Field-Flow Fractionation

Céline Guéguen, PhD, is Full Professor of Chemistry at the Université de Sherbrooke, Québec, Canada.Mohammed Baalousha, PhD, is Professor of Environmental Nanoscience and director of the Environmental Nanoscience & Analytics Laboratory at the University of South Carolina, Columbia, South Carolina, United States.S. Kim R. Williams is a Professor of Chemistry at the Colorado School of Mines, Golden, Colorado, United States

• Preface xi1 Field-Flow Fractionation Techniques 1P. Stephen Williams1.1 Introduction 11.2 Flow Field-Flow Fractionation 31.3 Hollow-Fiber Field-Flow Fractionation 101.4 Gravitational Field-Flow Fractionation 141.5 Sedimentation Field-Flow Fractionation 161.6 Thermal Field-Flow Fractionation 181.7 Electrical Field-Flow Fractionation 221.8 Magnetic Field-Flow Fractionation 241.9 Novel Techniques 271.9.1 Combined Fields 271.9.2 Two-Dimensional, Continuous Fractionation 28References 292 Field-Flow Fractionation User Guide 45Haiyang Dou, S. Kim Ratanathanawongs Williams, Mohammed Baalousha, and Céline Guéguen2.1 Theoretical FFF Background 452.2 Different Variants of FlFFF 472.3 Sample Properties Measured by FFF 482.4 Selection of Detectors 482.5 FFF Selection Strategy 502.6 Guidance for FFF Separation 502.6.1 Sample Pre-Preparation 522.6.2 Selection of Carrier Liquid 522.6.3 Verify Sample Loss in the FFF Channel 532.6.4 Optimize Field Strength 532.6.5 Optimize Channel Flow Rate 542.6.6 Evaluate Sample Overloading 542.6.7 Evaluate Sample Recovery 55Acknowledgments 55References 553 Polymers and Biohybrids 63Albena Lederer and Susanne Boye3.1 Polymer Architectures 643.2 FFF Systems for Polymer Characterization 663.3 FFF-Coupled Techniques for Polymer Characterization 683.4 FFF Separation of Polymers with Different Branching Topology, Composition, and Functionality 693.4.1 Hyperbranched Polyesters 703.4.2 Dendritic Glycopolymers 723.4.3 Single-Chain Nanoparticles 743.4.4 Flower-Like Polymer Structures by Self-Assembly 773.4.5 Polyethylene Block Copolymers 783.5 Biohybrids – Interaction Between Polymers and Biomolecules 803.5.1 Polymer-Dye/Drug Complexes 813.5.2 Biohybrid Structures Via Polymer–Protein Conjugation 843.5.3 Polyplexes: Conjugation of Polymers and DNA 883.5.4 Polymersomes 89References 914 Separation Techniques in Support of Elucidating Composition, Structure, and Function Relationships for Complex Polysaccharides 101Kaitlin C. Lesco, Lieve M. L. Laurens, and S. Kim Ratanathanawongs Williams4.1 Introduction 1014.2 Polysaccharide Structures 1024.3 Analytical Separation Techniques for Polysaccharides 1034.3.1 Asymmetrical Flow Field-Flow Fractionation 1034.3.2 Size Exclusion Chromatography 1044.3.3 Analytical Ultracentrifugation 1054.3.4 Anion Exchange Chromatography 1064.4 Online Detection Methods 1114.4.1 Light Scattering Detectors 1124.4.2 Detectors for Elucidation of Chemical Properties 1134.5 Comparing Techniques 1144.5.1 Resolution 1144.5.1.1 Size-Based Separation Techniques 1144.5.1.2 Monosaccharide-Based Separation Techniques 1174.5.2 Sample Recovery 1174.5.3 Carrier Fluid Flexibility 1184.5.4 MW or Size Range 1184.6 Factors Influencing Separation of Polysaccharides 1194.6.1 pH 1194.6.1.1 pH Effects on Polysaccharide Solubility 1194.6.1.2 pH Effects on Charge 1204.6.2 Ionic Strength and Composition 1204.6.2.1 Ionic Strength Effects on Separation 1214.6.2.2 Ionic Strength Effects on Polysaccharide Structures 1214.6.2.3 Ionic Composition 1224.7 Examples of the Separation of Polysaccharides and Their Aggregates 1224.7.1 Marine Polysaccharides 1224.7.1.1 Size-Based Separation Techniques 1274.7.1.2 Compositional and Charge-Based Separation Techniques 1274.7.2 Plant Polysaccharides 1284.7.2.1 Size-Based Separation Techniques 1294.7.2.2 Compositional and Charge-Based Separation Techniques 1304.7.3 Fungi Polysaccharides 1314.7.4 Mammalian Polysaccharides 1324.7.4.1 Size-Based Separation Techniques 1324.7.4.2 Compositional and Charge-Based