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• Electrochemistry of Ferrocene Derivatives at Highly Oriented Pyrolytic Graphite (HOPG): Quantification and Impact of Surface Adsorption
Cyclic voltammetry of three ferrocene derivatives – (ferrocenylmethyl) trimethylammonium (FcTMA+), ferrocenecarboxylic acid (FcCOOH), and ferrocenemethanol (FcCH2OH) – in aqueous solutions shows that the reduced form of the first two redox species weakly adsorbs on freshly cleaved surfaces of highly oriented pyrolytic graphite (HOPG), with the fractional surface coverage being in excess of 10% of a monolayer at a bulk concentration level of 0.25 mM for both compounds. FcCH2OH was found to exhibit greater and stronger adsorption (up to a monolayer) for the same bulk concentration. Adsorption of FcTMA+ on freshly cleaved surfaces of high quality (low step edge density) and low grade (high step edge density) HOPG is the same within experimental error, suggesting that the amount of step edges has no influence on the adsorption process. The amount of adsorption of FcTMA+ is the same (within error) for low grade HOPG, irrespective of whether the surface is freshly cleaved or left in air for up to 12 hours, while – with aging – high quality HOPG adsorbs notably more FcTMA+. The formation of an air-borne contaminating film is proposed to be responsible for the enhanced entrapment of FcTMA+ on aged high quality HOPG surfaces, while low quality surfaces appear less prone to the accumulation of such films. The impact of the adsorption of ferrocene derivatives on graphite on voltammetric studies is discussed. Adsorption is quantified by developing a theory and methodology to process cyclic voltammetry data from peak current measurements. The accuracy and applicability, as well as limits of the approach, are demonstrated for various adsorption isotherms.
• Assessment of Boron Doped Diamond Electrode Quality and Application to In Situ Modification of Local pH by Water Electrolysis
A protocol is described for the characterization of the key electrochemical parameters of a boron doped diamond (BDD) electrode and subsequent application for in situ pH generation experiments.
• Manipulation and Measurement of pH sensitive Ligand-Metal Binding Using Electrochemical Proton Generation and Metal Detection
Generator-detector electrodes can be used to both perturb and monitor pH dependant metal-ligand binding equilibria, in-situ. In particular, protons generated at the generator locally influence the speciation of metal (Cu2+) in the presence of ligand (triethylenetetraamine), with the detector employed to monitor, in real time, free metal (Cu2+) concentrations.