface to the Sixth Edition

THERE IS a continuing demand for the

Purification of Laboratory Chemicals

book, to the

extent that the 5th edition which was published in early 2003 was carefully translated into

Chinese (ISBN 978-7-5025-94367) by Ying-Jie Lin, Wei Liu, Hui-Ping Wang, Xiao-Bo Sun,

Qing-Shan Li and Jun-Gang Cao from Jilin University (People’s Republic of China) in 2007. In

response to the demand, it was timely to update the 5

edition to include the more recently

developed purification procedures, as well as add to the list of compounds for purification. The

latter comprise some commercially available compounds that have gained usefulness and

popularity in the past few years.

The first two chapters have been updated, sections of current interest have been expanded and

new sections added. Chapter 3 has been rewritten so that areas of work that have lost popularity

have been reduced in size or deleted and sections on recent, and now commonly adopted,

technologies have been inserted. Chapters 4, 5 and 6 are now completely reorganized, and each

is subdivided into several sections which will make it easier for the reader to locate compounds

of similar classification. Chapter 4 is subdivided into aliphatic, alicyclic, aromatic and

heterocyclic compounds, Chapter 5 has been subdivided into inorganic and metal-organic

compounds, and Chapter 6 has been subdivided into amino acids and peptides, proteins,

enzymes, DNA and RNA, carotenoids, carbohydrates, steroids and a miscellaneous section

which includes small biologically active substances such as antibiotics, coenzymes, co-factors,

lipids, phospholipids, polynucleotides and vitamins. Some useful compounds that have been

added recently to commercial catalogues have been included in these three chapters. A large

number of derivatives of previous entries with their physical properties and purifications have

been inserted together with extensive referencing to the original literature including

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references. This resulted in an increase in size of the 5th edition, in text and number of

compounds, by over 20%. The purifications of some 7400 substances are described. As in the

5th edition, substance entries are in alphabetical order within subsections and each substance is

defined by its Chemical Abstracts Service (CAS) Registry Number. An index of these numbers

with their respective page numbers at the end of the book will make it possible to locate the

purification of a desired substance readily and to check if the substance is contained in the book.

For this purpose we thank Rodney Armarego for setting up a

Macro

on the MacBook Pro

computer used for collating the CAS Registry Numbers for the index. There is also a General

Index of Contents.

Website references of distributors of substances and/or of equipment have been included in the

text. However, since these may change in the future, users should check for current websites of

suppliers. The bibliographies have been updated, and websites of a few publishers and book

suppliers have been included. Several texts with publication dates older than fifteen years have

been deleted except for a few very useful textbooks which are out of print and where recent

editions have not been produced. In these cases it is usually possible to obtain used copies from

good suppliers of old books, for which there are several websites, e.g. visit Google under “old

books suppliers”; also visit

websites such as <http//www.abebooks.com>,

<http//www.betterworld.com/usedbooks>, <http//www.booksandcollectibles.com.au/index>,

<http//www.ebay.com.au/>. Further information for almost every entry in Chapters 4, 5 and 6 of

the 6th edition can be obtained from the references to the original literature, which are cited

under each entry together with their respective

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reference(s).

We thank readers who have provided advice, constructive criticism and new information. We

are grateful for any further comments, suggestions, amendments and criticisms which could,

perhaps, be inserted in a second printing of this edition. We thank Joe Papa BS MS (EXAXOL in

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Clearwater, Florida, USA) in particular for sharing his experiences on the purification of several

inorganic substances in this and previous editions, and also for allowing us to use his analytical

results on the amounts of metal impurities at various stages of purification of several salts.

We thank Dr Pauline M. Armarego for assistance in the painstaking task of entering data into

respective files, for many hours of proofreading, correcting typographical errors and checking

CAS Registry Numbers against their respective entries.

One of us (W.L.F.A) owes a debt of gratitude to Dr Desmond (Des) J. Brown of the Research

School of Chemistry, ANU, for unfailing support and advice over several decades and for

providing data that was difficult to acquire not only for this edition but also for the previous five

editions of this book.

One of us (C.L.L.C) would like to acknowledge the support and friendship of her many research

staff and students (past and present at ANU and A*STAR). She especially thanks Drs Paul

Huleatt, Paul Bernardo, Felicity Moore and Brendan Burkett for their unfailing faith in her,

through chemical and personal journeys both in Singapore and Australia. The legacy of this book

is for Kimberley and Victoria Tse because it is cool to be a scientist!

We thank Mrs Joan Smith, librarian of the Research School of Chemistry, ANU, for her

generous help in many library matters which made the tedious task of checking references more

enduring.

W.L.F. Armarego & C.L.L. Chai

November 2008

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Preface to the First Edition

WE BELIEVE that a need exists for a book to help the chemist or biochemist who wishes to purify the reagents she or he uses. This need is

emphasised by the previous lack of any satisfactory central source of references dealing with individual substances. Such a lack must

undoubtedly have been a great deterrent to many busy research workers who have been left to decide whether to purify at all, to improvise

possible methods, or to take a chance on finding, somewhere in the chemical literature, methods used by some previous investigators.

