ELECTRON PROBE MICROANALYSIS AND ITS APPLICATION FOR ANALYTICAL DETERMINATION OF PHOSPHORUS
UDC 543.426
Keywords:
electron probe X-ray microanalysis, express analysis, determination of phosphorusAbstract
Electron probe X-ray microanalysis (EPMA) has been used to determine the content of phosphorus in the ferroalloys and the iron master alloys. This analytical method is useful for the express determination of phosphorus and has several advantages if compared with the well-known colorimetric method, which is achieved by adjusting the standard substance, the latter is used to keep the matrix effect. It has been determined that standards for the quantitative determination of phosphorus by EPMA should be homogeneous on the distribution of phosphorus in their volume, should have a clearly defined stoichiometry and should characterized by high stability on the impact of high-energy electrons. These standards could be vitreous or crystalline; however, they should possess sufficient hardness and fracture toughness. The last determine the conditions of standards polishing, which is a technological operation that should be performed in order to minimize the influence of the surface topography on the results of microanalysis. These conditions, among the investigated materials, is the best suited to the plates of single crystal synthetic monazite CePO4, which is a typical representative of the final stoichiometric number of mineralogical row and belongs to a broad family of refractory thermostable complex transition metal oxides. It is shown that the express WDS-EPMA method in the presence of an appropriate standard allows analytical determination of phosphorus in ferroalloys and ligatures and has significant advantage over spectrophotometric methods due to the rapid and nondestructive testing of alloys composition. Satisfactory agreement between the results of analysis that is conducted by using the WDS-EPMA method and standard spectrophotometric method confirms these data validity. The WDS-EPMA method has sufficient accuracy and shows reproducibility of the measurements. By using the WDS-EPMA method, 0.04-0.15 wt. % of phosphorus can be determined in the industrial ferroalloys. The data obtained allowed to apply this analytical technique for express analysis of trace phosphorus in industrial ferroalloys and the iron master alloys in order to control their production grade.
References
1. Karmanov N.S., Account of the background in wavelength dispersive X-Ray electron probe microanalysis based on the simulation of Bremsstrahlung X-radiation / Karmanov N.S., Kanakin S.V., Karmanova N.G. // J. Anal. Chem. – 2009. – V. 64. – № 4. – P. 372–378.
2. Козлов В.В. Системы рентгеноспектрального микроанализа Inca Energy и Inca Wave / В.В. Козлов // Перспективные технологии, обору-дование и системы для материаловедения и наноматериалов: Матери-алы конференции и семинара / под ред. проф. Л.В.Кожитова. – М.: Интерконтакт Наука; Усть-Каменогорск: ВКГТУ, 2008. – С. 106–122.
3. Количественный электронно-зондовый микроанализ: пер. с англ. А.И. Козленкова / под ред. Скотта В., Лава Г. – М.: Мир, 1986. – 352 с.
4. Scanning Electron Microscopy and X-ray Microanalysis: Third Edition / Goldstein J., Newbery D.E., Joy D.C. et al. – New York: Springer, 2003. – 689 p.
5. Черепин В.Т. Методы и приборы для анализа поверхности мате-риалов / В.Т. Черепин, М.А. Васильєв. – K: Наукова думка, 1982. – 400 c.
6. ГОСТ 13230.4-93. Ферросилиций. Метод определения фосфора.
7. ГОСТ 21876.5-76. Ферромарганец. Методы определения фосфо-ра.
8. Матвеев Д.В. Методика измерений структуры поверхности и эле-ментного состава образцов методами сканирующей электронной мик-роскопии и рентгеноспектрального анализа / Д.В. Матвеев, А.А. Мазил-кин. – Черноголовка: Изд. ИФТТ РАН, 2009. – 18 c.
9. Рид С.Дж.Б. Электронно-зондовый микроанализ и растровая элек-тронная микроскопия в геологии: пер. с англ. И.М. Романенко / С.Дж.Б. Рид. – М.: Технгосфера, 2008. – 232 с.
10. Scanning Electron Microscopy, X-Ray Microanalysis, and Analytical Electron Microscopy / Lyman C.E., Newbury D.E., Goldstein, et al. – New York: Plenum Press, 1990. – 407 p.
11. Measurement of chemical state change of phosphorus during mev-proton irradiation by a high-resolution wavelength-dispersive pixe system / Tada T., Wonglee S., Fukuda H. et al. // Int. J. of PIXE. – 2009. – V. 19. – № 1/2. – С. 9–15.
12. Лісняк В.В. Формування і фізико-хімічні властивості складних
d-металвмісних гетерогенних систем та їх каталітична активність у реак-ціях окиснення Н2, СО та СН4 [Текст] : дис. … д-ра хім. наук /
Лісняк В.В. – К, 2014. – 329 с.
13. Pennycook S.J. Scanning Transmission Electron Microscopy, Imaging and Analysis. / S.J. Pennycook, P.D. Nellist. – New York: Springer, 2011. – 762 p.
14. Beaman D.R. Electron Beam Microanalysis. / D.R. Beaman, J.A. Isasi. – Philadelphia: ASTM Press, 1972. – 79 p.
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