It is very important to minimize the waste generation for decontamination of the reactor coolant system in a nuclear facility. As an alternative to commercial decontamination technologies, an inorganic acid chemical decontamination (SP-HyBRID) process can be effectively applied to the decontamination because it can significantly reduce the waste generation. In this study, the decontamination of a contaminated reactor coolant pump shaft from a nuclear facility was conducted using the SP-HyBRID process. First, equipment for a mock-up test of the decontamination was prepared. Detailed experimental conditions for the decontamination were determined through the mock-up test. Under the detailed conditions, the contaminated shaft was successfully decontaminated. The dose rate on the shaft surface was greatly reduced from 1400 to 0.9 μSv/h, and the decontamination factor showed a very high value (>1500).