Finding variations in unitary operations in the synthesis and drying method, applied to the obtainment of Nb2O5/carbon xerogel, is the aim of in the present study. Feed (dispersion) preparation led to some variations in unit operations. Dispersion was spray dried at 115 ºC, 1.25 m 3 /min and 0.15 L/h; it presented 38. 024.4 kg/m 3 . Moisture content in the product reached 0.89 % dry basis; particle and tapped density reached 5,413.3 and 287.9 kg/m 3 , respectively; and spherical particle size ranged from 1 to 21 μm.