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• W2186751106 abstract "Introduction The Rh-Sn-Cl complex in HCl solutions has attracted interest in metal separation studies, since the addition of SnCl2 to Rh in HCl solutions markedly accelerates the Rh extraction from the aqueous to organic phases [1]. However, detailed structural parameters of the Rh-Sn-Cl complex in solution have been limited. This work investigated the coordination structure of the Rh-Sn-Cl complexes in HCl solutions based on Rh and Sn K-edge XAFS measurements. Experimental Sample solutions were prepared by adding SnCl2 to Rh in 3 M HCl solutions ([Rh]=0.1M). All of the XAFS spectra were measured in transmission mode at the NW10A station in the PF-AR. The experimental data were analyzed by WinXAS Ver. 2.3 [2] and fit using theoretical phase and amplitudes calculated from the program FEFF 8.2 [3]. The amplitude reduction factor, S0 2 was refined by the curve fits to the Rh and Sn solutions; their coordination number is known to be six. These values were found to be 0.89 for the Rh and 1.0 for the Sn and held constant using them during the fits of the Rh and Sn K-edge XAFS, respectively. The coordination number, CN, the bond distance, r, Debye-Waller factor, σ, and the shift in threshold energy, ΔE0, were allowed to vary in the fit. Results and Discussion Figure 1 shows the raw k-weighted Rh and Sn K-edge EXAFS spectra and the corresponding Fourier transforms (FT) of the Rh-Sn-Cl complex in 3 M HCl solutions ([Sn]/[Rh] = 1.0, 2.8). In the FT of the Rh K-edge EXAFS (1, 2), two significant peaks appeared at ~1.9 A and ~2.3 A. The peak at ~1.9 A corresponds to the Rh-Cl correlation. This peak shrinks with an increase in the [Sn]/[Rh] value (1.0→2.8), while the peak at ~2.3 A, related to the Rh-Sn correlation, increases. This means that the Cl in the inner sphere of Rh is replaced by the Sn. The obtained CN values (2.7(3) Cl and 2.7(5) Sn) at [Sn]/[Rh] = 2.8 are in good agreement with the Sn NMR result [4], which showed that the [RhCl3(SnCl3)3] 3is dominant at [Sn]/[Rh] ≈ 3. The curve fits to the Sn Kedge EXAFS spectrum indicate the presence of 1.1(3) Rh at 2.465(14) A and 3.2(5) Cl at 2.332(4) A. This verifies that the Sn predominantly exists as the [RhCl6-x(SnCl3)x] 3species (x ≤ 3) at [Sn]/[Rh] ≤ 3 [4]. The bond distance of the Sn-Rh correlation (2.465(14) A) is very similar to that obtained from the Rh k-edge EXAFS (2.453(13) A), indicating that the fitting quality is high." @default.
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• W2186751106 date "2007-01-01" @default.
• W2186751106 modified "2023-09-26" @default.
• W2186751106 title "Rh and Sn K-edge XAFS analysis of Rh-Sn-Cl complexes in hydrochloric acid solutions" @default.
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