Determination of lithium,beryllium,rubidium,cesium,niobium and tantalum in geochemical samples by inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry
ZHU Zhigang, LI Meili, FANG Xiaohong, PENG Liping, XIE Xinkan
Inner Mongolia Minerals Experiment Research Institute,Hohhot 010031,China
Abstract：In view of the characteristics of some geochemical samples, such as large variation range of the associated rare Li, Be, Rb, Cs, Nb and Ta, the high content of Nb and Ta which are easily hydrolyzed, the complicated process of traditional analysis method, and the difficulty to realize simultaneous determination, the sample was decomposed by heating at normal pressure with acid solution system of HF-HNO3-H2SO4 at 10∶5∶1 (volume ratio). The sample solution was extracted with 80 g/L tartaric acid solution to fully complex Nb and Ta. Then the aqua regia was added to fully extract the Li, Be, Rb and Cs into solution by heating. Li, Be, Rb, Nb, Cs and Ta were determined by inductively coupled plasma mass spectrometry (ICP-MS) using 7Li, 9Be, 85Rb, 93Nb, 133Cs and 181Ta as the isotopes for analysis. Li 670.784 nm {Ⅰ}, Be 234.861 nm {Ⅰ}, Rb 780.023 nm {Ⅰ}, Nb 316.340 nm {Ⅱ} and Ta 268.517 nm {Ⅱ} were used as analytical lines for the determination of Li, Be, Rb, Nb and Ta by inductively coupled plasma atomic emission spectrometry (ICP-AES). The method for the determination of Li, Be, Rb, Cs, Nb and Ta in geochemical samples by ICP-MS and ICP-AES was established. The linear correlation coefficients of the calibration curves of Li, Be, Rb, Cs, Nb, and Ta ranged from 0.999 4 to 0.999 9. The limit of detection and limit of quantification (based on ICP-MS) was 0.01-0.15 μg/g and 0.012-0.807 μg/g, respectively. The contents of Li, Be, Rb, Cs, Nb and Ta in certified reference materials of soil, stream sediment and tantalum ore as well as actual sample of a pegmatite mine in Namibia were determined according to the experimental method. The relative standard deviations (RSDs, n=7) of determination results were between 0.78% and 9.6%. The absolute values of the logarithmic difference between the measured and the certified values (|ΔlgC|, n=7) ranged from 0.000 2 to 0.020. The measured values of certified reference materials were basically consistent with the certified values. The spiked recoveries of actual samples were between 93% and 104%.
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