A new solvent-impregnated resin (SIR) was constructed using Amberlite XAD-2 and 3-hydroxy-2-naphthoic acid (3H2NA). The SIR was applied for stepwise extraction of Th(IV) and U(VI) from the coexistence ions dissolved in aqueous media at pHs of 3.0 and 7.0, respectively. The U(VI) and Th(IV) ions adsorbed on the minicolumn were consecutively eluted with 0.5 M and 4 M HCl solutions. They were then measured by Arsenazo III at their maximum absorption wavelengths. The characteristic parameters for the successful separation of these ions from the aqueous media were investigated. The SIR showed excellent reproducibility during the 800 subsequent extraction cycles.