Analytical Sciences

Abstract − Analytical Sciences, 25(1), 133 (2009).

Sealing Effect of Magic-Angle-Spinning Rotors in Solid-State NMR
Shigenobu HAYASHI
Research Institute of Instrumentation Frontier, National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba Central 5, 1-1-1 Higashi, Tsukuba, Ibaraki 305-8565, Japan
Several methods are proposed to check the sealing of a magic-angle-spinning (MAS) rotor. The intrusion of moisture into the MAS rotor is checked by trimethylphosphine oxide, which is highly hygroscopic. Its hydrated form is separately observed in 31P MAS NMR spectra from the crystalline (anhydrous) form. 1H MAS NMR can monitor the hydrated form, the crystalline form, and adsorbed water independently. Gas leakage from the MAS rotor is monitored by measuring 129Xe MAS NMR spectra of xenon (Xe) confined in zeolites as well as 3He MAS NMR spectra of 3He gas. The sealing effect of MAS rotors has been checked quantitatively using the above methods.