Abstract: This paper established a qualitative and semi-quantitative analysis detection method of the micro-arc oxidation titanium and titanium alloy layer of Na, Si, P, S and other impurity elements by X-ray fluorescence. At the same time, from the angle of technological process, we analyzed the impurity element types and sources, and verify the reliability of this method. The locking plates superficial layer contained P element, the average was 1.01%. The occipital plate superficial layer contained Si element, the average was 1.39%. The advantages of this detection method were convenient and fast, and the sample without pretreatment and so forth. So this detection method was the ideal method of qualitative and semi-quantitative analysis to the micro-arc oxidation of surgical implants.