氢化物发生-原子荧光光谱法测定纯锆中微量铋  

Determination of trace bismuth in pure zirconium by hydride generation-atomic fluorescence spectrometry

作　　者：杨峥 梁钪 张艳 刘喜山 庞晓辉 高颂 YANG Zheng;LIANG Kang;ZHANG Yan;LIU Xi-shan;PANG Xiao-hui;GAO Song(AECC Beijing Institute of Aeronautical Materials,Beijing 100095,China;Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation,Beijing 100095,China;Key Laboratory of Science and Technology on Aeronautical Materials Testing and Evaluation,Aeroengine Corporation of China,Beijing 100095,China;Aviation Key Laboratory of Science and Technology on Materials Testing and Evaluation,Beijing 100095,China)

机构地区：[1]中国航发北京航空材料研究院,北京100095 [2]航空材料检测与评价北京市重点实验室,北京100095 [3]中国航空发动机集团材料检测与评价重点实验室,北京100095 [4]材料检测与评价航空科技重点实验室,北京100095

出　　处：《冶金分析》2020年第11期63-67,共5页Metallurgical Analysis

摘　　要：纯锆被广泛应用于航空航天、航海和核反应堆等领域。铋元素对锆的耐腐蚀性有重要影响,准确测定纯锆中铋含量非常重要。实验建立了氢化物发生-原子荧光光谱法(HG-AFS)测定纯锆中微量铋元素的分析方法。采用HCl-HNO3-HF可将纯锆完全溶解;以硫脲-抗坏血酸为预还原剂,12g/L硼氢化钾溶液为还原剂,20%(体积分数)盐酸为测定介质,光电倍增管负高压为300V,灯电流为80mA,实现了HG-AFS对纯锆中铋的测定。实验表明锆基体对铋元素测定的干扰可忽略,因此配制标准溶液系列时不需要进行锆基体的匹配。铋校准曲线的线性范围为0.00005%~0.0010%,校准曲线线性相关系数r=0.9998;方法检出限为0.000002%。按照实验方法分析3个纯锆样品中铋,结果的相对标准偏差(RSD,n=10)为0.29%~0.75%;测定结果与电感耦合等离子体质谱法(ICP-MS)基本一致。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(12 g/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 300 V;the lamp current was 80 mA.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).

关 键 词：氢化物发生-原子荧光光谱法(HG-AFS) 纯锆 铋 

分 类 号：O657.31[理学—分析化学] TF801.3[理学—化学]