The scintillating polymer inclusion membrane (S-PIM) was developed for preconcentration and determination of α-emitting actinides from aqueous solution. The preparation of S-PIM involved physical immobilization of an extractant bis(2-ethylhexyl)phosphoric acid, primary scintillator 2,5-diphenyloxazole, and secondary scintillator 1,4-bis(2-methylstyryl)benzene in the plasticized cellulose triacetate matrix. The S-PIM was found to be effective for the quantitative sorption (94-98%) of trivalent lanthanides/actinides ( 1 4 7 Pm, 1 5 4 Eu and 2 4 1 Am), tetravalent actinides (Pu(IV)) and hexavalent actinides (U(VI)) from the aqueous solutions whose acidity had been adjusted to pH 2.5, 1.0 and 0.25mol/L, respectively with dilute HNO 3 . The interference of β-emitting lanthanides, in preconcentration and determination of α-emitting actinides using S-PIM, were also studied. The α-scintillation counting efficiency in the S-PIM was found to be 92-95% after discriminating the background noise. However, β-scintillation counting efficiency was found to be in the range of 12-25% depending upon the energy of β-particles. It was observed that β-scintillation pulses from 1 4 7 Pm and 1 5 4 Eu could be discriminated based on pulse height analysis. Thus, α-activities of the actinides sorbed in the sample of S-PIM could be directly measured in the presence of β-emitters by scintillation counting. However, the α-scintillation counting efficiency was reduced to 38% after discriminating β-scintillation pulses in the S-PIM. The preconcentration ability of S-PIM was examined in tap water and seawater spiked with 2 4 1 Am. The total α-activity of 46Bq (present in 100mL) could be preconcentrated and measured from tap water using S-PIM.