Evaluation of flow restrictors for open-tubular supercritical fluid chromatography at pressures up to 560 atm

✍ Scribed by Pinkston, J. David ;Hentschel, Rosemary T.

• Publisher: John Wiley and Sons
• Year: 1993
• Tongue: English
• Weight: 600 KB
• Volume: 16
• Category: Article
• ISSN: 0935-6304
• DOI: 10.1002/jhrc.1240160502

✦ Synopsis

Abstract

Proper performance of the flow restrictor is of crucial importance in supercritical fluid chromatography. This is especially the case when the restrictor is the interface between the chromatographic column and a detector operating at lower pressure than the column. The performance of three types of fixed flow restrictor, the “tapered”, the “integral”, and the “frit”, was examined. The test mixtures chosen covered a range of polarities and molecular weights. Polydimethylsiloxane with an average molecular weight of 10,000 was used as a low polarity probe. Two polyethylene glycol mixtures were chosen as higher polarity probes. One consisted of a mixture of polyethylene glycol standards with average molecular weights ranging from 200 to 1450. The other polyethylene glycol mixture had an average molecular weight of 2000. The polydimethylsiloxane standard did not elute when the frit restrictor was used. Satisfactory results were obtained when the tapered and integral restrictors were employed. All three restrictors provided satisfactory results for polyethylene glycol oligomers eluting up to approximately 40.5 MPa (400 atm). However, for oligomers eluting above this pressure, the peaks merged into a broad hump with the frit restrictor, while the tapered and integral restrictors provided satisfactory separations. The integral restrictor produced more evenly spaced, more well resolved peaks at the high‐pressure end of the chromatograms than did the tapered restrictor. This is shown to be due to differences in the rates of increase in mobile‐phase velocity with increasing pressure for the two restrictors.