Simultaneous determination of oxygen, nitrogen and hydrogen in tungsten and tantalum by pulse heating-time of flight mass spectrometry
HAN Wei-ru1, ZHOU Hai-shou1, CHEN Ran1, LI Ji-dong1SHEN Xue-jing2, YANG Qian-qian2, HU Shao-cheng2
1.Beijing General Research Institute for Non-ferrous Metals, Beijing 100088, China;#br#
2. China Iron & Steel Research Institute Group, Beijing 100081, China
Abstract：Oxygen, nitrogen and hydrogen in refractory metals tungsten and tantalum were simultaneously determined by the pulse heating-time of flight mass spectrometer under optimal instrument conditions with 0.15 g of nickel foil as flux agent and self-designed graphite crucible which consists of outer and inner crucibles. The calibration curves of oxygen and nitrogen were established with steel reference materials with oxygen and nitrogen that corresponded with tungsten and tantalum products. The calibration curve of hydrogen was established with titanium reference materials with hydrogen that corresponded with tungsten and tantalum products. In this method, the detection limits of oxygen, nitrogen and hydrogen were 0.5 μg, 0.5 μg, 0.4 μg, and the limits of quantitation were 1.7 μg, 1.7 μg, 1.2 μg, respectively. The relative standard deviations (RSDs) for the determination of oxygen, nitrogen and hydrogen in tungsten sample were 5.5%, 11.5%, 8.9% (n=11), while the RSDs for the determination of oxygen, nitrogen and hydrogen in tantalum sample were 12%, 24% and 22% (n=11). The determination results of oxygen, nitrogen and hydrogen were basically consistent with those of infrared absorption method and thermoconductivity.
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