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Comprehensive two-dimensional gas chromatography using partial modulation via a pulsed flow valve with a short modulation period
Talanta ( IF 5.6 ) Pub Date : 2017-09-04 , DOI: 10.1016/j.talanta.2017.08.095
Chris E. Freye , H. Daniel Bahaghighat , Robert E. Synovec

Partial modulation via a pulsed flow valve for comprehensive two-dimensional (2D) gas chromatography (GC × GC) is demonstrated, producing narrow peak widths, 2Wb, on the secondary separation dimension, 2D, coupled with short modulation periods, PM, thus producing a high peak capacity on the 2D dimension, 2nc. The GC × GC modulator is a pulse flow valve that injects a pulse of carrier gas at the specified PM, at the connection between the primary, 1D, column and the 2D column. Using a commercially available pulse flow valve, this injection technique performs a combination of vacancy chromatography and frontal analysis, whereby each pulse disturbance in the analyte concentration profile as it exits the 1D column results in data that is readily converted into a 2D separation. A three-step process converts the raw data into a format analogous to a GC × GC separation, incorporating signal differentiation, baseline correction and conversion to a GC × GC chromatogram representation. A 115-component test mixture with a wide range of boiling points (36–372 °C) of nine compound classes is demonstrated using modulation periods of PM = 50, 100, 250, and 500 ms, respectively. For the test mixture with a PM of 250 ms, peak shapes on 2D are symmetric with apparent 2Wb ranging from 12 to 45 ms producing a 2nc of ~ 10. Based on the average peak width of 0.93 s on the 1D separation for a time window of 400 s, the 1D peak capacity is 1nc ∼ 430. Thus, the ideal 2D peak capacity nc,2D is 4300 or a peak capacity production of 650 peaks/min using the PM of 250 ms. Additionally, for a PM of 50, 100 and 500 ms, the 2nc are 4, 7, and 12, respectively. Retention times on 2D, 2tR, are reproducible having standard deviations less than 1 ms. Finally, the processed data is shown to be quantitative, with an average RSD of 4.7% for test analytes.



中文翻译:

全面的二维气相色谱法,使用短调制周期的脉冲流量阀进行部分调制

演示了通过脉冲流量阀进行的部分调制,以进行全面的二维(2D)气相色谱(GC×GC),在二级分离尺寸2 D上产生了窄的峰宽2 W b,同时调制时间较短,P M,从而在2 D维2 n c上产生高峰值容量。GC×GC调节器是一种脉冲流量阀,可在指定的P M处在主色谱柱,1 D色谱柱和色谱柱2之间的连接处注入一个载气脉冲。D列。使用市售的脉冲流量阀,该注射技术来执行空缺色谱和前沿分析,由此在所述分析物的浓度分布的每个脉冲的干扰,因为它离开的组合1在被容易地转换成一个数据d柱结果2 d的分离。一个三步过程将原始数据转换为类似于GC×GC分离的格式,包括信号微分,基线校正和转换为GC×GC色谱图表示。分别使用P M = 50、100、250和500 ms的调制周期,演示了具有9种化合物的沸点范围广(36–372°C)的115组分测试混合物。对于带有P的测试混合物M为250 ms,2 D上的峰形是对称的,表观2 W b为12至45 ms,产生2 n c约为10。基于时间窗口的1 D分离的平均峰宽为0.93 s的400秒,1 d峰容量为1 ñ ç〜430因此,理想2D峰值容量ñ C,2D是4300或使用的峰值容量生产的650个峰/分钟P中号的250毫秒。此外,对于50、100和500 ms的P M2 n c分别是4、7和12。在2 D,2 t R上的保留时间是可重现的,标准偏差小于1 ms。最后,处理后的数据显示为定量数据,测试分析物的平均RSD为4.7%。

更新日期:2017-09-04
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