Determination of oxygen,nitrogen and hydrogen in vanadium-nitrogen alloy materials by pulse heating-time of flight mass spectrometry
DAN Juan1,2,CHEN Xiao-yi1,2,LIU Lin1,2,YANG Qian-qian3,HOU Hong-xia3
1.National Center for Quality Supervision and Inspection of Vanadium and Titanium Products,Panzhihua 617000,China; 2.Product Quality Supervision and Testing Institute of Panzhihua,Panzhihua 617000,China; 3.Central Iron & Steel Research Institute,Beijing 100081,China
Abstract：With the increasing inspection requirements on content of trace impurity elements, a simultaneous determination method of oxygen, nitrogen and hydrogen in vanadium-nitrogen alloy was developed. 0.050 g of sample after treatment was packed with clean nickel foil and put into nickel basket, which was then put into degassed high temperature graphite crucible. The analytical power was controlled at 4.5 kW. The content of oxygen, nitrogen and hydrogen in vanadium-nitrogen alloy materials was simultaneously determined by pulse heating-time of flight mass spectrometry using 12C+, 14N+ and 2H+ as the analytical line, respectively. The experimental results showed that the linear correlation coefficients of calibration curves under optimal conditions were higher than 0.999. The detection limit of oxygen, nitrogen and hydrogen in proposed method was 0.02, 0.06 and 0.002 μg/g, respectively. The proposed method was applied to the determination of oxygen (6.5-94.3 μg), nitrogen (12-264 μg) and hydrogen (0.10-8.8 μg) in vanadium-nitrogen alloy samples. The determination results were basically consistent with those obtained by pulse heating-infrared thermal conductivity detection method (IR/TCD). The relative standard deviations (RSD, n=7) of oxygen and nitrogen were less than 9%, while the standard deviation (SD, n=7) of hydrogen was not higher than 0.000 5%.
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DAN Juan,CHEN Xiao-yi,LIU Lin,YANG Qian-qian,HOU Hong-xia. Determination of oxygen,nitrogen and hydrogen in vanadium-nitrogen alloy materials by pulse heating-time of flight mass spectrometry. , 2016, 36(6): 8-12.
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