Rhenium is one of the rarest elements in the Earth’s crust with an average concentration of 1 × 10−7%. It has been widely used in various industrial fields due to its special physical and chemical properties. The rhenium in nature is precious but scattered, causing difficulty in accurate deter-mination of its content. The great industrial demand of rhenium requires its production in large amounts. This stimulates the development of analytical methods for its control in various mineral raw materials as well as in different technological products, including, electro stripping voltam-metry, spectrophotometry, X-ray fluorescence analysis spectrometry, ICP-AES and ICP-MS. ICP-MS has the advantages as follows: Low detection, little matrix effects, simple spectral lines, simulta-neous... determination of many elements, wide linear range and rapid determination of isotope ratios. In geology, it is used to detect trace elements and ultratrace elements in rock ore and groundwater. With the development and application of large-scale precise instruments, the pretreatment, separation, enrichment and determination methods of samples containing rhenium had some progresses. In this study, the research progress on separation and determination method of rhenium in ore samples in recent years was reviewed. The application of ICP-MS in the detection of rhenium was focally introduced. The merits and demerits of different methods were compared. The development direction on separation and analysis method of rhenium was prospected.