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Table of contents
Chapter 1 Literature review
1.1 Introduction
1.1.1 Sol-gel process
1.1.2 Mesoporous silica
1.1.3 Mesoporous silica thin films
1.2 Main approaches for electrode modification
1.2.1 Electrode modification by mesoporous silica films
1.2.2 Mesoporous silica films with vertically oriented pores for electrochemical application
1.2.3 Functionalisation of vertically oriented mesoporous silica films
1.2.4 Practical application of vertically oriented mesoporous silica films
1.3 Our research project
Chapter 2 Experimental part
2.1 Instrumental techniques
2.1.1 Electrochemistry
2.1.2 Spectroscopy
2.1.3 Microscopy
2.1.4 Profilometry
2.2 Protocol for synthesis of (3-azopropyl)triethoxysilane (AzPTES)
2.3 Mesoporous silica film preparation by electrochemically-assisted self-assembly
2.3.1 Sol preparation and film deposition
2.3.2 Surfactant extraction
2.3.3 Click reaction to prepare modified films
2.4 Electrochemical characterisation of mesoporous silica films
2.4.1 Characterisation with conventional probes
2.4.2 Characterisation with haemoglobin
2.5 Protocol for etching experiments
Chapter 3 Tuning the thinness of well-organised mesoporous silica film
3.1 Introduction
3.2 Investigating the deposition time parameter for obtaining the thinnest flawless films
3.3 Wet etching approach to control the thickness of mesoporous silica film
3.3.1 Control experiments
3.3.2 Effect of mesoporous silica film nature
3.3.3 Effect of the NH4F concentration
3.3.4 The effect of the etching agent
3.4 Conclusions
Chapter 4 Development of system based on Ru(bpy)32+ modified mesoporous silica thin film for glyphosate detection by electrochemiluminescence
4.1. Introduction
4.1.1 General information about Ru(bpy)32+ as electrochemiluminescence reactant
4.1.2 Immobilisation of Ru(bpy)32+ onto solid matrix
4.1.3 Glyphosate and its detection
4.2 Glyphosate detection by ECL – Ru(bpy)32+ complex system: solution approach
4.2.1 ITO working electrode
4.2.2 ITO working electrode modified by mesoporous silica film
4.3 Impregnation of Ru(bpy)32+ complex onto silica film surface
4.3.1 Electrode preparation
4.3.2 Characterisation of mesoporous silica films with physically adsorbed Ru(bpy)32+ complex
4.3.3 Electrochemical response in presence of glyphosate
4.4 Covalent immobilisation of Ru(bpy)2(bpy’)2+ onto mesoporous silica film surface
4.4.1 Ru(bpy)2(bpy’)2+ complex preparation
4.4.2 Huisgen “click” reaction
4.4.3 Characterisation of Ru(bpy)2(bpy)’-modified mesoporous silica films
4.4.4 Electrochemical response in presence of glyphosate
4.5 Analytical aspect of electrochemical detection of glyphosate
4.6 ECL measurements: challenges and complications in course of the project
4.7 Conclusions
General conclusion and perspectives
Appendix 1: Chemicals
Appendix 2: Determination of ammonium fluoride concentration
Appendix 3: Surfactant extraction from mesopores during etching
Appendix 4: Effect of pH on glyphosate detection using Ru(bpy)32+ glyphosate co-reactant system on ITO electrode
Appendix 5: NMR characterisation
Bibliography
