Effective and selective separation and recovery of the fission product palladium from high-level liquid waste are conducive not only to reducing its hazards to the public health and environment but also to alleviate the pressure on the increasing demand for natural palladium. Herein, the Pd extraction in an HNO solution with a nitrilotriacetate-derived triamide ligand NTAamide(-Oct) and the complexation between them were investigated. Using -octanol as a diluent, NTAamide(-Oct) demonstrated an excellent selectivity, strong extractability, and high loading capacity for Pd extraction. Combined with the results of single-crystal X-ray diffraction, Fourier transform infrared spectroscopy, electrospray ionization-mass spectroscopy, microcalorimetric titration, and slope analysis, the extracted complexes were determined as [PdL](NO) and [PdL][Pd(NO)] (where L denotes the NTAamide ligand) in 0.10 and 3.0 mol/L HNO solutions, respectively. The extraction model closely depended on the solvation state of Pd in the HNO solution. An ion-pair extraction model was proposed and discussed.
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