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A novel mesoporous silica-coated ferrocyanide (MSCFC) composite was successfully synthesized and evaluated as a dual-function material for simultaneous removal of 137 Cs + cations and 99 TcO 4 − anions from aqueous solutions. Sorption behavior of both radionuclides on MSCFC under different experimental conditions has been studied using a batch technique. Results revealed that about 100% of 137 Cs + and 97% of 99 TcO 4 − were removed by MSCFC in the pH ranges of 2.2–12.4 and 4.1–9.5, respectively. Sorption kinetic data were analyzed by pseudo-first-order, pseudo-second-order and intraparticle diffusion kinetic models, while Langmuir and Freundlich models were applied for the sorption isotherms. The maximum sorption capacity of MSCFC for radiocesium was determined and compared with other reported sorbents. Applicability of the coated ferrocyanide for simultaneous removal of 137 Cs + and 99 TcO 4 − from low-level liquid radioactive waste (LLLW) was also tested, and the data revealed that 99.91% and 98.34% were removed from 137 Cs + and 99 TcO 4 − , respectively. It is concluded that MSCFC exhibits excellent efficiency for simultaneous removal of the mixed radionuclides with different charge from LLLW. [ABSTRACT FROM AUTHOR]