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Full Description
Comprehensive, up-to-date, and user-centered one-stop reference on principles and applications of Field flow fractionation (FFF), a highly versatile separation technology
Field Flow Fractionation Principles and Applications offers a comprehensive and topical one-stop reference on field flow fractionation (FFF), an important separation technique which has been proven successful in the analysis of natural and engineered nanoparticles, pharmaceuticals, proteins, polymers, soils, and food.
After introductory chapters on theory, principles, and instrumentation, a tutorial-style user guide addresses typical users' questions and problems. In the application part, the separation of all relevant particle classes is discussed by international experts.
Sample topics covered in Field Flow Fractionation Principles and Applications include:
Historical perspectives of the technique, normal versus steric versus hyperlayer modes, retention resolution, and fractionation power
FFF techniques, including flow (asymmetric, frit inlet, and outlet), sedimentation, thermal, electric, and other novel techniques such as 2D
How to determine if FFF is the correct choice and if it is being implemented correctly, along with general optimization strategies including carrier fluid, calibration, and reproducibility
Sample overloading and recovery, detector selection, troubleshooting, and performance of other fractionation techniques
Both beginners and experienced chemists and researchers can confidently rely on Field Flow Fractionation Principles and Applications to confirm their own understanding and to improve their FFF methods and interpretation of their results.
Contents
Preface xi
1 Field-Flow Fractionation Techniques 1
P. Stephen Williams
1.1 Introduction 1
1.2 Flow Field-Flow Fractionation 3
1.3 Hollow-Fiber Field-Flow Fractionation 10
1.4 Gravitational Field-Flow Fractionation 14
1.5 Sedimentation Field-Flow Fractionation 16
1.6 Thermal Field-Flow Fractionation 18
1.7 Electrical Field-Flow Fractionation 22
1.8 Magnetic Field-Flow Fractionation 24
1.9 Novel Techniques 27
1.9.1 Combined Fields 27
1.9.2 Two-Dimensional, Continuous Fractionation 28
References 29
2 Field-Flow Fractionation User Guide 45
Haiyang Dou, S. Kim Ratanathanawongs Williams, Mohammed Baalousha, and Céline Guéguen
2.1 Theoretical FFF Background 45
2.2 Different Variants of FlFFF 47
2.3 Sample Properties Measured by FFF 48
2.4 Selection of Detectors 48
2.5 FFF Selection Strategy 50
2.6 Guidance for FFF Separation 50
2.6.1 Sample Pre-preparation 52
2.6.2 Selection of Carrier Liquid 52
2.6.3 Verify Sample Loss in the FFF Channel 53
2.6.4 Optimize Field Strength 53
2.6.5 Optimize Channel Flow Rate 54
2.6.6 Evaluate Sample Overloading 54
2.6.7 Evaluate Sample Recovery 55
Acknowledgments 55
References 55
3 Polymers and Biohybrids 63
Albena Lederer and Susanne Boye
3.1 Polymer Architectures 64
3.2 FFF Systems for Polymer Characterization 66
3.3 FFF-Coupled Techniques for Polymer Characterization 68
3.4 FFF Separation of Polymers with Different Branching Topology, Composition, and Functionality 69
3.4.1 Hyperbranched Polyesters 70
3.4.2 Dendritic Glycopolymers 72
3.4.3 Single-Chain Nanoparticles 74
3.4.4 Flower-Like Polymer Structures by Self-Assembly 77
3.4.5 Polyethylene Block Copolymers 78
3.5 Biohybrids - Interaction Between Polymers and Biomolecules 80
3.5.1 Polymer-Dye/Drug Complexes 81
3.5.2 Biohybrid Structures Via Polymer-Protein Conjugation 84
3.5.3 Polyplexes: Conjugation of polymers and DNA 88
3.5.4 Polymersomes 89
References 91
4 Separation Techniques in Support of Elucidating Composition, Structure, and Function elationships for Complex Polysaccharides 101
Kaitlin C. Lesco, Lieve M. L. Laurens, and S. Kim Ratanathanawongs Williams
4.1 Introduction 101
4.2 Polysaccharide Structures 102
4.3 Analytical Separation Techniques for Polysaccharides 103
4.3.1 Asymmetrical Flow Field-Flow Fractionation 103
4.3.2 Size Exclusion Chromatography 104
4.3.3 Analytical Ultracentrifugation 105
4.3.4 Anion Exchange Chromatography 106
4.4 Online Detection Methods 111
4.4.1 Light Scattering Detectors 112
4.4.2 Detectors for Elucidation of Chemical Properties 113
4.5 Comparing Techniques 114
4.5.1 Resolution 114
4.5.1.1 Size-Based Separation Techniques 114
4.5.1.2 Monosaccharide-Based Separation Techniques 117
4.5.2 Sample Recovery 117
4.5.3 Carrier Fluid Flexibility 118
4.5.4 MWor Size Range 118
