Table Of Content

Page i Tandem Techniques Page ii SEPARATION SCIENCE SERIES Editors: Raymond P. W. Scott, Colin Simpson and Elena D. Katz Quantitative Analysis using Chromatographic Techniques Edited by Elena D. Katz The Analysis of Drugs of Abuse Edited by Terry A. Gough Liquid Chromatography Column Theory by Raymond P. W. Scott Silica Gel and Bonded Phases Their Production, Properies and Use in LC by Raymond P. W. Scott Capillary Gas Chromatography by David W. Grant High Performance Liquid Chromatography: Principles and Methods in Biotechnology Edited by Elena D. Katz Tandem Techniques by Raymond P. W. Scott Page iii Tandem Techniques by Raymond P. W. Scott Georgetown University, Washington DC, USA and Birbeck College, University of London, UK Page iv Copyright © 1997 by John Wiley & Sons Ltd, Baffins Lane, Chichester West Sussex PO19 1UD, England National 01243 779777 International (+44) 1243 779777 e-mail (for orders and customer service enquiries): [email protected] Visit our Home Page on http://www.wiley.co.uk or http://www.wiley.com All Rights Reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, recording, scanning or otherwise, except under the terms of the Copyright Designs and Patents Act 1988 or under the terms of a licence issued by the Copyright Licensing Agency, 90 Tottenham Court Road, London W1P 9HE, UK, without the permission in writing of the Publisher Other Wiley Editorial Offices John Wiley and Sons, Inc., 605 Third Avenue, New York, NY 10158-0012, USA VCH Verlagsgesellschaft mbH, Pappelallee 3, D-69469 Weinheim, Germany Jacaranda Wiley Ltd, 33 Park Road, Milton, Queensland 4064, Australia John Wiley & Sons (Asia) Pte Ltd, Clementi Loop #02-01, Jin Xing Distripark, Singapore 129809 John Wiley & Sons (Canada) Ltd, 22 Worcester Road, Rexdale, Ontario M9W 1L1, Canada Library of Congress Cataloging-in-Publication Data Scott, Raymond P. W. (Raymond Peter William), 1924- Tandem techniques / Raymond P. W. Scott. p. cm. - (Separation science series) Includes bibiographical references and index. ISBN 0-471-96760-2 1. Chromatographic analysis. I. Title. II. Series. QD79.C4S3837 1997 96-42339 543'. 089-- dc20 CIP British Library Cataloguing in Publication Data: A catalogue record for this book is available from the British Library ISBN 0 471 96760 2 Typeset by the author Printed and bound in Great Britain by Bookcraft (Bath) Ltd. This book is printed on acid-free paper responsibly manufactured from sustainable forestation, for which at least two trees are planted for each one used for paper production. Page v CONTENTS Part 1 1 Introduction To Tandem Systems Chapter 1 3 Introduction To Tandem Techniques The Evolution of Analytical Instruments 3 Separation Techniques for Tandem Systems 7 Chromatography 7 Gas Chromatography 9 Gas Chromatography Columns. 13 Liquid Chromatography. 18 Liquid Chromatography Columns 19 Thin Layer Chromatography 25 The Function of the Chromatographic Column 27 Peak Dispersion 30 Capillary Electrophoresis 35 Zone Electrophoresis 36 Isotachophoresis 37 Isoelectric Focusing 38 Capillary Electrophoresis Apparatus 40 Synopsis 41 References. 43 Chapter 2 45 Identification Techniques For Tandem Use Introduction to Identification Techniques 45 Spectroscopy Involving the Absorption and Emission of 48 Electromagnetic Waves UV and Visible Spectroscopy 48 Fluorescence Spectroscopy 55 Infrared Spectroscopy 59 IR Spectroscopy Instrumentation 62 Raman Spectroscopy 66 Atomic Spectra 73 Atomic Absorption Spectroscopy 75 Chiro-Optical Measurements 76 Polarization Modulation 79 Practical Chiral Measuring Devices 80 Page vi Nuclear Magnetic Resonance Spectroscopy 82 The NMR Spectrometer 87 Mass Spectrometry 90 The Sector Mass Spectrometer 90 The Quadrupole Mass Spectrometer 94 The Ion Trap Detector 97 The Time of Flight Mass Spectrometer 99 Synopsis 101 References 103 Chapter 3 105 Interface Conduits Dispersion in Open Tubes 105 Gas Chromatography Columns and Connecting Tubes 105 Liquid Chromatography Columns and Connecting Tubes 113 Low Dispersion Connecting Tubes 122 Serpentine Tubes 126 Synopsis 128 References 129 Part 2 131 Gas Chromatography Tandem Systems Chapter 4 133 Gas Chromatography Ir Spectroscopy (Gc/Ir) Tandem Systems The Early GC/IR/M S Triplet System 134 Modem GC/IR Systems 138 Light Pipe Interfaces 138 The Cryostatic Interface 147 Thermogravimetric Analysis (TGA) Coupled with GC/IR and 153 GC/MS Synopsis 162 References 163 Chapter 5 165 Gas Chromatography / Mass Spectroscopy (Gc/Ms) Tandem Systems Vapor Concentrators 165 The Ryhage Concentrator 166 The Bieman Concentrator 167 Ion Sources Used in GC/M S 168 Electron Impact Ionization 168 Chemical Ionization 171 The Inductively Coupled Plasma Mass Spectrometer Ion Source 174