Chromatography

Mark F. Vitha is currently a Professor at Drake University.  He received his Ph.D. from the University of Minnesota.  He is the series editor for The Chemical Analysis Series (Wiley) and is a co-editor of the book High Throughput Analysis for Food Safety (Wiley, 2014). He has been named as a Levitt Teacher of the Year, a Windsor Professor of Science, and a Ronald D. Troyer Research Fellow at Drake.

• Preface ix1. Fundamentals of Chromatography 11.1 Theory 11.1.1 Component Separation 31.1.2 Retention Factor 61.1.3 Separation 111.1.4 Resolution and Theoretical Plates 131.2 Band Broadening 201.2.1 Diffusion 211.2.2 Linear Velocity 231.2.3 Broadening in Open Tubes with No Stationary Phase and No Retention 241.2.4 Broadening in Open Tubes with a Stationary Phase 281.2.5 Broadening in a Packed Column 341.2.6 Putting It All Together 431.2.7 Practical Consequences of Broadening Theory 451.3 General Resolution Equation 471.4 Peak Symmetry 511.5 Key Operating Variables 511.6 Instrumentation 531.7 Practice of The Technique 531.7.1 Quantitation 531.7.2 Internal Standards and the Method of Standard Additions 551.8 Emerging Trends and Applications 551.9 Summary 55Problems 56References 59Further Reading 592. Gas Chromatography 612.1 Theory of Gas Chromatographic Separations 612.1.1 GC Columns and Partitioning 642.2 Key Operating Variables that Control Retention 642.2.1 Adjusting Retention Time: Temperature 652.2.2 Adjusting Retention Time: Temperature Programming 672.2.3 Adjusting Retention Time: Mobile Phase Flow Rate 692.2.4 Adjusting Retention Time: The Column and the Stationary Phase 722.2.5 Adjusting Retention Time: Summary 782.2.6 Measures of Retention 782.3 Gas Chromatography Instrumentation 822.3.1 Carrier Gas Supply 832.3.2 The Injection Port and the Solute Injection Process 832.3.3 Oven/Column Compartment 972.3.4 Detectors 982.4 A More Detailed Look at Stationary Phase Chemistry: Kovats Indices and Mcreynolds Constants 1112.4.1 Kovats Retention Indices 1112.4.2 Stationary Phase Selection 1202.5 Gas Chromatography in Practice 1242.5.1 Syringe Washing 1242.5.2 Controls and Blanks/Ghost Peaks 1242.5.3 Autosamplers 1252.5.4 GC Septa 1252.5.5 Qualitative Analysis 1262.5.6 Quantitative Analysis 1262.5.7 Derivatization 1282.5.8 High-Speed GC 1282.5.9 Tandem GC 1292.5.10 Microfabricated GC 1292.6 A “Real-World” Application of Gas Chromatography 1312.6.1 GC and International Oil Trading 1312.7 Summary 136Problems 137References 143Further Reading 1443. Liquid Chromatography 1453.1 Examples of Liquid Chromatography Analyses 1453.2 Scope of Liquid Chromatography 1473.3 History of LC 1483.3.1 Modern Packing Materials 1493.4 Modes of Liquid Chromatography 1523.4.1 Normal Phase Liquid Chromatography (NPLC) 1523.4.2 Reversed-Phase Liquid Chromatography (RPLC) 1543.4.3 Ion-Exchange Chromatography (IEX) 1653.4.4 Hydrophilic Interaction Chromatography (HILIC) 1733.4.5 Size Exclusion Chromatography (SEC) 1753.4.6 Affinity Chromatography 1783.5 HPLC Instrumentation 1803.5.1 The Proportioning Valve 1813.5.2 Mixing Chamber 1813.5.3 Pumps 1813.5.4 Injection 1833.5.5 The Column and Particles 1853.5.6 Guard Columns 1873.5.7 Detectors 1883.6 Specific Uses of and Advances in Liquid Chromatography 2013.6.1 Chiral Separations 2023.6.2 Preparative-Scale Chromatography 2073.6.3 Ultra-High Performance Liquid Chromatography (UHPLC) for High-Speed Separations 2123.6.4 Tandem-Column Liquid Chromatography 2163.6.5 Two-Dimensional Liquid Chromatography (2D-LC) 2183.7 Application of LC – Analysis of Pharmaceutical Compounds in Groundwater 2243.7.1 Sampling 2253.7.2 Analysis Method for 21 Antibiotics – Sample Pretreatment 2253.7.3 Use of Internal Standards and Other Quality Assurance Issues 2273.7.4 LC Analyses 2283.7.5 Mass Spectrometric Selected Ion Monitoring Detection 2283.7.6 Results 2293.8 Summary 230Problems 230References 232Solutions 237Index 263

"Mark Vitha has written a book that will appeal to students, teachers, and perhaps professional analysts who need a refresher in the fundamentals of chromatography. The book consists of three sections of about equal length dealing with separation theory, gas chromatography (GC), and liquid chromatography (LC). The section on theory is especially strong. Vitha is an experienced educator who understands the undergraduate audience and explains concepts clearly. He uses analogies to help students with abstract ideas, something I have seen little of in the sciences. He also freely uses ideas and terms from thermodynamics that can be grasped by students who have studied physical chemistry"."Graduate students might want to use this book, with additional depth provided by their instructors and current and classic papers (many are referenced). Graduate students need more depth in areas such as solvent theory and the selection of solvents, for example, than is given in this book"."I taught instrumental methods to undergraduate students for many years using encyclopedic full-course texts. I wish there had been as fine a pedagogical tool as this more-focused new textbook at that time". (LC/GC- December 16)