Determination of trace bismuth in pure zirconium by hydride generation-atomic fluorescence spectrometry
YANG Zheng1, 2, 3, 4, LIANG Kang*1, 2, 3, 4, ZHANG Yan1, 2, 3, 4, LIU Xi-shan1, 2, 3, 4 PANG Xiao-hui1, 2, 3, 4, GAO Song1, 2, 3, 4
1. AECC Beijing Institute of Aeronautical Materials, Beijing 100095, China; 2. Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation, Beijing 100095, China; 3. Key Laboratory of Science and Technology on Aeronautical Materials Testing and Evaluation, Aeroengine Corporation of China, Beijing 100095, China; 4. Aviation Key Laboratory of Science and Technology on Materials Testing and Evaluation, Beijing 100095, China
Abstract：Pure zirconium is widely used in aerospace, navigation, nuclear reactor and other fields. As bismuth greatly influences on the corrosion resistance of zirconium, it is very important to accurately determine the bismuth content in pure zirconium. An analysis method for the determination of trace bismuth in pure zirconium by hydride generation-atomic fluorescence spectrometry (HG-AFS) was established. The results showed that pure zirconium sample could be completely dissolved with HCl-HNO3-HF. The determination of bismuth in pure zirconium by HG-AFS was realized under the following experimental conditions: thiourea-ascorbic acid was used as the pre-reducing agent; the potassium borohydride solution (12g/L) was selected as the reducing agent; 20% (volume fraction) hydrochloric acid was used as determination medium; the negative high voltage of photomultiplier tube was 300V; the lamp current was 80mA. It was found that the interference of zirconium matrix with the determination of bismuth could be ignored, so the matching of zirconium matrix was not required for the preparation of standard solution series. The linear range of calibration curve for bismuth was 0.00005%-0.0010%, and the linear correlation coefficient was r=0.9998. The limit of detection was 0.000002%. The contents of bismuth in three pure zirconium samples were analyzed by the proposed method. The relative standard deviations (RSD, n=10) of determination results were between 0.29% and 0.75%. The found results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).
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