Abstract: ²³⁹Pu in many soil samples should be analyzed to survey radioactive pollution level in nuclear facilities and its affinity environment efficiently. In order to input the opt conditions for column experiment, the experiments of the static adsorption coefficient of ²³⁹Pu to solid phase extraction disk with different contact time, concentration of HNO₃ and different temperature were carried out. The chemical procedure for the rapid separation and determination of ²³⁹Pu in soils had been formulated, which using solid phase extraction disk (Empore^TM Anion Exchange-SR) as extraction material and liquid scintillation spectrometry counting as measurement. In the procedure, soil sample usage was 10 g, and were leached by 8 mol/L HNO₃, the chemical recovery of the procedure was about 78.9%, and the minimum detectable concentration was 3.7 Bq/kg. It took less than 3 hours once and the presence of ¹³⁷Cs, ⁹⁰Sr-⁹⁰Y and natural uranium, ²⁴¹Am, ⁹⁹Tc did not interfere with the procedure, owning high DF of them. The procedure can be used extensively in determination of ²³⁹Pu in soils.