Sealing Effect of Magic-Angle-Spinning Rotors in Solid-State NMR

被引:12
作者
Hayashi, Shigenobu [1 ]
机构
[1] Natl Inst Adv Ind Sci & Technol, Res Inst Instrumentat Frontier, Tsukuba, Ibaraki 3058565, Japan
关键词
CHEMICAL-SHIFTS; SEALED SAMPLES; XE-129; RELAXATION; ZEOLITES; INSERT; PHASE;
D O I
10.2116/analsci.25.133
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
Several methods are proposed to check the sealing of a magic-angle-spinning (MAS) rotor. The intrusion Of moisture into C the MAS rotor is checked by trimethylphosphine oxide, which is highly hygroscopic. Its hydrated form is separately observed in (31)P MAS NMR spectra front the crystalline (anhydrous) form. (1)H MAS NMR can monitor the hydrated form, the crystalline form. and adsorbed water independently. Gas leakage from the MAS rotor is monitored by measuring (129)Xe MAS NMR spectra of xenon (Xe) confined in zeolites as well as (3)He MAS NMR spectra of (3)He gas. The sealing effect of MAS rotors has been checked quantitatively using the above methods.
引用
收藏
页码:133 / 136
页数:4
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