Separation Techniques 1324.8 Future Outlooks 1334.9 Acknowledgments 134References 1345 Field-Flow Fractionation Methods for the Characterization of Natural Nanoparticles in Waters and Soils 149Valentin de Carsalade Du Pont, Stéphane Faucher, and Gaëtane Lespes5.1 Introduction 1495.2 Sources, Occurrence, and Biophysicochemical Processes 1495.3 Analytical Investigations 1525.3.1 Preliminary 1525.3.2 Analytical Methodologies 1525.3.2.1 Sample Collection and Preparation 1535.3.2.2 Injected Amount 1555.3.2.3 Fractionation 1565.3.2.4 Detection 1635.3.2.5 Data Processing and Size Calibration 1675.4 Current and Future Trends 173References 1746 Field-Flow Fractionation Methods for the Characterization of Natural Applications, Challenges, and Considerations for Trace Element Analysis in Natural Waters Using Asymmetric Flow Field-Flow Fractionation - Ultraviolet - Inductively Coupled Plasma Mass Spectrometry (AF4-UV-ICPMS) 179Yu Wang, Chad W. Cuss, and William Shotyk6.1 Introduction 1796.2 Applications to the Analysis of TEs in Natural Waters 1806.2.1 Size Fraction Definition 1826.2.2 Case Studies 1866.3 Challenges and Troubleshooting Strategies 1876.3.1 Sample Losses 1886.3.2 Contamination and Carryover 1896.3.3 Troubleshooting Strategies 1916.4 Considerations and Future Needs 193References 1937 Online Coupling of Flow Field-Flow Fractionation (FlFFF) to Inductively Coupled Plasma Mass Spectrometry (ICPMS): Considerations for the Routine Separation and Analysis of Trace Elements at the Micro- and Nano-Scales 197Chad W. Cuss and Iain Grant-Weaver7.1 Introduction and Overview 1977.2 System Configuration and Components 1987.3 QA/QC and Other Analytical Considerations 2047.3.1 Trace Analysis and Initial Setup 2047.3.2 Calibration, SRMs, LODs, Recovery, and Memory Effects 2067.3.3 Data Analysis and Calculations 2087.4 Optimization 2117.4.1 AF4 Flow Program: Multielement Optimization 2117.4.2 ICP-MS Operating Conditions 2117.5 Further Routinization and Future Directions 213References 2158 Analysis of Proteins and Enzymes by Field-Flow Fractionation (fff) 219Ju Yong Lee and Wenwan Zhong8.1 Demands for Separation of Intact Proteins 2198.2 Separation Methods for Intact Proteins 2208.3 Introduction of AF4- or HF5-Based Protein Analysis 2238.3.1 FFF for Protein Fractionation Prior to MS Analysis in Proteomic Study 2238.3.2 FFF for Study of Protein Aggregation 2258.3.3 Application of Micro- and Nanoparticles Combining with Proteins 2278.3.4 Lipoproteins 2298.4 General Guidance for Applying AF4 and HF5 in Protein Analysis 2308.4.1 Membrane and Buffer of AF4 and HF5 for Proteomic Analysis 2308.4.2 Dimension and Thickness of Spacer and Flowrate Condition 2318.4.3 Detectors and Other Analytical Techniques 2328.4.4 Procedures Used in Development of an AF4- or HF5-Based Method for Protein Analysis 2348.5 Conclusion 236References 2369 Cell Sorting with FFF 241Gaëlle Begaud, Serge Battu, Philippe Cardot, Barbara Roda, Andrea Zattoni, and Pierluigi Reschiglian9.1 Introduction 2419.2 Common Features of Sedimentation FFF Methods 2429.2.1 Sample Preparation 2439.2.2 Hyperlayer Elution Mode 2459.3 Sedimentation Field-Flow Fractionation 2499.3.1 Apparatus 2499.3.1.1 Implementation of the Separation Channel 2499.3.1.2 The Speed Control Unit 2519.3.1.3 Rotating Seals 2529.3.1.4 Inlet/Outlet Tubing 2529.3.1.5 Channel Wall Materials, Mobile Phase, Recovery, and Decontamination Procedure 2539.3.1.6 Detection and Characterization of the Sample 2569.3.2 Practical Steps of Cell Sorting 2589.3.2.1 Biophysical Calibration of Fractogram 2589.3.2.2 Biological Calibration of the Fractogram 2619.3.2.3 Cell Reusability 2639.4 Gravitational FFF (GrFFF) 2659.4.1 Introduction 2659.4.2 GrFFF Separative Channel 2669.4.3 GrFFF Instrumental Setup 2679.4.4 GrFFF Separation Modes 2689.4.5 GrFFF Operations 2709.4.6 GrFFF Main Applications 2719.4.6.1 GrFFF for Cell Purging 2719.4.6.2 GrFFF of a Raw Sample 2739.4.6.3 Neega-df 277References 280Index 293