Dynamic thermal gradient gas chromatography

The use of negative axial thermal gradients in gas chromatography (TGGC) has intrigued chromatographers since the early 1950s because of the dramatic narrowing of analyte bands and concomitant raised expectations for improving resolving power. However, technical difficulties experienced in construction of TGGC instrumentation and control of the temperature along the column have made its implementation and, hence, detailed study difficult. In this work, we describe a TGGC system capable of rapidly producing and varying thermal gradient profiles by simultaneous use of resistive heating and convective cooling. Heating and cooling rates as high as 1200 and 2500 °C/min, respectively, allowed the creation of dynamic temperature gradients. The separation characteristics of TGGC with dynamically changing temperature gradients are demonstrated. A gradient velocity of 2.22 cm/s provided repetitive separations every 45 s, and injection band widths of 45 s duration were transformed into approximately 1-s peak widths. Peak tailing for basic compounds was nearly eliminated. Dynamic TGGC allows unique control over separations, oftentimes improving resolution and detection signal-to-noise. Thermally controlled elution in TGGC holds great promise for performing smart separations in which the separation time window is most efficiently utilized, and optimized separations can be quickly achieved. Rapid adjustment of relative compound elution can be used to greatly reduce GC method development time.