A process for the separation of metaxylene from aromatic C.sub.8 hydrocarbons, particularly from ethylbenzene and paraxylene, wherein a first phase is provided in which the mixture of aromatic hydrocarbons is selectively adsorbed, in vapor phase, into a catalytic bed consisting of zeolite of the Y type, preliminarily exchanged with potassium, and in a second phase a desorption is effected with a suitable solvent. The process, carried out at a temperature of 150.degree. to 200.degree. C. and preferably at atmospherical pressure, permits the recovery of metaxylene, substantially pure and at a concentration much higher than that of the starting mixture.