Abstract：The determination of trace cadmium in high-purity molybdenum is severely affected by multi-atomic ions such as molybdenum-oxygen and molybdenum-nitrogen, so it difficult to accurately analyze it even using high-resolution mass spectrometer. In order to effectively eliminate the interference, the reaction cell technique of tandem mass spectrometry was employed. 111Cd was selected as the analytical isotope. The variation trends of signal strength of 1000μg/mL Mo standard solution and 1000μg/mL Mo-1.000ng/mL Cd mixed standard solution as well as background equivalent concentration (BEC) were discussed under H2 mode and NH3 mode, respectively. The flow rate of gas was also optimized. Finally 0.4mL/min of NH3 was selected as the reaction gas. At this time, the BEC of Cd in 1000μg/mL Mo standard solution was about 0.8ng/L, indicating that the interference of multi-atomic ions such as molybdenum-oxygen and molybdenum-nitrogen could be effectively eliminated. Under the selected instrumental conditions, the linear correlation coefficient of calibration curve was higher than 0.9999, the detection limit of method was 2.7ng/g, and the recoveries were between 93% and 105%. The determination method of trace cadmium in high-purity molybdenum by inductively coupled plasma tandem mass spectrometry was established. The proposed method was applied for the analysis of high-purity molybdenum samples. The relative standard deviations (RSD, n=5) of measured results were between 0.50% and 4.2%
刘元元, 胡净宇. 电感耦合等离子体串联质谱法测定高纯钼中痕量镉[J]. 冶金分析, 2018, 38(5): 1-6.
LIU Yuan-yuan, HU Jing-yu. Determination of trace cadmium in high-purity molybdenum by inductively coupled plasma tandem mass spectrometry. , 2018, 38(5): 1-6.
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