Determination of nitrogen in Fe-base nanocrystal alloy by spark discharge atomic emission spectrometry
LI Yan-ping1,2, CAO Cheng1, ZHOU Shao-xiong*1,2, SHI Yi3, LI Shi-min3
1. China Iron ＆ Steel Research Institute Group, Beijing 100081, China; 2. Research and Development Center,Advance Technology ＆ Materials Co., Ltd., Beijing 100081, China; 3. Spectro Analytical Instruments GmbH of Germany, Beijing Representative Office, Beijing 100015, China
Abstract：In order to carry out the quality control analysis of nitrogen in production process of Fe-base nanocrystal alloy, the determination method of nitrogen in Fe-base nanocrystal alloy by spark discharge atomic emission spectrometry was proposed. Some questions in the determination of nitrogen were discussed, including the selection of spectral lines, the analytical conditions of nitrogen, the preparation of standard samples for internal control, the verification of sampling method, the division and treatment of analytical samples, the effects of interference by coexisting elements, and the fitting of calibration curve. The optimum analysis conditions for the determination of nitrogen were listed as below: the flow rate of high-purity argon (φ≥99.999%) was 180L/h, the flush time of argon was 2s, the precombustion (HEPS) time was 6s, the integral time was 2s, and the analytical line pair was N149.3nm/Fe149.7nm. Under the analytical conditions above, the calibration curve of nitrogen was prepared using the self-made standard sample of nitrogen-containing Fe-base nanocrystal alloy. Moreover, the effects of interference for coexisting elements were corrected. The content of nitrogen in Fe-base nanocrystal alloy sample was determined according to the experimental method. The standard deviation (RSD, n=8) of measured results was less than 7.0%. The found results were consistent with those obtained by impulse heating-thermal conductivity method. The proposed method was also applicable for the simultaneous determination of nitrogen and alloying elements in Fe-base nanocrystal alloy samples.
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