Determination of niobium in uranium-niobium-lead polymetallic ore by inductively coupled plasma mass spectrometry with hydrofluoric acid resistant injection system
GUO Xiaorui1,2,3, FAN Lei1,2,3, MAO Xiangju1,2,3, ZHANG Hongli1,2,3, WANG Tiantian1,2,3, YAO Mingxing*1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. Key Laboratory for Polymetallic Ores' Evaluation and Utilization, MNR, Zhengzhou 450006, China; 3. Key Laboratory of Comprehensive Utilization of Gold Resource in Henan Province, Zhengzhou 450006, China
Abstract：Accurate determination of niobium (Nb) in uranium-niobium-lead polymetallic ore plays an important role in beneficiation research and recycle of niobium. The uranium-niobium-lead polymetallic ore samples were digested in hydrofluoric acid by microwave digestion. The use of hydrofluoric acid resistant injection system avoided the corrosion of standard injection system by hydrofluoric acid. A new method for the determination of niobium in uranium-niobium-lead polymetallic ore by inductively coupled plasma mass spectrometry (ICP-MS) with hydrofluoric acid resistant injection system was established using 93Nb as analytical isotopes and 200 ng/mL185Re as internal standard. It was found in experiments that the mass spectrum intensity of the hydrofluoric acid resistant injection system was lower than that of the standard injection system, which would reduce the measurement sensitivity. Therefore, the instrument parameters were optimized: the peristaltic pump speed was 40 r/min and the plasma power was 1 590 W. Under the optimized instrument conditions, there was a good linear relationship between the mass spectrum intensity and mass concentration of niobium pentoxide in the range of 0.01-500 ng/mL. The correlation coefficient was 0.999 3, the limit of detection of the method was 0.228 ng/mL and the limit of quantification was 0.758 ng/mL. The content of niobium pentoxide in uranium-niobium-lead polymetallic ore sample was determined according to the experimental method. The found results were basically consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). The relative standard deviations (RSDs, n=9) were between 2.4% and 5.8%. The spiked recovery test was conducted according to the experimental method, and the recoveries were between 95% and 104%, which could meet the requirements in national geological and mineral industry standard (DZ/T 0130-2006).
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