The solubility of acephate in ethyl acetate, acetone, 2-propanol, and dichloromethane from (292.90 to 327.60) K were measured using a laser-monitoring observation under the atmospheric pressure. The experimental solubility data were correlated with a semiempirical equation. The results show that the solubilities of acephate in these four solvents all increase with the increase of temperature and that dichloromethane is the best solvent for the crystallization process of acephate.