Flame-assisted spray pyrolysis (FASP) is a versatile process for synthesis of nanoparticles from a broad choice of precursors and solvents. Water is an attractive solvent particularly for inexpensive inorganic precursors (e.g. metal nitrates) as it can effectively reduce the process cost. Furthermore when water usage is combined with a carbon-free fuel (e.g. H-2), nanoparticles can be made without forming CO2. Here such a FASP process is explored for synthesis of Bi2O3 and other oxide nanoparticles from aqueous precursor solutions. The flame temperature was measured by FTIR emission-transmission spectroscopy while powders were characterized by X-ray diffraction and N-2 adsorption. At low FASP fuel gas (H-2 or C2H2) flow rates or process temperatures, product powders had a bimodal crystal size distribution. Its large and small modes were made by droplet- and gas-to-particle conversion, respectively. Homogeneous Bi2O3 and CeO2 powders were obtained for sufficiently high flow rates of either C2H2 or H-2. Prolonged high temperature residence times promoted precursor evaporation from the spray droplets and yielded homogeneous nanostructured powders by gas-to-particle conversion. In contrast, FASP of aqueous solutions of aluminum nitrate yielded rather large particles by droplet-to-particle conversion at all fuel flows investigated. (C) 2012 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.