Abstract：During determination of trace Tl in converter graphite sphere sample by inductively coupled plasma mass spectrometry (ICP-MS), the coexisting elements, including Hg, Pb, and rare earth elements (Ir, Os, Re, etc) will cause polyatomic interference with the determination of 205Tl+ in the form of hydride polyatomic ions (1H204Hg+, 1H204Pb+) and rare earth compound ions (12C193Ir+, 14N191Ir+, 16O189Os+ and 18O187Re+). The sample was calcinated at 750 ℃ for 1 h and then dissolved with 10 mL HCl-10 mL HNO3-5 mL HF-3 mL HClO4 system. In tandem quadrupole (MS/MS) mode, the mass-to-charge ratio (m/z) of the first-stage mass filter (Q1) was set to 205, so that 205Tl+ entered the collision reaction pool with 12C193Ir+,14N191Ir+,16O189Os+,18O187Re+, etc. At the same time, O2 was introduced into the collision reaction cell, which could react with 205Tl+ to form 205Tl16O+, while the interference ions did not react with O2. The m/z of the second-stage mass filter (Q2) was set to 221, so that only 205Tl16O+ could pass through and entered the detector, thus eliminating the mass spectral interference. Based on this, a method for determination of trace Tl in converter graphite sphere by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) at oxygen reaction mode was established. The flow rate of O2 was optimized and 0.5 mL/min was selected. The matrix effect and the effect of internal standard correction were investigated. The results showed that the matrix effect could be ignored, and the influence of instrument signal drift on the determination could be overcome by the internal standard correction of 5 μg/L In. The linear range of this method was 0.01-1.00 μg/L, the linear correlation coefficient was 0.999 8, the limit of detection was 0.000 65 μg/g, and the limit of quantification was 0.002 0 μg/g. The recovery tests of Tl in converter graphite sphere sample were conducted according to the proposed method, and the recoveries were between 95% and 105%. The contents of Tl in converter graphite sphere samples were determined by the proposed method. The relative standard deviations(RSD,n=11) were between 1.6%-2.4%, and the results were basically consistent with graphite furnace atomic absorption spectrometry.
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