Online Electrochemical Detectors for Supercritical Fluid Chromatography

Online Electrochemical Detectors for Supercritical Fluid Chromatography
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用于超临界流体色谱的在线电化学检测器

DOI:
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发表时间:
1995
期刊:
影响因子:
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通讯作者:
A. Michael
A. Michael
中科院分区:
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文献类型:
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作者:
S. Dressman;A. Michael

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一个独立的电化学电池组成的工作和准参比电极涂有导电聚合物的薄膜被用作超临界流体色谱(SFC-EC)的柱后检测器。用循环伏安法测定了二茂铁、蒽、对苯醌和对苯二酚在C18填充柱上用未改性的、乙腈改性的和甲醇改性的CO2洗脱后的色谱图。在未改性的CO2中,在检测限、响应线性和峰形方面,二茂铁的SFC-EC检测的定量性能与下游FID获得的结果相似。EC检测器的基线信号在密度梯度洗脱期间保持平坦,而FID的基线信号中发生明显的漂移。然而,FID在含有约3%(v/v)乙腈或甲醇的移动的相中完全不可操作,EC检测器在改性流体中功能良好。因此,EC检测器与未改性的和改性的CO2移动的相兼容。这些新开发的SFC检测器的一个有价值的特征是它们与对SFC重要的分离条件的非常大部分的黑麦兼容
A self-contained electrochemical cell consisting of a working and a quasi-reference electrode coated with a thin film of a conductive polymer was used as a postcolumn detector for supercritical fluid chromatography (SFC-EC). Cyclic voltammetry was used to obtain chromatograms of ferrocene, anthracene, p-benzoquinone, and hydroquinone after they elution from a C 18 packed column with unmodified, acetonitrile-modified, or methanol-modified CO 2 . In unmodified CO 2 , the quantitative performance of the SFC-EC detection of ferrocene was similar to that obtained with a downstream FID with respect to detection limit, response linearity, and peak shape. The baseline signal of the EC detector remained flat during density gradient elution while a noticeable drift occurred in the baseline signal of the FID. Futhermore, whereas the FID was totally inoperable in a mobile phase containing ∼3% (v/v) of either acetonitrile or methanol, the EC detector functioned well in the modified fluids. Thus, the EC detector is compatible with both unmodified and modified CO 2 mobile phases. A valuable feature of these newly developed SFC detectors is they compatibility with a very large fraction of the rye of separation conditions that are important to SFC