A Method to Externally Adjust the Column Length in Gas Chromatography Using a Water Stationary Phase

IF 1.2 4区 化学 Q4 BIOCHEMICAL RESEARCH METHODS Chromatographia Pub Date : 2023-12-06 DOI:10.1007/s10337-023-04299-4
Kade L. Shepherd, Kevin B. Thurbide
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Abstract

A novel method for externally adjusting the column length during gas chromatography (GC) operation is introduced. The technique employs the controlled dehydration of a water stationary phase off a stainless-steel capillary column wall, which is then removed by the carrier gas. By halting the dehydration process (i.e. through adding water to the system) at specified times, partial column (i.e. coating) lengths are created as desired. For instance, since the phase is removed in a ‘peeling’ motion from inlet to outlet, then dehydrating 1/2 of the water coating away results in a 1/2 coated column remaining. This, in turn, acts analogous to a 1/2 column length in separations. In this way, direct and effective reduction in analyte retention time results from shortening column length. Adjustable lengths from 3/4 down to 1/10 of a full column are demonstrated. Good stability in maintaining new column lengths is realized, as analyte retention times vary by only about 1% RSD for most lengths and temperatures examined. Through calibration, column length can be predictably adjusted using system dehydration time, with changes being performed in a few minutes. Results indicate that this method could be useful for adjusting column length in-situ to accommodate various samples during GC operation.

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使用水固定相外部调节气相色谱柱长度的方法
本文介绍了一种在气相色谱(GC)操作过程中从外部调节色谱柱长度的新方法。该技术通过控制不锈钢毛细管柱壁上的水固定相脱水,然后通过载气将其去除。通过在指定时间停止脱水过程(即向系统中加水),可根据需要产生部分柱(即涂层)长度。例如,由于相从入口到出口是以 "剥离 "运动的方式去除的,因此脱水 1/2的水涂层会导致剩余 1/2的涂层柱。这反过来又类似于分离中的 1/2 柱长。这样,缩短色谱柱长度就能直接有效地减少分析物的保留时间。我们展示了从 3/4 到 1/10 全柱的可调长度。保持新的色谱柱长度具有良好的稳定性,因为在大多数长度和温度下,分析物保留时间的变化只有约 1% RSD。通过校准,可以利用系统脱水时间对色谱柱长度进行可预测的调整,并在几分钟内完成更改。结果表明,这种方法可用于在气相色谱操作过程中就地调整色谱柱长度,以适应各种样品。
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来源期刊
Chromatographia
Chromatographia 化学-分析化学
CiteScore
3.40
自引率
5.90%
发文量
103
审稿时长
2.2 months
期刊介绍: Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.
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