Chromatography

Basic Principles, Sample Preparations and Related Methods

Häftad, Engelska, 2013

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Beskrivning

Finally a book on chromatography which is easy to grasp for undergraduates and technicians; covers the area in sufficient depth while still being concise. The book includes all recent technology advances and has core textbook features further improving the learning experience.This book is the perfect introduction into a methodology which is the underlying principle of the vast majority of separation methods worldwide. Everyone working in a lab environment must be familiar with the basis of these technologies and Tyge Greibrokk, Elsa Lundanes and Leon Reubsaet succeed in delivering a text which is easy to read for undergraduates and laboratory technicians, and covers the area in sufficient depth while still being concise. The book includes all recent technology advances and has core textbook features further improving the learning experience.Importantly, the text does not only cover all major modern chromatography technology (thin layer, gas, high pressure liquid, and supercritical fluid chromatography) but also related methods, in particular electrophoretic technologies.

Produktinformation

Utgivningsdatum:2013-10-09
Mått:172 x 245 x 13 mm
Vikt:490 g
Format:Häftad
Språk:Engelska
Antal sidor:224
Förlag:Wiley-VCH Verlag GmbH
ISBN:9783527336203

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Analytisk kemi inom Naturvetenskap och teknik

Mer om författaren

Tyge Greibrokk has been professor of analytical chemistry since 1975 and also head of the Department of Chemistry at the University of Oslo. He retired as professor emeritus in 2012. Professor Greibrokk has (co)-authored more than 250 scientific papers and supervised more than 120 master students and 30 PhD students. He is elected member of the Norwegian Academy of Science and Letters, honorary member of the Norwegian Chemical Society, the recipient of several prizes and honors and has served as editor of Journal of Separation Science for many years. Léon Reubsaet took his academic degrees at the Free University Amsterdam and the Utrecht University. He has been professor in drug analysis since 2005 at the School of Pharmacy at the University of Oslo. He has (co)-authored approx. 70 scientific papers and supervised 40 master students and 8 PhD students. Since 2012 Professor Reubsaet is member of the editorial advisory board of Chromatographia. Elsa Lundanes obtained her academic degrees at the University of Oslo. She has been a professor of analytical chemistry since 1999. Professor Lundanes has (co)-authored more than 150 scientific papers, and supervised more than 100 master students and about 20 PhD students. She is elected member of the Norwegian Academy of Science and Letters.

