journal article·2022-12

X-ray Fluorescence Determination of Small Quantities of Hafnium in Nuclear Pure Zirconium-Based Materials

N. Ya. Varkentin, E. G. Vinokurov, O. A. Karavaeva, U. V. Bortnikova

Inorganic Materials· Volume 58· Issue 14
Publisher page

Abstract

Abstract An important chemical impurity in the composition of zirconium-based materials for nuclear power engineering is hafnium, the content of which should not exceed 0.05 and 0.01% for Russian and foreign alloy grades, respectively. Since the chemical properties of hafnium are similar to those of zirconium, determination of this element using classical methods of analytical chemistry is a challenging problem. Among the physical methods, the X-ray fluorescence method is the most expressive, which is important under conditions of continuous production. The X-ray fluorescence method for measuring the content of hafnium in zirconium-containing material has been tested by the example of potassium fluorozirconate, a precursor for obtaining alloys. Using various combinations of crystal analyzers, detectors, and collimators of a wave-dispersive spectrometer, the ratios of the intensities of the Hf and Zr analytical lines in the second order of reflection have been refined, and the degree of decrease in the fluorescence intensity of those lines has been determined. The X-ray fluorescence spectra of hafnium lines in potassium fluorozirconate have been studied for the content characteristic of nuclear-pure zirconium. The possibilities of recording the intensity of the Hf analytical lines and methods for eliminating the interference from the Zr lines in the second order of reflection are considered. The metrological characteristics of the determination of Hf using selected analytical lines have been calculated. It is shown that the error is the smallest and the detection limit is the lowest (0.001%) if the HfLβ1 line is used with certain settings of the wave-dispersive spectrometer (the X-ray tube operating mode, a combination of a crystal analyzer, a detector, and a collimator, and the amplitude discriminator settings). The proposed method of hafnium determination is applicable to the materials with a constant content of zirconium.
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OpenAlex topics: Nuclear Physics and Applications · Nuclear Materials and Properties · X-ray Diffraction in Crystallography

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References (17)

Show source-provided references
1. Zaimovskii, A.S., Nikulina, A.V., and Reshetnikov, N.G., Tsirkoniyevye splavy v yadernoi energetike (Zirconium Alloys in Nuclear Power), Moscow: Energoatomizdat, 1994.
2. Raparthi Shekhar, Arunachalam, J., Radha Krishna, G., et al., Determination of elemental composition of Zr-Nb alloys by glow discharge quadrupole mass spectrometry, At. Spectrosc., 2004, vol. 25, no. 4, pp. 157–164. https://doi.org/10.1039/b300158j10.1039/b300158j ↗
3. Tsutomu, M., Hideaki, M., and Takayoshi, K., Instrumental neutron activation analysis of hafnium in zirconium metal using internal standartization, J. Radioanal. Nucl. Chem., 2009, vol. 282, no. 1, pp. 49–52. https://doi.org/10.1007/s10967-009-0314-110.1007/s10967-009-0314-1 ↗
4. Dombrovskaya, M.A., Lisienko, D.G., and Shafar, O.Yu., Determination of hafnium in zirconium materials, Zavod. Lab. Diagn. Mater., 2019, vol. 85, no. 1, part 2, pp. 56–59. https://doi.org/10.26896/1028-6861-2019-85-1-II-56-5910.26896/1028-6861-2019-85-1-II-56-59 ↗
5. Steffan, I. and Vujicic, G., Analysis of zirconium alloys by inductively coupled plasma atomic emission spectrometry, J. Anal. At. Spectrom., 1994, vol. 9, pp. 785–789. https://doi.org/10.1039/JA994090078510.1039/JA9940900785 ↗
6. Asakura, H., Ikegami, K., Murata, M., and Wakita, H., Determination of components in refractories containing zirconia by X-ray fluorescence spectrometry, X-Ray Spectrom., 2000, vol. 29, no. 6, pp. 418–425. https://doi.org/10.1002/1097-4539(200011/12)29:6<<418: :AID-XRS445>>3.0.CO; 2-P10.1002/1097-4539(200011/12)29:6 ↗
7. Sarbajna, C., Durani, S., and Rajagopalan, V., Determination of hafnium in zircon by wavelength dispersive X-ray fluorescence spectrometry and inductively coupled plasma spectrometry, Indian Mineralogist, 2011, vol. 45, no. 1, pp. 217–226.
8. Afzal, M., Hanif, J., and Hanif, I., Determination of zirconium and hafnium in solution by X-Ray fluorescence spectrometry, J. Radioanal. Nucl. Chem., 1990, vol. 139, no. 2, pp. 203–214. https://doi.org/10.1007/BF0206180410.1007/BF02061804 ↗
9. GOST (State Standard) R 55410-2013: Refractories. Chemical analysis by X-ray fluorescence method, 2014.
10. Kalinkin, I.P., Mosichev, V.I., and Saidov, G.V., Spravochnik khimika i tekhnologa. Analiticheskaya khimiya, Chast’ 3 (New Handbook of Chemist and Technologist. Analytical Chemistry. Part III), St. Petersburg: Mir Sem’ya, 2004.
11. Majid, C.A., Hussain, M.A., and Saeed, K., Quantitative Microanalysis of Hafnium-Zirconium System by X-Ray Fluorescence, Rawalpindi: Pakist. Inst. Nucl. Sci. Technol., 1986.
12. Agarwal, R.M. and Jha, S.N., Determination of small concentration of hafnia in zirconia by selective excitation energy dispersive X-ray emission spectrometry, Fresenius J. Anal. Chem., 1994, vol. 349, pp. 434–437. https://doi.org/10.1007/BF0032292810.1007/BF00322928 ↗
13. Hasany, S.M., Rashid, F., and Rashid, A., Determination of traces of hafnium in zirconium oxide by wavelength dispersive X-Ray fluorescence spectrometry, J. Radioanal. Nucl. Chem., 1990, vol. 142, no. 2, pp. 505–514. https://doi.org/10.1007/BF0204032110.1007/BF02040321 ↗
14. Lisienko, D.G., Dombrovskaya, M.A., and Kubrina, E.D., Synthesis of materials and evaluation of metrological characteristics of a standard sample of potassium fluorozirconate composition, Stand. Obraztsy, 2016, no. 3, pp. 47–60.
15. Blokhin, M.A. and Shveitser, I.G., Rentgenospektral’nyi spravochnik (X-Ray Spectral Feference Book), Moscow: Nauka, 1982.
16. Varkentin, N.Ya. and Karavaeva, O.A., Influence of the instrumental parameters of an X-ray fluorescence wave-dispersive spectrometer on the metrological characteristics of measurements, Zavod. Lab. Diagn. Mater., 2019, vol. 85, no. 2, pp. 65–72. https://doi.org/10.26896/1028-6861-2019-85-2-65-710.26896/1028-6861-2019-85-2-65-7 ↗
17. Industry Instruction OI 001.639-2016: Hafnium, zirconium. X-ray fluorescence technique for measuring mass fractions in products of potassium fluorozirconate production, Glazov: Chepetsk. Mekh. Zavod, 2016.