Purification of Laboratory Chemicals (7th Edition).pdf

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Purification of Laboratory Chemicals

Seventh Edition

The John Curtin School of Medical Research

ANU College of Medicine, Biology, and Environment

The Australian National University, Canberra, A.C.T.

AUSTRALIA

Wilfred L. F. Armarego

Department of Pharmacy, National University of Singapore (NUS)

and

Institute of Chemical and Engineering Sciences

Agency for Science, Technology, and Research (A*STAR)

SINGAPORE

Christina Li Lin Chai

AMSTERDAM • BOSTON • HEIDELBERG • LONDON

NEW YORK • OXFORD • PARIS • SAN DIEGO

SAN FRANCISCO • SINGAPORE • SYDNEY • TOKYO

Butterworth-Heinemann is an imprint of Elsevier

The Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, UK

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Sixth edition 2008

Seventh edition 2013

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No responsibility is assumed by the publisher for any injury and/or damage to persons

or property as a matter of products liability, negligence or otherwise, or from any use or

operation of any methods, products, instructions or ideas contained in the material herein.

Because of rapid advances in the medical sciences, in particular, independent verification of

diagnoses and drug dosages should be made

British Library Cataloguing in Publication Data

A catalogue record for this book is available from the British Library

Library of Congress Cataloging-in-Publication Data

A catalog record for this book is available from the Library of Congress

ISBN: 978-0-12-382161-4

For information on all Butterworth-Heinemann publications

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Printed and bound in the US

12 13 14 15 16 10 9 8 7 6 5 4 3 2 1

HOW THIS BOOK SHOULD BE USED

Substances have been entered under their respective chapters, sections and subsections. In

these sections compounds have been entered in alphabetical order according to the more

commonly used name. However, because compounds can be named differently (some of

these other names have been included in brackets after their entries) and may be difficult to

find, it is advisable to obtain the page number of the entry from the Chemical Abstracts

Registry Numbers (CASRNs) Index at the end of the book. CASRNs of substances are

readily obtained from “SciFinder”, or better, from any commercial catalogue that sells these

compounds, as almost all of these have CASRNs inserted after the names of their products.

Also, in this book we could not insert some substances that can be formally included in more

than one section without repeating the entry. In such cases the compounds are entered in a

preferred section and are cross-referenced by inserting “see [CASRN]” or just “[CASRN]”.

Thus the cross-reference is its CASRN. The CASRNs Index provides the page numbers in

bold/italic type. If the CASRN of a desired substance is not in the CASRN Index, or its full

or abbreviated name is not in the General Index, then it will not be present in this book.

CASRNs are unique for each chemical substance and are such that they are internally

consistent. They are set up according to a specific formula. Refer to the first page of the

CASRNs Index to calculate the formula in order to check whether the number is a valid

number or not.

W.L.F.A. & C.L.L.C.

xxi

Preface to the Seventh Edition

THE SALES of the sixth edition, which appeared in April 2009, were high by about October 2009, and one of us

(WLFA) was approached by Ms Melanie Benson, Editorial Project Manager of Elsevier Science & Technology

Books (who was mainly responsible for the production of the 6th edition), about writing a 7th edition within 2–3

years. In the past, 6–9 years were allowed to lapse between editions. However, the attraction this time, was that we

were allowed to increase the size of the work by up to 249 pages. This has given us the opportunity to update all the

previous chapters in the light of current thinking on safety (personal and environmental), and to introduce two new

chapters. The award of five Nobel Prizes in the past ten years or so in Chemistry and one in Physics, of which three

were awarded for work on

Catalysis

and

the catalytic process

(2001, 2005 and 2010), and two for work on

Nanomaterials and Nanotechnology

(1996, 2010) have prompted us to write a new chapter on

Catalysts

and a new

chapter on

Nanomaterials and Nanotechnology.

Chemical suppliers have now made commercially available a large

number of catalysts as well as many nanomaterials of various sorts. Since the number of commercially available

catalysts are currently considerably larger than that of nanomaterials, the chapter on Catalysts is larger than that on

Nanomaterials and Nanotechnology, and had to be divided into two parts. The availability, preparation and

purification of a large range of these, are presented in these chapters. The other chapters have been updated and

expanded, also in keeping with the purpose of all previous editions which is to provide information for the

purification of commercially available laboratory materials. Of course, the General Subjects Index and the

Chemical Abstracts Registry Numbers (CASRNs) Index increased in size accordingly. Much of the cross-

referencing is done

via

CASRNs and a page of how to use this book through these is included before Chapter 1 to

assist the reader, not only to locate the pages where the required CASRNs are to be found, but also to let the reader

know whether a particular substance is included in this work. CASRNs can be readily obtained from chemical

catalogues or from SciFinder.

We would like to acknowledge Professor Martin Banwell FAA (Director, Research School of Chemistry, ANU) for

his generosity in allowing the use of IT services, and to Dr Emil Mittag (Research School of Chemistry, ANU) for

editing and updating the

Macro

program used for making the CASRNs Index.

We are greatly indebted to many people who have made valuable and constructive comments, and indicated errors,

in previous editions. The continued help from Joe Papa of BS MS (EXAXOL in Clearwater, Florida, USA) with the

preparation and purification of several inorganic compounds, particularly beryllium and cerium, is appreciated and

gratefully acknowledged.

One of us (W.L.F.A) owes a debt of gratitude to Professor Jill E. Gready (John Curtin School of Medical Research,

ANU) for her continued encouragement and for strongly supporting a Visiting Fellowship over a period of many

years.

We thank Dr Pauline M. Armarego for assistance in the painstaking task of proofreading and correcting

typographical errors as well as checking the General Index and the CASRNs Index.

We thank the ANU library and its staff, both on campus and at the ANU Print Repository, for their prompt and

unfailing assistance.

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

May 2012

CONTENTS

Preface to the Seventh Edition ................................................................................................. v

Preface to the First Edition ...................................................................................................... vi

Preface to the Second Edition .................................................................................................vi

Preface to the Third Edition .................................................................................................... vi

Preface to the Fourth Edition..................................................................................................vii

Preface to the Fifth Edition ................................................................................................. viii

Preface to the Sixth Edition ..................................................................................................... ix

CHAPTER 1

COMMON PHYSICAL TECHNIQUES USED IN PURIFICATION

INTRODUCTION .................................................................................................................... 1

THE QUESTION OF PURITY ................................................................................................ 1

SOURCES OF IMPURITIES ......................................................................................... 3

PRACTICES TO AVOID IMPURITIES ....................................................................... 3

Cleaning practice ........................................................................................................ 3

Silylation of glassware and plasticware ..................................................................... 4

SAFETY PRECAUTIONS ASSOCIATED WITH THE PURIFICATION

OF LABORATORY CHEMICALS ........................................................................................ 4

SOME HAZARDS OF CHEMICAL MANIPULATION IN PURIFICATION AND

RECOVERY OF RESIDUES ......................................................................................... 5

Perchlorates and perchloric acid ................................................................................. 5

Peroxides .................................................................................................................... 6

Heavy-metal-containing explosives ........................................................................... 6

Strong acids ................................................................................................................ 6

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