Abstract: In order to suit for the needs of analysis of different samples by micro-X-ray fluorescence spectrometer focused by polycapillary X-ray optics, several kinds of micro-X-ray fluorescence spectrometers were designed in this paper. The laser displacement sensor (LDS) was used to automatically control the distance between the irradiation spot of sample and exit of polycapillary X-ray optics so that it can decrease the measured error of irregular surface of archaeological object. Due to the lower transmission efficiency for the X-ray with energy for more than 25 keV, polycapillary X-ray optics could be used for the non-destructive analysis of ancient colored glaze that contains high concentration Pb. The elemental mappings of K, Ca, etc. in a grain rice were scanned by the micro-X-ray fluorescent spectrometer with the high power X-ray source. In the same time, a RMB 5 jiao coin was taken for example, and the methodology of dispersive energy of micro-X-ray diffraction was researched. The results show that the micro-X-ray fluorescent spectrometer can be widely used for the analysis of biological sample and archaeological object.