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Regioselective H/D exchange at the side-chain methyl group of ethylbenzene on dealuminated zeolite H-Y and formation of carbenium ions are observed for the first time by the novel in situ pulsed-flow 1H MAS NMR-UV/Vis technique. Hydride abstraction on Lewis acid sites lead to the formation carbenium ions which are protonated following Markovnikov's rule (see scheme).