Abstract
X-ray absorption fine structure (XAFS) measurements have been made at the Cs LIII absorption edge on 1) 0.04 M concentrations of CsBr in 0.04 M Dibenzo-18-Crown-6 ethers (D18C6) in acetonitrile solution, and 2) crystalline CsBr, CsCl and CsF powders that were used as standards. Due to the many difficulties associated with obtaining high quality XAFS data on these systems, a custom-manufactured 5 mil thick Sc foil was used in conjunction with a Soller slit assembly to improve the XAFS signal to noise ratio by almost a factor of 6. XAFS analyses of the Cs-D18C6 solution show the presence of a 1:1 Cs-D18C6 complex with the Br counter-ion still in contact with the Cs atom. These results are consistent with previous wet chemical studies. The choice of a heavy backscattering Br anion reduces the error in determining the presence of a single backscattering counter ion among the lighter backscattering oxygen and carbon atoms of the crown ether complex. The ability of XAFS to directly probe the anion contact pairing to Cs complexed to a macrocycle opens many exciting avenues for improving extraction methodologies.
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Kemner, K.M., Hunter, D.B., Elam, W.T., Bertsch, P.M. (1996). Cesium XAFS Studies of Solution Phase Cs-Ionophore Complexation. In: D’Amico, K.L., Terminello, L.J., Shuh, D.K. (eds) Synchrotron Radiation Techniques in Industrial, Chemical, and Materials Science. Springer, Boston, MA. https://doi.org/10.1007/978-1-4615-5837-8_10
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DOI: https://doi.org/10.1007/978-1-4615-5837-8_10
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