DATA TREATMENT IN SEQUENCED TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY

VEGA, JORGE R.; SISKOVA, ALENA; CLEMENTI, LUIS A.; BEREK, DUSAN ; MEIRA, GREGORIO R.

Salzburg

Simposio; 30th International Symposium on Chromatography; 2014

30th International Symposium on Chromatography

Liquid chromatography at limiting condition of desorption (LC LCD) is a fractionation technique useful for the separation of some polymers blends. It employs barriers of small molecules for the selective deceleration of more adsorbing species, while other non-affected macromolecules elute in the SEC mode [1]. The LC LCD peaks can be online forwarded into a size exclusion chromatography (SEC) system, for evaluation of average molar masses. This last procedure is called sequenced two-dimensional liquid chromatography (S2D LC) [2]. Data treatment of the chromatograms obtained in a S2D LC procedure is difficult because: (i) some species (partially or totally) unaffected by the barriers suffer of band broadening (BB) in the first-dimension LC LCD column, which in turn depend on the analyzed species and their molar masses; (ii) an additional BB is introduced by the SEC column and intermediate capillaries, valves, and fittings; and (iii) molar masses are calculated on the basis of a molar mass calibration that is determined for the SEC system only, and therefore a proper synchronization of the chromatogram with the calibration is required. In this work, a data treatment method is proposed for properly evaluating the S2D LC chromatograms. Initially, a calibration of the BB introduced by the different components of the experimental setup is implemented. Then, a numerical method is proposed for correcting the BB and synchronizing the chromatogram with the available molar mass calibration.