Abstract: The sample (2.00 mL) was decomposed with 10 mL of hydrochloric acid, and nitric acid 3 mL, evaporeted to 2-3 mL. Then 2 mL of 100 g·L-1 tartaric acid solution were added and the solution was diluted to 100 mL with HCl(5+95) solution, and ICP-AES was applied to the determination of stibium, bismuth, cobalt, nickel and arsenic in the sample solution. Analytical spectral lines of 206.836, 223.061, 228.615, 231.604, 193.696 nm were chosen for the determination of Sb, Bi, Co, Ni and As respectively. Linear relationships between values of emission intensity and mass concentration of the 5 elements were kept in definite ranges, with detection limits (3s) in the range of 0.005-0.130 mg·L-1. The proposed method was applied to the analysis of copper electrowinning solution, giving results in consistency with those given by FAAS. Values of recovery found by standard addition method were in the range of 95.8%-108%, and values of RSD′s (n=11) in the range of 0.70%-6.4%.