Abstract:A quantitative analysis method for the determination of seventeen impurity elements(including aluminum, bismuth, cadmium, cobalt, chromium, copper, iron, gallium, indium, manganese, magnesium, nickel, lead, tellurium, vanadium, titanium and zinc) in crude selenium materials by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The sample was dissolved with mixed acid of nitric acid and hydrochloric acid (V (HNO3)∶V (HCl)=5∶10). Selenium was volatilized and removed using mixed hydrochloric acid-hydrobromic acid in presence of little sulfuric acid. After removing sulfuric acid fume by heating, the solution was determined in 15 %(V/V) hydrochloric acid-nitric acid mixed medium(V (HNO3)∶V (HCl)=3∶1). Since the volatilization of selenium was not conducted in volatilizing furnace, the operation was simple and the volatilization efficiency was high. The testing elements had no volatilization loss. Moreover, the residual selenium and coexisting elements had no interference in the determination. The detection limit of method was 0.000 2-0.179 4 μg/mL, and the limit of quantitation was 0.1-15.0 μg/g. The correlation coefficient of calibration curve was higher than or equal to 0.999 9 when the mass concentration of elements was in range of 0-10 μg/mL. The proposed method was applied to the determination of seventeen impurity elements in crude selenium samples. The determination results were consistent with those obtained by nonferrous industrial standard analysis methods. The average recoveries were between 92% and 112%. The relative standard deviations (RSD, n=7) were less than 10% except for trace elements (Cd, Co, Cr, Ga, In and V) with low content.
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