A fast temperature-programmed second-dimension column for comprehensive two-dimensional gas chromatography

• Published in: Analytical and bioanalytical chemistry 2023-05, Vol.415 (13), p.2435-2446
• Main Authors: Cai, Huamin, Stearns, Stanley D.
• Format: Article
• Language: English
• Subjects: Air cooling; Analysis; Analytical Chemistry; Biochemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatography; Column chromatography; Comprehensive 2D Chromatography; Compressed air; Cooling; Direct flow; Equipment and supplies; Food Science; Gas chromatography; Gasoline; Heating; Laboratory Medicine; Lag time; Methods; Monitoring/Environmental Analysis; Naphthalene; Research Paper; Retention time; Sensors; Temperature requirements; Temperature sensors; Two dimensional analysis
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-022-04443-3

The short analysis time and constant temperature environment in the second dimension of two-dimensional comprehensive chromatography frequently causes wraparound problems, especially for complex high boilers. This problem can be solved by temperature programming on the second column, but since this requires heating and cooling the column in a matter of seconds, it is difficult to implement. In this study, we describe a method of accomplishing rapid heating and cooling with a resistively heated column cooled by compressed air. Critical to this method is minimizing the lag time between the actual temperature and the reported temperature by using the column heating element as the temperature sensor, virtually eliminating the danger of overshooting the temperature setpoint. This technique facilitates a ramp rate of up to 100 °C/s with minimal overshooting—well beyond the requirements of gas chromatography. A single-layer column bundle design allows a compressed-air cooling device to cool the column from 200 to 50 °C at an average rate of −21 °C/s. The secondary dimension temperature programming is facilitated by the longer secondary dimension time made possible by the direct flow modulation method. We evaluated the performance of the single-layer column bundle and demonstrated this method by applying it to a gasoline sample. We also compared this method with the traditional isothermal approach and found that use of the secondary temperature program reduced the naphthalene retention time from 12.1 to 6.3 s and its peak width at half height from 846 to 126 ms. Graphical abstract