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Thermogravimetric analysis (TGA) is investigated for determination of the OH surface density (OH/ nm 2 ) and carbon content of silica and titania powders made by flame aerosol and sol-gel processes. It is shown that it is possible to distinguish between physically adsorbed and chemically bound water and to rapidly determine the OH surface density even of small powder samples (<0.2 g) by TGA calibrated with LiAlH 4 titration data. The high accuracy of the OH surface density determination by TGA is confirmed further with additional LiAlH4 titration data of silica powders and by comparison with the specifications of commercially available silica Aerosil and titania P25 powders. Furthermore, by connecting a CO2 sensor or a mass spectrometer to the TGA balance, it is possible to verify the carbon content and determine other components (organic residues) of the powders. Thereby, it is shown that flame-made powders have high purity while the preparation conditions of sol-gel powders greatly affect their purity. At a water-toprecursor ratio of 1000:1, no organic residues are detected in sol-gel powders, while lower ratios result in residues in the product powder from the precursor, solvent, or catalyst.

Control and quanti®cation of particle size distribution is of importance in the application of nanoscale particles. For this reason, polydispersity in particle size has been the focus of many simulations of particle growth, especially for nanoparticles synthesized from aerosols such as fumed silica, titania and alumina. Single-source aerosols typically result in close to a log-normal distribution in size and micrograph evidence generally supports close to spherical particles, making such particles ideal candidates for considerations of polydispersity. Small-angle X-ray scattering (SAXS) is often used to measure particle size in terms of the radius of gyration, R g , using Guinier's law, as well as particle surface area, S/V, from the Porod constant B and the scattering invariant Q. In this paper, the uni®ed function is used to obtain these parameters and various moments of the particle size distribution are calculated. The particle size obtained from BET analysis of gas adsorption data directly agrees with the moment calculated from S/V. Scattering results are also compared with TEM particle-counting results. The potential of scattering to distinguish between polydisperse single particles and polydisperse particles in aggregates is presented. A generalized index of polydispersity for symmetric particles, PDI = BR g 4 /(1.62G), where G is the Guinier prefactor, is introduced and compared with other approaches to describe particle size distributions in SAXS, speci®cally the maximum-entropy method.

An overview of recent advances in the synthesis of nanoparticles by flame aerosol processes is given. In flame processes with gaseous precursors emphasis is placed on reactant mixing and composition, additives, and external electric fields for control of product characteristics. Thermophoretic sampling can monitor the formation and growth of nanoparticles, while the corresponding temperature history can be obtained by non-intrusive Fourier transform infrared spectroscopy. Furthermore, synthesis of composite nanoparticles for various applications is addressed such as in reinforcement or catalysis as well as for scale-up from 1 to 700 g/h of silica-carbon nanostructured particles. In flame processes with liquid precursors using the so-called flame spray pyrolysis (FSP), emphasis is placed on reactant and fuel composition. The FSP processes are quite attractive as they can employ a wide array of precursors, so a broad spectrum of new nanosized powders can be synthesized. Computational fluid dynamics (CFD) in combination with gas-phase particle formation models offer unique possibilities for improvement and possible new designs for flame reactors.

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