惠泊宁, 李维敏, 任洁, 梁伟, 文惠民, 周军. 电感耦合等离子体原子发射光谱法测定N36锆合金中微量钼和铅[J]. 分析测试技术与仪器, 2019, 25(1): 15-21. DOI: 10.16495/j.1006-3757.2019.01.004
引用本文: 惠泊宁, 李维敏, 任洁, 梁伟, 文惠民, 周军. 电感耦合等离子体原子发射光谱法测定N36锆合金中微量钼和铅[J]. 分析测试技术与仪器, 2019, 25(1): 15-21. DOI: 10.16495/j.1006-3757.2019.01.004
HUI Bo-ning, LI Wei-min, REN Jie, LIANG Wei, WEN Hui-min, ZHOU Jun. Determination of Trace Molybdenum and Lead in N36 Zirconium Alloy by Inductively Coupled Plasma Optical Emission Spectrometry[J]. Analysis and Testing Technology and Instruments, 2019, 25(1): 15-21. DOI: 10.16495/j.1006-3757.2019.01.004
Citation: HUI Bo-ning, LI Wei-min, REN Jie, LIANG Wei, WEN Hui-min, ZHOU Jun. Determination of Trace Molybdenum and Lead in N36 Zirconium Alloy by Inductively Coupled Plasma Optical Emission Spectrometry[J]. Analysis and Testing Technology and Instruments, 2019, 25(1): 15-21. DOI: 10.16495/j.1006-3757.2019.01.004

电感耦合等离子体原子发射光谱法测定N36锆合金中微量钼和铅

Determination of Trace Molybdenum and Lead in N36 Zirconium Alloy by Inductively Coupled Plasma Optical Emission Spectrometry

  • 摘要: 建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定N36锆合金中微量钼和铅的分析方法.讨论了样品溶解、基体效应干扰、谱线选择和观测方式等对测定结果的影响.采用均匀试验设计确定最适合的仪器测定参数,包括等离子气流量、辅助气流量、雾化气流量和等离子体发生器功率.结果表明,锆基体对测定结果有较大影响,在试验中采用基体匹配消除干扰,在试验设计优化的仪器测定参数下,使用N36锆合金样品对方法的精密度与准确度进行验证,相对标准偏差(RSD,n=11)低于5%,加标回收率为93%~104%.所建立的方法快捷、简便、准确,满足核用N36锆合金中微量钼和铅元素的分析要求.

     

    Abstract: A method for the determination of trace molybdenum and lead in N36 zirconium alloy by inductively coupled plasma optical emission spectrometry(ICP-AES) was set up. The effects of sample dissolution methods, the matrix interference, analysis spectral line, plasma view, etc., were discussed. The method of uniform experimental design was used to investigate the optimal conditions of plasma gas flow, auxiliary gas flow, nebulizer gas flow and RF power. The results showed that the zirconium matrix has a fairly great effect on the determination results. In the study, matrix matching was used to eliminate the interference. The precision and accuracy of the method were validated by using the N36 zirconium alloy sample with the instrument parameters optimized by the uniform experimental design. The relative standard deviation (RSD, n=11) was less than 5%, and the recovery was between 93% and 104%. This method is rapid, simple, accurate, and meets the analytical requirements for trace molybdenum and lead in N36 zirconium alloy for nuclear reactor.

     

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