Development of a membraneless extraction module for the extraction of volatile compounds: application in the chromatographic analysis of vicinal diketones in beer.
A membraneless extraction module (MLEM) for the sample preparation of volatile compounds and its use for the chromatographic analysis of vicinal diketones in beer are reported. The extraction process is based on the same principles of gas diffusion (GD) and pervaporation (PV); however it does not use a membrane. This module has a lower chamber where the sample continuously flows, while volatile compounds evaporate to the headspace. Inside the module there is a suspended small reactor, where a small volume of a suitable acceptor solution is placed. This extraction module was tested in the determination of vicinal diketones (VDKs) in beer (CV=5%; LOD=4 microg L(-1)), showing applicability with real samples. Several parameters of the extraction process, such as temperature, sample flow and extraction time, were studied and optimized. This module proved to be a good tool for the sampling of volatile compounds, since the extraction is made without using a membrane avoiding all the robustness problems related with its use.
Chromatographic analysis of methylglyoxal and other α-dicarbonyls using gas-diffusion microextraction.
Many α-dicarbonyl compounds such as methylglyoxal, diacetyl and pentane-2,3-dione are important quality markers of processed foods. They are produced by enzymatic and chemical processes, the Maillard reaction is the most known chemical route for α-dicarbonyl formation. In the case of methylglyoxal, there are obstacles to be overcome when analysing this compound due to its high reactivity, low volatility and low concentration. The use of extraction techniques based on the volatilization of methylglyoxal (like solid-phase microextraction) showed to be ineffective for the methylglyoxal extraction from aqueous solutions. Therefore, derivatization is typically applied to increase analyte's volatility. In this work a new methodology for the extraction and analysis of methylglyoxal and also diacetyl and pentane-2,3-dione from selected food matrices is presented. It is based on a gas-diffusion microextraction step followed by high performance liquid chromatographic analysis. It was successfully applied to port wines, black tea and soy sauce. Methylglyoxal, diacetyl and pentane-2,3-dione were quantified in the following concentration ranges: 0.24-1.74 mg L(-1), 0.1-1.85 mg L(-1) and 0.023-0.15 mg L(-1), respectively. The main advantages over existing methodologies are its simplicity in terms of sample handling, not requiring any chemical modification of the α-dicarbonyls prior to the extraction, low reagent consumption and short time of analysis.
Effect of superficial gas velocity on the particle temperature distribution in a fluidized bed with heat production
The heat transfer behavior of particles and gas in an olefin polymerization fluidized bed was numerically analyzed using an in-house developed 3-D computational fluid dynamics discrete element model (CFD-DEM). First the implementation of the model was verified by comparing simulation results with analytical results. A constant volumetric heat production rate was implemented in the particle energy equation to mimic the heat production due to the polymerization reaction. It was found that the probability density function (PDF) of the particle temperature becomes more homogeneous with increasing superficial gas velocity. Furthermore, instantaneous snapshots of the thermal driving force (the difference between the single particle temperature and bed-average gas temperature, Tp− ) for different heat production rates provide detailed insight in the particle temperature distribution inside the fluidized bed. The time- and bed-averaged particle convective heat transfer coefficient, which was calculated by Gunn׳s correlation, was found to be independent of the superficial gas velocity. This is explained by the fact that the relative velocity of gas and particles in the emulsion phase, where most of the particles and gas interact, is hardly influenced when increasing the gas superficial velocity. From the spatial distribution of Nusselt number, it becomes apparent that the high heat transfer regions are found in the wake of rising bubbles, whereas low heat transfer rates are found in the clouds of the bubbles.