Abstract：The content of Co in superalloys is relatively high. During the determination of As in superalloys by inductively coupled plasma mass spectrometry (ICP-MS), the analysis of As will be seriously interfered by 59Co16O+, which is always a research difficulty in the determination of trace As in superalloys by ICP-MS. O2 was introduced to the collision/reaction cell at tandem quadrupole (MS/MS) mode, and the first-level mass filter (Q1) was set to m/z=75. 75As+ could react with O2 to generate 75As16O+, while the interfering ions could not react with O2. The secondary mass filter (Q2) was set to m/z=91. Only 75As16O+ passed through and was detected by the detector, thus avoiding the mass spectrum interference of 59Co16O+. Based on this, a new method for the determination of trace As in superalloys by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) was established. A series of standard solutions with 1.000 ng/mL As and 1.000-1 000 μg/mL Co were used to investigate the mass spectrum interference of Co to As in the two modes, i.e., single quadrupole and tandem quadrupole (MS/MS). The results showed that the recoveries of As were all about 100% at MS/MS mode. It indicated that the serious interference caused by Co could be eliminated successfully through two mass selections at MS/MS mass transfer mode, where O2 was used as the reactant gas. The flow rate of O2 was optimized, and 0.375 mL/min was finally selected. The linear range of the method was 1.00-100 ng/mL with the linear correlation coefficient of 1.000 0. The limit of detection and the limit of quantification was 0.006 7 μg/g and 0.023 μg/g, respectively. The content of As in pure cobalt standard sample was determined according to the experimental method. Meanwhile, the standard addition recovery test was carried out. The recoveries were between 96% and 102%. The established method was applied to determine As in nickel-based superalloy reference materials and superalloy samples. The found results were basically consistent with the certified values or those obtained by atomic fluorescence spectrometry. The relative standard deviations (RSD, n=6) of the determination results of actual samples were between 1.6% and 2.8%.
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