Concentrations of dissolved rare earth metal oxides, Nd2O3, and Pr2O3 or their mixtures in different fluoride electrolytes composed of NdF3, PrF3, and LiF at ca. 1040 °C were monitored using a graphite probe inserted into the electrolyte during the dissolution process. Fast voltage sweeps of 100 V/s were applied to the graphite probe, and the current response was measured. As the oxide concentration in the diffusion layer towards the electrode depletes, a passive layer is, at a certain point, formed on the probe, resulting in a current drop. The magnitude of the peak current attained before the formation of the passive layer reflects the concentration of the dissolved oxide and, thus, is applied to determine the oxide concentration. The oxide concentration in the electrolyte samples determined using the inert gas fusion technique showed a good correlation to the peak current determined by the probe.