Aerosols of diameter smaller than 100 nm, usually are referred as nanoparticles or ultrafines, have received considerable interests lately as a source of building blocks to novel materials. However, our capabilities for charactering these materials are greatly limited by lack of appropriate diagnostic tools. The objective of this work is to develop new aerosol-based techniques for the characterization of nanoparticles and nanocomposites. The scope of this dissertation can be categorized in two ways. First, to provide knowledge of just how reactive a material is, we develop particle ion-mobility spectrometry and Single Particle Mass Spectrometry methods to probe the intrinsic size-dependent reactivity of individual metal particles. And second, the development of a new Time-of-Flight mass spectrometer (TOFMS) combined with a temperature jump (T-Jump) technique to study particle-particle reaction, and probe the reactivity of nanocomposite materials under combustion-like condition.