This work describes the electrochemical extraction on a reactive cathode (Cu, Ni) of two lanthanides Ln (Ln = Nd and Gd) from molten LiF-CaF2 medium at 840 and 920 A degrees C for Nd and 940 A degrees C for Gd. Extraction runs have been performed and the operating conditions (cathodic material and temperature) optimized. The titration of the Nd and Gd concentrations in the melt during extraction used square wave voltammetry. At the end of each run, the residual Ln content was checked by ICP-AES; the extraction efficiencies of the two lanthanides were found to be more than 99.8% on both reactive substrates.