Determination of molybdenum in coal tailing from Yunnan Province by inductively coupled plasma atomic emission spectrometry with graphite digestion
LAI Yongfeng, WU Weiming*
Key Laboratory of Testing and Tracing of Rare Earth Products for State Market Regulation, Jiangxi University of Science and Technology,Ganzhou 341000,China
Abstract：The mass fraction of molybdenum in one coal tailing from Yunnan Province is about 5%, which has high economic and social value. Therefore, it is of great significance to determine molybdenum accurately for extracting molybdenum from coal tailing. The molybdenum in mineral is hardly dissolved with the conventional acid dissolution method. The sample were calcinated at 600 ℃ for 60 min to remove carbon. Then, it was digested with 10 mL of aqua regia at 170 ℃ for 30 min. After that, 5 mL of hydrofluoric acid and 2 mL of perchloric acid were added, and the solution was further digested at 170 ℃ to almost dry. The residue was dissolved with water, and the content of molybdenum in the solution was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Consequently, a method for determination of molybdenum in coal tailing was established by ICP-AES after graphite digestion. The interference tests indicated that the main coexisting elements such as iron, magnesium and calcium had no interference with the determination of molybdenum. The mass concentration of molybdenum showed a good linear relationship with its corresponding emission intensity, and the linear correlation coefficient of the calibration curve was greater than 0.999 5. The limit of detection of method was 0.000 2%. The proposed method was applied to the determination of molybdenum in coal tailing samples from Yunnan Province. The relative standard deviation (RSD, n=10) of determination results was less than 1%. The recoveries were between 98% and 101%. The contents of molybdenum in coal tailing sample and certified reference material of molybdenum concentrate (wMo=1.51%) were determined according to the proposed method. The results were basically consistent with those obtained by thiocyanate spectrophotometry.
赖永锋, 吴伟明. 石墨消解-电感耦合等离子体原子发射光谱法测定云南某地煤尾矿中钼[J]. 冶金分析, 2023, 43(3): 52-56.
LAI Yongfeng, WU Weiming. Determination of molybdenum in coal tailing from Yunnan Province by inductively coupled plasma atomic emission spectrometry with graphite digestion. , 2023, 43(3): 52-56.
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