Evaluation of injection methods for fast, high peak capacity separations with low thermal mass gas chromatography

Fitz, Brian D.; Mannion, Brandyn C.; To, Khang; Hoac, Trinh; Synovec, Robert E.

doi:10.1016/j.chroma.2015.03.009

Cited by 8 publications

(4 citation statements)

References 32 publications

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“…Using this linear fit, one can estimate the peak capacity, n c , at unit resolution (R s = 1). 27 Indeed, a remarkable n c of 14 is achieved for this 200 ms separation window. If used in GC × GC mode, a P M of 200 ms could be applied, and this high peak capacity would be provided.…”

Section: ■ Results and Discussionmentioning

confidence: 85%

“…As expected for an isothermal separation, later eluting analytes are wider ( w b ∼ 26 ms for benzyl alcohol versus ∼6.5 ms for acetone), and the w b increases linearly with k ′ ( R 2 of 0.9778). Using this linear fit, one can estimate the peak capacity, n c , at unit resolution ( R s = 1) . Indeed, a remarkable n c of 14 is achieved for this 200 ms separation window.…”

Section: Resultsmentioning

confidence: 99%

“…In fact, the performance of the modulator speaks to the need to improve the performance of GC so much more efficient 1 D separations are achieved, such as providing 1 w b of ∼200−400 ms concurrently with a P M of ∼100 ms, so the sampling density is more appropriate. Recent advances in GC technology have been very promising in this regard, 29,30 such as resistively heated temperature programming, 27,31,32 with extension to micro-GC formats. 33−35 Developments in axial thermal gradient GC 36 and flow field thermal gradient GC 37 are also very promising platforms for potential integration with pulse flow valve modulation.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…In fact, the performance of the modulator speaks to the need to improve the performance of GC so much more efficient 1 D separations are achieved, such as providing 1 w b of ∼200–400 ms concurrently with a P M of ∼100 ms, so the sampling density is more appropriate. Recent advances in GC technology have been very promising in this regard, , such as resistively heated temperature programming, ,, with extension to micro-GC formats. − Developments in axial thermal gradient GC and flow field thermal gradient GC are also very promising platforms for potential integration with pulse flow valve modulation. Additionally, modulation from the 2 D to 3 D dimensions in GC 3 is naturally well suited to take advantage of partial modulation, as the second dimension peaks with 2 w b of ∼200 to 400 ms are readily achieved. ,, Indeed, this direction with GC 3 -TOFMS is reported herein.…”

Section: Resultsmentioning

confidence: 99%

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Development of Ultrafast Separations Using Negative Pulse Partial Modulation To Enable New Directions in Gas Chromatography

et al. 2019

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Partial modulation via a pulse flow valve operated in the negative pulse mode is developed for highspeed one-dimensional gas chromatography (1D-GC), comprehensive two-dimensional (2D) gas chromatography (GC × GC), and comprehensive three-dimensional gas chromatography (GC 3 ). The pulse flow valve readily provides very short modulation periods, P M , demonstrated herein at 100, 200, and 300 ms, and holds significant promise to increase the scope and applicability of GC instrumentation. The negative pulse mode creates an extremely narrow, local analyte concentration pulse. The reproducibility of the negative pulse mode is validated in a 1D-GC mode, where a pseudosteady-state analyte stream is modulated, and 8 analytes are baseline resolved (resolution, R s ≥ 1.5) in a 200 ms window, providing a peak capacity, n c , of 14 at unit resolution (R s = 1.0). Additionally, the pulse width, p w , of the pulse flow valve "injection" relationship to peak width-at-base, w b , resolution between peaks and detection sensitivity are studied. To demonstrate the applicability to GC × GC, a high-speed separation of a 20-component test mixture of similar, volatile analytes is shown. Analytes were separated on the second-dimension column, 2 D, with 2 w b ranging from 7 to 12 ms, providing an exceptional 2 D peak capacity, 2 n c , of ∼12 using a modulation period (P M ) of 100 ms. Next, a 12 min separation of a diesel sample using a P M of 300 ms is presented. The 1 w b is ∼4 s, resulting in a 1 n c of ∼180, and 2 w b is ∼18 ms, resulting in a 2 n c of ∼17, thus achieving a n c,2D of ∼3000 in this rapid GC × GC diesel separation. Finally, GC 3 with time-of-flight mass spectrometry (TOFMS) detection using a P M of 100 ms applied between the 2 D and 3 D columns is reported. Narrow third dimension, 3 D, peaks with 3 w b of ∼15 ms were obtained, resulting in a GC 3 peak capacity, n c,3D , of ∼35 000 in a 45 min separation.

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Section: ■ Results and Discussionmentioning

confidence: 85%

Section: Resultsmentioning

confidence: 99%