An experimental study was conducted to assess the solid hold-up distribution in a fluidized bed of zirconia and aluminum nanoparticles. For this purpose, two different techniques, radioactive densitometry and fibre optic measurement, were used. The results showed that while the fluidization of these nanoparticles occurs in the agglomeration state, it performs homogeneously in terms of phase concentration. This matter is important especially when a polymerization reaction should take place uniformly on the surface of nanoparticles, where the monomer is the fluidizing gas. Both techniques presented uniform solid hold-up distribution over the cross-section, although the fibre optic method overestimated the overall solid concentration, which was obtained based on bed expansion results. The radioactive densitometry was, however, capable of properly predicting the phase concentration within the bed according to the bed expansion observation. Finally, the effect of bulk density on the fluidization of nanoparticles was discussed by comparing the fluidization of different types of particulate materials.