ABSTRACTNickel‐metal hydride (NiMH) batteries hold not only the base metals but valuable rare earth elements (RREs) like La, Ce, Pr, and Nd. Given the importance of resource recycling and assured supply of the contained metals in such wastes, the present study has focused on the development of an XRF method able to fully characterize these residues. In this study, a robust method for the chemical characterization of the anode and cathode by wavelength‐dispersive x‐ray fluorescence spectrometry was developed. For that, NiMH batteries were manually disassembled to obtain the active materials used in the anode and cathode, where critical raw materials are used. The results showed that NiMH batteries' anode is valuable due to the high concentrations of La, Ce, Nd, and Pr, apart from Ni. Besides, the cathode is quite rich in Ni. The different composition of these two materials justifies the need for a recycling process that separates these fractions in order not to dilute the number of RREs and Ni that can be recovered from these batteries when they are disposed of.
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