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1.
J Chromatogr A ; 1577: 72-81, 2018 Nov 23.
Article in English | MEDLINE | ID: mdl-30348497

ABSTRACT

The development of the reversed fill/flush modulator represents a significant advancement in flow-modulated, comprehensive two-dimensional gas chromatography (GC × GC). Compared to the forward flush/fill modulator, the reversed-flow modulator is less susceptible to baseline anomalies and peak tailing as a result of modulator channel overfilling or insufficient purging of high concentration analytes. Flow reversal requires the addition of a bleed capillary not present in the forward-flow modulator. Selecting the appropriate restriction of the bleed capillary is critical. If the bleed capillary is too restrictive, eluate from the first-dimension column can split between the modulator channel and second-dimension column, which also results in baseline artifacts. To gain a better understanding of the reversed-flow modulator, a comprehensive pneumatic model was developed. The model was validated by comparing calculated and measured hold-up times. The errors in calculated hold-up times were less than 1% of the measured values. The model can be used to predict first-dimension eluate splitting and determine the optimal bleed capillary dimensions to prevent its occurrence. Calculation of the modulator hold-up time can be used to determine the maximum collection time to ensure comprehensive analysis and optimal flush times for partial fill operation.


Subject(s)
Chromatography, Gas/instrumentation , Chromatography, Gas/methods , Models, Theoretical , Reproducibility of Results
2.
J Chromatogr A ; 1387: 95-103, 2015 Mar 27.
Article in English | MEDLINE | ID: mdl-25704768

ABSTRACT

The development of new efficient conversion processes to transform heavy petroleum fractions into valuable products, such as diesel, requires improved chemical knowledge of the latter. High-temperature comprehensive gas chromatography (HT-GC × GC) has proven to be a powerful technique for characterizing such complex samples. This paper reports on an evaluation of the performances of four different differential flow modulators, including two original ones that have not been previously described in the literature, in terms of dispersion, peak intensity, peak capacity and overloading. These modulators, all of which are based on Agilent capillary flow technology (CFT), are forward fill/flush (FFF) differential flow modulators with an integrated collection channel or an adjustable channel (new) and reverse fill/flush (RFF) differential flow modulators with an integrated collection channel (new) or an adjustable channel. First, the optimization of the collection channel dimensions is described. Second, an RFF and an FFF differential flow modulator possessing the same collection channel were compared. The reverse differential flow modulation significantly reduced band broadening compared to forward differential flow modulation, and the peak intensity doubled for every modulated peak when an RFF differential flow modulator was used. Then, an RFF differential flow modulator and CO2 dual-jet modulator were compared. Whereas the percentages of separation space used were similar (61% with the HT-GC × GC method using a cryogenic modulator and 59% with the method using an RFF differential flow modulator), the peak capacities were at least three times more important with differential flow modulation due to the greater length of the column used in the second dimension. The results demonstrate that the RFF differential flow modulator is an excellent tool for studying heavy petroleum cuts. It demonstrates the best performances and it is the most versatile modulator. In its two-plate version, it gives more flexibility regarding the set of columns, the flow rates and the modulation periods that can be used compared with the others.


Subject(s)
Chemistry Techniques, Analytical/instrumentation , Chemistry Techniques, Analytical/methods , Chromatography, Gas , Hot Temperature , Petroleum/analysis
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