Abstract：There is serious mass spectrometry interference during the determination of trace P and S in superalloys by inductively coupled plasma mass spectrometry, thus affecting the determination results. The sample was dissolved with aqua regia-hydrofluoric acid. The mass-to-charge ratio (m/z) of the first-order mass filter (Q1) were set as 31 and 32 at the mode of tandem quadrupole (MS/MS), respectively. Then O2 was injected into collision/reaction cell. 31P+ and 32S+ would react with O2 to generate 31P16O+ and 32S16O+, while the interfering ions could not react with O2. The m/z of the second-order mass filter (Q2) were set as 47 and 48, respectively. Therefore, only 31P16O+ and 32S16O+ were passed and detected by the detector, which avoided the mass spectrometry interference. Accordingly, the method for the determination of trace P and S in superalloys by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) was established. The flow rate of O2 was optimized to be 0.375 mL/min. The linear range of the method was 1.00-100 μg/L, and the linear correlation coefficients were not less than 0.999 7. The limit of detection for P and S was 0.075 μg/g and 0.086 μg/g, and the limit of quantification was 0.23 μg/g and 0.26 μg/g, respectively. The certified reference material of high-purity nickel was selected as the determination object, and the contents of P and S were determined according to the experimental method. Meanwhile, the spiked recovery tests of blank were conducted. The recoveries were between 96% and 109%. The established method was applied to the determination of P and S in superalloy certified reference materials and superalloy samples, and the found results were basically consistent with the certified values and those obtained by inductively coupled plasma atomic emission spectrometry or high frequency combustion infrared absorption method. The relative standard deviations (RSD,n=6) of the determination results of actual sample were between 2.0% and 4.7%.
郭红巧, 胡净宇, 侯艳霞, 齐荣, 刘晓波. 电感耦合等离子体串联质谱法测定高温合金中痕量磷和硫[J]. 冶金分析, 2021, 41(11): 1-7.
GUO Hongqiao, HU Jingyu, HOU Yanxia, QI Rong, LIU Xiaobo. Determination of trace phosphorus and sulfur in superalloys by inductively coupled plasma tandem mass spectrometry. , 2021, 41(11): 1-7.
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