ABSTRACT The processing and control of liquid radioactive waste (LRW) in nuclear power plants (NPP) are critical aspects of nuclear energy management. This study details the principles of the methods and the measuring instruments used for control, and highlights the features and advantages of chemical and radiometric control in radioactive waste processing. The purpose is to systematize and analyze the results and methods used for chemical and radiometric monitoring, treatment technologies, and adherence to regulatory standards. The paper presents findings from an operating NPP with water–water energy reactor power units, showcasing the novelty of systematizing monitoring methods at each stage of LRW processing and ensuring compliance with regulatory standards. Moreover, the chemical and radiometric indicators in the LRW were analysed, which provides insight into the dynamics of waste processing and classification. In addition, the application of Pearson correlation analysis allowed us to identify the relationships between chemical and radiometric indicators in the LRW, which provides valuable information for waste management practices. The selection of appropriate chemical and radiometric methods is crucial given the complexity of LRW characteristics, making this study relevant for enhancing LRW monitoring and management practices.