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This study examines how the height and width of peaks exiting the secondary column of a comprehensive two-dimensional gas chromatography (GC × GC) separation are affected by the width of the pulse introduced to the secondary column. A flow-modulated GC × GC apparatus was assembled that allowed input pulse widths to be controlled precisely over a range of 10 to 70 ms. GC × GC chromatograms were obtained using secondary columns containing a polyethylene glycol stationary phase with internal diameters of 0.25 and 0.32 mm. The area, height, and width of peaks emerging from the secondary column were found to be accurately modeled by the convolution of a rectangular function with a Gaussian distribution. The rectangular function represents the input pulse, and the Gaussian distribution represents the broadening that occurs in the secondary column. The minimum peak width that could be produced by the secondary column was determined for a wide range of compounds. Injection pulse widths that matched a compound's minimum peak width produced peaks that were 25% wider than the minimum width and had heights that were 76% of the maximum possible peak height. Increasing the injection width significantly above the minimum width yielded substantially broader peaks with only a modest increase (< 25%) in peak height., (© 2022. Springer-Verlag GmbH Germany, part of Springer Nature.)

The present research is focused on the use and evaluation of hydrogen, as a more sustainable alternative to helium, within the context of fast flow modulation comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry. In such a respect, a comparison was made between the two mobile phases in terms of speed and overall chromatography performance. All experiments were carried out by using the following column set: low polarity with dimensions 10 m × 0.25 mm ID × 0.25 µm d f and medium polarity with dimensions 2 m × 0.10 mm ID × 0.10 µm d f . Fundamental gas chromatography parameters (efficiency, resolution) were measured under different experimental conditions, using the two carrier gases. Efficiency was measured in both the first and second dimensions, using a probe compound under isothermal conditions; after defining the optimum carrier gas conditions, a mixture containing 20 pesticides was analyzed to measure resolution, again in the first and second dimensions, using a temperature program. It was found (as expected) that a similar chromatography performance could be attained when using hydrogen, albeit with a circa 25% reduction in analysis time. Signal-to-noise ratios of the pesticides were calculated, using both carrier gases, with such values generally reduced (on average by 14%) when using hydrogen. Finally, a comparison was made between mass spectral profiles obtained analyzing the pesticides and fatty acid methyl esters using the two mobile phases. Even though mass spectral differences were observed, the ion profiles could be considered generally similar., (© 2022. Springer-Verlag GmbH Germany, part of Springer Nature.)