首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Fast temperature programming on a stainless-steel narrow-bore capillary column by direct resistive heating for fast gas chromatography
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Fast temperature programming on a stainless-steel narrow-bore capillary column by direct resistive heating for fast gas chromatography

机译:通过直接电阻加热在不锈钢窄口毛细管柱上进行快速温度编程,以进行快速气相色谱分析

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摘要

A direct resistive-heating fast temperature programming device for fast gas chromatography was designed and evaluated. A, stainless-steel (SS) capillary column acted both as a separation column and as a heating element. A fast temperature controller with the deviation derivative proportional-integral-derivative (DDPID) control algorithm, which was suitable for ramp control using ramip-to-setpoint function, was used to facilitate the fast pulse heating. The SS resistive-heating column can generate linear temperature ramps up to 10 degrees C/s and can re-equilibrium from 250 degrees C down to 50 degrees C within 30s. With n-alkanes as the test analytes, the relative standard deviations (RSDs) of retention time were between 0.19 and 0.59% and the RSDs of their peak areas were less than 4% for all but one. The results indicated that this technique could be used for both qualitative and quantitative analysis. Phenolic and nitroaromatic compounds were also analyzed by using the SS resistive-heated system. The combination of a short narrow-bore SS column and rapid heating rates provides sufficient separation efficiency for relatively simple mixtures at drastically reduced analysis time. The total analysis time including equilibration time was less than 2 min for all test mixtures in this study. (C) 2007 Elsevier B.V. All rights reserved.
机译:设计并评估了一种用于快速气相色谱的直接电阻加热快速温度编程装置。不锈钢(SS)毛细管柱既充当分离柱又充当加热元件。使用具有偏差微分比例积分微分(DDPID)控制算法的快速温度控制器,该算法适用于使用“ Ramp-to-setpoint”功能的斜坡控制,以促进快速脉冲加热。 SS电阻加热塔可以产生高达10摄氏度/秒的线性温度上升,并且可以在30秒内从250摄氏度重新平衡至50摄氏度。以正构烷烃为测试分析物,保留时间的相对标准偏差(RSD)在0.19至0.59%之间,除一个峰外,所有峰面积的RSD均小于4%。结果表明,该技术可用于定性和定量分析。还使用SS电阻加热系统分析了酚和硝基芳族化合物。短口径SS色谱柱和快速加热速率的结合,可以在大大减少分析时间的情况下为相对简单的混合物提供足够的分离效率。对于本研究中的所有测试混合物,包括平衡时间在内的总分析时间少于2分钟。 (C)2007 Elsevier B.V.保留所有权利。

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