In this study, Taguchi robust design as a statistical route was utilized to optimize the variables of spraying in non-solvent process in order to achieve KClO 4 nanoparticles. The experimental factors of the spraying in non-solvent technique, which may be effective in KClO 4 particle size, were optimized efficiently via Taguchi method. The procedure operating conditions, i.e., KClO 4 concentration, solvent ratio, non-solvent identity, and spray steps, were considered at triple levels. The role of these operating conditions on the size of resulted KClO 4 particles was evaluated quantitatively by analysis of variance (ANOVA). It was found that the particle size of KClO 4 prepared by spraying in non-solvent technique might be adjusted efficiently by tuning the main parameters at the corresponding optimum level. Moreover, the optimal conditions for the preparing of KClO 4 nanoparticles via the studied method were proposed. The ANOVA exhibited that 3 % (w/v) as KClO 4 concentration, CHCl 3 as type of nonsolvent, solvent to non-solvent ratio of 1:6, and single-step spraying are optimal conditions for the production of KClO 4 nanoparticles by spraying in non-solvent. Experimental data revealed that at optimum conditions of the process, the average particle size of produced KClO 4 is about 41 nm. Meantime, KClO 4 nanoparticles were prepared by supercritical carbon dioxide anti-solvent process for comparison. It was found that the size of the produced KClO 4 particles is about 55 nm.