In order to widen the scope of laser ablation/ICP-MS, calibration curves were prepared by using aqueous standard solutions instead of using standard solid materials. The decontaminated sample was irradiated by a Q-switched Nd/YAG laser beam (150mJ, 1064nm) for 220s and the ablated sample was trapped in 10ml of 0.1 moll^-1 nitric acid. More than 30% of the ablated sample were recovered in the solution as tiny particulates. The solution was directly introduced into the ICP-torch through a pneumatic nebulizer for the analysis by MS. Because the ionization efficiency of tiny particles was almost the same as that of aqueous ions, a series of aqueous standard solutions was employed for the preparation of calibration curves. Important experimental factors (e.g., argon flow rate, acidity of solution, and tube length) were studied in detail and optimized to obtain the highest signal intensity. The accuracy of the analytical data was significantly improved when the matrix element such as iron or zirconium was used as internal standard. The proposed method was applied to the determination of Cr, Ni, Mo, and Co in reference materials for steel and zircaloy. For the latter sample, laser irradiation was allowed to continue for 30min to ablate the sufficient amount of particles. The analytical results were in good agreement with the certified values.