Basic Gas Chromatography

Basic Gas Chromatography, Third Edition provides a brief 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. : This book provides a quick need-to-know introduction to gas chromatography; still the most widely used instrumental analysis technique, and is intended to assist new users in gaining understanding quickly and as a quick reference for experienced users.

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 xi

Preface to the Second Edition xiii

Preface to the First Edition xv

Acknowledgments xvii

1 Introduction 1

A Brief History 1

Definitions 3

Overview: Advantages and Disadvantages 9

Instrumentation and Columns 12

References 14

2 Basic Concepts and Terms 15

Definitions, Terms, and Symbols 15

The Rate Theory 25

The Achievement of Separation 34

References 35

3 Instrument Overview 37

Carrier Gas 38

Flow Control and Measurement 39

Sample Inlets and Sampling Devices 42

Capillary Columns 46

Temperature Zones 47

Detectors 49

Data Systems 50

Reference 50

4 Capillary Columns 51

Types of Capillary Columns 51

Capillary Column Tubing 54

Advantages of Capillary Columns 55

Column Selection 57

Column Quality Testing: The Grob Test Mix 65

Special Troubleshooting Considerations for Capillary Columns 66

Guidelines for Selecting Capillary Columns 67

References 68

5 Stationary Phases 69

Selecting a Column 69

Common and Important Stationary Phases 81

Other Common Stationary Phases 83

References 86

6 Temperature Programming 87

Advantages and Disadvantages of TPGC 89

Requirements for TPGC 90

Example Temperature Programmed Chromatograms 91

Special Topics 96

References 98

7 Inlets 99

Inlet Fundamentals 99

Split Inlet 101

Splitless Inlet 104

On‐Column Inlet 106

Programmed Temperature Vaporizer (PTV) 107

Related Topics 108

References 111

8 Classical Detectors: FID, TCD, and ECD 113

Classification of Detectors 115

Common Detector Characteristics 117

Flame Ionization Detector (FID) 124

Thermal Conductivity Detector (TCD) 128

Electron Capture Detector (ECD) 131

Other Detectors 134

References 136

9 Qualitative and Quantitative Analysis 139

Qualitative Analysis 139

Quantitative Analysis 145

Statistics of Quantitative Calculations 145

Quantitative Analysis Methods 148

Summary 154

References 154

10 GC‐MS and Spectrometric Detectors 157

Gas Chromatography–Mass Spectrometry (GC‐MS) 158

Gas Chromatography–Mass Spectrometry–Mass Spectrometry (GC‐MS‐MS) 171

Gas Chromatography–Fourier Transform Infrared Spectrometry (GC‐FITR) 172

Gas Chromatography–Vacuum Ultraviolet (GC‐VUV) Spectrometry 172

References 174

11 Sampling Methods 177

Overview 177

Liquid–Liquid Extraction (LLE) 179

Solid–Liquid Extraction: Soxhlet Extraction and Accelerated Solvent Extraction (ASE) 182

Solid‐Phase Extraction 183

Liquid–Vapor or Solid–Vapor Extraction: Headspace Extraction 186

Solid-phase microextraction (SPME) 188

QuEChERS (Quick, Easy Cheap, Effective, Rugged, Safe) 192

Additional Techniques and Summary 193

References 194

12 Multidimensional Gas Chromatography 197

Overview 197

Fundamental Principles of Multidimensional Chromatography 198

Heart Cutting 202

Comprehensive Two‐Dimensional GC (GC×GC) 203

LC‐GC with Heart Cutting 206

Comprehensive LC×GC 206

References 208

13 Packed Column GC 211

Columns 211

Solid Supports and Stationary Phases 213

Liquid Stationary Phases 214

Solid Stationary Phases 215

Gas Analysis 218

Analysis of Other Inorganics 221

Inlets and Liquid Sampling for Packed Columns 221

Special Columns and Applications 222

References 224

14 Special Topics 225

Fast GC 225

Chiral Analysis by GC 228

Analysis of Nonvolatile Compounds 229

Pyrolysis 233

Inverse GC 233

Additional Theory 234

Activity Coefficients 236

References 238

15 Troubleshooting GC Systems 241

Preventing Problems 241

Troubleshooting Problems 243

Appendix A Acronyms, Symbols and Greek Symbols 251

Appendix B Some Internet Sites for Gas Chromatography 255

Appendix C Other Books On Gas Chromatography 257

Index 259

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