This document describes a method for measuring 238Pu and 239 + 240 isotopes in soil by alpha spectrometry samples using chemical separation techniques. The method can be used for any type of environmental study or monitoring. These techniques can also be used for measurements of very low levels of activity, one or two orders of magnitude less than the level of natural alpha-emitting radionuclides. The test methods described in this document can also be used to measure the radionuclides in sludge, sediment, construction material and products following proper sampling procedure[2][3][4][5][7][8]. The mass of the test portion required depends on the assumed activity of the sample and the desired detection limit. In practice, it can range from 0,1 g to 100 g of the test sample.