Experimental method for low-temperature reaction studies in sealed samples by 13C CP/MAS NMR |
| |
| Institution: | 1. Ames Laboratory Institute for Physical Research and Technology, Ames, Iowa 50011, USA;2. Department of Chemical Engineering, Iowa State University, Ames, Iowa 50011 USA;3. Department of Chemistry, Iowa State University, Ames, Iowa 50011, USA;1. School of Mechanical and Power Engineering, Nanjing TECH University, Nanjing, Jiangsu 211816, China;2. Centre for Precision Engineering, Harbin Institute of Technology, Harbin, Heilongjiang 150001, China;3. School of Material and Science, Shenyang Ligong University, Shenyang, Liaoning 110159, China |
| |
| Abstract: | A new, simple, and inexpensive technique is presented for monitoring high-resolution solid-state NMR of 13C at temperatures ranging between 85 and 450 K. In this procedure, the reaction conditions are controlled by preparing samples at 77 K in 5 mm NMR tubes, while attached to a vacuum system. The NMR tubes are prefitted with a rotor for spinning. After preparation, the samples are sealed, transferred to the double-resonance MAS NMR probe, and analyzed, all while the sample temperature is maintained as low as 85 K. The spinning rates vary from 3.0 kHz at 85 K to 5.2 kHz at 300 K using nitrogen drive gas. Probe design and performance, sample-preparation procedure, and details of the low-temperature experiment are described. In general, the technique may be applied in studies of low-temperature reaction mechanisms and kinetics. 13C CP/MAS spectra of ethylene adsorbed on silica-supported ruthenium catalyst are presented to illustrate its performance and possible application. |
| |
| Keywords: | |
| 本文献已被 ScienceDirect 等数据库收录！ |
|
