Fluorometric determination of samarium and europium in rare earth minerals with β-diketoneternary complex

This communication reported the optimum conditions for the fluorometric determination of these ions, and the method was adopted in the simultaneous determination of samarium and europium in xenotime and monazite minerals. From the experimental results on the effect of diverse ions and the extraction pH of the aqueous phase, it became clear that TTA-TOPO hexane method was the best system for the determination of samarium and europium because of the highest fluorescence sensitivity of the ternary complex, and also because the lower extraction pH eliminated the effect of diverse ions. Moreover, the very high detection limit (2 ppb) of Sm was achieved by the use of a red sensitive photomultiplier. Which was used at 644 nm, and that of Eu (0.02 ppb) at 614 nm. The procedure was established as follows: The rare earth minerals (xenotime, monazite) sample was treated with hot conc. H2SO4 and twice precipitated with 0.5 mol dm-3 oxalic acid (pH was adjusted to 2.0 -- 2.2). Then the precipitate was filtered and ignited to give the rare earth oxide. Fifty milligrams of the oxide was dissolved in HCl and diluted with water in order to obtain the solution containing 5 μg cm-3 rare earth oxide. An aliquot of the solution ((1.0 -- 3.0) cm3) was adjusted to pH 5.5 with sodium acetate and shaken with 1 x 10-4 mol dm-3 TTA- 2 x 10-2 mol dm-3 TOPO hexane solution. Then the fluorescence intensity of the organic layer was measured at 644 nm for Sm and 614 nm for Eu. In this procedure, the recovery of Sm and Eu was found to be about 96%. Xenotime contained 0.70% of Sm and 0.004% of Eu, and monazite contained 1.84% of Sm and 0.003% of Eu. (J.P.N.)