Abstract
A set of ICP-AES techniques has been developed for determination of rated elements: Ti, Si, P, Al, Cu, Mo, V, Sn, and Zr in ferrotitanium; Ni, Fe, Cu, Co, and As in ferronickel; Si, Cr, and P in ferrochrome silicon; Zr, Si, Al, P, and Cu in zirconium ferrosilicon; Mn, Si, and P in manganese ferrosilicon. Combination of the multielement ICP-AES method which allows precise determination of the elements in ferroalloys in a wide range of concentrations and the microwave preparation of samples in closed autoclaves which excludes the loss of the components to be determined provides the rapidity of the analysis procedure. The composition of solutions for opening samples of ferroalloys and the temperature–time modes of microwave sample preparation in an autoclave are substantiated. Conditions for ICP-AES determination of the rated elements in ferroalloys are studied. Analytical lines of the elements to be determined free from significant spectral overlaps are chosen. The dilution rates of the solutions are determined. The method of internal standard was used to improve the reproducibility of the analytical signal for Ti determination in ferrotitanium, Si and Cr in ferrochrome silicon, and all rated elements in manganese ferrosilicon and ferronickel. The spectrometer was calibrated using model solutions and solutions of standard samples with additions of the certified solutions of the elements to be determined. To determine Ti, Si, P, Al, Cu, V, and Zr in ferrotitanium; Ni, Fe, Cu, and Co in ferronickel; Si, Cr, and P in ferrochrome silicon; Zr, Si, Al, P, and Cu in zirconium ferrosilicon; Si and P in manganese ferrosilicon, a multidimensional graduation by two analytical lines was used. The correctness of the determination was evaluated in analysis of standard samples of ferroalloys and comparative analysis of the obtained results with the data of standard methods: comparison of the variances according to the Fisher criterion did not reveal any significant difference between them, whereas the use of the modified Student test showed the absence of a systematic error.
Similar content being viewed by others
REFERENCES
Mizin, V.G., Ferrosplavy: spravochnik (Ferroalloys: Handbook), Moscow: Metallurgiya, 1992.
Gasik, M.I. and Lyakishev, N.P., Teoriya i tekhnologiya elektrometallurgii ferrosplavov: uchebnik dlya vizov (Theory and Technology of Electrometallurgy of Ferroalloys: Manual for Higher Education Institutions), Moscow: Intermet Inzhiniring, 1999, p. 18.
Reznik, I.D., Ermakov, G.P., and Shneerson, Ya.M., Nikel’. Tom 2. Okislennye nikelevye rudy. Kharakteristika rud. Pirometallurgiya i gidrometallurgiya okislennykh nikelevykh rud (Nickel, Vol. 2: Oxidized Nickel Ores. Characteristic of Ores. Pyrometallurgy and Hydrometallurgy of Oxidized Nickel Ores), Moscow: Nauka i Tekhnologiya, 2001.
GOST (State Standard) 17001.4-86: Ferrosilicozirconium, Methods for Determination of Zirconium, Moscow: Izd. Standartov, 1986.
GOST (State Standard) 17001.5-86: Ferrosilicozirconium, Methods for Determination of Phosphorus, Moscow: Izd. Standartov, 1986.
GOST (State Standard) 17001.7-86: Ferrosilicozirconium, Methods for Determination of Cuprum, Moscow: Izd. Standartov, 1986.
GOST (State Standard) 17001.6-86: Ferrosilicozirconium, Methods for Determination of Silicon, Moscow: Izd. Standartov, 1986.
GOST (State Standard) 17001.8-86: Ferrosilicozirconium, Methods for Determination of Aluminum, Moscow: Izd. Standartov, 1986.
Yakubenko, E.V., Voitkova, Z.A., Chernikova, I.I., and Ermolaeva, T.N., Microwave sample preparation for detection of Si, P, V, Cr, Mn, Ni, Cu, and W using inductively coupled plasma atomic emission spectrometry in engineering steels, Inorg. Mater., 2015, vol. 51, no. 14, pp. 1370–1374.
Tormysheva, E.A., Melikhova, E.V. and Ermolaeva, T.N., Analysis of refractory materials for metallurgy by the ICP-AES method, Inorg. Mater., 2011, vol. 47, no. 14, pp. 1544–1547.
Spirina, S.V., Gritsenko, N.N., Snezhko, E.A., et al., Application of the method of emission spectrometry with inductively coupled plasma for the analysis of the chemical composition of ferroalloys, fluxes, slags, sludges and dusts, Ekol. Prom. Ekol. Monit. Metrol. Standart. Sertif., 2013, no. 4, pp. 88–94.
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.
Chernikova, I.I., Tomilina, E.A., Kukina, V.A., and Ermolaeva, T.N., Optimization of the conditions of microwave sample preparation in the analysis of ferrovanadium and ferroniobium by the method of ICP-AES, Zavod. Lab., Diagn. Mater., 2017, vol. 83, no. 2, pp. 12–17.
Chernikova, I.I., Ostroukhova, U.A., and Ermolaeva, T.N., Microwave sample preparation in analysis of ferrotungsten, silicocalcium and ferroboron by inductively coupled plasma atomic emission spectrometry, Zavod. Lab., Diagn. Mater., 2018, vol. 84, no. 2, pp. 11–17.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
The authors declare that they have no conflicts of interest.
Additional information
Translated by A. Muravev
Rights and permissions
About this article
Cite this article
Chernikova, I.I., Tumneva, K.V., Bakaldina, T.V. et al. Improvement of Sample Preparation in ICP-AES Analysis of Ferroalloys. Inorg Mater 56, 1384–1390 (2020). https://doi.org/10.1134/S0020168520140034
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0020168520140034