Abstract：During the determination of trace Sc, Ir and Pt in high purity hafnium by single quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS), the interferences from matrix oxide and double charge ion of Zr are serious. The sample was dissolved with nitric acid and hydrofluoric acid. The tandem mass spectrometry (MS/MS) mode was used for analysis. Only target ions and interfering ions were allowed to enter collision/reaction cell (CRC) after filtration of the first quadrupole mass filter(Q1).After O2 was injected into the CRC as the reaction gas, the mass-to-charge ratio of the second quadrupole mass filter (Q2) was set to 61 and 191, respectively, then the target ion products passed through Q2 and entered the detector in the form of 45Sc16O+ and 191Ir+, thus eliminating the interference of double charge of Zr with Sc and matrix oxide with Ir. After NH3 was injected into the CRC, the mass-to-charge ratio of Q2 was set to 232, then the target ion products passed through Q2 and entered the detector in the form of 198Pt(NH3)2+, thus eliminating the interference of matrix oxide with Pt. Cs was used as internal standard element to correct Sc, and Tl was used to correct Ir and Pt. The calibration curve was prepared with matrix matching method to overcome the influence of matrix effect. Accordingly, a method for determination of Sc, Ir and Pt in high purity hafnium by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS) was established. The calibration curves were prepared with the mass concentration of Sc, Ir and Pt as x-coordinate, and the ratio of signal intensity of Sc, Ir and Pt against internal standard element as y-coordinate. The results showed that the linear ranges for Sc, Ir and Pt were all 2-50 ng/mL. The linear correlation coefficients were all higher than 0.999 5. The limits of detection were in range of 0.001 1-0.006 0 μg/g, and the limits of quantification were in range of 0.004-0.020 μg/g. The contents of Sc, Ir and Pt in 1# high purity hafnium sample were determined parallelly for 11 times according to the experimental method. The results were basically consistent with those obtained by glow discharge mass spectrometry (GDMS). The relative standard deviations (RSD, n=11) were all less than 15%. 2# high purity hafnium sample was determined according to the experimental method. Moreover, the standard addition recovery tests were conducted. The recoveries were between 96% and 102%.
墨淑敏, 邱长丹, 李爱嫦, 祝利红, 李娜. 电感耦合等离子体串联质谱法测定高纯铪中钪铱铂[J]. 冶金分析, 2022, 42(9): 9-15.
MO Shumin, QIU Changdan, LI Aichang, ZHU Lihong, LI Na. Determination of scandium,iridium and platinum in high purity hafnium by inductively coupled plasma tandem mass spectrometry. , 2022, 42(9): 9-15.
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