Analysis of Ultra-Trace Impurities in High Purity Molybdenum Powder through Inductively Coupled Plasma Tandem Mass Spectrometry
FU Liang1, 2, SHI Shu-yun2*, TANG You-gen2, WANG Hai-yan2
1. Collaborative Innovation Center of Green Development for Wuling Mountain Areas, Yangtze Normal University, Chongqing 408100, China
2. School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China
Abstract：An analytical method for the determination of ultra-trace impurities in high purity molybdenum was established by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS). In MS/MS mode, H2 was used as the reaction gas to measure Si and Ca through the H2 on-mass method. O2 was employed as the reaction gas to measure the Cd via the O2 on-mass method, and P, As, Se, Ta, Sn, Sb, Ba, and W were measured by the O2 mass-shift method. NH3/He was adopted as the reaction gas, so that Na, Mg, Al, K, and V could be measured by NH3/He on-mass method, and Ti, Cr, Mn, Fe, Co, Ni, Cu, and Zn could be measured by the NH3/He mass- shift method. Pb, Bi, Th, and U were measured in single quadropole (SQ) mode without gas. Compared with conventional collision/reaction cell (CRC) inductively coupled plasma mass spectrometry (ICP-MS), the background equivalent concentration (BEC) and detection limit of analyte in this method were lower, and the mass spectrum interference could be eliminated more thoroughly. Under optimized working conditions, the calibration curves of analytes showed good linearity with linear correlation coefficient (R2)≥0.999 7. The detection limit was 0.04～50.1 ng·L-1, the spike recoveries were 92.2%～107.4% and the relative standard deviation (RSD) was ≤4.3%, indicating that the proposal method has excellent accuracy and precision. The results of the sample analysis showed that the method can be used for the determination of 28 impurity elements in high purity molybdenum powder with purity of 5N (≥99.999%).
Key words：ICP-MS/MS; High purity molybdenum powder; Impurity elements; Mass-shift; On-mass
符 靓，施树云，唐有根，王海燕. 高纯钼粉中超痕量杂质的质谱分析[J]. 光谱学与光谱分析, 2018, 38(08): 2588-2594.
FU Liang, SHI Shu-yun, TANG You-gen, WANG Hai-yan. Analysis of Ultra-Trace Impurities in High Purity Molybdenum Powder through Inductively Coupled Plasma Tandem Mass Spectrometry. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2018, 38(08): 2588-2594.
