Inorganic Materials

, Volume 54, Issue 14, pp 1392–1396 | Cite as

Analysis of Siliceous Refractories by Inductively Coupled Plasma Atomic Emission Spectroscopy in Combination with Microwave Sample Preparation

  • E. V. YakubenkoEmail author
  • O. V. Tolmachyeva
  • I. I. Chernikova
  • T. N. Ermolaeva


In this paper, we developed a methodology for the determination of Al2O3, SiO2, CaO, and Fe2O3 in siliceous refractories by using inductively coupled plasma atomic emission spectroscopy (ICP-AES) with microwave sample preparation in an autoclave. We proposed the composition of the acid mixture and the stepwise microwave heating regime that ensure the completeness of sample dissolution and exclude the decompression of the autoclave leading to the loss of analytes in the form of volatile compounds. Cd was anticipated to be used as an internal standard. Calibrated dependences for the determination of normalized macro- and microelements in terms of oxides by ICP-AES were obtained using the method of three standards. The correctness of the developed methodology was confirmed by the analysis of state standard samples and comparison with the results of the Al2O3, SiO2, CaO, and Fe2O3 determination in accordance with GOST. The developed technique makes it possible to reduce both the time required for the analysis by 11 times and the consumption of concentrated acids by 8 times.


siliceous (dinas) refractories microwave sample preparation inductively coupled plasma atomic emission spectrometry 



