This thesis presents the results of a spectroelectrochemical investigation into the interactions of two flotation collectors (mercaptobenzothiazole (MBT) and dithiophosphate (DTP)) with gold electrode and nanorods surfaces. The relevant compounds and ligands of these two collectors were characterised and identified by Raman spectroscopy and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR). Gold nanorods (Au NRs) with average aspect ratio of 4.04 ± 0.08 were synthesised and reacted with MBT and DTP. Gold particle flotation was investigated using controlled potential techniques. Electrochemical techniques have also been used to investigate the open circuit potential (OCP) and controlled potential oxidation of chalcopyrite. The interaction of collectors with gold electrode surfaces was investigated using in situ surface-enhanced Raman scattering (SERS) spectroscopy. The SERS surface for a gold electrode was generated by electrochemically roughening using an oxidation-reduction cycling (ORC).