Basic Gas Chromatography

HAROLD M. MCNAIR, PHD, is Professor Emeritus of Chemistry at Virginia Tech, and is known internationally as a leading researcher and educator in the field of gas chromatography. JAMES M. MILLER, PHD, is Professor Emeritus of Chemistry at Drew University, where he taught for 36 years. NICHOLAS H. SNOW, PHD, is Professor of Chemistry and Biochemistry at Seton Hall University. He is widely published in gas chromatography and has been teaching GC to new students for over 30 years.

• Preface to the Third Edition xiPreface to the Second Edition xiiiPreface to the First Edition xvAcknowledgments xvii1 Introduction 1A Brief History 1Definitions 3Overview: Advantages and Disadvantages 9Instrumentation and Columns 12References 142 Basic Concepts and Terms 15Definitions, Terms, and Symbols 15The Rate Theory 25The Achievement of Separation 34References 353 Instrument Overview 37Carrier Gas 38Flow Control and Measurement 39Sample Inlets and Sampling Devices 42Capillary Columns 46Temperature Zones 47Detectors 49Data Systems 50Reference 504 Capillary Columns 51Types of Capillary Columns 51Capillary Column Tubing 54Advantages of Capillary Columns 55Column Selection 57Column Quality Testing: The Grob Test Mix 65Special Troubleshooting Considerations for Capillary Columns 66Guidelines for Selecting Capillary Columns 67References 685 Stationary Phases 69Selecting a Column 69Common and Important Stationary Phases 81Other Common Stationary Phases 83References 866 Temperature Programming 87Advantages and Disadvantages of TPGC 89Requirements for TPGC 90Example Temperature Programmed Chromatograms 91Special Topics 96References 987 Inlets 99Inlet Fundamentals 99Split Inlet 101Splitless Inlet 104On‐Column Inlet 106Programmed Temperature Vaporizer (PTV) 107Related Topics 108References 1118 Classical Detectors: FID, TCD, and ECD 113Classification of Detectors 115Common Detector Characteristics 117Flame Ionization Detector (FID) 124Thermal Conductivity Detector (TCD) 128Electron Capture Detector (ECD) 131Other Detectors 134References 1369 Qualitative and Quantitative Analysis 139Qualitative Analysis 139Quantitative Analysis 145Statistics of Quantitative Calculations 145Quantitative Analysis Methods 148Summary 154References 15410 GC‐MS and Spectrometric Detectors 157Gas Chromatography–Mass Spectrometry (GC‐MS) 158Gas Chromatography–Mass Spectrometry–Mass Spectrometry (GC‐MS‐MS) 171Gas Chromatography–Fourier Transform Infrared Spectrometry (GC‐FITR) 172Gas Chromatography–Vacuum Ultraviolet (GC‐VUV) Spectrometry 172References 17411 Sampling Methods 177Overview 177Liquid–Liquid Extraction (LLE) 179Solid–Liquid Extraction: Soxhlet Extraction and Accelerated Solvent Extraction (ASE) 182Solid‐Phase Extraction 183Liquid–Vapor or Solid–Vapor Extraction: Headspace Extraction 186Solid-phase microextraction (SPME) 188QuEChERS (Quick, Easy Cheap, Effective, Rugged, Safe) 192Additional Techniques and Summary 193References 19412 Multidimensional Gas Chromatography 197Overview 197Fundamental Principles of Multidimensional Chromatography 198Heart Cutting 202Comprehensive Two‐Dimensional GC (GC×GC) 203LC‐GC with Heart Cutting 206Comprehensive LC×GC 206References 20813 Packed Column GC 211Columns 211Solid Supports and Stationary Phases 213Liquid Stationary Phases 214Solid Stationary Phases 215Gas Analysis 218Analysis of Other Inorganics 221Inlets and Liquid Sampling for Packed Columns 221Special Columns and Applications 222References 22414 Special Topics 225Fast GC 225Chiral Analysis by GC 228Analysis of Nonvolatile Compounds 229Pyrolysis 233Inverse GC 233Additional Theory 234Activity Coefficients 236References 23815 Troubleshooting GC Systems 241Preventing Problems 241Troubleshooting Problems 243Appendix A Acronyms, Symbols and Greek Symbols 251Appendix B Some Internet Sites for Gas Chromatography 255Appendix C Other Books On Gas Chromatography 257Index 259