Abstract：The content of impurity elements in beryllium directly affects the properties of beryllium materials. The accurate determination of their contents is of great significance. The beryllium metal pebble sample was dissolved in hydrochloric acid-nitric acid system. The isotopes of 7Li, 114Cd, 147Sm, 153Eu, 157Gd and 163Dy were determined at standard mode, and 27Al, 52Cr, 55Mn, 56Fe, 60Ni and 208Pb were determined at the mode of helium collision cell kinetic energy discrimination (KED) with helium flow rate of 6.0 mL/min. Thus, a method for determination of twelve trace impurity elements (Li, Al, Cr, Mn, Fe, Ni, Cd, Sm, Eu, Gd, Dy and Pb) in beryllium metal pebble by inductively coupled plasma mass spectrometry (ICP-MS) was established. The matrix effect investigated, and it was overcome through stepwise dilution of sample solution to reduce the matrix concentration and online correction with internal standard. Considering that the contents of Fe and Al in beryllium metal pebble were higher than other impurity elements, the sample solution with dilution factor of 200 was used for determination of Fe and Al, while the dilution factor of 50 was used for determination of other elements. The internal standard of 45Sc was used to correct Li, Al, Cr, Mn, Fe and Ni. The internal standard of 103Rh was used to correct Cd and Sm. The internal standard of 187Re was used to correct Eu, Gd, Dy and Pb. The experimental results showed that the linear correlation coefficients of calibration curves for elements were all higher than 0.999 5, the limits of detection were 0.002-2.90 μg/g, and the limits of quantification were 0.006-9.67 μg/g. The proposed method was applied for determination of twelve trace impurity elements (Li, Al, Cr, Mn, Fe, Ni, Cd, Sm, Eu, Gd, Dy and Pb) in beryllium metal pebble sample with purity grade of Be-2. Moreover, the standard addition recovery tests were conducted. The relative standard deviations (RSD,n=6) of determination results were between 0.76% and 7.0%, and the recoveries were between 95% and 118%. The standard method of GJB 2513A-2008 was used for comparison. It was found that the absolute errors between the two methods were all within the tolerance range specified in the standard method.
郭文韬, 王雷, 孟祥娥, 方哲, 王超刚, 王瑞. 电感耦合等离子体质谱法测定金属铍珠中痕量杂质元素[J]. 冶金分析, 2023, 43(9): 28-34.
GUO Wentao, WANG Lei, MENG Xiang'e, FANG Zhe, WANG Chaogang, WANG Rui. Determination of trace impurity elements in beryllium metal pebble by inductively coupled plasma mass spectrometry. , 2023, 43(9): 28-34.
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