Determination of ten elements in zirconium ores by lithium metaborate fusion-inductively coupled plasma atomic emission spectrometry
WANG Li-qiang1,2, WANG Jia-song*1,2, WU Liang-ying1,2, ZENG Jiang-ping1,2,3 FANG Peng-da1,2, ZHENG Zhi-kang1,2
1. Tianjin Center of Geolofical Survey, China Geological Survey, Tianjin 300170, China; 2. North China Center for Geoscience Innovation, Tianjin 300170, China; 3. Key Laboratory of Geological Environment of Muddy Coastal Zone, China Geological Survey, Tianjin 300170, China
Abstract：Zirconium ore was an important strategic ore resource. The accurate analysis of zirconium as well as its intergrowth useful and harmful elements had great significance on the comprehensive evaluation and utilization of zirconium ore resources. However, zirconium ore was insoluble, and hydrolytic precipitation of Zr and Hf easily occured in sample preparation process. Based on the selection of sample pretreatment method and the optimization of instrumental working conditions, the analysis method of ten elements (in oxides, including Zr, Hf, K, Na, Ca, Mg, Al, Fe, Ti and Mn) in zirconium ore by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established after lithium metaborate fusion and dilute sulfuric acid-tartaric acid extraction. The sample was prepared according to the fusion decomposition characteristic by lithium metaborate. The sample treatment effect was good when the mass of flux was five times of sample mass. The hydrolysis of Zr and Hf could be inhibited by adding tartaric acid into dilute sulfuric acid extracting solution. The working conditions for the instruments were set as follows: the power of generator was 1.3kW; the sample injection speed was 1.0mL/min; the flow rate of atomized gas was 0.7L/min; Zr 343.823nm, Hf 277.336nm, K 766.490nm, Na 589.592nm, Ca 317.933nm, Mg 285.213nm, Al 396.153nm, Fe 238.204nm, Ti 334.940nm and Mn 257.610nm were selected as the analytical lines; the influence of matrix effect was eliminated by preparing the calibration curve using matrix matching method. The linear correlation coefficients of the calibration curves for testing elements were all higher than 0.9990. The limit of detection was 1.57-58.8μg/g. The proposed method was applied to the determination of Zr, Hf, K, Na, Ca, Mg, Al, Fe, Ti and Mn (in oxides) in certified reference materials of zirconium ore (GBW07156 and GBW07157). The relative standard deviations (RSD, n=10) of determination results were between 0.67% and 4.1%. The relative errors (RE) were 0.13%-4.8%. The contents of elements (in oxides) in actual sample were determined according to the experimental method. The relative standard deviations (RSD, n=5) of determination results were between 0.27% and 4.4%. The zirconium ore could be rapidly and completely decomposed. The hydrolysis of Zr and Hf could be effectively avoided. The proposed method was applicable for the accurate analysis of ten elements in zirconium ore.
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