Ultraviolet/visible (UV/vis) spectroscopy was used to determine qualitatively and quantitatively Cu2+, Co2+, Co3+, and Fe3+ in oxidized Cu-Co ore leachates. The mineralogical and chemical characteristics of the three oxidized Cu-Co ore samples considered were determined using Fourier transform infrared spectroscopy (FTIR), X-ray powder diffractometry (XRD), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), and X-ray fluorescence spectrometry (XRF). The results showed that Cu and Co in the samples were in the form of carrollite (Co2CuS4), malachite (Cu2CO3(OH)(2), and heterogenite (CoO(OH)). The samples contained (2.73% Cu and 0.19% Co), (2.82% Cu and 0.07% Co), and (0.03% Cu and 0.05% Co), respectively. Gangues were mainly constituted of quartz, goethite, and hematite. The ultraviolet/visible (UV/vis) results indicated that the wavelengths of absorbance of the metal ions in dilute ethylenediaminetetraacetic acid aqueous solution (pH approximate to 3.5) were Fe3+ (293 nm), Cu2+ (821 nm), Co3+ (344 nm), and Co2+ (512 nm). The molar concentrations of the metal ions obtained using the UV/vis method compared well with the results obtained using the atomic absorption spectroscopy (AAS) method. UV/vis spectroscopy was also used to monitor the conversion of Co3+ into Co2+ using different reducing agents. The results showed that the molar concentration of Co2+ in the aqueous solutions increased with the addition of reducing agents, of about 80.95% (copper foil), 61.22% (ferrous sulfate), and 20.35% (sodium sulfite), respectively.