电感耦合等离子体质谱法测定核级海绵锆中痕量硼

doi:10.13228/j.boyuan.issn1000-7571.011335

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摘要硼的存在会严重影响核级海绵锆的中子平衡和反应堆的正常运转,因此,需要准确测定核级海绵锆中痕量硼。在采用电感耦合等离子体质谱法(ICP-MS)测定核级海绵锆中痕量硼时,锆基体干扰比较严重,必须对其进行校正或消除。实验用硝酸和氢氟酸溶解样品,以¹¹B为测定同位素,采用标准加入法克服基体干扰,建立了ICP-MS测定核级海绵锆中痕量硼的方法。结果表明,在优化的实验条件下,硼质量浓度在0.50~10.00 μg/L范围内与其对应的信号强度呈线性关系,相关系数为0.999 5,方法检出限为0.038 μg/g,定量限为0.125 μg/g。按照实验方法测定6个核级海绵锆样品中硼,结果的相对标准偏差(RSD)为2.3%,加标回收率为102%;采用分光光度法进行方法对照试验,两种方法测定结果基本一致。

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	荆慧
	罗凤焱
	李洁
	耿来垚
	赵峰
	盛红伍

关键词 ：电感耦合等离子体质谱法(ICP-MS), 标准加入法, 核级海绵锆, 硼

Abstract：The presence of boron will seriously affect the neutron balance of nuclear-grade zirconium sponge and the normal operation of the reactor. Therefore, it is necessary to accurately determine the trace amounts of boron in nuclear-grade sponge zirconium. During the determination of trace boron in nuclear-grade zirconium sponge by inductively coupled plasma mass spectrometry (ICP-MS), the interference of zirconium matrix is relatively serious, which must be corrected or eliminated. The sample was dissolved with nitric acid and hydrofluoric acid. ¹¹B was selected as the determination isotope. The matrix interference was overcome by the standard addition method. The determination method of trace boron in nuclear-grade zirconium sponge by ICP-MS was established. The results showed that the mass concentration of boron had a linear relationship with its corresponding signal intensity in the range of 0.50-10.00 μg/L under the optimized experimental conditions. The correlation coefficient was 0.999 5. The limit of detection was 0.038 μg/g. The limit of quantification was 0.125 μg/g. The content of boron in six samples of nuclear-grade zirconium sponge was determined according to the experimental method. The relative standard deviation (RSD) of the measurement results was 2.3%, and the spiked recovery was 102%. The spectrophotometry was used for control test, and the results of two methods were basically consistent.

Key words： inductively coupled plasma mass spectrometry (ICP-MS) standard addition method nuclear-grade zirconium sponge boron

收稿日期: 2020-11-13

ZTFLH:	O657.63
	TF841.4

作者简介: 荆慧(1992—),女,助理研究员,硕士,主要从事材料研究及分析工作;E-mail:15822218752@163.com

引用本文:

荆慧, 罗凤焱, 李洁, 耿来垚, 赵峰, 盛红伍. 电感耦合等离子体质谱法测定核级海绵锆中痕量硼[J]. 冶金分析, 2021, 41(8): 72-75. JING Hui, LUO Fengyan, LI Jie, GENG Laiyao, ZHAO Feng, SHENG Hongwu. Determination of trace boron in nuclear-grade zirconium sponge by inductively coupled plasma mass spectrometry. , 2021, 41(8): 72-75.

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