Ore sample, pretreated at 650 ℃, was decomposed with aqua regia. Gold in the sample solution was then pre-concentrated by adsorbing with polyurethane foam plastic, released with thiourea solution, and determined by inductively coupled plasma-atomic emission spectrometry and flame atomic absorption spectrometry. Based on the characteristic of the copper matte and sinter containing copper, the effects of sample dissolving condition, matrix effect and interference of coexisting elements were investigated. The accuracy, precision and detection limit were discussed. The results of test show that both of the two methods were suitable for determining the contents of gold in copper matte and sintered copper material.