Journal of Analytical Chemistry

, Volume 72, Issue 3, pp 279–288 | Cite as

X-ray fluorescence determination of La, Ce, Pr, Nd, and Sm in industrial sediments of calcium sulfate using linear regression analysis



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.


energy-dispersive X-ray fluorescence analysis inductively coupled plasma mass spectrometry linear regression analysis lanthanides overlapping of spectral lines 


Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.


  1. 1.
    Zinin, D.S. and Bushuev, N.N., Russ. J. Appl. Chem., 2014, vol. 87, no. 11, p. 1611.CrossRefGoogle Scholar
  2. 2.
    Bushuev, N.N., Zinin, D.S., and Levin, B.V., Khim. Tekhnol., 2014, vol. 15, no. 9, p. 549.Google Scholar
  3. 3.
    Bushuev, N.N. and Zinin, D.S., Russ. J. Inorg. Chem., 2016, vol. 61, no. 2, p. 161.CrossRefGoogle Scholar
  4. 4.
    Gleisberg, B., Ly, B.M., and Gorski, B., J. Radioanal. Nucl. Chem., 1991, vol. 147, no. 1, p. 95.CrossRefGoogle Scholar
  5. 5.
    Rimskaya-Korsakova, M.N., Dubinin, A.V., and Ivanov, V.M., J. Anal. Khim., 2003, vol. 58, no. 9, p. 870.Google Scholar
  6. 6.
    Nikolaeva, I.V., Palesskii, S.V., Koz’menko, O.A., and Anoshin, G.N., Geochem. Int., 2008, no. 10, p. 1016.CrossRefGoogle Scholar
  7. 7.
    Eid, M.A., Broekaert, J.A.C., and Tschopel, P., Fresenius’ J. Anal. Chem., 1992, vol. 342, no. 1, p. 107.CrossRefGoogle Scholar
  8. 8.
    Marathe, S.M., Biswas, S.S., Patil, P.B., and Murty, P.S., Microchim. Acta, 1992, vol. 109, no. 5, p. 261.CrossRefGoogle Scholar
  9. 9.
    Bakhtiarov, A.V., Rentgenospektral’nyi fluorestsentnyi analiz v geologii i geokhimii (X-Ray Fluorescence Analysis in Geology and Geochemistry), Leningrad: Nedra, 1985.Google Scholar
  10. 10.
    Losev, N.F. and Smagunova, A.N., Osnovy rentgenospektral’nogo fluorestsentnogo analiza (Fundamentals of X-Ray Fluorescence Analysis), Moscow: Khimiya, 1982.Google Scholar
  11. 11.
    Makarskii, I.V. and Revenko, A.G., Analitika Kontrol’, 2000, vol. 4, no. 5, p. 437.Google Scholar
  12. 12.
    Lal, M., Choudhury, R.K., Joseph, D., Bajpai, H.N., and Tyer, C.S.P., J. Radioanal. Nucl. Chem., 1989, vol. 137, no. 2, p. 127.CrossRefGoogle Scholar
  13. 13.
    Labrecque, J.J., Beusen, J.M., and Van Grieken, R.E., X-Ray Spectrom., 1986, vol. 15, no. 1, p. 13.CrossRefGoogle Scholar
  14. 14.
    Smirnova, I.S., Bushuev, N.N., and Nabiev, A.G., Zavod. Lab., 1990, vol. 56, no. 2, p. 39.Google Scholar
  15. 15.
    Chandola, L.C., Machado, I.J., and Mohile, A.N., Microchim. Acta, 1976, vol. 66, no. 3, p. 399.CrossRefGoogle Scholar
  16. 16.
    Chandola, L.C., Machado, I.J., and Mohile, A.N., J. Radioanal. Chem., 1976, vol. 34, no. 2, p. 389.CrossRefGoogle Scholar
  17. 17.
    Aisueva, T.S., Belozerova, O.Yu., Finkel’shtein, A.L., Bryantseva, N.Yu., and Skornikova, S.A., Analitika Kontrol’, 2013, vol. 17, no. 4, p. 386.Google Scholar
  18. 18.
    Willis, J.P. and McNew, E.B., Adv. X-Ray Anal., 1997, vol. 41, p. 829.Google Scholar
  19. 19.
    Khudonogova, E.V., Suvorova, D.S., and Revenko, A.G., Analitika Kontrol’, 2015, vol. 19, no. 4, p. 347.Google Scholar
  20. 20.
    Aivazyan, S.A., Mkhitaryan, V.C., Prikladnaya statistika i osnovy ekonometriki (Applied Statistics and Fundamentals of Econometrics), Moscow: YuNITI, 1998, p. 621.Google Scholar
  21. 21.
    Alley, B.J. and Myers, R.H., Anal. Chem., 1965, vol. 37, no. 13, p. 1685.CrossRefGoogle Scholar
  22. 22.
    Molchanova, E.I., Smagunova, A.N., and Shcherbakov, I.V., J. Anal. Chem., 2011, vol. 66, no. 9, p. 824.CrossRefGoogle Scholar
  23. 23.
    Bushuev, N.N., Nabiev, A.G., Petropavlovsky, I.A., and Smirnova, I.S., Russ. J. Appl. Chem., 1988, vol. 61, no. 10, p. 1973.Google Scholar
  24. 24.
    Bushuev, N.N. and Zinin, D.S., Khim. Prom-st. Segodnya, 2014, no. 5, p. 16.Google Scholar
  25. 25.
    Bushuev, N.N. and Zinin, D.S., Khim. Prom-st. Segodnya, 2015, no. 4, p. 6.Google Scholar
  26. 26.
    Kirsanov, D., Panchuk, V., Goydenko, A., Khaydukova, M., Semenov, V., and Legin, A., Spectrochim. Acta, Part B, 2015, vol. 113, p. 126.CrossRefGoogle Scholar
  27. 27.
    Lemberge, P. and Van Espen, P.J., X-Ray Spectrom., 1999, vol. 28, no. 2, p. 77.CrossRefGoogle Scholar
  28. 28.
    Adams, M.J. and Allen, J.R., Analyst, 1998, vol. 123, no. 4, p. 537.CrossRefGoogle Scholar
  29. 29.
    Barbalat, Yu.A., Kalinkin, I.P., Mosichev, V.I., Saidov, G.V., and Sverdlova, O.V., Novyi spravochnik khimika i tekhnologa (New Handbook of Chemist and Process Engineer), vol. 6: Analiticheskaya khimiya (Analytical Chemistry), St. Petersburg: Mir i Sem’ya, 2004, part 3, p. 56.Google Scholar

Copyright information

© Pleiades Publishing, Ltd. 2017

Authors and Affiliations

  • D. S. Zinin
    • 1
  • N. N. Bushuev
    • 1
  • V. V. Kuznetsov
    • 1
  1. 1.Mendeleev University of Chemical Technology of RussiaMoscowRussia

Personalised recommendations