A novel macroporous silica-based 2,6-bis(5,6-dibutyl-1,2,4-triazine-3-yl)pyridine (BDBTP) material, BDBTP/SiO2-P, was prepared through impregnation and immobilization of BDBTP and octanol into the pores of the SiO2-P particles. The adsorption of 10 typical fission and nonfission elements contained in highly active liquid waste (HLW) onto BDBTP/SiO2-P was investigated by examining the effect of contact time and the HNO3 concentration in the range of 0.1-5.0 M. Pd(II), a weak Lewis acid and an electron-pair acceptor, was strongly complexed with nitrogen, a weak Lewis base and an electron-pair donor. BDBTP/SiO2-P showed excellent adsorption ability and high selectivity for Pd(II) over all the tested metals. The separation of Pd(II) from a simulated HLW was performed by BDBTP/SiO2-P packed column. Pd(II) was effectively eluted with 0.2 M thiourea and separated from the others. It demonstrated that in HNO3, application of the macroporous silica-based BDBTP/SiO2-P material in partitioning and recovery of Pd(II) from HLW is promising. (C) 2010 American Institute of Chemical Engineers AIChE J, 56: 3074-3083, 2010