Visualizing and studying frictional heating effects in reversed-phase liquid chromatography using infrared thermal...

Column temperature control is a fundamental component of liquid chromatography experiments. However, it is typically monitored indirectly by tracking the temperature of an adjacent heating element that exchanges heat with the column in a controlled environment. The practice of not directly measuring the column temperature means that uncontrolled contributions of heat, such as frictional heating inside the column, can be overlooked. The present work describes the use of a high-resolution infrared thermal imaging camera to directly measure the column heat map during mobile phase flow. The approach was used to measure the longitudinal temperature gradient formed with three common mobile phases: water, methanol, and acetonitrile, in two 50 mm reversed-phase columns, a 1.7 μm particle-packed column and a polystyrene divinylbenzene monolith. In a close approximation to an adiabatic environment, the temperature gradients (ΔT) observed with the 1.7 μm particle column at a linear velocity of 5.8 mm/s were up to +16.6 and + 12.8 °C above an ambient temperature of 23 °C for water and acetonitrile, respectively. In the case of water, the measured temperature gradient values (ΔT) were within 1% difference of theoretically-calculated values and on average within 10% for acetonitrile. By contrast, the ΔT observed in the monolith was negligible. The elevated temperatures that are generated through friction in sub-2 μm particle columns may be particularly important to consider for the design of experiments that measure structural features of temperature-sensitive analytes, such as biomolecules. While frictional heating is one important application of the thermal imaging approach described, the technique can be used to provide a data-rich profile of heat exchange in numerous experimental configurations, chromatographic or otherwise.