Innehållsförteckning

Preface xiii1 General Concepts 11.1 Introduction 11.2 Migration and Retention 21.2.1 General 21.2.2 Mobile and Stationary Phases 31.2.3 Chromatograms 31.2.4 Retention Factor 31.3 Band Broadening 51.3.1 Eddy Diffusion 61.3.2 Longitudinal Diffusion 61.3.3 Resistance to Mass Transfer 71.3.4 Combined Band Broadening in a Column 81.3.5 Band Broadening outside the Column 91.4 Measuring Column Efficiency 91.4.1 Plate Numbers 91.4.2 Coupling Columns 101.4.3 Plate Height 101.4.3.1 Reduced Plate Height 111.4.4 Effective Plate Number 111.4.5 Asymmetry 111.5 Resolution 111.5.1 Increasing the Resolution 131.6 Peak Capacity 131.7 Two-Dimensional Systems 131.8 Increased Performance 14References 152 Gas Chromatography 172.1 Introduction 172.2 Mobile Phase/Carrier Gas 172.3 Injection Systems 192.3.1 Packed Column Injector (Evaporation Injector) 202.3.2 Injection Systems for Capillary Columns 212.3.2.1 Split Injection 212.3.2.2 Splitless Injection 222.3.2.3 On-Column Injection 222.3.2.4 Large-Volume Injectors 232.3.2.5 Headspace Techniques 232.4 Columns 242.4.1 Packed Columns 252.4.2 Open Tubular Columns 252.5 Detectors 262.5.1 Introduction 262.5.2 Thermal Conductivity Detector 282.5.3 Flame Ionization Detector 282.5.4 Nitrogen–Phosphorus Detector 302.5.5 Electron Capture Detector 312.5.6 Mass Spectrometry 322.5.6.1 Positive Ionization 332.5.6.2 Negative Ionization 332.5.6.3 Gas Chromatography–Mass Spectrometry (GC–MS) Interfacing 332.5.7 Other Detectors 352.5.7.1 The Flame Photometric Detector 352.5.7.2 The Chemiluminescent Detector 352.5.7.3 The Electrolytic Conductivity Detector 352.5.7.4 The Photoionization Detector 352.5.7.5 The Atomic Emission Detector 362.5.7.6 Fourier Transform Infrared Detector 362.6 Stationary Phases 362.6.1 GSC – Adsorption Chromatography 362.6.2 GLC – Partition Chromatography 372.6.2.1 Matrix 372.6.2.2 Choosing the Stationary Phase 372.6.2.3 Types of Stationary Phases in GLC 382.6.2.4 Stationary Phase (Film) Thickness 402.6.2.5 Temperature 412.7 Two-Dimensional Separations 422.8 Qualitative and Quantitative Analyses 432.9 Derivatization 44References 463 High-Performance Liquid Chromatography (HPLC) 473.1 Introduction 473.2 Solvents and Solvent Delivery 473.2.1 Maintenance 493.2.2 Automation 503.3 Injection 503.3.1 Techniques 503.3.1.1 Constant Volume Injection 503.3.1.2 Variable Volume Injection 513.3.1.3 Volumes and Precision 513.3.2 Dilution and Refocusing 513.3.2.1 Injection Volume Related to Solvent Elution Strength 513.3.2.2 Timed Injection 523.3.2.3 Carryover 523.3.2.4 Combination with Solid-Phase Extractors 523.3.3 Calculation of Maximum Injection Volumes 533.3.4 Calculating the Dilution of the Analyte in the Column 543.4 Columns 543.4.1 Packed Columns 543.4.1.1 Column Dimensions and Materials 543.4.1.2 Effect on Detection 553.4.1.3 Solvent Saving 553.4.1.4 Column Efficiency 563.4.1.5 Column Lifetime 573.4.1.6 Peak Shapes 573.4.1.7 Flow and Backpressure 583.4.1.8 Conventional Totally Porous Particles 583.4.1.9 Core–Shell Particles 583.4.1.10 Ultrahigh-Pressure LC (UHPLC or UPLC) 593.4.2 Monolithic Columns 593.4.3 Microchip Columns 603.4.4 Open Tubular Columns 613.4.5 Temperature Control 613.4.6 Preparative LC and Flash Chromatography 633.5 Stationary Phases and