Based on studies on the chemical phase-analysis methods for rubidium in some mineral ores from Hunan Shizhuyuan mine, the occurrence state and mass fraction of rubidium in minerals were preliminarily determined by using inductively coupled plasma optical emission spectrometer (ICP-OES), combined with XRD, SEM, electron probe and MLA. After the phase separation of rubidium was determined and appropriate selective reagents and reaction conditions were selected, rubidium in mica, rubidium in fluorite, rubidium in silica-aluminum oxide, rubidium in feldspar, and rubidium in insoluble minerals were all analyzed. Then, a method for rubidium phase analysis was developed. It is found that this analysis method is characterized by lower detection limit, high precision, good reproducibility, wider linear range, and simple and rapid process. Based on an experiment on the interference of alkali metallic elements in minerals, reasonable analysis methods were selected according to different concentrations of K, Na and Li, so as to obtain accurate results with less interference.