  1. 1.
    Kashcheev, I.D., Strelov, K.K., and Mamykin, P.S., Khimicheskaya tekhnologiya ogneuporov: uchebnoe posobie (Chemical Technology of Refractories: Manual), Moscow: Intermet Inzhiniring, 2007.Google Scholar
  2. 2.
    Wiltsche, H., Brenner, I.B., Knapp, G., and Prattes, K., Simultaneous determination of As, Bi, Se, Sn, and Te in high alloy steels–re-evaluation of hydride generation inductively coupled plasma atomic emission spectrometry, J. Anal. At. Spectrom., 2007, vol. 22, pp. 1083–1088.CrossRefGoogle Scholar
  3. 3.
    Recknagel, S., Richter, S., Reinholdsson, F., et al., An intercomparison study of analytical methods for the determination of magnesium in low alloy steel, Steel Res. Int., 2012, vol. 83, no. 2, pp. 146–149.CrossRefGoogle Scholar
  4. 4.
    Hlaváčková, I. and Hlaváček, I., Multi-element analysis of some high silicon content ferroalloys by inductively coupled plasma atomic emission spectrometry, J. Anal. At. Spectrom., 1994, vol. 9, pp. 251–255.Google Scholar
  5. 5.
    Bukhbinder, G.L., Korotkov, V.A., Arak, M.N., and Shikhareva, N.P., Analysis of cathode copper in iCAP 6000 Series ICP emission spectrometers, Zavod. Lab., Diagn. Mater., 2011, vol. 77, no. 3, pp. 11–13.Google Scholar
  6. 6.
    Karachevtsev, F.N., Zagvozdkina, T.N., and Dvoretskov, R.M., Determination of silicon in nickel alloys by ICP-AES combined with microwave sample preparation, Tr. Vseross. Inst. Aviats. Mater., 2015, no. 12, pp. 55–60.Google Scholar
  7. 7.
    Dvoretskov, R.M., Karachevtsev, F.N., Zagvozdkina, T.N., and Mekhanik, E.A., Determination of the alloying elements of nickel-based alloys designed for aviation application by inductively coupled plasma atomic emission spectrometry in combination with the microwave digestion method, Inorg. Mater., 2014, vol. 50, no. 14, pp. 1421–1425.CrossRefGoogle Scholar
  8. 8.
    Romanova, N.B., Pechishcheva, N.V., Shunyaev, K.Yu., et al., Determination of tungsten, titanium, molybdenum, niobium, and vanadium in steels and nickel-based alloys by inductively coupled plasma atomic emission spectroscopy, Zavod. Lab., Diagn. Mater., 2013, vol. 79, no. 3, pp. 3–7.Google Scholar
  9. 9.
    Maiorova, A.V., Vorontsova, K.A., Pechishcheva, N.V., et al., Determination of silica in ore raw materials by inductively coupled plasma atomic emission spectroscopy, Zavod. Lab., Diagn. Mater., 2013, vol. 79, no. 12, pp. 9–15.Google Scholar
  10. 10.
    Simakov, V.A., Vasil’ev, G.A., Grigor’ev, D.V., and Sulkhanov, I.V., Determination of the general components of manganese ores using inductively coupled plasma atomic emission spectroscopy, Zavod. Lab., Diagn. Mater., 2013, vol. 79, no. 7-1, pp. 3–6.Google Scholar
  11. 11.
    Tormysheva, E.A., Smirnova, E.V., and Ermolaeva, T.N., Determination of iron oxide (III), calcium oxide, and aluminum oxide in manganese refractories by ICP-AES under microwave sample decomposition, Vestn. Voronezh. Gos. Univ. Ser. Khim. Biol. Farm., 2010, no. 1, pp. 51–55.Google Scholar
  12. 12.
    Nerobeeva, I.V. and Ermolaeva, T.N., Determination of boron in high-aluminum semiproduct by inductively coupled plasma atomic emission spectroscopy, Inorg. Mater., 2009, vol. 45, no. 14, pp. 1580–1583.CrossRefGoogle Scholar
  13. 13.
    Shaverina, A.V., Tsygankova, A.R., and Saprykin, A.I., Development of direct and combined ICP-AES methods for silicon analysis, Vserossiiskaya konferentsiya po analiticheskoi spektroskopii, Tezisy dokladov (All-Russ. Conf. on Analytical Chemistry, Abstracts of Papers), Krasnodar, 2012, p. 81.Google Scholar
  14. 14.
    Shaverina, A.V., Tsygankova, A.R., Shelpakova, I.R., and Saprykin, A.I., ICP-AES analysis of high-purity silicon, Inorg., Mater., 2013, vol. 49, no. 14, pp. 1283–1287.Google Scholar
  15. 15.
    Yakubenko, E.V., Voitkova, Z.A., and Ermolaeva, T.N., Microwave sample preparation of the refractories and refractory materials for determination of magnesium, aluminum, silicon, calcium, and iron (III) oxides using ICP-AES, Zavod. Lab., Diagn. Mater., 2014, vol. 80, no. 3, pp. 15–19.Google Scholar
  16. 16.
    Doronina, M.S., Karpov, Yu.A., and Baranovskaya, V.B., Advanced techniques for sample processing of the reusable metal-containing raw material (review), Inorg. Mater., 2017, vol. 53, no. 14, pp. 1391–1398.CrossRefGoogle Scholar
  17. 17.
    Korsakova, N.V., Toropchenova, E.S., Krigman, L.V., et al., Analysis of silicate materials using the microwave-assisted sample preparation, Inorg. Mater., 2010, vol. 46, no. 14, pp. 1513–1517.CrossRefGoogle Scholar
  18. 18.
    Kubrakova, I.V. and Toropchenova, E.S., Microwave sample preparation for geochemical and ecological studies, J. Anal. Chem., 2013, vol. 68, no. 6, pp. 467–476.CrossRefGoogle Scholar
  19. 19.
    Domanskii, A.I., Orlov, Yu.I., Rumyantsev, P.F., and Shidlovskaya, O.V., Kinetic regularities of the interaction of aluminum oxide and silicon dioxide single crystals with phosphoric acid, Glass Phys. Chem., 2007, vol. 33, no. 1, pp. 55–61.CrossRefGoogle Scholar
  20. 20.
    Tikhonov, V.N., Analiticheskaya khimiya alyuminiya (Analytical Chemistry of Aluminum), Moscow: Nauka, 1971.Google Scholar

Copyright information

© Pleiades Publishing, Inc. 2018

Authors and Affiliations

  • E. V. Yakubenko
    • 1
    • 2
    Email author
  • O. V. Tolmachyeva
    • 2
  • I. I. Chernikova
    • 1
    • 2
  • T. N. Ermolaeva
    • 1
  1. 1.Lipetsk State Technical UniversityLipetskRussia
  2. 2.PJSC NovolipetskLipetskRussia

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