Due to the impact of lead-zinc mining and smelting, the soil of lead-zinc orefield and nearby areas has been widely polluted. Moreover, theconcentration of lead and zinc was high, and their concentration range was wide.Furthermore, the impact of overlapping interference between low concentration Asand high Pb was serious, and the lack of soil standards of lead and zinc was alsoa problem. According to these problems, the present work studied an effectivesolution to setting up the EDXRF analysis of Pb, As, Cd, Cu and Zn of soil onlead-zinc orefield. The measurable concentration of Pb was 4.4-23 600 μg?g-1,and that of Zn was 7.0-39 400 μg?g-1. The detection limit was 1.1 μg?g-1 forPb and 0.9 μg?g-1 for Zn. The average relative error was 7.6% for Pb and 6.2%for Zn.fluorescence (EDXRF)