Thermogravimetric analysis (TGA) was used to evaluate microstructural evolution and binder segregation during drying of particulate suspensions of submicrometer alumina. The addition of 2 and 4 wt.% poly(vinyl alcohol) (PVA) binder decreased the evaporation rate by similar to 12 and similar to 20%, respectively, during the constant rate drying period. Increasing the PVA molecular weight (MW) extended the drying time also. At 4 wt.% addition, an acrylic emulsion binder did not affect the drying behavior but at 2 wt.% addition, the initial evaporation rate decreased by approximately 24%. It is shown that the TGA can be used to determine the drying stages of a particulate suspension during drying.