We have studied the micro x-ray fluorescence (XRF) and 2D- or 3D-XRF analysis in the laboratory by using polycapillary optics. A confocal 3D micro-XRF instrument was applied for solid/liquid interface analysis. 2D elemental maps of x-ray fluorescence for the solid surface of an Fe plate after Cu was deposited by chemical plating were obtained. The 2D images could be taken in the solution. This result suggests that this 3D micro-XRF method is useful for in-situ monitoring of chemical reactions on solid-liquid interfaces. Furthermore, we have reported a new application of polycapillary x-ray optics. Two independent straight polycapillary optics were arranged between the sample and an x-ray energy dispersive detector. X-ray fluorescence emitted from the sample was collimated by the first capillary, and then it was introduced into the second capillary. By adjusting the angle between two capillary optics, only the x-rays totally reflected on the inner wall of the second capillary could be detected by the x-ray detector. This result suggests that we can use these polycapillary optics for x-ray energy filtering optics.