Basic Gas Chromatography 2nd Edition by Harold M. McNair


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Basic Gas Chromatography nd Edition by Harold McNair
BASIC GAS CHROMATOGRAPHYBASIC GAS CHROMATOGRAPHYSecond EditionHAROLD M. MCNAIRJAMES M. MILLERA JOHN WILEY & SONS, INC., PUBLICATIONCopyright © 2009 by John Wiley & Sons, Inc. All rights reservedPublished by John Wiley & Sons, Inc., Hoboken, New JerseyPublished simultaneously in CanadaNo 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 as permitted under Section 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, Inc., 222 Rosewood Drive, Danvers, MA 01923, (978) 750-8400, fax (978) 750-4470, or on the web at Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 111 River Street, Hoboken, NJ 07030, (201) 748-6011, fax (201) 748-6008, or online at of Liability/Disclaimer of Warranty: While the publisher and author have used their best efforts in preparing this book, they make no representations or warranties with respect to the accuracy or completeness of the contents of this book and specifi cally disclaim any implied warranties of merchantability or fi tness for a particular purpose. No warranty may be created or extended by sales representatives or written sales materials. The advice and strategies contained herein may not be suitable for your situation. You should consult with a professional where appropriate. Neither the publisher nor author shall be liable for any loss of profi t or any other commercial damages, including but not limited to special, incidental, consequential, or other damages.For general information on our other products and services or for technical support, please contact our Customer Care Department within the United States at (800) 762-2974, outside the United States at (317) 572-3993 or fax (317) 572-4002.Wiley also publishes its books in a variety of electronic formats. Some content that appears in print may not be available in electronic formats. For more information about Wiley products, visit our web site at of Congress Cataloging-in-Publication Data:McNair, Harold Monroe, 1933–Basic gas chromatography / Harold M. McNair, James M. Miller. — 2nd ed.p. cm.Includes index.ISBN 978-0-470-43954-8 (cloth)1. Gas chromatography. I. Miller, James M., 1933– II. Title.QD79.C45M425 2009543′.85—dc222009013332Printed in the United States of America10 9 8 7 6 5 4 3 2 1CONTENTSPREFACE TO THE SECOND EDITION ixPREFACE xiACKNOWLEDGMENTS xiii1 INTRODUCTION 1A Brief History / 1Defi nitions / 3Overview: Advantages and Disadvantages / 9Instrumentation / 11References / 132 INSTRUMENT OVERVIEW 14Carrier Gas / 15Flow Control and Measurement / 16Sample Inlets and Sampling Devices / 20Columns / 23Temperature Zones / 24Detectors / 27Data Systems / 27References / 28vvi CONTENTS3 BASIC CONCEPTS AND TERMS 29Defi nitions, Terms, and Symbols / 29The Rate Theory / 40A Redefi nition of H / 50The Achievement of Separation / 51References / 524 STATIONARY PHASES 53Selecting a Column / 53Classifi cation of Stationary Phases for GLC / 54Liquid Stationary Phases (GLC) / 65Solid Stationary Phases (GSC) / 69References / 695 PACKED COLUMNS AND INLETS 71Solid Supports / 71Liquid Stationary Phases / 73Solid Stationary Phases (GSC) / 74Gas Analysis / 76Analysis of Other Inorganics / 80Inlets for Liquid Samples and Solutions / 80Special Columns / 81Upgrading for Capillary Columns / 82References / 836 CAPILLARY COLUMNS AND INLETS 84Types of OT Columns / 84OT Column Tubing / 86Advantages of OT Columns / 89Column Selection / 91Capillary Inlet Systems / 97Miscellaneous Topics / 100References / 1027 DETECTORS 104Classifi cation of Detectors / 105Detector Characteristics / 108Flame Ionization Detector (FID) / 115Thermal Conductivity Detector (TCD) / 119CONTENTS viiElectron Capture Detector (ECD) / 122Other Detectors / 125References / 1278 QUALITATIVE AND QUANTITATIVE ANALYSIS 129Qualitative Analysis / 129Quantitative Analysis / 135References / 1449 PROGRAMMED TEMPERATURE 145Temperature Effects / 145Advantages and Disadvantages of PTGC / 147Requirements of PTGC / 149Theory of PTGC / 151Special Topics / 153References / 15510 GAS CHROMATOGRAPHY–MASS SPECTROMETRY (GC–MS) 156Instrumentation / 157History / 165Limitations of GC–MS Systems / 166Data Analysis / 167References / 16911 MULTIDIMENSIONAL GAS CHROMATOGRAPHY 170Overview / 170Fundamental Principles of Multidimensional Chromatography / 171GC×GC with Heart Cutting / 174Comprehensive GC×GC / 175LC×GC with Heart Cutting / 178Comprehensive LC×GC / 179Summary / 180References / 18112 SAMPLING METHODS 183Overview / 183Liquid–Liquid Extraction (LLE) / 185viii CONTENTSSolid–Liquid Extraction: Soxhlet Extraction and Accelerated Solvent Extraction (ASE) / 188Liquid–Solid Extraction: Solid-Phase Extraction (SPE) / 189Liquid- or Solid-Vapor Extraction: Headspace Extraction / 191Solid-Phase Micro-extraction (SPME) / 193Additional Techniques and Summary / 195References / 19713 SPECIAL TOPICS 198Fast GC / 198Chiral Analysis by GC / 201GC Analysis of Nonvolatile Compounds / 202References / 20514 TROUBLESHOOTING GC SYSTEMS 207APPENDIX I SYMBOLS AND ACRONYMS 215APPENDIX II GUIDELINES FOR SELECTING CAPILLARY COLUMNS 218APPENDIX III GC: HOW TO AVOID PROBLEMS 220APPENDIX IV CALCULATION OF SPLIT RATIO FOR SPLIT INJECTION ON OT COLUMNS 222APPENDIX V OPERATING CONDITIONS FOR CAPILLARY COLUMNS 224APPENDIX VI OV LIQUID PHASES PHYSICAL PROPERTY DATA 225APPENDIX VII SOME COMPRESSIBILITY CORRECTION FACTORS (J) 227APPENDIX VIII SOME INTERNET WEBSITES FOR GAS CHROMATOGRAPHERS 228APPENDIX IX OTHER BOOKS ON GAS CHROMATOGRAPHY 230INDEX OF APPLICATIONS 231INDEX 233 PREFACE TO THE SECOND EDITION When the fi rst edition of this book was published in 1998, gas chromatography (GC) was already a mature, popular separation method. Grob ’ s encyclopedic Modern Practice of Gas Chromatography was already in its third (1995) edition. But the fi eld has not remained static, and there is much new informa-tion that necessitates an update, a second edition of our book. In the meantime, Grob ’ s book (now coedited with Barry) is in its fourth edition (2004) and comprises over 1000 pages. Miller ’ s book on Chromatography is also in its second edition (2005). Our objectives have remained the same, as has our intention to keep the book small, basic, and fundamental. Several topics that were contained in the Special Topics chapter of the fi rst edition have been expanded in the second. They are Gas Chromatography – Mass Spectrometry (GC – MS) and Special Sampling Methods, now entitled simply Sampling Methods. In addition, a new chapter on Multidimensional GC has been added. Also, two new topics have been added to the Special Topics chapter, namely, Fast GC and the GC Analysis of Nonvolatile Compounds. The latter includes the original section on Derivatization, supplemented with Inverse GC and Pyrolysis GC. The entire book has been updated with new references, resources, and websites. The textual material for the two new chapters ( 11 and 12 ) has been written by Nicholas Snow and Gregory Slack, both former students of McNair. They are established chromatography authors in their own right, and we welcome them and thank them for their contributions. Further information about them can be found on the Acknowledgments page. ixx PREFACE TO THE SECOND EDITIONWe would be remiss if we did not repeat our expression of gratitude that is included in our original Preface. Many persons have helped us and taught us, including our mentors, students, and many other colleagues. We are also indebted to our wives and families for their support and encouragement. Thank you all. H arold M. M c N air J ames M. M iller PREFACE A series of books on the Techniques in Analytical Chemistry would be incom-plete without a volume on gas chromatography (GC), undoubtedly the most widely used analytical technique. Over 40 years in development, GC has become a mature method of analysis and one that is not likely to fade in popularity. In the early years of development of GC, many books were written to inform analysts of the latest developments. Few of them have been kept up - to - date and few new ones have appeared, so that a satisfactory single introductory text does not exist. This book attempts to meet that need. It is based in part on the earlier work by the same title, Basic Gas Chromatography , co - authored by McNair and Bonelli and published by Varian Instruments. Some material is also drawn from the earlier Wiley book by Miller, Chromatography: Concepts and Contrasts. We have attempted to write a brief, basic, introduction to GC following the objectives for titles in this series. It should appeal to readers with varying levels of education and emphasizes a practical, applied approach to the subject. Some background in chemistry is required: mainly general organic chemistry and some physical chemistry. For use in formal class work, the book should be suitable for undergraduate analytical chemistry courses and for intensive short courses of the type offered by the American Chemical Society and others. Analysts entering the fi eld should fi nd it indispensable, and industrial chemists working in GC should fi nd it a useful reference and guide. Because the IUPAC has recently published its nomenclature recommenda-tions for chromatography, we have tried to use them consistently to promote a unifi ed set of defi nitions and symbols. Also, we have endeavored to write in xixii PREFACEsuch a way that the book would have the characteristics of a single author, a style especially important for beginners in the fi eld. Otherwise, the content and coverage are appropriately conventional. While open tubular (OT) columns are the most popular type, both open tubular and