ADVANCED COMBUSTION ENGINEERING RESEARCH CENTER

HomeMembershipPersonnel • Research • StudentsLaboratories • Products • Publications • Annual Conference Library •

Huang, EC

1988

Direct Coupling of Capillary Supercritical Fluid Chromatography to High Resolution Mass Spectrometry with Minimum Modification

Huang, E.C.; Jackson, B.J.; Markides, K.E. and Lee, M.L.
Chromatographia, 25, 51-54, 1988. 4 pgs. Funded by US Department of Energy and Gas Research Institute.

It is estimated that the majority of analyses by supercritical fluid chromatography (SFC) involves the use of the flame ionization detector (FID) or the UV-absorbance detector. Unfortunately, each of these detectors can only be used when the SFC mobile phase and the sample being chromatographed fill certain requirements; the FID is limited to the use of only a few supercritical mobile phases, and the UV-absorbance detector can be used only when the sample molecules contain chromophores. The demand for a universal detector for SFC has intensified as the range of applicability of the technique has expanded. Coupled chromatography/mass spectrometry systems are among the most powerful analytical instruments available today for the analysis of organic mixtures. The successful marriage of gas chromatography/mass spectrometry (GC/MS) and the considerable progress in coupling liquid chromatography with the mass spectrometer (LC/MS) have naturally led to studies of SFC/MS.

The coupling of a capillary supercritical fluid chromatograph with a high resolution double focusing mass spectrometer has been accomplished without any modifications to the pumping or ion source systems. The interface utilizes a direct insertion probe (DIP), which was originally designed for the direct analysis of solid samples, together with a frit restrictor as a decompression device. The DIP is placed opposite to the SFC restrictor, and it provides sufficient heat to prevent cluster formation and cooling resulting from the expansion of the supercritical fluid into the vacuum environment. Excellent mass spectra of standard polycyclic aromatic hydrocarbons under chemical-ionization (CI) conditions using methane as the reagent gas, and under charge-exchange (CE) conditions using CO2 as the charge exchange medium were obtained.