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Possibilities and limitations of fast GC with narrow-bore columns

机译:窄口径色谱柱快速气相色谱的可能性和局限性

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摘要

In this work, two narrow-bore capillary columns with different internal diameters (I.D.) 0.15 mm (15 in length, 0.15 pin film thickness) and 0.10 mm, (10 in length, 0.10 mu m film thickness) with the same stationary phase (5% diphenyl 95% dimethylsiloxane), phase ratio and separation power were compared with regard to their advantages, practical limitations and applicability in fast GC on commercially available instrumentation. The column comparison concerns fast GC method development, speed and separation efficiency, the sample transfer into the column utilizing split and splitless inlet, sample capacity, detection (analysing compounds of a wide range of polarities and volatilities - even n-alkanes C-16 - C-28 and selected pesticides) and ruggedness (in the field of ultratrace analysis of pesticide residues in real matrix). Under conditions corresponding to speed/separation efficiency trade-off 0.10 mm I.D. versus 0.15 min I.D. column provides a speed gain of 1.74, but all other parameters investigated were better for the 0.15 min I.D. column concerning more efficient sample transfer from inlet to the column using splitless injection, no discrimination with split injection. Better sample capacity (three times higher for the 0.15 min than for the 0.10 mm I.D. column) resulted in improved ruggedness and simpler fast GC-MS method development.
机译:在这项工作中,两根窄孔毛细管柱的内径(ID)为0.15 mm(长度为15,针厚为0.15针膜厚)和0.10 mm(长度为10,膜厚为0.10μm),固定相相同(比较了5%(二苯基95%)二甲基硅氧烷,相比和分离能力的优势,实际局限性以及在市售仪器上进行快速气相色谱分析的适用性。色谱柱比较涉及快速的气相色谱方法开发,速度和分离效率,利用不分流进样和不分流进样口将样品转移到色谱柱中,样品容量,检测(分析多种极性和挥发性的化合物-甚至包括正构烷烃C-16- C-28和选定的农药)和耐用性(在超痕量分析实基质中农药残留的领域)。在与速度/分离效率相对应的条件下,需要权衡0.10 mm I.D.内径0.15分钟色谱柱可提供1.74的速度增益,但对于0.15分钟的内径,所研究的所有其他参数均更好。使用不分流进样可更高效地将样品从进样口转移到色谱柱,而分流进样则无区别。更好的样品容量(0.15分钟内径比0.10 mm内径色谱柱高三倍)可提高耐用性并简化快速GC-MS方法的开发。

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