The invention concerns a method and a device for separating at least one catalyst and/or adsorbent from a homogeneous mixture of catalysts and/or adsorbents, said catalysts or adsorbents containing one or more metal, semi-metal or non-metal contaminant(s) deposited on said catalysts or adsorbents, such as Fe, Hg, Ni, V, C, Cl, Na, S, N, Si, P and As. The separation method and device make it possible to separate catalysts or adsorbents depending on the presence or absence of contaminant and also depending on the content of contaminants, from a sorting threshold corresponding to a content and defined by the operator. The grains of catalysts or of adsorbents pass in front of the LIBS detection system, which detects the contaminant according to the wavelength(s) characterising said contaminant, the analyser associated with the LIBS processes the signal sent by the detector by comparing same with a setpoint value representing the sorting threshold and sends a signal to a means for discharging the catalyst grains i