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Table of contents
Chapter I: Literature review
1.1 Electrochemistry and sensing
1.2 Types of electrochemical sensors
1.2.1 Potentiometric sensors
1.2.2 Conductometric sensors
1.2.3 Amperometric sensors
1.3 Types of working electrodes
1.3.1 Mercury electrodes
1.3.2 Solid electrodes
1.4 Modified electrodes
1.4.1 The Sol-gel process
1.4.2 Mesoporous silica modified electrodes
1.4.3 Configurations of mesoporous silica modified electrodes
1.4.4 Composite electrodes
1.4.5 Silica coated electrodes
1.5 Mesoporous silica thin films
1.5.1 Vertically oriented mesoporous silica thin films
1.5.2 Electrochemically assisted self-assembly (EASA) process
1.5.3 Mesoporous silica thin film applications
1.6 Use of pesticides in agriculture
1.6.1 Paraquat and diquat
1.6.2 Isoproturon
1.6.3 Other herbicides
1.7 Electrochemical detection of herbicides
1.8 Brief introduction of research project
Chapter II: Experimental section
2.1 Chemicals
2.2 Electrodes and electrochemical apparatus
2.2.1 Working electrodes
2.2.2 Reference electrodes
2.2.3 Counter electrode
2.2.4 Electrochemical cells
2.2.5 Electrochemical apparatus
2.2.6 Electrodes preparation
2.3 Protocols for mesoporous silica film preparation
2.3.1 3-Aminopropyltriethoxysilane (APTES) electrografting
2.3.2 Sol gel preparation and thin film electrodeposition (monolayer films)
2.3.3 Sol preparation and thin film deposition (multi-layered films)
2.4 Electrochemical techniques for analysis
2.4.1 Cyclic voltammetry (CV)
2.4.2 Square wave voltammetry (SWV)
2.4.3 Stripping voltammetry
2.4.4 Electrochemical impedance spectroscopy (EIS)
2.5 Analytical techniques for chemical and structural analysis
2.5.1 Ion chromatography
2.5.2 Scanning electron microscopy (SEM)
2.5.3 Transmission electron microscopy (TEM)
2.5.5 Silica thin film Characterization by profilometry
2.5.6 X-ray photoelectron spectroscopy (XPS)
Chapter III: Improved adhesion of mesoporous silica thin films on glassy carbon electrodes by electrografting of 3-aminopropyltriethoxysilane
3.1 Introduction
3.2 Electrochemical modification and characterization of glassy carbon electrodes
3.2.1 Electrochemical Characterization of APTES electrografting
3.2.2 Electrogeneration and Characterization of the mesoporous silica films
3.2.3 Characterization of modified GCE by neutral and anionic redox species
3.2.4 Characterization of modified electrodes by scanning electron microscopy (SEM) .
3.2.5 Silica film characterization by transmission electron microscopy (TEM)
3.2.6 X-ray photoelectron spectroscopy analysis of GCE modification
3.3 Functionalization of the mesoporous silica with click chemistry
3.4 Conclusions
Chapter IV: Electrochemical detection of paraquat at mesoporous silica thin films modified glassy carbon electrodes
4.1 Introduction
4.2 Electrode modification
4.3 Electrochemistry of paraquat
4.3.1 Effect of charge on redox analytes at their electrochemical behaviour
4.3.2 Electrochemical behavior of paraquat at mesoporous silica modified GCE
4.3.3 Investigation of paraquat electrochemical behavior by square wave voltammetry .
4.3.4 Influence of ionic strength on SWV signal intensity
4.3.5 Effect of electrolytes nature on SWV response
4.3.6 Electrochemical impedance spectroscopic (EIS) analysis of electrolyte solutions .
4.3.7 Effect of solution pH on SWV response
4.3.8 Effect of Debye length and mesochannels Interaction on sensitivity
4.4 Square wave voltammetric analysis with low concentration of paraquat
4.4.1 Analysis of real samples spiked with paraquat
4.5 Conclusions
Chapter V: Studies of electrode modification and electrode geometry effect on paraquat sensing
5.1 Introduction
5.2 Electrochemical deposition and characterization of monolayer films
5.2.1 Microscopic characterization of electrode modification
5.2.2 Film thickness measurements by profilometry
5.2.3 Paraquat accumulation by CV at modified electrodes
5.2.4 SWV analysis of paraquat on monolayer thin films
5.2.5 Conclusions
5.3 Multi-layered silica thin films
5.3.1 Characterization of multi-layered silica films
5.3.2 Microscopic characterization of multi-layered silica film modification
5.3.3 Paraquat electrochemistry at multilayer silica thin films
5.3.4 Paraquat detection on multilayer silica thin films
5.3.5 Conclusion
5.4 Microelectrode arrays fabrication and modification with silica thin films
5.4.1 Microelectrode arrays fabrication
5.4.2 Electrochemical characterization of microelectrode arrays
5.4.3 Microelectrode arrays modification by silica thin films
5.4.4 Electrochemical characterization of microelectrode arrays modification
5.4.5 Scanning electron microscopic characterization of microelectrode arrays modification
5.4.6 Paraquat detection at silica thin films modified microelectrode arrays
5.5 Conclusions
Chapter VI: Electrochemical Characterization and detection of isoproturon at mesoporous silica modified and unmodified glassy carbon electrodes
6.1 Introduction
6.2 Results and discussion
6.2.1 Cyclic voltammetric Characterization of isoproturon
6.2.2 Scan rate studies of isoproturon
6.2.3 Effect of repetitive scans at peak intensity
6.2.4 Effect of supporting electrolyte on electrochemical behavior of isoproturon
6.3 Analytical detection of isoproturon
6.3.1 Effect of preconcentration time
6.3.2 Quantitative analysis of isoproturon by SWV
6.4 Conclusions
Conclusions and perspectives
Conclusions et perspectives
References
