Thermal desorption modulation for comprehensive two-dimensional gas chromatography using a simple and inexpensive segmented-loop fluidic interface

Author(s)

Mucedola, Vanessa ; Vieira, Luis C. S. ; Pierone, Danilo ; Gobbi, Angelo L. ; Poppi, Ronei J. ; Hantao, Leandro W.

• Document type: Journal article
• Source: Talanta; v. 164, p. 470-476, MAR 1 2017.
• Web of Science Citations: 5

Abstract

In this study, we introduce a modulation strategy for comprehensive two-dimensional gas chromatography (GCxGC) by using a simple and consumable-free modulator. This ``Do-It-Yourself{''} interface comprised a 1.0 mx0.25 mm segment of MTX-5 metallic column and a low-cost DC power supply. Thermal desorption modulation (TDM) was attained using a dual-stage heater-based modulator in a novel segmented-loop configuration. TDM was achieved by alternating analyte trapping and thermal desorption. Former process relied on analyte partition to sorbent phase, while latter explored direct resistive heating. Introduction of an intermediate delay segment between the two stages mitigated analyte breakthrough, improving peak symmetry and chromatographic efficiency. This feature was critical to acquire reliable GCxGC modulation using such simple heater-based device. The effects of important modulation variables on 2D separations were investigated, including TDM stage length, dimension of delay loop, and outlet pressure. Significant advances and limitations of proposed TDM strategy were carefully determined. Proposed GCxGC prototype by using an in-oven TDM modulator was successfully applied to a series of challenging matrices, including petroleum distillates, biodiesel, and essential oil. This open-hardware, cost-effective modulator was easy to install and operate, as it circumvented the need for sophisticated components (e.g. moving parts and cooling systems). Therefore, our modulator is a compelling alternative to existing GCxGC solutions to operate in resource-limited laboratories. (AU)

• FAPESP's process: 15/05059-9 - Development and evaluation of Consumable-free planar microfluidic modulators for comprehensive two-dimensional gas chromatography
• Grantee: Leandro Wang Hantao
• Support Opportunities: Regular Research Grants
• FAPESP's process: 14/00228-4 - Myology of the shoulder, arm, forearm in paca (Cuniculus paca, L.1766)
• Grantee: Juliana Aparecida Do Carmo Emidio e Silva
• Support Opportunities: Scholarships in Brazil - Scientific Initiation