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一种直热式快速气相色谱快速升温装置的设计

许峰, 观文娜, 廉玫, 徐媛, 关亚风   

  1. 中国科学院大连化学物理研究所仪器分析化学研究室, 大连 116023
  • 收稿日期:2006-11-22 修回日期:1900-01-01 出版日期:2007-06-10 发布日期:2007-06-10
  • 通讯作者: 关亚风

Design of a Direct-heating Fast Temperature Programming Device for Fast Gas Chromatography

XU Feng, GUAN Wen-Na, LIAN Mei, XU Yuan, GUAN Ya-Feng*   

  1. Department of Instrumentation & Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2006-11-22 Revised:1900-01-01 Online:2007-06-10 Published:2007-06-10
  • Contact: GUAN Ya-Feng

摘要: 用大电流脉冲直接加热不锈钢毛细管柱, 将脉冲间隔调整到正好使柱管局部完成热平衡, 用快速PID技术控制脉冲频率和宽度, 设计了一种直热式快速升温装置. 该装置最高升温速率可达到5 ℃/s, 升温范围 40~150 ℃, 程序升温线性相关系数大于0.9996, 最大功耗74 W, 加热平均功耗小于50 W, 在34 s内完成nC8~nC17 10种正构烷烃的分离, 保留时间重复精度误差RSD在0.22%~0.55%之间, 降温和平衡时间仅为30 s. 与常规气相色谱仪相比, 该装置分析挥发性和半挥发性有机物速度可提高20倍以上, 专用于快速气相色谱仪.

关键词: 快速气相色谱, 快速程序升温, 直接电阻加热技术, 直热式色谱柱

Abstract: A direct-heating fast temperature programming device for fast gas chromatography was designed and evaluated. A metal capillary column was used both as a separation column and as a heating element. Pulsed current heating strategy was used to heat the column, and at the same time, gave the time lag for self-equilibrium of the metal tubing during a temperature programming. A fast PID control was used to facilitate the fast pulse heating. The correlation coefficients of temperature programming curves were more than 0.9996 between 40—150 ℃, with tunable heating rates varying from 1 to 5 ℃/s. The power consumption of the device was 74 W max, and was less than 50 W on average. The separation time was within 34 s for n-alkanes(nC8nC17), with relative standard deviations of the retention times between 0.22% and 0.55%. The cool down time plus the equilibration time is less than 30 s. The device is suitable for the analysis of semi-and volatile organic compounds in portable GC.

Key words: Fast gas chromatography, Fast temperature programming, Direct resistive heating technique, Direct-heating column

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