Characterisation of surfaces modified with phthalocyanines through click chemistry for applications in electrochemical sensing
- O'Donoghue, Charles St John Nqwabuko
- Authors: O'Donoghue, Charles St John Nqwabuko
- Date: 2018
- Subjects: Electrodes, Carbon , Phthalocyanines , X-ray photoelectron spectroscopy , Electrochemistry , Electrochemical sensors , Hydrazine , Click chemistry
- Language: English
- Type: text , Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10962/58046 , vital:27038
- Description: One form of surface modification was primarily investigated in this work on glassy carbon electrodes. The form of modification is comprised of a series of steps in which electrografting is first applied to the glassy carbon surface, which is then followed up with click chemistry to ultimately immobilise a phthalocyanine onto the surface. The modified glassy carbon electrodes and surfaces were characterised with a combination of scanning electrochemical microscopy, X-ray photoelectron spectroscopy and various electrochemical methods. In this work, three alkyne substituted phthalocyanines were used. Two novel phthalocyanines, with nickel and cobalt metal centres, were studied alongside a manganese phthalocyanine reported in literature. Each of the three phthalocyanines was modified at the peripheral position with a 1-hexyne group, via a glycosidic bond, yielding the terminal alkyne groups that were used for subsequent click reactions. In situ diazotisation was used to graft 4-azidoaniline groups to the surface of the glassy carbon electrode. The azide bearing 4- azidoaniline groups were thus used to anchor the tetra substituted phthalocyanines to the surface of the electrodes. This method yielded successful modification of the electrodes and lead to their application in sensing studies. The modified electrodes were primarily used to catalyse the common agricultural oxidising agent hydrazine.
- Full Text:
- Authors: O'Donoghue, Charles St John Nqwabuko
- Date: 2018
- Subjects: Electrodes, Carbon , Phthalocyanines , X-ray photoelectron spectroscopy , Electrochemistry , Electrochemical sensors , Hydrazine , Click chemistry
- Language: English
- Type: text , Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10962/58046 , vital:27038
- Description: One form of surface modification was primarily investigated in this work on glassy carbon electrodes. The form of modification is comprised of a series of steps in which electrografting is first applied to the glassy carbon surface, which is then followed up with click chemistry to ultimately immobilise a phthalocyanine onto the surface. The modified glassy carbon electrodes and surfaces were characterised with a combination of scanning electrochemical microscopy, X-ray photoelectron spectroscopy and various electrochemical methods. In this work, three alkyne substituted phthalocyanines were used. Two novel phthalocyanines, with nickel and cobalt metal centres, were studied alongside a manganese phthalocyanine reported in literature. Each of the three phthalocyanines was modified at the peripheral position with a 1-hexyne group, via a glycosidic bond, yielding the terminal alkyne groups that were used for subsequent click reactions. In situ diazotisation was used to graft 4-azidoaniline groups to the surface of the glassy carbon electrode. The azide bearing 4- azidoaniline groups were thus used to anchor the tetra substituted phthalocyanines to the surface of the electrodes. This method yielded successful modification of the electrodes and lead to their application in sensing studies. The modified electrodes were primarily used to catalyse the common agricultural oxidising agent hydrazine.
- Full Text:
Electrode surface modification using metallophthalocyanines and metal nanoparticles : electrocatalytic activity
- Authors: Maringa, Audacity
- Date: 2015
- Subjects: Phthalocyanines , Nanoparticles , Electrocatalysis , Scanning electron microscopy , X-ray photoelectron spectroscopy , Electrochemistry , Scanning electrochemical microscopy
- Language: English
- Type: Thesis , Doctoral , PhD
- Identifier: vital:4541 , http://hdl.handle.net/10962/d1017921
- Description: Metallophthalocyanines and metal nanoparticles were successfully synthesized and applied for the electrooxidation of amitrole, nitrite and hydrazine individually or when employed together. The synthesized materials were characterized using the following techniques: predominantly scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), electrochemistry and scanning electrochemical microscopy (SECM). Different electrode modification methods were used to modify the glassy carbon substrates. The methods include adsorption, electrodeposition, electropolymerization and click chemistry. Modifying the glassy carbon substrate with MPc (electropolymerization) followed by metal nanoparticles (electrodeposition) or vice versa, made a hybrid modified surface that had efficient electron transfer. This was confirmed by electrochemical impedance studies with voltammetry measurements having lower detection potentials for the analytes. This work also describes for the first time the micropatterning of the glassy carbon substrate using the SECM tip. The substrate was electrografted with 4-azidobenzenediazonium salt and then the click reaction was performed using ethynylferrocene facilitated by Cu⁺ produced at the SECM tip. The SECM imaging was then used to show the clicked spot.
- Full Text:
- Authors: Maringa, Audacity
- Date: 2015
- Subjects: Phthalocyanines , Nanoparticles , Electrocatalysis , Scanning electron microscopy , X-ray photoelectron spectroscopy , Electrochemistry , Scanning electrochemical microscopy
- Language: English
- Type: Thesis , Doctoral , PhD
- Identifier: vital:4541 , http://hdl.handle.net/10962/d1017921
- Description: Metallophthalocyanines and metal nanoparticles were successfully synthesized and applied for the electrooxidation of amitrole, nitrite and hydrazine individually or when employed together. The synthesized materials were characterized using the following techniques: predominantly scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), electrochemistry and scanning electrochemical microscopy (SECM). Different electrode modification methods were used to modify the glassy carbon substrates. The methods include adsorption, electrodeposition, electropolymerization and click chemistry. Modifying the glassy carbon substrate with MPc (electropolymerization) followed by metal nanoparticles (electrodeposition) or vice versa, made a hybrid modified surface that had efficient electron transfer. This was confirmed by electrochemical impedance studies with voltammetry measurements having lower detection potentials for the analytes. This work also describes for the first time the micropatterning of the glassy carbon substrate using the SECM tip. The substrate was electrografted with 4-azidobenzenediazonium salt and then the click reaction was performed using ethynylferrocene facilitated by Cu⁺ produced at the SECM tip. The SECM imaging was then used to show the clicked spot.
- Full Text:
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