Abstract
Industrial sediments of calcium sulfate semihydrate obtained from industrial extraction phosphoric acid and containing 0.3–4.5 wt % of impurity La−Sm are investigated by energy-dispersive X-ray fluorescence analysis (XRFA) and a procedure for the quantitative determination of cerium lanthanides in the sediments is developed. The use of linear regression analysis of X-ray fluorescence spectra of multielement industrial samples and models of individual compounds NaLn(SO4)2 · H2O (cp grade) allowed us to resolve overlaps of spectral L-series lines for La–Sm, eliminate the background, and perform the regression assessment of line intensities of these elements. On this basis, we developed a procedure for the determination of La, Ce, Pr, Nd, and Sm in CaSO4 · 0.5H2O sediments with limits of detection (wt %): 0.022, 0.013, 0.011, 0.008, and 0.008, respectively. In concentration ranges (wt %) La (0.05–0.99), Ce (0.1–4.9), Pr (0.005–0.49), Nd (0.02–0.99), and Sm (0.005-0.19), the relative standard deviation RSD (n = 10, P = 0.95) was 18−27, 9−18, 20−31, 17−26, and 19−31%, respectively. A comparison of the results of XRFA with the data of inductively coupled plasma mass spectrometry confirms the accuracy of the results obtained according to OST (Branch Standard) 41-08-221-04.
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Original Russian Text © D.S. Zinin, N.N. Bushuev, V.V. Kuznetsov, 2017, published in Zhurnal Analiticheskoi Khimii, 2017, Vol. 72, No. 3, pp. 226–236.
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Zinin, D.S., Bushuev, N.N. & Kuznetsov, V.V. X-ray fluorescence determination of La, Ce, Pr, Nd, and Sm in industrial sediments of calcium sulfate using linear regression analysis. J Anal Chem 72, 279–288 (2017). https://doi.org/10.1134/S1061934817030157
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DOI: https://doi.org/10.1134/S1061934817030157