Crystallization of L-ornithine-L-aspartate (LOLA) by drowning out was investigated using methanol as an antisolvent for the production of the anhydrous form of LOLA. Spherical agglomerates of LOLA crystal were prepared by precipitation in a semibatch crystallizer. It was found that the size of LOLA agglomerates was influenced by the experimental conditions such as the temperature, feed concentration, feeding rate and agitation speed. The increase in the agglomerate size of LOLA from 40 μm to 180 μm was observed by increasing temperature and decreasing agitation speed and feeding rate.