Determination of 69 impurity elements in high-purity rhenium powder by pulsed glow discharge mass spectrometry

An analytical method for the determination of impurity elements in high-purity rhenium powder based on pulsed glow discharge mass spectrometry (Pulsed-GDMS) was established in this study. The experimental results indicated that the forming difficulty of rhenium powder due to high elasticity modulus could be effectively overcome using an ultra-high-pressure sample preparation system, which stepwise increased the pressure to 200 t, in combination with a thickened polytetrafluoroethylene cup as mold. The pressed powder sample obtained could meet the analytical requirements. The instrument conditions were systemically optimized and the optimal discharge parameters were obtained as follows: the pulse voltage was 950 V, the flow rate of discharge gas was 400 mL/min, the pulse duration was 90 μs, and the pre-sputtering time was 35 min. The MS interference was investigated in detail, and the appropriate isotopes and resolution mode were selected for testing elements. The limits of detection of method ranged from 0.001 to 0.98 μg/g, and the lower limits of quantification ranged from 0.003 to 3.3 μg/g. The contents of 69 impurity elements in high-purity rhenium powder were determined according to the experimental method, and the relative standard deviations (RSD, n=7) of determination results were all less than 25%. The proposed method was compared with inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and atomic absorption spectrometry (AAS). Except for the measurement result of W, which had certain deviation with ICP-MS due to the excitation characteristics of powder sample, the determined results of other elements were basically consistent with those obtained by other methods, indicating that the proposed method had good accuracy and reliability.