Abstract:
Inductively coupled plasma tandem mass spectrometry(ICP-MS/MS) has great advantages in the analysis of trace and ultra-trace impurity elements in high-purity refractory metals. In this study, the high matrix introduction(HMI) ICP-MS/MS method was employed to analyze specific interfering elements in high-purity refractory metals, such as trace silver(Ag) in high-purity niobium(Nb), trace platinum(Pt) in high-purity hafnium(Hf), and trace gold(Au) in high-purity tantalum(Ta). The HMI parameters were optimized: the carrier gas flow was 0.45 L/min, and the dilution gas flow was 0.65 L/min, enabling direct quantification using calibration curves without matrix matching.The reaction mode and action mechanism of O
2/NH
3 in tandem quadrupole mass spectrometer(MS/MS) mode was investigated to eliminate the mass spectral interference of matrix on tested elements. Ag was analyzed in the O
2 on-mass mode(primary mass filter Q1=107, secondary mass filter Q2=107) with the flow rate of 0.50 mL/min. Pt and Au were analyzed in the NH
3 mass shift mode(Pt: Q1=194, Q2=228; Q1=195, Q2=229. Au: Q1=197, Q2=231) with the flow rate of 0.75 mL/min and 0.50 mL/min, respectively. The linear ranges of Ag, Pt, and Au were 0.10-50.0 ng/mL,with correlation coefficients(r) all greater than 0.999.The limits of detection were in range of 0.001-0.035 μg/g. The standard solution of Ag, Pt, and Au with known concentration was added into high-purity Nb, Hf and Ta matrixes for the standard addition recovery tests. Moreover, the precision investigations of measurement results were also conducted. The experimental results showed that the spiked recoveries of Ag, Pt, and Au were between 83.0% and 113.0%. The relative standard deviations(RSD, n=6) of determination results were between 3.0% and 7.9%. The proposed method was applied for the analysis of three high-purity refractory metals, and the results were compared with those obtained by glow discharge mass spectrometry(GDMS). It was found that the determination results of two analysis methods were basically consistent.