Determination of trace gallium, indium, thallium, cadmium andgermanium in lead ore by inductively coupled plasmamass spectrometry with closed digestion
Abstract：The lead deposit usually contained high-grade various scattered elements, so the accurate determination of Ga, In, Tl, Cd and Ge in lead ore has important significance to the saving, development and utilization of ore resources. The sample was digested in closed system. During the digestion process, H2SO4 (1+4) was added to precipitate and separate Pb matrix under heating in water bath. 69Ga, 115In, 205Tl, 114Cd and 72Ge were selected as the analytical isotopes. 103Rh was used as internal standard to correct Ga, In, Cd and Ge, while 187Re was used as internal standard to correct Tl. The determination of trace scattered elements in lead ore (i.e., Ga, In, Tl, Cd and Ge) was realized by inductively coupled plasma mass spectrometry (ICP-MS). The results showed that the background equivalent concentrations of Ga, Tl and Cd at standard (STD) mode were one magnitude order higher than the kinetic energy discrimination (KED) mode, while the background equivalent concentrations of In and Ge at the above two modes were similar. Therefore, the KED mode was selected for determination of Ga, Tl and Cd, and STD mode was selected for determination of In and Ge. The flow rate of He gas at KED mode was optimized, and 5.8mL/min was selected. The correlation coefficients of linear equations were not less than 0.9992. The detection limit of Ga, In, Tl, Cd and Ge was 0.0520, 0.0392, 0.0196, 0.0212 and 0.0437μg/g, respectively. The proposed method was applied for determination of Ga, In, Tl, Cd and Ge in actual sample of lead ore. The relative standard deviations (RSD, n=6) of determination results were between 1.3% and 5.0%. The recoveries were between 86% and 112%. The contents of these five elements in certified reference material of lead ore were determined according to the experimental method, and the results were consistent with the certified values.
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