Abstract: The method for determining concentrations of As, Sb, S, and Cu, Pb, Zn which are above 100 μg/g, within arsenic ore and stibium ore by inductively coupled plasma-atomic emission spectrometry(ICP-AES)with aqua regia digestion is reported in this paper. The experimental conditions such as placement time, solution acidity, and the influence of oxidant and complexing agents on As, Sb, S and the other elements were studied. The relative error (RE) was determined to be between -0.17% and 7.74% with a RSD (n=5) of <2% if the concentrations of As, Sb, S in the samples were in the range of 0.74-39.7%. However, the RE was from -2.5% to 4.79% and RSD(n=5) was <2% if the Sb concentration is lower than 100-500 μg/g. The RE was determined to be between -10.3% and 10.3% with a RSD(n=5) of generally less than 5% if the Cu, Pb and Zn concentrations were more than 100 μg/g. No accurate data were obtained for Cu, Pb and Zn if the concentrations were lower than 100 μg/g, limited by the large dilution factor of 1000. The accuracy and precision of the method were validated by reference materials.