Abstract：The metal ions in Huayangchuan uranium-niobium-lead polymetallic ore were packed by silicon crystal nucleus and hardly leached. Moreover, niobium was easily hydrolyzed and precipitated, which brought difficulty to the determination of niobium in sample. The sample was treated by microwave digestion with hydrofluoric acid-nitric acid-tartaric acid mixture system. Thus, a determination method of niobium in Huayangchuan uranium-niobium-lead polymetallic ore by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established with Nb 309.418 nm as analytical line. The obtained microwave digestion procedures were listed as follows: the temperature was increased from room temperature to 180 ℃ in range of 0-30 min, and from 180 ℃ to 200 ℃ in range of 30-60 min, and then cooling by blowing in range of 60-90 min. The experimental results showed that the mass concentration of niobium in range of 0.10-2.00 μg/mL had good linearity to its corresponding emission intensity with correlation coefficient of 0.999 946. The detection limit was 0.002%. The major component in sample, i.e., silicon dioxide, had been reacted with hydrofluoric acid during sample preparation and released in form of silicon tetrafluoride. Moreover, the mass concentrations of other coexisting elements in sample solution were less than 80 μg/mL, so the matrix effect could be ignored. The experimental method was applied to the determination of Huayangchuan polymetallic ore samples with mass fraction of niobium in range of 0.030 2%~0.189%. The relative standard deviations (RSD, n=6) were between 3.1% and 3.9%. Since niobium and tantalum were usually associated, and their elemental properties and ore potentiality were highly similar, the certified reference material of tantalum ore with certified value of niobium was selected as the determination object. The results of experimental method were basically consistent with the certified values. The proposed method was compared with the national standard method of GB/T 17415.2-2010. The results indicated that the determination values of niobium in Huayangchuan polymetallic ore samples by the above two methods were consistent.
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