Their Properties in HPLC 643.5.1 Normal-Phase Materials for Adsorption Chromatography 643.5.1.1 Separation Principles 643.5.1.2 Silica 653.5.1.3 Alumina, Titania, and Zirconia 653.5.1.4 Silica with Bonded Polar Functional Groups 663.5.1.5 Hydrophilic Interaction Liquid Chromatography (HILIC) 673.5.1.6 Carbon Materials 683.5.2 Reversed-phase Materials 683.5.2.1 Separation Principles 683.5.2.2 Retention 693.5.2.3 The Solvation Parameter Model 703.5.2.4 Silica-based Reversed-phase Materials 713.5.2.5 Hybrid Materials and Hydrosilated Materials 723.5.2.6 Organic Polymer-based Materials 723.5.2.7 Ion Pair Chromatography on Reversed-Phase Columns 723.5.2.8 Hydrophobic Interaction Chromatography 733.5.3 Ion Exchange Materials 733.5.3.1 Elution 743.5.3.2 Retention 743.5.4 Chromatofocusing 743.5.4.1 Ion Chromatography for Inorganic Ions 753.5.5 Size Exclusion Materials 763.5.5.1 Separation Principles 763.5.5.2 Materials 763.5.5.3 Mobile Phases 773.5.6 Materials for Chiral Separations 773.5.6.1 Separation Principle 773.5.6.2 Materials 783.5.7 Affinity Materials 783.5.7.1 Separation Principle 783.5.7.2 Affinity Materials for Chromatography and Microarrays 793.6 Detectors 803.6.1 UV Detection 813.6.1.1 Some Common Chromophores 823.6.1.2 Choosing the Right Wavelength 823.6.1.3 Flow Cells 823.6.1.4 Filter Photometric Detection 833.6.1.5 Spectrophotometric Detection 833.6.1.6 Diode Array Detectors 833.6.2 Mass Spectrometric Detection 853.6.2.1 Electrospray Ionization 863.6.2.2 Atmospheric Pressure Chemical Ionization 883.6.2.3 Atmospheric Pressure Photoionization 893.6.2.4 Inductively Coupled Plasma Ionization 903.6.2.5 Mass Analysis 913.6.2.6 The Quadrupole Mass Analyzers 913.6.2.7 The Ion Trap Analyzers 923.6.2.8 The Time-of-Flight Analyzers 923.6.2.9 The FTMS Analyzers 933.6.2.10 Fragmentation in Mass Spectrometry 943.6.3 Fluorescence Detection 953.6.3.1 Filter Fluorimeters 973.6.3.2 Spectrofluorimeters 973.6.3.3 Chemiluminescence Detection 973.6.4 Electrochemical Detection 983.6.4.1 Amperometric Detection 983.6.4.2 Coulometric Detector 993.6.5 Light Scattering Detection 1003.6.6 Refractive Index Detection 1003.6.7 Other Detectors 1023.6.7.1 The Conductivity Detector 1023.6.7.2 The Corona Discharge Detector 1023.6.7.3 Radioactivity Detectors 1023.6.7.4 Ion Mobility Spectrometry 1033.6.7.5 Chemiluminescent Nitrogen Detector 1033.6.7.6 Chirality Detection 1033.7 Increased Performance 1033.7.1 Speed 1033.7.2 Efficiency 1033.7.3 Resolution 1033.7.4 Detection 1033.7.5 Column Lifetime 104References 1044 Thin Layer Chromatography (TLC) 1054.1 Introduction 1054.2 Sample Application 1054.3 Stationary Phases 1064.3.1 TLC versus HPTLC 1064.3.2 Adsorbents 1074.3.3 Chemically Bonded Phases 1074.4 Mobile Phases 1074.5 Elution and Development 1084.5.1 Vertical Linear Development 1084.5.2 Horizontal Development 1094.5.3 Two-Dimensional Development 1104.5.4 Gradient Development 1114.5.5 Overpressured Layer Chromatography (OPLC) 1114.6 Rf Value 1114.7 Detection 1124.7.1 Instrumental Detection 1134.7.2 TLC–MS 1145 Supercritical Fluid Chromatography 1155.1 Introduction 1155.2 Mobile Phases 1185.2.1 CO2 as Mobile Phase 1185.2.2 Mobile Phase Delivery 1195.3 Gradient Elution 1205.4 Injection 1215.5 Columns 1225.6 Restrictors 1245.7 Detectors 