Two Dimensional One Pulse (TOP) processing...
27Al MAS 300MHz spectrum of YAG for TOP processing
D.Massiot, J.Hiet, N.Pellerin, F.Fayon, M.Deschamps, S.Steuernagel, P.J.Grandinetti
'Two dimensional One Pulse MAS of Half-Integer Quadrupolar Nuclei'
Journal of Magnetic Resonance 181 310-315 (2006)
TOP reconstruction protocol (only
available from dm2006 versions)
Download the TOP example files [Download]
and extract the zip file to a directory of you choice.
Load the "YAG 300 001 BL.1R" 1D file
[Menu/File/Open. The 1D files shows multiple spinning sidebands arising from
the satellite transitions of AlO6 and AlO4
Load the default decomposition parameters
[Menu/Decomposition/Load Fit]. This decomposition file only contains a fit
of the <+/-3/2> spinning sidebands allowing an exact measurement of the
spinning rate (31244.29Hz).
Generate the 2D TOP spectrum by calling
Click the "baseline correct" to add a baseline correction after the 1D->2D
Click the "separate slices" to separate the reconstructed spinning sideband
slices by nulls
Click the "to 2D" button to execute or "Quit" to exit
You should now have a 2D spectrum looking
like this (after rescaling with [Menu/Graph/Parameters change "level div" to
In this spectrum you see
+ the AlO6 sharp line with its satellite
transition (right most intense line)
+ the AlO4 second order broadened central
transition, only showing up in the central slice (N=0) with its <+-3/2>
transition on the left side (sharp ridge) and even some contributions of the
Build the sum spectrum (equivalent to
synchronized acquisition) by calling [Menu/Tools/TOP/Proj all] and obtain the
spectrum below showing clearly the <1/2>, <3/2> and <5/2> transitions (from
right to left) of the AlO4 contribution
Go to the left panel button and select "ssb"
from the projection list ("no proj" by default) and build the projection
again [Menu/Tools/TOP/Proj N#0] and obtain the spectra of the satellite
transitions alone (by ignoring the N=0 central transition).