Institute of Analytical Chemistry, Radlinskeho 9, 81237 Bratislava, Slovak Republic.
J Chromatogr A. 2011 May 27;1218(21):3186-9. doi: 10.1016/j.chroma.2011.03.042. Epub 2011 Apr 12.
Retentivity tuning in comprehensive two dimensional GC separations of aliphatics (linear and cyclic hydrocarbons) and aromatics in gasoline by changing the carrier gas flows in the column series at constant working temperature parameters of both columns is discussed. Comprehensive 2D techniques studied include GC×GC with cryogenic and differential flow modulation and non-modulated transfer (NMT). In all configurations, the first dimension was a non-polar column and the second dimension a polar column. Using three different flows (0.6, 1.0 and 1.4mL/min) of helium carrier gas in cryogenic modulated GC×GC illustrated that, as expected, retention of the solutes on the (1)D and (2)D columns increased but the separation quality was nearly constant. A change of carrier gas pressure (p(m)=175-125kPa) on the (1)D and (2)D columns joint point at constant inlet pressure (p(i)=525kPa) in NMT, induces an increase of the carrier gas flow rate on the (1)D and a decrease on the (2)D column, respectively. The higher retentivity of the (2)D column improved the group type separation of aliphatic/cyclic hydrocarbons and aromatics and a higher distribution of aromatics on the 2D retention plane was noted. Retentivity tuning was also performed in flow modulated GC×GC by operating the (1)D column at 0.8mL/min and the (2)D column at 20 and 26mL/min. The higher retentivity at 20mL/min improved the group type separation of aliphatic/cyclic hydrocarbons and aromatics in the 2D retention plane.
讨论了通过在恒定工作温度参数下改变柱串联中的载气流速来调整脂肪族(线性和环状烃类)和芳烃在汽油中的全二维 GC 分离的保留值。研究的全二维技术包括使用低温和差分流量调制以及非调制转移(NMT)的 GC×GC。在所有配置中,第一维是非极性柱,第二维是极性柱。使用氦载气的三种不同流量(0.6、1.0 和 1.4mL/min)在低温调制 GC×GC 中说明了,正如预期的那样,溶质在(1)D 和(2)D 柱上的保留增加了,但分离质量几乎保持不变。在 NMT 中,在(1)D 和(2)D 柱连接点处改变载气压力(p(m)=175-125kPa)而保持入口压力(p(i)=525kPa)不变,分别导致(1)D 柱上载气流速增加和(2)D 柱上载气流速减少。(2)D 柱较高的保留性改善了脂肪族/环状烃类和芳烃的分组分离,并且注意到芳烃在 2D 保留平面上的分布更高。通过以 0.8mL/min 的流速操作(1)D 柱并以 20 和 26mL/min 的流速操作(2)D 柱,在流量调制 GC×GC 中也进行了保留值调整。20mL/min 时较高的保留性改善了脂肪族/环状烃类和芳烃在 2D 保留平面上的分组分离。