Determination of beryllium, cesium, gallium, thallium, niobium, tantalum, zirconium, hafnium, uranium and thorium in geological sample by inductively coupled plasma mass spectrometry with alkali fusion
LIU Huan, KANG Jia-hong, WANG Yu-xue
Research Institute No.240, The China National Nuclear Corporation, Shenyang 110032, China
Abstract:After geological sample was treated by alkali fusion method with potassium hydroxide, a determination method of ten elements (including beryllium, cesium, gallium, thallium, niobium, tantalum, zirconium, hafnium, uranium and thorium) was established with beryllium, cesium, thallium, hafnium, uranium and thorium corrected by rhodium, gallium, niobium, tantalum and zirconium corrected byrhenium. The silver crucible, nickel crucible and corundum crucible were selected for melting of blank sample, respectively. The results showed that the blank response signals of elements in silver crucible were lower compared to the nickel crucible and corundum crucible. The fusion conditions were also optimized as follows: the melting temperature was 600℃ and the melting time was 8min. The deionized water and 2% (volume fraction) nitric acid were used as blank solution for test respectively, and the response signal values of elements were recorded and compared with those obtained by actual geological samples. The results showed that their influence could be ignored. Under the optimized experimental conditions, the linear correlation coefficients of calibration curves of elements were all higher than 0.9990. The detection limits of the method were 0.023-0.049μg/g, and the low limits of determination limit were 0.078-0.16μg/g. Ten elements including beryllium, cesium, gallium, thallium, niobium, tantalum, zirconium, hafnium, uranium and thorium in the certified reference materials for the chemical composition of rock were determined according to the experimental method. The results were basically consistent with the certified values. The relative errors (RE) were between -8.3% and 9.6%, and the relative standard deviations (RSD, n=11) were all not more than 4.2%. The proposed method was applied for the determination of two actual geological samples from the field and the certified reference materials for the chemical composition of rock were added for the spiked recovery test. The recoveries of these ten elements were between 96% and 102%.
刘环, 康佳红, 王玉学. 碱熔-电感耦合等离子体质谱法测定地质样品中铍铯镓铊铌钽锆铪铀钍[J]. 冶金分析, 2019, 39(3): 26-32.
LIU Huan, KANG Jia-hong, WANG Yu-xue. Determination of beryllium, cesium, gallium, thallium, niobium, tantalum, zirconium, hafnium, uranium and thorium in geological sample by inductively coupled plasma mass spectrometry with alkali fusion. , 2019, 39(3): 26-32.
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