多维色谱技术快速检测电子气中痕量气体杂质的方法研究

Research on the Method of Rapid Detection of Trace Gas Impurities in Electronic Degrade Gas by Multidimensional Chromatography

采用多维气相色谱,通过不同色谱柱的组合变换、配合反吹、中心切割等操作技术,分别对六氟化硫、四氟化碳、氢气3种电子气中的6~7种杂质检测进行了方法开发。使用气体稀释法作出了5个浓度下氢气中各组分的响应校准曲线,线性良好,最低浓度点0.05×10^-6 mol/mol时的RSD均小于10%。系统地描述了3种电子气检测方法的开发过程和经验技巧,计算了检出限,均远好于市场检测需求,其中六氟化硫各组分检出限在20.3×10^-9~30.3×10^-9 mol/mol,四氟化碳各组分检出限在16.2×10^-9~25.5×10^-9 mol/mol,氢气各组分检出限在8.1×10^-9~15.6×10^-9 mol/mol,方法重复性好、检测效率高,可作为标准操作规范向社会开放共享。

In this work,the multi-dimensional gas chromatography was used,as long as the back-flush and center-cut technology,to developing the analyzing method of 6~7 impurities in three electronic grade gases:sulfur hexafluoride,carbon tetrafluoride and hydrogen with the combination of different chromatographic columns.The gas dilution method was used to make a response calibration curve for each component in hydrogen at 5 concentrations.The linearity was good,and the RSD at the lowest concentration point of 0.05×10^-6 mol/mol was less than 10%.The development process and experience skills of three electronic grade gas analysis methods were systematically described.The limits of detection were calculated,which are far better than the market detection requirements.The detection limits of each component were 20.3×10^-9~30.3×10^-9 mol/mol,16.2×10^-9~25.5×10^-9 mol/mol and 8.1×10^-9~15.6×10^-9 mol/mol for sulfur hexafluoride,carbon tetrafluoride and hydrogen,respectively.The methods had good repeatability and high detection efficiency,and could be shared with the society as a standard operating specification.