Although commercially available laboratory chemicals are usually satisfactory, as supplied, for most purposes in scientific and technological

work, it is also true that for many applications further purification is essential.

With this thought in mind, the present volume sets out, first, to tabulate methods, taken from the literature, for purifying some thousands of

individual commercially available chemicals. To help in applying this information, two chapters describe the more common processes currently

used for purification in chemical laboratories and give fuller details of new methods which appear likely to find increasing application for the

same purpose. Finally, for dealing with substances not separately listed, a chapter is included setting out the usual methods for purifying specific

classes of compounds.

To keep this book to a convenient size, and bearing in mind that its most likely users will be laboratory-trained, we have omitted manipulative

details with which they can be assumed to be familiar, and also detailed theoretical discussion. Both are readily available elsewhere, for example

in Vogel's very useful book

Practical Organic Chemistry

(Longmans, London, 3rd ed., 1956), or Fieser's

Experiments in Organic Chemistry

(Heath, Boston, 3rd ed., 1957).

For the same reason, only limited mention is made of the kinds of impurities likely to be present, and of the tests for detecting them. In many

cases, this information can be obtained readily from existing monographs.

By its nature, the present treatment is not exhaustive, nor do we claim that any of the methods taken from the literature are the best possible.

Nevertheless, we feel that the information contained in this book is likely to be helpful to a wide range of laboratory workers, including physical

and inorganic chemists, research students, biochemists, and biologists. We hope that it will also be of use, although perhaps to only a limited

extent, to experienced organic chemists.

We are grateful to Professor A. Albert and Dr D.J. Brown for helpful comments on the manuscript.

D.D.P., W.L.F.A. & D.R.P.

1966

Preface to the Second Edition

SINCE the publication of the first edition of this book, there have been major advances in purification procedures. Sensitive methods have been

developed for the detection and elimination of progressively lower levels of impurities. Increasingly stringent requirements for reagent purity

have gone hand-in-hand with developments in semiconductor technology, in the preparation of special alloys and in the isolation of highly

biologically active substances. The need to eliminate trace impurities at the micro- and nanogram levels has placed greater emphasis on

ultrapurification technique. To meet these demands the range of purities of laboratory chemicals has become correspondingly extended.

Purification of individual chemicals thus depends more and more critically on the answers to two questions-Purification from what, and to what

permissible level of contamination. Where these questions can be specifically answered, suitable methods of purification can usually be devised.

Several periodicals devoted to ultrapurification and separations have been started. These include "Progress in Separation and Purification" (vol.

1) Ed. E.S. Perry, Wiley-Interscience, New York, vols. 1-4, 1968-1971, and

Separation and Purification Methods,

Ed. E.S.Perry and C.J.van

Oss, Marcel Dekker, New York, vol. 1, 1973. Nevertheless, there still remains a broad area in which a general improvement in the level of

purity of many compounds can be achieved by applying more or less conventional procedures. The need for a convenient source of information

on methods of purifying available laboratory chemicals was indicated by the continuing demand for copies of this book even though it had been

out of print for several years.

We have sought to revise and update this volume, deleting sections that have become more familiar or less important, and incorporating more

topical material. The number of compounds in Chapters 3 and 4 have been increased appreciably. Also, further details in purification and

physical constants are given for many compounds that were listed in the first edition.

We take this opportunity to thank users of the first edition who pointed out errors and omissions, or otherwise suggested improvements or

additional material that should be included. We are indebted to Mrs S.Schenk who emerged from retirement to type this manuscript.

D.D.P., W.L.F.A. & D.R.P.

1980

Preface to the Third Edition

THE CONTINUING demand for this monograph and the publisher's request that we prepare a new edition are an indication that

Purification of

Laboratory Chemicals

fills a gap in many chemists' reference libraries and laboratory shelves. The present volume is an updated edition that

contains significantly more detail than the previous editions, as well as an increase in the number of individual entries and a new chapter.

Additions have been made to Chapters 1 and 2 in order to include more recent developments in techniques (e.g. Schlenk-type,

p. 10), and

chromatographic methods and materials. Chapter 3 still remains the core of the book, and lists in alphabetical order relevant information on

4000 organic compounds. Chapter 4 gives a smaller listing of

750 inorganic and metal-organic substances, and makes a total increase of ca

13% of individual entries in these two chapters. Some additions have also been made to Chapter 5.

We are currently witnessing a major development in the use of physical methods for purifying large molecules and macromolecules, especially of

biological origin. Considerable developments in molecular biology are apparent in techniques for the isolation and purification of key

biochemicals and substances of high molecular weight. In many cases something approaching homogeneity has been achieved, as evidenced by

electrophoresis, immunological and other independent criteria. We have consequently included a new section, Chapter 6, where we list upwards

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