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Updated: Aug 22, 2025

Synthesis of Zeolites Using the ADOR Assembly-Disassembly-Organization-Reassembly Route
Published on: April 3, 2016
Direct Identification of Zeolite Beta Polymorphs by Solid-State 29Si Nuclear Magnetic Resonance Spectroscopy
Yury G Kolyagin1,2, Alexander V Yakimov1, Dmitry S Zasukhin1
1Department of Chemistry, Lomonosov Moscow State University, Leninskye Gory 1, Building 3, 119991 Moscow, Russia.
Abstract:
Stacking disorder and polymorphism in zeolite and zeolite-like materials hinder their structural characterization. In this work, we propose an advanced approach based on applying "pure shift" solid-state 29Si nuclear magnetic resonance (NMR) spectroscopy for the structural investigation of zeolitic materials containing intergrown polymorphs. The approach developed in the case study of zeolite beta allows for the resolution of 21 29Si signals, attributing them to non-equivalent T sites in polymorphs A, B, and C, reconstruction of individual 29Si magic angle spinning NMR spectra for each polymorph, and determination of the polymorph composition with higher accuracy than X-ray diffraction. The results reveal that two widely used synthetic routes for zeolite beta, alkaline and fluoride synthesis, lead to different polymorph compositions. These findings indicate that "pure shift" solid-state 29Si NMR can serve as a superior tool for the elucidation of polymorphism in zeolites.
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