Abstract: Based on nuclear materials accounting evaluation and considerable techniques research of spent fuel reprocessing facilities, in order to fulfill the requirements of nuclear material accounting & control and improve the timeliness of abnormal operation of spent fuel reprocessing facilities, near-real-time accounting technology for nuclear materials and process monitoring technology in Purex process was investigated and analyzed in this paper. The primary measuring equipment and advanced instruments, as well as the structure of integrated data information system and its operation and maintenance requirements were also addressed out. Combining with the traditional methods of material balanced area and key measurement points, aiming at the significance quality of nuclear materials, adding suitable process monitoring and strategic observation points, adopting model development and verification, analyzing methods optimization and evaluation, information management system integration technology, and overall management and control of Purex process setting in the whole life cycle of reprocessing facilities, near-real-time nuclear material accounting and control will be achieved in equipment, pipes, valves, tanks, and so on.