A High-Pressure Reactor Coupled To Synchrotron Radiation Photoionization Mass Spectrometry

A high-pressure reactor was designed and coupled to synchrotron radiation photoionization mass spectrometry (SR-PIMS), which realizes the molecular-beam sampling and detection of gaseous products of high-pressure reactions. The reaction pressure can be controlled by varying the size of the pinhole of the pressure-bearing pipe. As tested by the Fischer-Tropsch synthesis (FTS) catalyzed by Co/SiO2 at 230 degrees C, the reaction pressure of our setup can reach 1.3 MPa with a pinhole size of 50 mu m and 0.16 MPa with a pinhole size of 150 mu m. The FTS products were successfully online detected by SR-PIMS, and the photoionization efficiency spectra of selected products were acquired for unambiguous identification of the detected signals. Meanwhile, time-resolved SR-PIMS spectra were acquired with a temporal resolution of 10 s. The characterization results demonstrate that the product distribution (C-2-C-4, C-5-C-11, and C12+) of FTS depends on the reaction pressure, where a high pressure facilitates the formation of long-chain hydrocarbons. With the advantages of detecting unstable intermediates and distinguishing isomers, this setup will be useful for fundamental studies of high-pressure heterogeneous catalytic reactions.