Abstract: This paper covers the simultaneous determination of Fe, Zn, Ca, Mg and Cu in the milk sample by inductively coupled plasma atomic emission spectrometry. The milk sample was digested under high pressure with nitric acid and hydrogen peroxide in the tightly sealed microwave system, which is under controlled through the advanced procedure, then the sample solution in the PTFE vessel was transferred to a 25mL volumetric flask after cooling. The above mentioned metal iron were determined simultaneously by inductively coupled plasma atomic emission spectrometry, in which the operation conditions were determined through optimum test. The process of test was not only simple but test time was saved due to amount element were determined at the same time. Precision test and recovery test indicated the results of test by this method is believable. The proposed method has been applied satisfactorily to the analysis of imported milk powder.