Abstract: In order to improve the accuracy of determination of copper in copper tailing,the microwave digestion was used in preparation of sample solution,and the standard addition calibration technique was used in the flame atomic absorption spectrometry(FAAS) to reduce effectively interference of coexistent elements in real sample solution.At first,the copper concentration and the linear ranges were preliminarily determined by standard curve method.Then,the amount of standard addition was confirmed.According to analytical results,we found that the correlation coefficients of method were 0.9998 in standard addition calibrating curves.The recovery and the RSD of method is in range of 100.75%～103.00% and 0.44%～3.7% respectively.The test showed that the proposed method is simple and rapid and reliable.