Determination of niobium pentoxide, zirconium dioxide and titanium dioxide in waste powder of lanthanum glass by inductively coupled plasma atomic emission spectrometry
1. National Engineering Research Centre of Rare Earth Metallurgy and Funcional Materials, Baotou 014030, China; 2. Baotou Research Institute of Rare Earths, Baotou 014030, China
Abstract：The sample was melted with sodium hydroxide and sodium peroxide at high temperature, and the melt was extracted with hot water. Thus, silicon, boron and sodium salts was separated from precipitate under alkaline condition. After the precipitate was dissolved with hydrochloric acid and hydrofluoric acid, the content of Nb2O5, ZrO2 and TiO2 was simultaneously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) with Nb 309.418 nm, Zr 257.139 nm and Ti 334.941 nm as analytical lines. Consequently, a determination method of Nb2O5, ZrO2 and TiO2 in waste powder of lanthanum glass was established. The optical sample fusion conditions were explored as follows: 3.0 g of sodium hydroxide and 1.5 g of sodium peroxide were added into 0.5 g of sample followed by fusion at 750 ℃ for 10 min. The optimal analysis lines were selected by spectral line, background profile, signal-to-background ratio and signal intensity. The results showed that the mass concentration of matrix below 0.1 mg/mL had no influence on the determination. The interference of coexisting elements including La, Ni, Ce, Ba, Sr, Si and B could be ignored. The linear range of Nb2O5, ZrO2 and TiO2 was 1.00-15.0 μg/mL,1.00-10.0 μg/mL and 1.00-15.0 μg/mL, respectively. The linear correlation coefficients of calibration curves were all 0.999 9. The detection limits were between 0.013% and 0.016%. The content of Nb2O5, ZrO2 and TiO2 in actual sample of waste powder of lanthanum glass was determined according to the experimental method. The relative standard deviations (RSD, n=11) were between 0.59% and 1.2%. The results were consistent with those obtained by X-ray fluorescence spectrometry (Nb2O5), gravimetry(ZrO2) and titration method(TiO2).
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