Two series of FeZSM-5 catalysts prepared from Na+ and NH4+ ZSM-5 precursors are studied in the selective reduction of NOx using NH3 and urea as reducing agents. All Fe-containing catalysts are active for NOx reduction in the SCR-NH3 reaction with ex-NH4+ catalysts being more active than ex-Na+ materials and the activity depending (to a minor extent within each series of catalysts) upon [Fe]. Catalysts with Bronstead acid sites also show a small transient deNO(x) activity at low temperatures. All catalysts are less active for the SCR-urea reaction but the ex-Na+ catalysts retain far more deNO(x) activity than the ex-NH4+ materials. NH3 TPD shows that strongly binding Bronstead acid sites are present on the ex-NH4+ materials and H+-treated parent zeolites while Urea TPD shows that the mode of decomposition of urea differs as a function of initial zeolite counter-ion. Urea TPSR shows that the reaction between adsorbed urea and gaseous NO/O-2 is related to [Fe]. It is proposed that the decreased activity of the ex-NH4(+) catalysts in the SCR-urea reaction is due to a less favourable mode of decomposition over these catalysts. Furthermore it is suggested that the Bronstead acidity plays some part in this less favoured decomposition. (c) 2005 Elsevier B.V. All rights reserved.