packed columns are treated throughout, and their advantages, disadvantages, and applications are contrasted. In addition, special chapters are devoted to each type of column. Chapter 2 introduces the basic instrumen-tation and Chapter 7 elaborates on detectors. Other chapters cover stationary phases (Chapter 4 ), qualitative and quantitative analysis (Chapter 8 ), programmed temperature (Chapter 9 ), and troubleshooting (Chapter 11 ). Chapter 10 briefl y covers the important special topics of GC – MS, derivatiza-tion, chiral analysis, headspace sampling, and solid - phase micro - extraction (SPME) for GC analysis. We would like to express our appreciation to our former professors and many colleagues who have in one way or another aided and encouraged us and to those students who, over the years, have provided critical comments that have challenged us to improve both our knowledge and communication skills. H arold M. M c N air J ames M. M iller ACKNOWLEDGMENTS The authors wish to acknowledge that two chapters, 11 (Multidisciplinary Gas Chromatography) and 12 (Sampling Methods), have been provided for our book by the following colleagues: 1. Professor Nicholas H. Snow, Department of Chemistry and Biochemistry, Center for Academic Industry Partnership, Seton Hall University, South Orange, NJ, 07079 ( [email protected] ) and 2. Dr. Gregory C. Slack, Director of Research and Technology Transfer, Clarkson University, Potsdam, NY, 13699 ( [email protected] ). Both of these authors wish to acknowledge the support of their respective educational institutions. Snow also gratefully acknowledges Sanofi - Aventis, which established Seton Hall ’ s Center for Academic Industry Partnership and provided fi nancial support. Also, LECO Corporation is acknowledged for providing instrumentation and technical assistance for his GC × GC work. We also wish to express our appreciation to Mike Shively and the Restek Corporation of Bellefonte, PA for providing the multidimensional gas chro-matogram used on the front cover. H arold M. M c N air J ames M. M iller xiiiINDEX OF APPLICATIONSAcetone, 76, 85Air contaminants, 133Alcohols, 76, 89, 131Aldrin, 55, 124Amines, 82, 100Amino acids, 82Aqueous solutions, 76Arochlor, 90Aromatics, 68, 85, 133Benzene, 64, 68, 85, 93, 133, 167, 199BETX, 68BTX, 1992-Butanone, 56, 76, 85Cadaverine, 100Carbon dioxide, 74, 78Carbon monoxide, 74, 78Chlorinated hydrocarbons, 85, 90Cola drink, 178Cyclohexane, 64Essential oils, 2, 10, 149Ethane, 74, 78, 93231Basic Gas Chromatography, Second Edition, by Harold M. McNair and James M. MillerCopyright © 2009 John Wiley & Sons, Inc.Ethion, 11Ethylbenzene, 68, 85Freons, 82Gases, fi xed, 74, 75, 87Gas, natural, 93Gases, rare, 75, 78, 87Gas, shale oil, 78Gasoline, 132, 178Heptachlor, 124n-Heptane, 56, 148Homologous series, 148Hydrocarbons, 89, 132, 133, 148, 167Hydrocarbons, light, 78, 82, 93Hydrogen, 74, 77, 78Insecticides, 11, 55, 124Kelthane, 55Lindane, 124232 INDEX OF APPLICATIONSMalathion, 11, 55MEK, see 2-ButanoneMethane, 74, 75, 78, 93Nitrogen, 75, 78, 87Noble gases, 75, 78, 87Oil shale gas, 78Orange oil, 10, 149Oxygen, 75, 78, 87Oxygenates in gasoline, 178Parathion, methyl, 11PCBs, 90Peppermint oil, 2Pesticides, 11, 55, 82Phthalates, 82Polyethylene, 154Polymers, 154, 205n-Propanol, 56Putrescine, 100Simulated distillation, 82Solvents, 76, 82, 85Sulfur oxides, 82Test mixture, 89, 171THF, 56, 76, 85Toluene, 68, 76, 85, 199Triacylglycerols, 181Volatile organics, 85Water, 76Xylenes, 68, 76, 82, 85, 133, 199INDEXAbsorption, 6Accelerated solvent extraction (ASE), 188Accuracy, defi nition of, 135–136Achievement of separation, 51–52Activity coeffi cient, 65Adjusted retention volume, 32See also Retention volumeAdsorbents for GSC, 69, 74–75Adsorption, 6Advantagesof GC, 9of OT columns, 89–90Analyte, see SoluteArea normalization, 138Asymmetry of peaks, 35–36Attenuator, 120Autosampler, 23Average linear carrier gas velocity, 18Azeotropes, 11Backfl ushing, 77Baseline, 108Base peak, 161233Basic Gas Chromatography, Second Edition, by Harold M. McNair and James M. MillerCopyright © 2009 John Wiley & Sons, Inc.Bleeding, see Stationary phaseBonded phases, 94Calibration, 142–143Capacity factor, see Retention factorCapacity ratio, see Retention factorCapillary columns, see Columns, open tubular (OT)Capillary direct interface, 158–159Carbowax, 55, 66, 69, 73See also Polyethylene glycolsCarrier gas, 15–16choice of, 15, 48–49, 121, 201, 219defi nition of, 3detector requirements, 15effect on effi ciency in OT columns, 48–49, 121optimum velocity, 46–47purity of, 16Chemical ionization (CI), 160Chiral separations, 201–202Chromatogram, 5, 7–8Chromatograph, 11–12, 14–15234 INDEXChromatographyadvantages of, 9books, 230classifi cation of, 4defi nition of, 3disadvantages of, 11gas-liquid, GLC, 4, 54–63, 81–82gas-solid, GSC,



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