Sodium aluminate liquor was diluted and neutralized with water and oxalic acid in the presence of surface-active polymers polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) and sodium carboxymethylcellulose (NaCMC). Dynamic light scattering experiments showed that the final precipitate had diameters between 80 – 300 nm when precipitated in the presence of PVP, and 600 – 800 nm when precipitated in the presence of NaCMC. The initial sols prepared using oxalic acid without surfactant had diameters of 200 – 300 nm. Scanning Electron Microscopy, SEM, Energy Dispersive Analysis by X-rays, EDAX, and X-ray diffraction were used for imaging, chemical and structural analysis of the final dialyzed particles. Transmission Electron Microcopy, TEM, images of the sols trapped and dried between nitrocellulose membranes showed that the initial particles were nearly spherical and bimodal in particle size. Larger particles had diameter of about 176 nm but were not pure solid alumina. A small fraction of initial particles had diameters much smaller than 176 nm. The discrepancies between initial and final precipitates indicate a complex precipitation pathway.