Determination of tantalum, uranium and ytterbium in coal by microwave digestion and high resolution inductively coupled plasma mass spectrometry based on matrix matching
SHEN Jian1,2, WANG Bing2, XU Qianru2, MIN Hong2, ZHANG Linping*1, LIU Shu*2
1. Chemical Engineering and Biotechnology, Key Laboratory of Science and Technology of Eco-Textile, Ministry of Education, Donghua University,Shanghai 201620, China; 2. Technical Center for Industrial Product and Raw Material Inspection and Testing of Shanghai Customs,Shanghai 200135, China
摘要 煤中Ta、U、Yb的测定对煤炭地球化学研究和产地溯源具有重要意义。在采用高分辨电感耦合等离子体质谱(HR-ICP-MS)测定煤中Ta、U、Yb时,基体效应较为严重,导致测定结果偏高。采用8 mL HNO3-1 mL HF微波消解煤炭样品,优化了消解体系、消解程序、复溶时间等前处理条件,选用181Ta、238U、172Yb为测定同位素,采用低分辨率模式测定U,高分辨率模式测定Ta、Yb,以Rh内标结合基体匹配法克服基体效应,实现了煤中Ta、U、Yb的HR-ICP-MS测定。在优化的实验条件下,在1.000~20.00 μg/L范围内,被测元素与内标元素信号强度的比值与被测元素质量浓度呈现良好的线性相关,相关系数不小于0.999 9,各元素的检出限在0.002~0.008 μg/g之间,定量限在0.007~0.027 μg/g之间。将实验方法应用于煤炭标准样品中Ta、U、Yb的测定,测定值与认定值基本一致,相对标准偏差(RSD,n=6)为2.3%~4.3%。选取俄罗斯其他烟煤及无烟煤、澳大利亚其他烟煤、蒙古炼焦煤、印度尼西亚褐煤及其他烟煤6个代表性样品,按照实验方法进行测定,测定结果表明,Ta、U在俄罗斯其他烟煤样品中含量最高,Yb在澳大利亚其他烟煤样品中含量最高,印度尼西亚褐煤中3种元素含量均最低。
Abstract：The determination of Ta, U and Yb in coal is of great significance for coal geochemical research and origin traceability. During the determination of Ta, U and Yb in coal by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS), the matrix effect was relatively serious, which resulted in higher measurement results. The coal samples were dissolved with 8 mL of HNO3 and 1 mL of HF by microwave digestion. The pretreatment conditions such as digestion system, digestion procedure and resolution time were optimized. 181Ta, 238U and 172Yb were selected as the test isotopes. U was determined at low resolution mode, while Ta and Yb were determined at high resolution mode. The matrix effect was overcome with Rh as internal standard and matrix matching. Consequently, the determination of Ta, U and Yb in coal by HR-ICP-MS was realized. Under the optimized experimental conditions, the ratio of the signal intensity between the analyzed element to the internal standard element showed a good linear relationship with the concentration of the analyzed element in range of 1.000-20.00 μg/L. The correlation coefficient was not less than 0.999 9. The limits of detection were between 0.002 μg/g and 0.008 μg/g, and the limits of quantitation were between 0.007 μg/g and 0.027 μg/g. The experimental method was applied to the determination of Ta, U and Yb in coal certified reference materials, and the results were basically consistent with the certified values. The relative standard deviations (RSD, n=6) were between 2.3% and 4.3%. Six representative coal samples, including other bituminous coal and anthracite from Russian, Australian other bituminous coal, Mongolian coking coal, lignite coal and other bituminous coal from Indonesian, were determined according to the experimental method. The results showed that the contents of Ta and U in Russian other bituminous coal samples were the highest, the content of Yb in Australian other bituminous coal samples was the highest, while the contents of three elements in Indonesian lignite were all the lowest.
沈健, 王兵, 徐倩茹, 闵红, 张琳萍, 刘曙. 微波消解-基体匹配高分辨电感耦合等离子体质谱法测定煤中钽铀镱[J]. 冶金分析, 2022, 42(6): 30-36.
SHEN Jian, WANG Bing, XU Qianru, MIN Hong, ZHANG Linping, LIU Shu. Determination of tantalum, uranium and ytterbium in coal by microwave digestion and high resolution inductively coupled plasma mass spectrometry based on matrix matching. , 2022, 42(6): 30-36.
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