The determination of /sup 90/Sr in soil by tri-n-butyl phosphate (TBP) is often interfered with iron which is always present in soil sample. Based on the method given by the U.S. Environmental Protection Agency, HClO/sub 4/ is added to remove iron ions while the soil sample is analyzed with TBP. The effect of different concentrations of HClO/sub 4/ on extraction yield of iron and chemical yield of yttrium is investigated. The experimental results show that 2N HClO/sub 4/ is the optimum concentration. The chemical yield of yttrium can reach about 60 percent, and all iron ions can be removed. This method has successfully been applied to analyze the soil samples taken from the site of the nuclear power plant in North Taiwan.