A high-pressure reactor coupled to synchrotron radiation photoionization mass spectrometry

• Published in: Review of scientific instruments 2020-09, Vol.91 (9), p.093102-093102
• Main Authors: You, Rui, Yu, Shengsheng, Yang, Jiuzhong, Pan, Yang, Huang, Weixin
• Format: Article
• Language: English
• Subjects: Chemical synthesis; Fischer-Tropsch process; Ions; Isomers; Mass spectrometry; Photoionization; Pinholes; Scientific apparatus & instruments; Scientific imaging; Silicon dioxide; Spectroscopy; Synchrotron radiation; Synchrotrons; Temporal resolution
• ISSN: 0034-6748; 1089-7623
• DOI: 10.1063/5.0014144

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 °C, the reaction pressure of our setup can reach 1.3 MPa with a pinhole size of 50 µm and 0.16 MPa with a pinhole size of 150 µm. 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 (C2–C4, C5–C11, 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.