Determination of thallium in rock sample by inductively coupled plasma mass spectrometry with ether extraction separation
GAO Xiao-fei1,2,3, ZHAO Yi-fan1,2,3, MAO Xiang-ju1,2,3, ZHANG Hong-li*1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Key laboratory of Evaluation and Multipurpose Utilization of Polymetallic Ores Ministry of Land and Resources, Zhengzhou 450006, China
Abstract：The accurate determination of thallium content in rock samples was of great significance for the monitoring of thallium pollution in mineral mining and processing. Since the content of thallium in rock sample was usually very low, the separation and enrichment of thallium should be conducted before determination of thallium to eliminate the interference of many matrix elements. The rock sample was decomposed with hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid. The hydrobromic acid was added into sample solution to react with Tl3+ to form thallium bromide complex. The thallium bromide complex was then extracted with ether, realizing the separation of thallium from matrix elements. The ether extract liquor was heated on electric hot plate at 60℃ to remove ether by volatilization. The residual ether was further removed by digestion with heating and addition of nitric acid. After leaching with nitric acid and hot water, the content of thallium was determined by inductively coupled plasma mass spectrometry (ICP-MS) with 5.0ng/mL 185Re as internal standard and 205Tl+ as determination object. Thus, the determination method of thallium in rock sample was realized. The experimental results showed that the mass concentration of thallium in the range of 5.00-40.00ng/mL was linear to the ratio of signal intensity to thallium and internal standard. The correlation coefficient was 0.9998. The detection limit of method was 0.0049ng/mL. The proposed method was applied for the analysis of rock actual samples. The relative standard deviations (RSD, n=6) of determination results were all less than 5%. The spiked recoveries were between 96% and 103%. The content of thallium in certified reference material of rock was determined, and the found results were basically consistent with the certified values
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