A flow-through column electrolytic cell for supercritical fluid chromatography.
A flow-through column electrolytic cell for supercritical fluid chromatography.
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用于超临界流体色谱的流通柱电解池。
DOI：
10.1002/jssc.201700317
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发表时间：
2017
影响因子：
3.1
通讯作者：
H. Hakamata
中科院分区：
文献类型：
--
作者：
Kazuhiro Yamamoto;T. Ueki;Naoyuki Higuchi;Kouji Takahashi;Akira Kotani;H. Hakamata
提出了一种新型的流通柱电解槽作为超临界流体色谱电流信号的检测器。该电池由两个电极及其固定器组成，一个工作电极和一个对电极由192根碳串制成，这些碳串由直径为10μm的400根碳纤维填充到热缩管内。这些电极被放置在由聚醚醚酮块制成的夹持器的中心，并通过聚四氟乙烯膜过滤器进行分离。为了评价该电解槽的灵敏度，将二茂铁标准溶液注入到与电解槽相连的超临界流体色谱系统中。二茂铁通过硅胶柱洗脱，流动相为超临界二氧化碳和含有乙酸铵的甲醇改进剂的混合物。二茂铁的当前峰面积与二茂铁的浓度在10-400molμ/L范围内呈良好的线性关系(r=0.999)。此外，从3的信噪比估计，柱上的检测下限为9.8亿×10-13兆摩尔。
A novel flow-through column electrolytic cell was proposed as a detector to obtain current signals for supercritical fluid chromatography. The electrochemical cell consisted of two electrodes and its holder, and a working and a counter electrode were fabricated from 192 carbon strings, which were composed of 400 carbon fibers of 10 μm in diameter filled into a heat-shrinkable tube. These electrodes were placed in the center of a holder made from polyether ether ketone blocks and they were separated by polytetrafluoroethylene membrane filters. To evaluate the sensitivity of this cell, a standard solution of ferrocene was injected into the supercritical fluid chromatography system connected to the electrolytic cell. The ferrocene was eluted through a silica gel column using a mixture of a mobile phase of supercritical CO2 and a modifier of methanol containing ammonium acetate. The current peak area of ferrocene correlated to the ferrocene concentration in the range of 10-400 μmol/L (r = 0.999). Moreover, the limit of detection on the column estimated from a signal-to-noise ratio of 3 was 9.8 × 10-13 mol.