1245.8 Current Performance 125References 1266 Electrophoresis and Potential-Driven Chromatography 1276.1 Introduction 1276.2 Theory 1276.2.1 Secondary Effects 1286.2.2 Electroosmosis 1296.3 Gel Electrophoresis Techniques 1306.3.1 Gels 1306.3.1.1 Polyacrylamide Gels 1306.3.1.2 Agarose Gels 1316.3.2 Instrumentation 1316.3.2.1 Sample Application 1316.3.2.2 Separation 1326.3.2.3 Detection 1326.3.3 Zone Electrophoresis 1336.3.4 Isoelectric Focusing 1346.3.5 Two-Dimensional Separations 1346.3.6 Selected Applications 1346.3.6.1 Protein Separations 1346.3.6.2 Separation of DNA/RNA 1356.4 Capillary Electrophoresis 1356.4.1 Instrumentation 1366.4.1.1 High-Voltage Supply 1366.4.1.2 Capillaries 1366.4.1.3 Sample Introduction 1376.4.1.4 Detection 1396.4.2 CE Zone Electrophoresis 1406.4.3 Other CE Separation Principles 1426.4.3.1 Isoelectric Focusing 1426.4.3.2 Gel Electrophoresis in CE 1426.4.3.3 Gel-Free Sieving 1426.4.3.4 Isotachophoresis 1436.4.4 Micellar Electrokinetic Capillary Chromatography (MEKC) 1436.5 Potential-Driven Chromatography (Electrochromatography – CEC) 1456.5.1 Instrumentation 1456.5.2 Mobile Phases 1456.5.3 Columns and Stationary Phases 1466.5.4 CEC in Separation Science 146References 1477 Chromatography on a Chip 1497.1 Introduction 1497.2 Sample Introduction 1497.3 Columns and Stationary Phases 1517.3.1 Open Channel Columns 1527.3.2 Packed Columns 1527.3.3 Monolithic Columns 1527.3.4 COMOSS 1527.4 Flow Management 1527.5 Detection 153Reference 1548 Field-Flow Fractionation 1558.1 Introduction 1558.2 Types of FFF 1568.2.1 Flow FFF 1568.2.2 Thermal FFF 1578.2.3 Sedimentation FFF 1588.3 Applications 158Reference 1599 Sample Preparation 1619.1 Introduction 1619.1.1 Recovery 1629.1.2 Enrichment 1629.2 Liquid–Liquid Extraction 1649.2.1 Back Extraction 1679.3 Solid-Phase Extraction (SPE) 1689.3.1 Normal Phase 1709.3.2 Reversed Phase 1729.3.3 Ion Exchange 1729.3.4 Mixed-Mode Ion Exchange 1759.3.5 MIP 1759.3.6 RAM 1769.3.7 SPE Hardware 1769.3.7.1 Disks 1779.4 SPME 1789.4.1 Adsorption/Extraction 1789.4.2 Desorption/Injection 1799.4.2.1 SPME–GC 1809.4.2.2 SPME–HPLC 1809.4.3 SPME Fiber Materials and Extraction Parameters 1809.4.3.1 pH 1819.4.3.2 Ionic Strength 1819.4.3.3 Water and Organic Solvents 1819.4.3.4 Temperature 1819.4.3.5 Agitation 1819.4.3.6 Extraction Time 1829.5 Protein Precipitation 1829.6 Membrane-Based Sample Preparation Techniques 1839.6.1 Microdialysis 1839.6.1.1 Perfusion Flow Rate 1849.6.1.2 Diameter and Length 1849.6.1.3 Cutoff 1849.6.1.4 Membrane Chemistry 1849.6.1.5 Application of Microdialysis 1859.6.1.6 How to Analyze the Dialysate? 1859.6.2 LPME 1859.6.2.1 Two-Phase LPME 1869.6.2.2 Three-Phase LPME 1869.6.2.3 Enrichment in LPME 1869.6.2.4 Donor Phase pH 1879.6.2.5 Acceptor Phase pH 1879.6.2.6 Composition of the SLM 1879.6.2.7 Extraction Time 188References 18810 Quantitation 18910.1 Introduction 18910.2 Calibration Methods 19210.2.1 External Standard 19210.2.2 Internal Standard 19310.2.3 Standard Addition 19410.3 Method Validation 19610.3.1 Validation Parameters 19610.3.1.1 Linearity and Range 19710.3.1.2 Repeatability 19710.3.1.3 Accuracy 19710.3.1.4 Selectivity 19710.3.1.5 Robustness 19710.3.1.6 Stability 19810.3.2 Validation Procedure: A Simple Example 198Reference 199Index 201