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Varian Solid-State NMR User Manual
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User Guide:
Solid-State NMR
V
arian NMR Spectrometer Syst
ems
With VNMR 6.1C Software
Pub
. No
. 01-99916
2-00, Rev
. C04
02
2
Table of Contents
Default Chapter
4
Table of Contents
4
Safety Precautions
8
Introduction
12
Chapter 1. Overview of Solid-State NMR
14
Line Broadening
14
Spin-Lattice Relaxation Time
15
Solids Modules, Probes, and Accessories
15
Chapter 2. CP/MAS Solids Operation
16
CP/MAS Solids Modules
16
Figure 1. Attenuator Control Graph for INOVA Systems
18
Figure 2. Attenuator Control Graph for Mercury Systems
18
Table 1. Background Nuclei of Rotor Material
19
Rotor Characteristics and Composition
20
Preparing Samples
21
Table 2. Typical Spin Rates with Associated Bearing and Drive Values
21
Spinning the Sample
22
Figure 3. Spinner Speed Control Window
25
Figure 4. Spinner Speed Control Window
27
Adjusting Homogeneity
29
Figure 5. Typical MAS Spectrum of Adamantane
31
Adjusting the Magic Angle
32
Figure 6. Coarse Adjustment of Sample Angle
32
Table 3. Reference Materials and 13 C Chemical Shifts
32
Figure 7. FID Display of Kbr on Angle
34
Figure 8. FID Display of Kbr 1/2 Turn off Angle
34
Figure 9. Typical Hexamethylbenzene (HMB) Spectrum
34
Calibrating the CP/MAS Probe
35
Table 4. Bessel Filter Outputs
35
Referencing a Solids Spectrum
37
XPOLAR1-Cross-Polarization
38
Figure 10. XPOLAR1 Pulse Sequence
38
Table 5. Wideline Experiment Commands and Parameters
38
Optimizing Parameters and Special Experiments
41
Figure 11. Array of Contact Times
41
Figure 12. TOSS Experiment on Alanine (Spectrum and Sequence)
42
Figure 13. Protonated Carbon Suppression of Alanine (Spectrum and Sequence)
43
Figure 14. Rotating-Frame Spin-Lattice Relaxation Measurements Sequence
43
Useful Conversions
44
Figure 15. Pulse Sequence for Measuring H T
44
Chapter 3. Wideline Solids Module Operation
46
Wideline Solids Module
46
Figure 16. Solids Cabinet Layout, Open Front View
48
Wideline Experiments
50
SSECHO Pulse Sequence
51
Data Acquisition
51
Standard Wideline Samples
53
Table 6. Rotor Synchronization Controls
53
Data Processing
55
Table 7. Rotor Controller Gain Setting and Typical Ranges
55
Chapter 4. Cramps/Multipulse Module Operation
56
Introduction to Multipulse Experiments
56
Cramps/Multipulse Module Hardware
57
Multipulse Experiments and User Library
60
Multipulse Tune-Up Procedure (FLIPFLOP)
60
Figure 17. Real Channel FID Pattern
62
Figure 18. FLIPFLIP FID at Exact 90 ° Pulse
62
Figure 19. FLIPFLOP "Tram Tracks
63
Figure 20. FLIPFLOP Desired FID
63
CRAMPS Experiment (BR24 or MREV8)
64
H CRAMPS Experiment (BR24 or MREV8)
64
How to Obtain Good CRAMPS Spectra
65
Figure 21. Adipic Acid Spectrum
65
Quadrature 1H CRAMPS
66
Fast MAS Assisted with a Multiple-Pulse Cycle (Wahuhahs)
67
Table 8. Multiacquisition Quadrature Corrections for MREV8
67
Table 9. Multiacquisition Quadrature Corrections for BR24
67
FLIPFLOP - Pulse Width and Phase Transient Calibration
68
Figure 22. Pulse Sequence for Flipflop.C
68
BR24 and CYLBR24 - Multiple Pulse Line Narrowing (24-Pulse Cycle)
69
Figure 23. BR24 Pulse Sequence
69
MREV8 and CYLMREV - Multiple Pulse Line Narrowing (8-Pulse Cycle)
70
Figure 24. MREV8 Pulse Sequence
70
Wahuha and Wahuhahs - MP-Assisted High-Speed Spinning (4-Pulse Cycle)
71
Figure 25. Wahuha Pulse Sequence
71
Chapter 5. Solid-State NMR Accessories
72
Pneumatics/Tachometer Box
72
