Two methods of analyzing particles were interfaced to a low pressure chemical vapor deposition (CVD) reactor to evaluate whether or not particles were formed in the gas phase during the growth of aluminum films using tertiaryamine complexes of alane. A laser light scattering particle counter was used to detect large (>200 nm) particles in real time and established that the appearance of particles corresponded to the flow of precursor into the CVD reactor. A particle impaction system was used to collect particles (>20 nm) for analysis using analytical electron microscopy and electron diffraction. This established that the particles were crystalline aluminum and that the particle sizes ranged from 20–700 nm. The median size was 85 nm.