Identification of tetrahedrally ordered Si-O-Al environments in molecular sieves by \27Al\-29Si REAPDOR NMR
Résumé
The silicon sites tetrahedrally connected to aluminum in framework positions of a molecular sieve may be identified by a selective reintroduction of the hetero-nuclear 27Al–29Si dipolar interaction through Rotational Echo Adiabatic Passage DOuble Resonance (REAPDOR) NMR. In this rotor synchronized 29Si MAS experiment, an effective dipolar dephasing of the Si–O–Al, over Si–O–Si, environments is shown to aid in the identification of silicon sites in the immediate vicinity of aluminum. Application of the method in the structurally interesting and novel molecular sieve ETAS-10 provides valuable insights on the details of aluminum substitution in the zeolite lattice and further leads to the first direct NMR estimate of Al–Si distance (rAl–Si=323±5 pm) in ETAS-10.