Abstract: Plutonium is one of the most concerned environmental contaminated nuclides in the context of radioactive survey and nuclear emergency monitoring. The determination of plutonium in environmental soil samples involves three analytical steps, sample digestion, chemical separation and measurement. In order to improve the efficiency of the digestion and separation, the method for microwave-assisted digestion of soil sample and chemical separation of plutonium was studied. A procedure combining microwave assisted digestion for soil sample dissolution, anion exchange for chemical separation of plutonium and inductively coupled plasma mass spectrometry (ICP-MS) for plutonium content measurement was developed and tested. The recovery for the procedure is more than 99% for ²³⁹Pu in 5 g soil sample extracted by 6 mol/L HCl with the ratio of 4∶1 mL/g to 5∶1 mL/g between reagent volume and soil weight. Meanwhile, over 94% of ²³⁹Pu is recovered when 1 g soil sample is totally digested by the mixtures of HF, HNO₃ and HCl, and in which the concentration of HF is 13.2 mol/L. The concentration of ²³⁹Pu in IAEA-375 soil reference material determined by this procedure is consistent with the certified value. A detection limit of 84 mBq/kg is obtained for the procedure by analyzing ²³⁹Pu in 1 g soil sample.