Adiabatic packed column supercritical fluid chromatography using a dual-zone still-air column heater.

ABSTRACT

An approach to conducting SFC separations under pseudo-adiabatic condition utilizing a dual-zone column heater is described. The heater allows for efficient separations at low pressures above the critical temperature by imposing a temperature profile along the column wall that closely matches that for isenthalpic expansion of the fluid inside the column. As a result, the efficiency loss associated with the formation of radial temperature gradients in this difficult region can be largely avoided in packed analytical scale columns. For elution of n-octadecylbenzene at 60 °C with 5% methanol modifier and a flow rate of 3 mL/min, a 250 × 4.6-mm column packed with 5-micron Kinetex C18 particles began to lose efficiency (8% decrease in the number of theoretical plates) at outlet pressures below 142 bar in a traditional forced air oven. The corresponding outlet pressure for onset of excess efficiency loss was decreased to 121 bar when the column was operated in a commercial HPLC column heater, and to 104 bar in the new dual-zone heater operated in adiabatic mode, with corresponding increases in the retention factor for n-octadecylbenzene from 2.9 to 6.8 and 14, respectively. This approach allows for increased retention and efficient separations of otherwise weakly retained analytes. Applications are described for rapid SFC separation of an alkylbenzene mixture using a pressure ramp, and isobaric separation of a cannabinoid mixture.