Introduction to modern liquid chromatography,2d ed.

1 Introduction, 1 1.1 Liquid versus Gas Chromatography, 2 1.2 Modern versus Traditional LC Procedures, 3 1.3 How Did Modem LC Arise?, 8 1.4 The Literature of LC, 9 1.5 About the Book, 12 References, 13 Bibliography, 13 2 Basic Concepts and Control of Separation, 15 2.1 The Chromatographic Process, 16 2.2 Retention in LC, 22 2.3 Band Broadening, 27 2.4 Resolution and Separation Time, 34 2.5 The Control of Separation, 37 References, 81 Bibliography, 82 3 Equipment, 83 3.1 Introduction, 84 3.2 Extracolumn Effects, 86 3.3 Mobile-Phase Reservoirs, 88 3.4 Solvent Pumping (Metering) Systems, 90 3.5 Equipment for Gradient Elution, 103 XIII xiv Contents 3.6 Sample Injectors, 110 3.7 Miscellaneous Hardware, 117 3.8 Integrated and Specialized Instruments, 119 3.9 Laboratory Safety, 123 References, 123 Bibliography, 124 4 Detectors, 125 4.1 Introduction, 126 4.2 Detector Characteristics, 127 4.3 UV-Visible Photometers and Spectrophotometers, 130 4.4 Differential Refractometers, 140 4.5 Fluorometers, 145 4.6 Infrared Photometers, 147 4.7 Electrochemical (Amperometric) Detectors, 153 4.8 Radioactivity Detectors, 158 4.9 Conductivity Detectors, 161 4.10 Summary of the Characteristics of Most-Used Detectors, 161 4.11 Other Detectors, 165 References, 165 Bibliography, 166 5 The Column, 168 5.1 Introduction, 169 5.2 Characteristics and Use of Different Column Packings, 173 5.3 Available Column Packings, 183 5.4 Column Packing Methods, 202 5.5 Column Evaluation and Specifications, 218 5.6 Column Techniques, 225 5.7 Reduced Parameters and Limiting Column Performance, 234 References, 243 Bibliography, 245 6 Solvents, 246 6.1 Introduction, 247 6.2 Physical Properties, 251 Contents xv 6.3 Intermolecular Interactions Between Sample and Mobile-Phase Molecules, 255 6.4 Solvent Strength and "Polarity," 257 6.5 Solvent Selectivity, 260 6.6 Purification of LC Solvents, 265 References, 267 Bibliography, 268 7 Bonded-Phase Chromatography, 269 7.1 Introduction, 270 7.2 Preparation and Properties of Bonded-Phase Packings, 272 7.3 Mobile-Phase Effects, 281 7.4 Other Separation Variables, 289 7.5 Special Problems, 294 7.6 Applications, 301 7.7 The Design of a BPC Separation, 316 References, 319 Bibliography, 321 8 Liquid-Liquid Chromatography, 323 8.1 Introduction, 323 8.2 Essential Features of LLC, 325 8.3 Column Packings, 327 8.4 The Partitioning Phases, 332 8.5 Other Separation Variables, 336 8.6 Special Problems, 336 8.7 Applications, 338 8.8 The Design of an LLC Separation, 342 References, 347 Bibliography, 348 9 Liquid-Solid Chromatography, 349 9.1 Introduction, 351 9.2 Column Packings, 361 9.3 Mobile Phases, 365 9.4 Other Separation Variables, 389 xvi Contents 9.5 Special Problems, 391 9.6 Applications, 398 9.7 The Design of an LSC Separation, 405 References, 407 Bibliography, 409 10 Ion-Exchange Chromatography, 410 10.1 Introduction, 410 10.2 Column Packings, 414 10.3 Mobile Phases, 419 10.4 Other Separation Variables, 426 10.5 Special Problems, 427 10.6 Applications, 429 10.7 The Design of an Ion-Exchange Separation, 445 References, 450 Bibliography, 452 11 Ion-Pair Chromatography, 453 11.1 Introduction, 454 11.2 Column Packings, 457 11.3 Partitioning Phases, 458 11.4 Other Separation Variables, 470 11.5 Special Problems, 471 11.6 Applications, 473 11.7 The Design of an Ion-Pair Separation, 477 References, 481 Bibliography, 482 12 Size-Exclusion Chromatography, 483 12.1 Introduction, 484 12.2 Column Packings, 487 12.3 Mobile Phases, 500 12.4 Other Separation Variables, 503 12.5 Molecular-Weight Calibration, 509 12.6 Recycle Chromatography, 519 12.7 Problems, 522 Contents xvii 12.8 Applications, 525 12.9 The Design of an SEC Separation, 534 References, 538 Bibliography, 540 13 Quantitative and Trace Analysis, 541 13.1 Introduction, 542 13.2 Peak-Size Measurement, 545 13.3 Calibration Methods, 549 13.4 Selection of Calibration Method, 556 13.5 Trace Analysis, 560 References, 573 14 Qualitative Analysis, 575 14.1 Retention Data for Sample Characterization, 576 14.2 Qualitative Analysis of Sample Bands from Analytical-Scale LC Separations, 589 14.3 On-Line Spectroscopic Analysis of LC Peaks, 603 References, 612 Bibliography, 614 15 Preparative Liquid Chromatography, 615 15.1 Introduction, 615 15.2 Separation Strategy, 617 15.3 Experimental Conditions, 623 15.4 Operating Variables, 641 15.5 Applications, 647 15.6 A Preparative Separation Example, 654 References, 661 16 Gradient Elution and Related Procedures, 662 16.1 Gradient Elution, 663 16.2 Column Switching and Stationary-Phase Programming, 694 16.3 Flow Programming, 712 16.4 Temperature Programming, 715 xviii Contents 16.5 Practical Comparison of Various Programming and Column-Switching Procedures, 715 References, 717 Bibliography, 718 17 Sample Pretreatment and Reaction Detectors, 720 17.1 Introduction, 720 17.2 Sample Cleanup, 722 17.3 Sample Derivatization, 731 17.4 Reaction Detectors, 740 17.5 Automation of Sample Pretreatment, 746 References, 748 Bibliography, 750 18 Selecting and Developing One of the LC Methods, 752 18.1 Introduction, 753 18.2 Developing a Particular Separation, 762 18.3 Special Applications, 776 References, 779 19 Troubleshooting the Separation, 781 19.1 Troubleshooting the Equipment, 782 19.2 Separation Artifacts, 791 19.3 Troubleshooting Analytical Errors, 813 References, 823 Appendix I Suppliers of LC Equipment, Accessories, and Columns, 824 Appendix II Miscellaneous Tables Used by Workers in LC, 833 II. 1 The Gaussian or Error Function, 833 II.2 Reduced Plate-Height Data for "Good" Columns, 836 II.3 Viscosity of Solvent Mixtures, 836 II.4 Particle Size Expressed as Mesh Size, 838 References, 839 Contents xix List of Symbols, 840 List of Abbreviations, 844