Determination of 27Al-29Si connectivities in zeolites with 2D 27Al→29Si RAPT-CPMG-HETCOR NMR

被引:19
作者
Kennedy, Gordon J. [1 ]
Wiench, Jerzy W. [2 ,3 ]
Pruski, Marek [2 ,3 ]
机构
[1] ExxonMobil Res & Engn Co, Corp Strateg Res, Annandale, NJ 08801 USA
[2] Iowa State Univ, Ames Lab, Ames, IA 50011 USA
[3] Iowa State Univ, Dept Chem, Ames, IA 50011 USA
关键词
ZSM-4; MAZ; zeolite; NMR; HETCOR;
D O I
10.1016/j.ssnmr.2008.04.002
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
The recently introduced concept of the combined use of rotor assisted population transfer (RAPT) and Carr-Purcell-Meiboom-Gill (CPMG) techniques to boost the sensitivity of cross polarization (CP) based NMR experiments is applied to a synthetic zeolite (ZSM-4). The sensitivity was increased by a factor of similar to 4, which enabled acquisition of a high quality two-dimensional Al-27-Si-29 HETCOR (heteronuclear correlation) spectrum. By separating the resonances in two dimensions, through-space connectivities between spins were revealed and the effective resolution was improved in both dimensions, which allowed determination of the existing ambiguities in spectral assignments in this material. The spectra provided clear indication of random distribution of aluminum and silicon within the ZSM-4 network. Additionally, unexpected correlations were observed between different components of in homogeneously broadened Si-29 and Al-27 lines, which are most likely due to differences in the second coordination sphere environments. (c) 2008 Elsevier Inc. All rights reserved.
引用
收藏
页码:76 / 81
页数:6
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