SFC Using LC Columns

Figure 8 demonstrates the pressure-programming separation of methylphenylsiloxane oligomers using diethyl ether as the supercritical fluid. The critical temperature, pressure and density are 194°C, 3.6 MPa and 0.264 g cm"3, respectively. The initial inlet pressure is 4.4 MPa and the pressure is programmed at 0.1 MPa min"1 for 10 min, 0.05 MPa min-1 for the next 10 min and 0.025 MPa min"1 for the rest of the analysis. The pressure drop across the column is maintained at 0.49 MPa using a two-pump system. The temperature is kept constant at 225°C and the analytes are detected by UV at 215 nm.

Figure 8 Pressure-programming SFC separation methylphenylsiloxane oligomers using diethyl etherasthe mobile phase. Column: Develosil ODS-5 (5 ^m ODS), 300 x 0.5 mm i.d. Mobile phase: diethyl ether. Initial inlet pressure: 4.4 MPa. Pressure programmed at 0.1 MPa min-1 for 10 min, 0.05 MPa min-1 for the next 10 min and 0.025 MPa min-1 for the rest of the analysis. Pressure drop: 0.49 MPa. Temperature: 225°C. Sample: OV-17 dissolved in tetrahydrofuran. Detector: UV (215 nm). (Reproduced with permission from Takeuchi et al. (1987). Retention behaviour in liquid and supercritical fluid chromatography using methanol or diethyl as mobile phase. Chromatographia 23: 932.)

Figure 8 Pressure-programming SFC separation methylphenylsiloxane oligomers using diethyl etherasthe mobile phase. Column: Develosil ODS-5 (5 ^m ODS), 300 x 0.5 mm i.d. Mobile phase: diethyl ether. Initial inlet pressure: 4.4 MPa. Pressure programmed at 0.1 MPa min-1 for 10 min, 0.05 MPa min-1 for the next 10 min and 0.025 MPa min-1 for the rest of the analysis. Pressure drop: 0.49 MPa. Temperature: 225°C. Sample: OV-17 dissolved in tetrahydrofuran. Detector: UV (215 nm). (Reproduced with permission from Takeuchi et al. (1987). Retention behaviour in liquid and supercritical fluid chromatography using methanol or diethyl as mobile phase. Chromatographia 23: 932.)

Ether is toxic and flammable. Even a small leakage of the mobile phase should be avoided for safety reasons.

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