Abstract
The separation of lanthanides from calcium compounds in the form of oxalates from hot nitric acid solutions of Ln(NO3)3 and Ca(NO3)2 with the insertion of oxalic acid and a Ln2(C2O4)3 · nH2O crystal seed was studied by mass-spectrometric, atomic emission, microscopic, X-ray diffraction, and fluorescence analyses. The produced single-phase precipitate was found to contain an isomorphic impurity of La–Sm oxalates, while calcium oxalate remained in the hot nitric acid solution (95°С) saturated with oxalic acid. This facile and efficient method provides Ln2(C2O4)3 · nH2O (n = 9.5 mol) in one step in a 80.1 rel. % yield, with the major phase being at least 99.4 wt %. The unit cell parameters were determined for the crystals of the isomorphic lanthanide oxalate mixture: a = 11.243(2) A, b = 9.591(2) A, c = 10.306(2) A; α = γ = 90°, β = 114.12(1)°; Z = 2; V = 1013.7(5) A3.
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