摘要
该文建立了聚变堆燃料循环系统中氢氘组分的微气相色谱定量分析方法。采用MnCl_(2)溶液改性的氧化铝色谱柱(4~6 m×0.53 mm)为分离柱,考察了改性液含量、色谱柱长和载气流量对氢氘组分分析的影响,在液氮低温(77 K)条件下实现了H_(2)、HD和D_(2)混合物的分离。结果表明,19%MnCl_(2)溶液处理的色谱柱分离氢同位素的效果优于15%MnCl_(2)溶液处理的色谱柱;柱越长,H_(2)和HD的分离效果越好,当色谱柱长度大于5 m时,H_(2)和HD组分可以完全分离,分离度大于1.5;HD和D2的最小理论塔板高度分别为0.013 cm和0.016 cm。He中H_(2)、HD、D23组分氢同位素在0%~10%含量范围内的线性相关系数均不低于0.993,检出限(LOD)分别为600.1、343.8、654.5μL/L。方法的相对标准偏差为0.34%~1.5%。该法是一种快速、准确、实用的氢同位素分析方法,有望用于聚变堆D/T燃料循环系统氢同位素气体的测定。
A micro gas chromatography was established for the quantitative analysis of hydrogen and deuterium components in fusion reactor fuel cycle system.An alumina column(4~6 m × 0. 53 mm)was modified with MnCl_(2) solution.Effects of concentration of modified liquid,length of column and flow rate of carrier gas on the analysis of H/D components were studied.The mixture of H_(2),HD and D_(2) were separated at LN2 cryogenic temperature(77 K).The results indicated that the column treated with 19%MnCl_(2) solution was better than that treated with 15% MnCl_(2) solution for the separation of hydrogen isotopes.The longer the column length,the better the separation effect of H_(2) and HD. Under the experimental conditions,H_(2) and HD components could be completely separated when the column length was longer than 5 m,and the peak resolution between H_(2) and HD was larger than 1. 5,resulting in the effective separation of the hydrogen isotope.Furthermore,the minimum values of HETP for HD and D_(2) were 0. 013 cm and 0. 016 cm in the experiment,respectively.As for the three hydrogen isotopes in He,there were good linear relationships for the three components in the concentrations range of 0%-10%,with their correlation coefficients not less than 0. 993 and the detection limits(LODs)of 600. 1,343. 8,654. 5 μL/L for H_(2),HD and D_(2),respectively.The peak area relative standard deviations(RSDs)were in the range of 0. 34%-1. 5%.The method is a rapid,accurate and applicable analysis method for hydrogen isotope,which is expected to be applied to the analysis of hydrogen isotope gases in the D/T fuel cycle system of fusion reactor.
作者
刘振兴
杨洪广
赵崴巍
杨丽玲
LIU Zhen-xing;YANG Hong-guang;ZHAO Wei-wei;YANG Li-ling(Anhui CNNC Tongyuan Technology Co.,Ltd.,Anqing 231400,China;China Institute of Atomic Energy,Beijing 102413,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2022年第2期266-270,共5页
Journal of Instrumental Analysis
基金
国家磁约束核聚变能研究专项资助(2017YFE0300300,2011GB111006)。
关键词
氢氘组分
燃料循环
微气相色谱
hydrogen deuterium components
fuel cycle
micro gas chromatography
