Bruker BioSpin Solid State NMR - Page 310

310 (327) BRUKER BIOSPIN User Manual Version 002
Figures
Figure 3.39. Mounting a Triple Insert Into a Triple Probe ............................................................. 49
Figure 3.40. Example of a 600 WB NMR Instrument Site ............................................................. 51
Figure 3.41. Short Display, Pulse Routing Only for C/N/H DCP or REDOR Experiment, observing
13C (above) and 15N (below).................................................................................. 52
Figure 3.42. Long Display, Pulse and Receiver Routing............................................................... 53
Figure 3.43. Pulse on F2, Observe on F1 - Routing ..................................................................... 54
Figure 3.44. The edasp Display for a System with two Receiver Channels .................................. 54
4 Basic Setup Procedures 55
Figure 4.1. Routing for a Simple One Channel Experiment ........................................................ 57
Figure 4.2. Probe Connections to the Preamplifier..................................................................... 59
Figure 4.3. Pop-up Window for a New Experiment..................................................................... 60
Figure 4.4. ased Table with Acquisition Parameters for the KBr Experiment............................... 61
Figure 4.5. Graphical Pulse Program Display ............................................................................ 62
Figure 4.6. Display Example of a Well-tuned Probe ................................................................... 63
Figure 4.7. Display Example of an Off-Matched and Off-Tuned Probe........................................ 64
Figure 4.8. Display Example Where Probe is Tuned to a Different Frequency ............................ 64
Figure 4.9. FID and Spectrum of the 79Br Signal of KBr used to Adjust the Magic Angle ........... 65
Figure 4.10. Routing for a Double Resonance Experiment using High Power Stage for H and X-nu-
cleus ....................................................................................................................... 66
Figure 4.11. Routing for a Double Resonance Experiment, Changed for Proton Observation ....... 67
Figure 4.12. Proton Spectrum of Adamantane at Moderate Spin Speed ....................................... 68
Figure 4.13. Setting the Carrier on Resonance............................................................................ 69
Figure 4.14. Expanding the Region of Interest............................................................................. 70
Figure 4.15. Save Display Region to Menu.................................................................................. 70
Figure 4.16. The popt Window ....................................................................................................71
Figure 4.17. The popt Display after Proton p1 Optimization ......................................................... 72
Figure 4.18. Adamantane 13C FID with 50 msec aq. setsh Display ............................................. 74
Figure 4.19. Adamantane 13C FID with 50 msec aq. setsh with Optimized Z-Shim Value............. 74
Figure 4.20. A cp Pulse Sequence .............................................................................................. 76
Figure 4.21. Hartmann-Hahn Optimization Profile........................................................................ 77
Figure 4.22. Hartmann-Hahn Optimization Profile Using a Square Proton Contact Pulse ............. 78
Figure 4.23. Display Showing α-Glycine Taken Under Adamantane Conditions, 4 scans.............. 79
Figure 4.24. Optimization of the Decoupler Offset o2 at Moderate Power, Using cw Decoupling .. 80
Figure 4.25. Glycine with cw Decoupling at 90 kHz RF Field ....................................................... 81
Figure 4.26. Glycine Spectrum with Spinal64 Decoupling at 93 kHz RF field ................................ 83
5 Decoupling Techniques 89
Figure 5.1. Optimization of TPPM Decoupling, on Glycine at Natural Abundance....................... 90
Figure 5.2. Geometry for the FSLG Condition............................................................................ 93
Figure 5.3. FSLG Decoupling Pulse Sequence Diagram ............................................................ 94
Figure 5.4. Adamantane, FSLG-decoupled, showing the (downscaled) C-H J-couplings. ........... 94
Figure 5.5. Shape with Phase Gradients ................................................................................... 96
Figure 5.6. Pulse Program for Hahn Echo Sequence ................................................................. 98
6 Practical CP/MAS Spectroscopy on Spin 1/2 Nuclei 99
7 Basic CP-MAS Experiments 105
Figure 7.1. Pulse Program for CP with Flip-back Pulse............................................................ 105
Figure 7.2. Pulse Program for CPTOSS. ................................................................................. 107