Poliak Marina, Kochman Maya, Amirav Aviv
School of Chemistry, Sackler Faculty of Exact Sciences, Tel Aviv University, Tel Aviv 69978, Israel.
J Chromatogr A. 2008 Apr 4;1186(1-2):189-95. doi: 10.1016/j.chroma.2007.09.030. Epub 2007 Sep 18.
Pulsed flow modulation (PFM) is based on higher flow rate time compression of the first GC column effluent, which prior to the injection into the second column is stored for a few seconds in a standard fused silica wide bore transfer line. We constructed the PFM device with two standard 1/16 in. brass compression fittings with the insertion of the two columns inside the wide bore 0.53 mm i.d. fused silica storage transfer line for the elimination of dead volumes. This simple arrangement provides a combination of flexibility in the length of the sample storage transfer line hence comprehensive two-dimensional gas chromatography (GC x GC) cycle time, inert sample path and full elimination of cooling gas consumption. A record short second column injection time of 20 ms is demonstrated. Practical injection times are the sample collection time (such as 4s) divided by the second to first column flow rate ratio (such as 20/0.7), which is typically around 150 ms. Due to the low cost of the device it can also be considered for use with non comprehensive time segmented GC x GC to remove a few accidental coelutions. PFM-GCxGC excels with high second column capacity due to the use of 0.32 mm i.d. columns with high flow rates as the second dimension GC x GC column. As a result, PFM-GCxGC can have up to two orders of magnitude higher second column sample capacity and linear dynamic range for improved reduction of adverse matrix interference effects due to column overloading.
脉冲流调制(PFM)基于对第一根气相色谱柱流出物的更高流速时间压缩,在注入第二根色谱柱之前,其在标准的大口径熔融石英传输线中存储几秒钟。我们构建的PFM装置由两个标准的1/16英寸黄铜压缩接头组成,将两根色谱柱插入内径为0.53 mm的大口径熔融石英存储传输线内,以消除死体积。这种简单的布置提供了样品存储传输线长度的灵活性,从而实现了全二维气相色谱(GC×GC)循环时间、惰性样品路径以及完全消除冷却气体消耗的组合。展示了20毫秒的创纪录短的第二根色谱柱进样时间。实际进样时间是样品收集时间(如4秒)除以第二根色谱柱与第一根色谱柱的流速比(如20/0.7),通常约为150毫秒。由于该装置成本低,它也可考虑用于非全二维时间分段GC×GC,以消除一些意外的共洗脱。由于在二维气相色谱(GC×GC)中使用内径为0.32 mm的色谱柱和高流速,PFM-GC×GC在第二根色谱柱容量方面表现出色。因此,PFM-GC×GC的第二根色谱柱样品容量和线性动态范围可提高多达两个数量级,以改善因柱过载导致的不利基质干扰效应的降低。