Rechargeable Ni-MH batteries contain strategic metal values which are worth to be recovered. In the present work, a preliminary sequential chemical and electrochemical procedure is proposed, in order to reclaim materials bearing Ni, Co and rare earth elements (REE) from Ni-MH spent batteries. Initially, spent batteries are disassembled to separate the electrode materials (anode and cathode), which are then leached with an aqueous solution of 5w% sulphuric acid. The metal content of this solution is checked by atomic absorption spectrometry techniques. The obtained solution is pH-adjusted (with NaOH), until pH is between 4.0 and 4.3; then, it is heated up to 70°C to precipitate a rare earth elements sulphate (Nd, La, Pr, Ce), as determined by means of x-ray fluorescence techniques. The solids-free solution is then electrolyzed, in order to recover a Ni-Co alloy. The electrolysis conditions were established through a cyclic voltammetry technique.