The unique chemical, electromagnetic and mechanical properties of nanosize particles have generated a demand for a supply of uniform and well characterized particles to develop new applications. Although flame synthesis has been successfully scaled up to commercial production of micron and sub-micron particulates, control of nano-particle size, shape, phase composition, and aggregate size is difficult because flame temperature, residence time and precursor loading all influence these parameters. A Fourier transform infrared spectrometer was interfaced to a diffusion flame reactor to measure these parameters during the production of TiO 2 and SiO 2 by oxidation of TiCl 4 and SiCl 4 , respectively. Rayleigh scattering theory was used to generate spectra to match measured infrared absorbance spectra based on particle size, shape and number density. The approach successfully monitored changes in particle size and shape as a function of process conditions. Theoretical spectra matched to in-situ measurements identified shapes, ranging from spheres to needles. These shapes were confirmed by post -process transmission electron microscopy.Recently, nanosize particles (diameters below 100 nm) have demonstrated enhanced properties in a number of applications. For example, ceramic layers formed from nano-particles demonstrate improved adhesion, ductility, and mechanical strength (7). Changes in chemical, physical and mechanical properties compared to bulk materials, such as a lower melting point, are attributed to the relative number of atoms or molecules on the surface of the particle becoming comparable to that inside the particle (7). The predominant methods of preparing these particles are based on aerosol processes, such as flames (2), tube furnaces (3), gas-condensations (¥), thermal plasmas (5), etc., designed to provide sufficient temperature to promote gas-to-particle conversion. However, until now, only flame 170