A systematic study of salting-out precipitation is carried out to obtain the operational limits within which this precipitation method can be applied for the production of fines (mean particle size < 10 mum) with acceptable quality and productivity. The model substances: glycine and sodium chloride are salted-out from their aqueous solutions by using ethanol as antisolvent. The main operational parameter is the initial supersaturation of the solutions. It is shown that the smallest particles can be produced at the limits of the metastability domain determined by three optional process parameters: the initial solution concentration, the equilibrium solubility and the operational time. The product quality (crystallinity, polymorphic states, aggregation) and productivity considerably change with the operational conditions. (C) 2004 Elsevier B.V. All rights reserved.