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Table of contents
Introduction
Chapter I. Nanotechnology, metrology and size characterization
1. Generalities about nanomaterials
1.1. History
1.2. Definitions
1.3. Classification of nanomaterials
1.3.1. Dimensional based classification
1.3.2. Classification based on chemical composition and structure
1.3.3. Origin based classification
1.4. Fabrication methods
1.4.1. Top-down method
1.4.2. Bottom-up method
1.5. Properties of nanoparticles
1.5.1. Surface effect
1.5.2. Quantum confinement effect
1.6. Applications
1.6.1. Catalysis
1.6.2. Environmental applications
1.6.3. Medical applications
1.6.4. Optical applications
2. Characterization of nanomaterials
2.1. Size characterization techniques
2.1.1. Equivalent diameter
2.1.2. Dynamic light scattering
2.1.3. Single particle inductive coupled plasma mass spectrometry SP-ICP-MS
2.1.4. Multi angle light scattering
2.1.5. Electronic microscopy
2.1.6. Atomic force microscopy
2.1.7. Particle tracking analysis
2.1.8. Small-angle X-ray scattering
2.1.9. Tunable resistive pulse sensing (TRPS)
2.1.10. Numerous techniques and numerous mesurands
3. Fractionations techniques
3.1. Field Flow Fractionation
3.2. Size exclusion chromatography
3.3. Analytical ultracentrifugation and centrifugal liquid sedimentation
4. Metrology
4.1. International system of units
4.2. Metrological Traceability
4.3. Measurement uncertainties
References
Chapter II. Field-Flow Fractionation techniques: state of the art
Abstract
1. FFF principle
1.1. Elution modes
1.2. Theoretical formalization
1.3. Working hypotheses of the FFF retention theory
1.4. Practice versus classical theory
1.5. Variants of the classical retention model
1.5.1. Steric model
1.5.2. Model tacking into account the interaction particle-wall
1.5.3. Experimental correction for particle−wall interaction
1.5.4. Models based on different assumptions
2. Flow-FFF and Asymmetrical Flow-FFF
2.1. The different steps in AF4 analysis
2.2. AF4 applications
2.3. Strength and weakness of AF4-multidetector
Scope of the work
References
Chapter III. Materials and methods
Abstract
1. AF4-multidetector instrumentation
1.1. Determination of the effective channel thickness
1.2. Determination of the retention time
1.3. Determination of the void time
1.4. Determination of the focusing position
1.5. Determination of the recovery rate
2. Zeta potential analyses
2.1. Measurement of the zeta potential of particle suspensions
2.2. Measurement of the zeta potential of membranes
3. Scanning electron microscopy analyses
4. Particle standards
5. Experimental approach and method validation of AF4 method
References
Chapter IV: Study of the mechanisms governing the retention inside the AF4 channel and application of the δw model for the characterisation of nanoparticle hydrodynamic diameter
Abstract:
1. Study of the retention behaviour of spherical nanoparticles in AF4 channel using the classical model
1.1. Influence of the carrier ionic strength on the particle retention
1.2. Influence of the membrane nature on the particle retention and recovery rate
1.3. Influence of the particle size on the particle retention
1.4. Influence of the particle nature on the particle retention
1.5. Lessons retained from preliminary tests on retention behaviour of spherical nanoparticles in AF4 channel
2. Application of the δw model to AF4 for the size characterization of nanoparticles
2.1. Determination of the channel thickness in the case of the δw model
2.2. Effect of the ionic strength and of the particle size on δw
2.3. Validation of the model
Conclusion
References
Chapter V. Implementation and evaluation of a retention model taking into account particle-wall interactions for the measurement of nanoparticle hydrodynamic diameter by asymmetrical flow field-flow fractionation
Abstract
1. Introduction
2. Theory
3. Materials and methods
3.1. Instrumentation
3.2. Reagents and Samples
4. Results and discussion
4.1. Zeta potential of the membrane
4.2. Characterization of the particles standard
4.3. Determination of the void time
4.4. Channel thickness determination
4.4.1. Effective channel thickness as a physical parameter
4.4.2. Effective thickness as a correction factor
Conclusion
Chapter VI. Metrological validation of a retention model taking in account particle-wall interactions for the measurement of nanoparticle hydrodynamic diameter by asymmetrical flow field-flow fractionation
Abstract:
1. Introduction
2. Theory
2.1 FFF theory
3. Materiel and methods
3.1. Nanoparticles Standards for size values
3.2. Instrumentation
4. Results and discussion
4.1. Program operation and uncertainty propagation
4.2. Determination of the standard uncertainty of the inputs parameters
4.3. Result of the rh probability density function
4.4. Metrological traceability
Conclusion
References
Chapter VII: A novel approach to directly determine the channel thickness: feasibility study
Abstract
1. On the measurement of the effective channel thickness
2. Characteristics of the ideal method for the direct measurement of weff
2.1. Principle of chromatic confocal sensor
3. Evaluation of the experimental set-up
4. Future enhancements of the measurement set-up
Conclusion
References
Conclusions and perspectives
Résumé étendu en français
Annex I: Conference paper 19th International Congress of Metrology – CIM2019



