Download Solid State NMR: AVANCE Solids User Manual - Pascal-Man

Transcript
Contents
5.4
5.5
5.6
6
6.1
6.2
6.3
6.4
6.5
7
7.1
7.2
7.3
7.4
8
8.1
8.2
8.3
9
9.1
9.2
9.3
Basic CP-MAS Experiments ..............................................61
Introduction ...................................................................................... 61
Pulse Calibration with CP ............................................................. 61
Total Sideband Suppression TOSS ................................................... 62
SELTICS .......................................................................................... 66
Non-Quaternary Suppression (NQS) ................................................ 69
Spectral Editing Sequences: CPPI, CPPISPI and CPPIRCP ............. 72
FSLG-HETCOR ..................................................................75
Introduction ......................................................................................
Pulse Sequence Diagram for FSLG HETCOR ...................................
Setting FSLG HETCOR Experiments ................................................
Results ............................................................................................
75
76
77
81
Modifications of FSLG HETCOR .......................................83
Carbon Decoupling During Evolution ................................................ 84
HETCOR with DUMBO, PMLG or w-PMLG, Using Shapes ................ 85
The Sequence pmlghet ................................................................. 85
w-pmlghet .................................................................................... 88
edumbohet ................................................................................... 89
dumbohet ..................................................................................... 90
HETCOR with Cross Polarization under LG Offset ............................ 91
RFDR .................................................................................93
9.4
Experiment ...................................................................................... 94
Set-up .............................................................................................. 94
Data Acquisition ............................................................................... 95
Set-up 2D Experiment .................................................................. 95
Spectral Processing ......................................................................... 96
10
Proton Driven Spin Diffusion (PDSD) ...............................99
10.1
10.2
10.3
10.4
10.5
11
11.1
11.2
11.3
4
Possible Approaches for non-13C Samples ...................................... 57
Hints, Tricks, Caveats for Multi-nuclear (CP-)MAS Spectroscopy ...... 58
Setup for Standard hetero-nuclear Samples 15N, 29SI, 31P ............. 58
Pulse Sequence Diagram ............................................................... 101
Basic Setup .................................................................................... 101
2D Experiment Setup .................................................................. 101
Acquisition Parameters .................................................................. 103
Processing Parameters ............................................................... 104
Adjust the Rotational Resonance Condition for DARR/RAD ............ 104
Example Spectra ............................................................................ 106
SUPER ............................................................................. 109
Overview ........................................................................................ 109
Pulse Program ............................................................................... 110
Experiment Setup .......................................................................... 110
Experiment setup ....................................................................... 110
Setup 2D Experiment ...................................................................111
BRUKER BIOSPIN
User Manual Version 001