1.安徽中核桐源科技有限公司,安徽 安庆 231400
2.中国原子能科学研究院,北京 102413
刘振兴,博士,副研究员,研究方向:同位素分离技术,E-mail:zxliu11@sina.com
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刘振兴,杨洪广,赵崴巍等.微气相色谱法分析氢氘同位素组分气体[J].分析测试学报,2022,41(02):266-270.
LIU Zhen-xing,YANG Hong-guang,ZHAO Wei-wei,et al.Analysis of Hydrogen Deuterium Components by Micro Gas Chromatography[J].Journal of Instrumental Analysis,2022,41(02):266-270.
刘振兴,杨洪广,赵崴巍等.微气相色谱法分析氢氘同位素组分气体[J].分析测试学报,2022,41(02):266-270. DOI: 10.19969/j.fxcsxb.21040601.
LIU Zhen-xing,YANG Hong-guang,ZHAO Wei-wei,et al.Analysis of Hydrogen Deuterium Components by Micro Gas Chromatography[J].Journal of Instrumental Analysis,2022,41(02):266-270. DOI: 10.19969/j.fxcsxb.21040601.
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D,2,的最小理论塔板高度分别为0.013 cm和0.016 cm。He中H,2,、HD、D,2, 3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、654.5 μL/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 LN,2, 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.
氢氘组分燃料循环微气相色谱
hydrogen deuterium componentsfuel cyclemicro gas chromatography
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