Varian Solid-State NMR - Default Chapter; Table of Contents

01-999162-00 C0402 VNMR 6.1C User Guide: Solid-State NMR 4
Table of Contents
SAFETY PRECAUTIONS .................................................................................... 8
Introduction ...................................................................................................... 12
Chapter 1. Overview of Solid-State NMR ...................................................... 14
1.1 Line Broadening ......................................................................................................... 14
1.2 Spin-Lattice Relaxation Time ..................................................................................... 15
1.3 Solids Modules, Probes, and Accessories ................................................................... 15
Chapter 2. CP/MAS Solids Operation ............................................................ 16
2.1 CP/MAS Solids Modules ............................................................................................ 16
2.2 Rotor Characteristics and Composition ...................................................................... 20
2.3 Preparing Samples ...................................................................................................... 21
2.4 Spinning the Sample ................................................................................................... 22
2.5 Adjusting Homogeneity .............................................................................................. 29
2.6 Adjusting the Magic Angle ......................................................................................... 32
2.7 Calibrating the CP/MAS Probe ................................................................................... 35
2.8 Referencing a Solids Spectrum ................................................................................... 37
2.9 XPOLAR1—Cross-Polarization ................................................................................. 38
2.10 Optimizing Parameters and Special Experiments ..................................................... 41
2.11 Useful Conversions ................................................................................................... 44
Chapter 3. Wideline Solids Module Operation .............................................. 46
3.1 Wideline Solids Module .............................................................................................. 46
3.2 Wideline Experiments ................................................................................................. 50
3.3 SSECHO Pulse Sequence ........................................................................................... 51
3.4 Data Acquisition ......................................................................................................... 51
3.5 Standard Wideline Samples ........................................................................................ 53
3.6 Data Processing ........................................................................................................... 55
Chapter 4. CRAMPS/Multipulse Module Operation ...................................... 56
4.1 Introduction to Multipulse Experiments ..................................................................... 56
4.2 CRAMPS/Multipulse Module Hardware .................................................................... 57
4.3 Multipulse Experiments and User Library .................................................................. 60
4.4 Multipulse Tune-Up Procedure (FLIPFLOP) ............................................................. 60
4.5
1
H CRAMPS Experiment (BR24 or MREV8) ........................................................... 64
4.6 How to Obtain Good CRAMPS Spectra ..................................................................... 65
4.7 Quadrature 1H CRAMPS ........................................................................................... 66
4.8 Fast MAS Assisted with a Multiple-Pulse Cycle (WaHuHaHS) ................................ 67
4.9 FLIPFLOP - Pulse Width and Phase Transient Calibration ........................................ 68
4.10 BR24 and CYLBR24 - Multiple Pulse Line Narrowing (24-pulse cycle) ................ 69
4.11 MREV8 and CYLMREV - Multiple Pulse Line Narrowing (8-pulse cycle) ........... 70
4.12 WaHuHa and WaHuHaHS - MP-Assisted High-Speed Spinning (4-pulse cycle) .... 71