Laser-supported high-temperature MAS NMR for time-resolved in situ studies of reaction steps in heterogeneous catalysis

Solid State Nucl Magn Reson. 1996 Apr;6(2):147-56. doi: 10.1016/0926-2040(95)01214-1.

Abstract

The temperature of zeolite samples containing various adsorbed molecules was rapidly changed (within 15 s) from room temperature to 600 K by means of a laser beam. The location of the sealed glass ampoule in a boron nitride container decreases the temperature gradient in the sample and avoids laser-induced reactions. The technique facilitates time-dependent magic-angle-spinning (MAS) NMR spectroscopy of high-temperature reactions which take place within 60 s. The H-D exchange in the hydrogen form of zeolites loaded with fully deuterated molecules, the methanol-to-gasoline conversion and the catalytic ethylbenzene disproportionation in zeolites were monitored by 13C and 1H MAS NMR by means of a "stop and go" method.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Benzene Derivatives / chemistry
  • Carbon Isotopes
  • Catalysis
  • Deuterium / chemistry
  • Hot Temperature
  • Hydrogen / chemistry
  • Lasers
  • Magnetic Resonance Spectroscopy / instrumentation
  • Magnetic Resonance Spectroscopy / methods*
  • Methanol / chemistry
  • Zeolites / chemistry

Substances

  • Benzene Derivatives
  • Carbon Isotopes
  • Zeolites
  • Hydrogen
  • Deuterium
  • ethylbenzene
  • Methanol