The coordination states of multivalent dysprosium complexes of potassium bis(trifluoromethylsulfonyl) amide (K[NTf2]) were investigated by Raman spectroscopy. The concentration dependence of the deconvoluted Raman spectra was investigated for 0.23−0.45 mol kg−1 Dy(III), and a mixed sample of Dy(II)/Dy(III) (molar ratio 1/3), in K[NTf2]. Using conventional analysis, the solvation number, n, of the dysprosium complexes was determined to be 4.12 for Dy(II) and 5.09 for Dy(III). The electrochemical behavior of [DyIII(NTf2)5]2– in K[NTf2] melts was also investigated in this study. It is speculated that the first reduction peak at approximately +2.24 V probably corresponds to the formation of [DyII(NTf2)4]2–. Electrochemical analysis revealed that the reduction peak of [DyIII(NTf2)5]2– at approximately +0.81 V at 483 K is based on an electrodeposition reaction from [DyIII(NTf2)5]2– to Dy(0). The diffusion coefficient and activation energy of [DyIII(NTf2)5]2– in K[NTf2] melts were measured in the range 473–493 K by semi-integral and semi-differential analyses. Furthermore, the nucleation behavior of [DyIII(NTf2)5]2– was evaluated using chronoamperometry. The results indicated that the nucleation mechanism of Dy nuclei changed from instantaneous to progressive nucleation when the overpotential became more negative than the deposition potential of Dy(0). The electrodeposits were identified as mostly the metallic state by X-ray photoelectron spectroscopy.
We studied the stepwise formation constants (β) of water-soluble diglycolamide (DGA) and dioxaoctanediamide (DOODA) for the mutual separation of Ln in a solvent extraction system. TODGA (N,N,N',N'-tetraoctyl-diglycolamide) and DOODA(C8) (N,N,N',N'tetraoctyl-dioxaoctanediamide) exhibit opposite behaviors in extracting both light and heavy Ln through Ln-patterns. Metal complexes of two-and three-folding with watersoluble DOODA and DGA, respectively, were found, and each β value was calculated using distribution ratios. Taking β, their distribution ratio, D, and separation factor, SF, values into consideration, the suitable separation conditions (aqueous phase: 30 mM DOODA(C2) in 1 M HNO3; organic phase: 0.1 M TODGA in n-dodecane
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