Perovskitic mixed oxides prepared through flame-spray pyrolysis possess a good stability in high-temperature application, viz. the catalytic flameless combustion of methane. Some preparation operating parameters are here analysed, such as O-2 pressure drop along the spraying nozzle, O-2 discharge velocity and flow rate. These parameters have been correlated with specific surface area, activity and durability of the prepared samples, as well as with flame temperature, varied by using different fuel mixtures. It was found that specific surface area increases with increasing O-2 velocity and flow rate and with decreasing the combustion enthalpy of the solvent mixture. This reflects on both activity and durability of the catalyst. (c) 2006 Elsevier B.V. All rights reserved.