[Show abstract][Hide abstract] ABSTRACT: Comprehensive two-dimensional gas chromatography (GC×GC) suffers from the impossibility to operate both dimensions at their optimum carrier gas velocity at the same time due to the different inner diameters of the columns typically employed. The use of multiple parallel capillary columns in the second dimension (GC×multi-GC) is studied as a means to achieve simultaneous optimum-velocity operation. A programme written in Microsoft Excel(®) was developed to calculate the efficiency of the two dimensions in GC×multi-GC for different numbers of columns in the second dimension. With the aid of this programme the appropriate number of columns was selected. Columns with maximum repeatability were specifically manufactured to grand suitable performance, i.e. to avoid band broadening effects caused by inter-column variations. 1D-GC experiments were carried out on the columns separately and combined in parallel. The performance of the parallel column set was consistent with that of the individual columns, with over 9100plates generated (approximately 10,000plates/m). A GC×multi-GC set-up was successfully installed. Model experiments proved the possibility to operate both dimensions at their optimum linear velocity simultaneously. The suitability of the novel second dimension column format to perform multidimensional separations was also shown for a number of selected applications.
Full-text · Article · Aug 2013 · Journal of Chromatography A
[Show abstract][Hide abstract] ABSTRACT: When the typical column combinations are used, comprehensive two-dimensional gas chromatography (GC×GC) suffers from the impossibility to operate both dimensions at their optimum carrier gas velocities at the same time. This as a result of the flow mismatch caused by the different dimensions of the columns used. The objective of the present study was the development of monolithic second dimension columns which would allow simultaneous optimum-velocity operation. With monolithic GC columns the optimum performance can be obtained at any given flow rate by varying the bed structure and column diameter. Different divinylbenzene-based monolithic columns were prepared and evaluated in terms of permeability and performance. Plate heights of less than 0.18mm and plate generation rates up to 600 plates/s were achieved. 1D-GC experiments performed on short monolithic columns showed a good resolving power thanks to the elevated retention and the good selectivity. A peak capacity up to 12 peaks per 4-5s was obtained for low-boiling alkanes, confirming the potential for fast separations. Excellent repeatability in terms of retention times (RSD<0.5%) and peak widths (RSD<1.5%) was observed. The columns prepared were successfully used in the second dimension of a GC×GC setup with a standard non-polar first dimension. Model experiments proved the possibility to operate both dimensions at their optimum linear velocity simultaneously. The suitability of the novel second dimension column format to perform multidimensional separations was shown for selected applications.
Full-text · Article · Oct 2012 · Journal of Chromatography A
[Show abstract][Hide abstract] ABSTRACT: A new chip-based liquid-liquid extraction technique for sample preparation of aqueous samples for GC was developed. Extraction is performed in a segmented flow system with additional mixing provided by an etched channel structure. The dimensions of the device are optimized to allow benefiting of the advantages of chip technology without suffering from the limitations of over-miniaturization. Phase separation is performed with a novel phase separator developed in house. The instrumental set-up is simple. The results obtained for selected test analytes show that the extraction is quantitative (recoveries = 92-110%, RSD < 6%) for a wide range of hydrophobicities (LogK(o/w) = 0.86-4.79). The performance at different flow rates (0.5-6.0 mL/min) and flow ratios (β = 1-10) was evaluated, confirming the flexibility and the possibility to perform enrichment. The results obtained for a few selected applications demonstrate the suitability of the method to perform quick, simple and reliable sample preparation for analytes of interest in real samples.
Full-text · Article · Aug 2011 · Journal of Chromatography A
[Show abstract][Hide abstract] ABSTRACT: The trace-level analysis of unknown pollutants in water requires the use of fast and sensitive methods which also provide structural information. In the present preliminary study, solid phase extraction (SPE), programmed temperature vaporisation (PTV) and gas chromatography (GC) with mass spectrometric (MS) detection are combined. A fully automated SPE system was connected to a GC via a PTV injector. The PTV injector was selected because of its robustness (over 100 analyses) when analysing real-life samples. The mass spectrometer was used in the full-scan mode to allow compound identification. The technique is applied to the determination of a series of priority pollutants in water from the river Rhine and Meuse. In this way tributhylphosphate and caffeine were detected. The results of this analysis were confirmed by RIZA both qualitative as well as quantitative.