Abstract
The plumbing of a commercial supercritical fluid chromatograph was modified by replacing all the connector tubing with the shortest possible lengths (65 cm) of 75 µm ID tubes. Heat exchangers controlling column temperatures and column outlet temperature were bypassed. The UV detector flow cell was replaced with an experimental cell with a 75 µm inlet tube, and a 2 µL internal volume. All these steps were taken to minimize extra-column dispersion. The extra-column dispersion was decreased from ≈ 80 µL2 in the commercial instrument to roughly 2 µL2 with the modifications. Reduced plate heights as low as 1.65 were obtained using a 20 × 3 mm column packed with 1.8 µm particles. This is a remarkably low value for such a short column. The optimum flow was ≈ 2.5 mL min−1. The system pressure drop at optimum was 220 bar (320 bar pump pressure), but increased rapidly with flow rate, to 450 bar (550 at pump) at 3.5 mL min−1.
References
Wahab MF, Wimalasinghe RM, Wang Y, Barhate CL, Patel DC, Armstrong DW (2016) Salient sub-second separations. Anal Chem 88:8821–8826
Ismail OH, Pasti L, Ciogli A, Villani C, Kocergin J, Anderson S, Gasparrini F, Cavazzini A, Catani M (2016) Pirkle-type chiral stationary phase on core-shell and fully porous particles: are superficially porous particles always the better choice toward ultrafast high-performance enantioseparations? J Chromatogr A 1466:96–104
Khundadze N, Pantsulaia S, Fanali C, Farkas T, Chankvetadze B (2018) On our way to sub-second separations of enantiomers in high-performance liquid chromatography. J Chromatogr A 2018(1572):37–43
Ciogli A, Ismail OH, Mazzoccanti G, Villani C, Gasparrini F (2018) Enantioselective ultra high performance liquid and supercritical fluid chromatography: the race to the shortest chromatogram. J Sep Sci 41:1307–1318
Perrenoud AG-G, Veuthey J-L, Guillarme D (2012) Comparison of ultra-high performance supercritical fluid chromatography and ultra-high performance liquid chromatography for the analysis of pharmaceutical compounds. J Chromatogr A 1266:158–167
Berger TA (2016) Instrument modifications that produced reduced plate heights < 2 with sub-2 μm particles and 95% of theoretical efficiency at k = 2 in supercritical fluid chromatography. J Chromatogr A 1444:129–144
Berger TA (2019) High-speed, high-efficiency achiral SFC on a 3 × 20-mm column packed with 1.8-μm particles facilitated by a low-dispersion chromatograph. Chromatographia 82:537–543
Berger TA (2017) Preliminary kinetic evaluation of an immobilized polysaccharide sub-2 μm column using a low dispersion supercritical fluid chromatograph. J Chromatogr A 1510:82–88
De Pauw R, Shoykhet K, Desmet G, Broeckhoven K (2015) Understanding and diminishing the extra-column band broadening effects in supercritical fluid chromatography. J Chromatogr A 1403:132–137
Barhate CL, Wahab MF, Tognarelli DJ, Berger TA, Armstrong DW (2016) Instrument idiosyncracies affect in the performance of ultrafast chiral and achiral supercritical fluid chromatography. Anal Chem 88:8664–8672
Berger TA (2016) Characterizing pressure issues due to turbulent flow in tubing, in ultra-fast chiral supercritical fluid chromatography at up to 580 bar. J Chromatogr A 1475:86–94
De Pauw R, Choikhet K, Desmet G, Broeckhoven K (2014) Occurence of turbulent flow conditions in supercritical fluid chromatography. J Chromatogr A 1361:277–285
Sternberg JC (1996) Extracolumn contributions to chromatographic bandspreading. In: Giddings JC, Kelly RA (eds) Advances in chromatography, vol 2. Marcel Dekker, New York
Acknowledgements
The author wishes to acknowledge the gift of the experimental 20 × 3 mm, 1.8 µm RX-Sil column by Agilent Technologies in Wilmington, Delaware, and for the custom detector flow cell specially fabricated by Agilent in Waldbronn, Germany.
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Berger, T.A. Reduced Plate Height of 1.65 on a 20 × 3 mm Column Packed with 1.8 µm Particles in Supercritical Fluid Chromatography (SFC). Chromatographia 82, 971–974 (2019). https://doi.org/10.1007/s10337-019-03722-z
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DOI: https://doi.org/10.1007/s10337-019-03722-z