4.6 Factors Influencing Separation of Polysaccharides 119
4.6.1 pH 119
4.6.1.1 pH Effects on Polysaccharide Solubility 119
4.6.1.2 pH Effects on Charge 120
4.6.2 Ionic Strength and Composition 120
4.6.2.1 Ionic Strength Effects on Separation 121
4.6.2.2 Ionic Strength Effects on Polysaccharide Structures 121
4.6.2.3 Ionic Composition 122
4.7 Examples of the Separation of Polysaccharides and Their Aggregates 122
4.7.1 Marine Polysaccharides 122
4.7.1.1 Size-Based Separation Techniques 127
4.7.1.2 Compositional and Charge-Based Separation Techniques 127
4.7.2 Plant Polysaccharides 128
4.7.2.1 Size-Based Separation Techniques 129
4.7.2.2 Compositional and Charge-Based Separation Techniques 130
4.7.3 Fungi Polysaccharides 131
4.7.4 Mammalian Polysaccharides 132
4.7.4.1 Size-based Separation Techniques 132
4.7.4.2 Compositional and Charge-Based Separation Techniques 132
4.8 Future Outlooks 133
4.9 Acknowledgments 134
References 134
5 Field-Flow Fractionation Methods for the Characterization of Natural Nanoparticles in Waters and Soils 149
Valentin de Carsalade du pont, Stéphane Faucher, and Gaëtane Lespes
5.1 Introduction 149
5.2 Sources, Occurrence, and Biophysicochemical Processes 149
5.3 Analytical Investigations 152
5.3.1 Preliminary 152
5.3.2 Analytical Methodologies 152
5.3.2.1 Sample Collection and Preparation 153
5.3.2.2 Injected Amount 155
5.3.2.3 Fractionation 156
5.3.2.4 Detection 163
5.3.2.5 Data Processing and Size Calibration 167
5.4 Current and Future Trends 173
References 174
6 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) 179
Yu Wang, Chad W. Cuss, and William Shotyk
6.1 Introduction 179
6.2 Applications to the Analysis of TEs in NaturalWaters 180
6.2.1 Size Fraction Definition 182
6.2.2 Case Studies 186
6.3 Challenges and Troubleshooting Strategies 187
6.3.1 Sample Losses 188
6.3.2 Contamination and Carryover 189
6.3.3 Troubleshooting Strategies 191
6.4 Considerations and Future Needs 193
References 193
7 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 197
Chad W. Cuss and Iain Grant-Weaver
7.1 Introduction and Overview 197
7.2 System Configuration and Components 198
7.3 QA/QC and Other Analytical Considerations 204
7.3.1 Trace Analysis and Initial Setup 204
7.3.2 Calibration, SRMs, LODs, Recovery, and Memory Effects 206
7.3.3 Data Analysis and Calculations 208
7.4 Optimization 211
7.4.1 AF4 Flow Program: Multielement Optimization 211
7.4.2 ICP-MS Operating Conditions 211
7.5 Further Routinization and Future Directions 213
References 215
8 Analysis of Proteins and Enzymes by Field-Flow Fractionation (FFF) 219
Ju Yong Lee and Wenwan Zhong
8.1 Demands for Separation of Intact Proteins 219
8.2 Separation Methods for Intact Proteins 220
8.3 Introduction of AF4- or HF5-Based Protein Analysis 223
8.3.1 FFF for Protein Fractionation Prior to MS Analysis in Proteomic Study 223
8.3.2 FFF for Study of Protein Aggregation 225
8.3.3 Application of Micro- and Nanoparticles Combining with Proteins 227
8.3.4 Lipoproteins 229
8.4 General Guidance for Applying AF4 and HF5 in Protein Analysis 230
8.4.1 Membrane and Buffer of AF4 and HF5 for Proteomic Analysis 230
8.4.2 Dimension and Thickness of Spacer and Flowrate Condition 231
8.4.3 Detectors and Other Analytical Techniques 232
8.4.4 Procedures Used in Development of an AF4- or HF5-Based Method for
Protein Analysis 234
8.5 Conclusion 236
References 236
9 Cell Sorting with FFF 241
Gaëlle Begaud, Serge Battu, Philippe Cardot, Barbara Roda, Andrea Zattoni, and Pierluigi Reschiglian
9.1 Introduction 241
9.2 Common Features of Sedimentation FFF Methods 242
9.2.1 Sample Preparation 243
9.2.2 Hyperlayer Elution Mode 245
9.3 Sedimentation Field-Flow Fractionation 249
9.3.1 Apparatus 249
9.3.1.1 Implementation of the Separation Channel 249
9.3.1.2 The Speed Control Unit 251
9.3.1.3 Rotating Seals 252
9.3.1.4 Inlet/Outlet Tubing 252
9.3.1.5 ChannelWall Materials, Mobile Phase, Recovery, and Decontamination Procedure 253
9.3.1.6 Detection and Characterization of the Sample 256
9.3.2 Practical Steps of Cell Sorting 258
9.3.2.1 Biophysical Calibration of Fractogram 258
9.3.2.2 Biological Calibration of the Fractogram 261
9.3.2.3 Cell Reusability 263
9.4 Gravitational FFF (GrFFF) 265
9.4.1 Introduction 265
9.4.2 GrFFF Separative Channel 266
9.4.3 GrFFF Instrumental Setup 267
9.4.4 GrFFF Separation Modes 268
9.4.5 GrFFF Operations 270
9.4.6 GrFFF Main Applications 271
9.4.6.1 GrFFF for Cell Purging 271
9.4.6.2 GrFFF of a Raw Sample 273
9.4.6.3 NEEGA-DF 277
References 280
Index 291