Polyacrylate and hydroxamate flocculants are commonly used to aid solid-liquid separation of bauxite residue from pregnant liquor in the Bayer process. This study presents the direct examination of the bauxite residue flocculation with polyacrylate and hydroxamate flocculants, using the focussed beam reflectance measurement (FBRM) probe to monitor aggregate dimensions. The key difference between polyacrylate and hydroxamate flocculation was found to be the way the aggregates developed post-shear, with hydroxamate flocculation exhibiting a greater degree of post-shear flocculation. Polyacrylate aggregates were found to be more dense and shear resistant, while the hydroxamate aggregates exhibited greater fines capture and lower solids in the supernatant. The solids remaining in the supernatant after flocculation were found to differ for each flocculant, with the polyacrylate system having relatively more coarse particles within the solid and the hydroxamate system being relatively finer and more iron rich. The observed results are discussed in terms of the different way in which each polymer is considered to adsorb onto the residue material. (C) 2008 Elsevier B.V. All rights reserved