Rotor Synchronization Operation
72
C0402 VNMR 6.1C User Guide: Solid-State NMR
72
Figure 26. Pneumatics/Tachometer Box for CP/MAS Probes
73
Figure 27. Different Modes of the Rotor Synchronization Accessory
73
Figure 28. Base of a Varian High-Speed Spinning Rotor
74
Figure 29. Doty Double Bearing Rotor
74
Rotor Speed Controller Accessory Operation
76
Variable Temperature Operation with Solids
78
Chapter 6. Solid-State NMR Experiments
80
XPOLAR-Cross-Polarization, UNITY
81
Figure 30. TOSS Pulse Sequence
82
Figure 31. Protonated Carbon Suppression Sequence
83
Figure 32. Rotating-Frame Spin-Lattice Relaxation Measurements Sequence
83
Figure 33. Pulse Sequence for Measuring H T
84
XPOLAR1-Cross-Polarization
85
Figure 34. XPOLAR1 Pulse Sequence
85
XPWXCAL-Observe-Pulse Calibration with Cross-Polarization
87
Figure 35. XPWXCAL Pulse Sequence
88
XNOESYSYNC-Rotor Sync Solids Sequence for Exchange
89
Figure 36. XNOESYSYNC Pulse Sequence
89
MASEXCH1-Phase-Sensitive Rotor Sync Sequence for Exchange
90
Figure 37. MASEXCH1 Pulse Sequence
91
HETCORCP1-Solid-State HETCOR
92
WISE1-Two-Dimensional Proton Wideline Separation
93
XPOLWFG1-Cross-Polarization with Programmed Decoupling
93
XPOLXMOD1-Waveform Modulated Cross-Polarization
95
Figure 38. XPOLXMOD1 Pulse Sequence
95
VACP-Variable Amplitude Cross-Polarization
97
Figure 39. VACP Pulse Sequence
97
XPOLEDIT1-Solids Spectral Editing
98
Figure 40. XPOLDIT1 Pulse Sequence
98
3QMAS1-Triple-Quantum 2D for Quadrupole Nuclei
99
Figure 41. 3QMAS1 Pulse Sequence
99
Table 10. Multiacquisition Quadrature Corrections for CORY24
100
PASS1-2D Sideband Separation for CP/MAS
101
Figure 42. PASS1 Pulse Sequence
101
CPCS-Cross-Polarization with Proton Chemical Shift Selection
102
Figure 43. CPCS Pulse Sequence
102
CPCOSYPS-Cross-Polarization Phase-Sensitive COSY
103
CPNOESYPS-Cross-Polarization Phase-Sensitive NOESY
104
Figure 44. CPCOSYPS Pulse Sequence
104
Figure 45. CPNOESYPS Pulse Sequence
105
R2SELPULS1-Rotation Resonance with Selective Inversion
106
Figure 46. R2SELPULS1 Pulse Sequence
107
DIPSHFT1-Separated Local Field Spectroscopy
108
Figure 47. DIPSHFT1 Pulse Sequence
108
SEDRA2-Simple Excitation of Dephasing Rotational-Echo Amplitudes
109
Figure 48. SEDRA2 Pulse Sequence
110
REDOR1-Rotational Echo Double Resonance
111
Figure 49. REDOR1 Pulse Sequence
112
DOUBLECP1-Double Cross-Polarization
113
Figure 50. DOUBLECP1 Pulse Sequence
114
T1Cp1-T
115
Figure 51. T1CP1 Pulse Sequence
115
T1CP1-T 1 Measurement with Cross-Polarization
115
HAHNCP1-Spin 1/2 Echo Sequence with CP
116
Figure 52. HAHNCP1 Pulse Sequence
116
SSECHO1-Solid-State Echo Sequence for Wideline Solids
117
Figure 53. SSECHO1 Pulse Sequence
118
WLEXCH1-Wideline Solids Exchange
119
Figure 54. WLEXCH1 Pulse Sequence
120
HS90-90-Degree° Phase Shift Accuracy
121
Figure 55. HS90 Pulse Sequence
121
MREVCS-Multiple Pulse Chemical-Shift Selective Spin Diffusion
122
Figure 56. MREVCS Pulse Sequence
122
MQ_SOLIDS-Multiple-Quantum Solids
123
Figure 57. MQ_SOLIDS Pulse Sequence
123
SPINDIFF-Spin Diffusion in Solids
124
FASTACQ-Multinuclear Fast Acquisition
124
Figure 58. SPINDIFF Pulse Sequence
124
NUTATE-Solids 2D Nutation
125
Figure 59. FASTACQ Pulse Sequence
125
Figure 60. NUTATE Pulse Sequence
126
Index
128
4
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Varian Solid-State NMR Specifications
General
Brand
Varian
Model
Solid-State NMR
Category
Measuring Instruments
Language
English
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