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首页> 外文期刊>Science & justice: journal of the Forensic Science Society >Preparation and characterization of micro-bore wall-coated open-tubular capillaries with low phase ratios for fast-gas chromatography-mass spectrometry: Application to ignitable liquids and fire debris
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Preparation and characterization of micro-bore wall-coated open-tubular capillaries with low phase ratios for fast-gas chromatography-mass spectrometry: Application to ignitable liquids and fire debris

机译：快速气相色谱 - 质谱法的微孔壁涂覆的张开管状毛细管的制备与表征 - 用于可燃液体和火碎片的应用

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Fast Gas Chromatography (GC) allows for analysis times that are a fraction of those seen in traditional capillary GC. Key modifications in fast GC include using narrow, highly efficient columns that can resolve mixtures using a shorter column length. Hence, a typical fast GC column has an inner diameter of 100-180 mu m. However, to maintain phase ratios that are consistent with typical GC columns, the film thickness of fast GC stationary phases are also low (e.g., 0.1-0.18 mu m). Unfortunately, decreased film thickness leads to columns with very low sample capacity and asymmetric peaks for analytes that are not sufficiently dilute. This paper describes micro-bore (50 pm i.d.) capillary columns with thick films (1.25 mu m), and low phase ratios (10). These columns have greater sample capacity yet also achieve minimum plate heights as low as 110 mu m. Hence, separation efficiency is much higher than would be obtained using standard GC columns. The capillary columns were prepared in-house using a simple static-coating procedure and their plate counts were determined under isothermal conditions. The columns were then evaluated using temperature programming for fast GC-MS analysis of ignitable liquids and their residues on fire debris exemplars. Temperature ramps of up to 75 degrees C min(-1) could be used and separations of ignitable liquids such as gasoline, E85 fuel, and lighter fluid (a medium petroleum distillate) were complete within 3 min. Lastly, simulated fire debris consisting of ignitable liquids burned on carpeting were extracted using passive headspace absorption-elution and the residues successfully classified.
机译：快速气相色谱（GC）允许分析时间是传统毛细血管GC中观察到的分析时间。快速GC中的键修改包括使用窄的高效列，可以使用较短的柱长来解析混合物。因此，典型的快速GC柱具有100-180μm的内径。然而，为了保持与典型GC柱一致的相比，快速GC固定相的膜厚度也低（例如，0.1-0.18μm）。不幸的是，薄膜厚度下降导致具有非常低的样品能力和不充分稀释的分析物的样品能力和不对称峰的柱。本文描述了具有厚膜（1.25μm）和低相比（10）的微孔（50mp I.D.）毛细管柱。这些柱具有更大的样品能力，尚不到低至110μm的最小板高度。因此，分离效率远高于使用标准GC列获得的。使用简单的静态涂布程序内部制备毛细管柱，并在等温条件下测定它们的板数。然后使用温度规划评估柱，用于快速GC-MS分析可点燃液体及其残留物的火碎片样品。可以使用高达75摄氏度的温度斜坡（-1），并在3分钟内完成可燃液体如汽油，E85燃料和较轻的液体（备体石油馏分）的分离。最后，使用被动顶空吸收洗脱和成功分类的残留物提取由在地毯上燃烧的可点燃液体组成的模拟的火碎片。

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