Xu Feng, Guan Wenna, Yao Guiyan, Guan Yafeng
Department of Instrumentation & Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457, Zhongshan Road, Dalian 116023, China.
J Chromatogr A. 2008 Apr 4;1186(1-2):183-8. doi: 10.1016/j.chroma.2007.08.063. Epub 2007 Sep 1.
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 ramp-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.
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升温装置。一根不锈钢（SS）毛细管柱既作为分离柱又作为加热元件。采用了具有偏差导数比例积分微分（DDPID）控制算法的快速温度控制器，该算法适用于使用斜坡到设定点函数的斜坡控制，以促进快速脉冲加热。SS电阻加热柱可产生高达10℃/s的线性温度斜坡，并能在30秒内从250℃重新平衡至50℃。以正构烷烃作为测试分析物，除一种情况外，保留时间的相对标准偏差（RSD）在0.19%至0.59%之间，其峰面积的RSD小于4%。结果表明，该技术可用于定性和定量分析。还使用SS电阻加热系统对酚类和硝基芳香族化合物进行了分析。短窄内径SS柱与快速升温速率的结合，在大幅缩短分析时间的情况下，为相对简单的混合物提供了足够的分离效率。本研究中所有测试混合物的包括平衡时间在内的总分析时间均小于2分钟。
