Determination of impurities in high-purity niobium(V) oxide by high-resolution continuum source graphite furnace atomic absorption spectrometry after sorption preconcentration
Autor: | Yu. A. Karpov, E. N. Kareva, V. V. Eskina, O. A. Dal’nova, V. B. Baranovskaya |
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Rok vydání: | 2017 |
Předmět: |
Sorbent
010401 analytical chemistry Analytical chemistry Niobium Oxide chemistry.chemical_element Sorption 010402 general chemistry Mass spectrometry 01 natural sciences Chloride 0104 chemical sciences Analytical Chemistry chemistry.chemical_compound chemistry Impurity medicine Graphite furnace atomic absorption medicine.drug |
Zdroj: | Journal of Analytical Chemistry. 72:649-655 |
ISSN: | 1608-3199 1061-9348 |
Popis: | Method of sorption–atomic-absorption determination of Co, Cr, Cu, Fe, Mn, and Ni in samples of high-purity Nb2O5 with heterochain S,N-containing sorbents was developed. The method is based on the sorption preconcentration of trace impurities followed by their determination by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). Selectivity of three original inhouse synthesized S,N-containing heterochain sorbents was studied. The recoveries of Co, Cr, Cu, Fe, Mn, and Ni using heterochain sorbents OKS, MTH, and GLSH were 100, 80, and 76%, correspondingly. Sorbent “OKS”, which provided the quantitative recovery of trace impurities, was chosen for further research. The sorption conditions for chloride solutions of different acidities (0.1–3 M HCl) were studied and optimized. Using the conditions established for the sorption and HR CS GFAAS analysis, trace Co, Cr, Cu, Fe, Mn, and Ni were determined in high purity Nb2O5 with a relative error less than 5%. The trueness control of the obtained results is confirmed by the “added–found” method. The developed method allows us to determine concentrations of analytes: 0.02–0.20 ppm Co, 2.0–3.3 ppm Cr, 0.2–1.5 ppm Cu, 6.0–21.0 ppm Fe, 0.6–0.8 ppm Mn, and 2.8–3.5 ppm Ni. The proposed methodology can be successfully extended to the determination of various trace elements in other high-purity inorganic materials. |
Databáze: | OpenAIRE |
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