Bruker BioSpin Solid State NMR

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Practical CP/MAS Spectroscopy on Spin 1/2 Nuclei

User Manual Version 002 BRUKER BIOSPIN 103 (327)

- subtract 2 dB from pl1 (more is not required since the transmitter will usually

put out 50% more power at

N frequency)

- set p15 = 3 ms

- acquire 4-8 scans

- optimize HH condition, acquire reference spectrum with aq=25-35 ms

Si on DSS

- load α-glycine

C reference spectrum

- set observe nucleus to

Si in edasp

- add 2 dB to sp0

- acquire 4 scans with aq = 35 ms

- optimize HH condition, acquire reference spectrum

P on ADP (ammonium dihydrogen phosphate NH

)

- load α-glycine

C reference spectrum

- set observe nucleus to

P in edasp

- add 6 dB to pl1

- optimize HH condition, acquire 2 scans, reduce rg appropriately.

Main Page

Default Chapter3
- Table of Contents3
- Contents3
1 Introduction9
- Disclaimer10
- Safety Issues10
- Contact for Additional Technical Assistance10
2 Test Samples11
- Test Samples12
- Test Samples13
- Table 2.1. Setup Samples for Different NMR Sensitive Nuclei13
3 General Hardware Setup15
- Connections to the Preamplifier15
  - Figure 3.1. All Connections to the Back of the Preamplifier16
  - General Hardware Setup16
- Figure 3.2. Transmitter Cables (Only) Wired to Back of the Preamplifier17
- Figure 3.3. the Edasp Setpreamp Display18
- Figure 3.4. Additional Connections to the Preamplifier Stack19
- RF Connections between Preamplifier and Probe20
- Figure 3.5. Matching Box Setup for High Power X-BB Preamplifiers20
- RF-Filters in the RF Pathway21
- Figure 3.6. Standard Double Resonance CP Experiment, Bypassing the Proton Preamp22
- Figure 3.7. Standard CP Experiment, Proton Preamp in Line22
- Figure 3.8. Triple Resonance Experiment, Without X-Y Decoupling23
- Figure 3.9. Triple Resonance Experiment, with X-Y Decoupling23
- Figure 3.10. Triple Resonance 1H/19F-Experiment24
- Figure 3.11. 19F/1H Combiner/Filter Set24
- Connections for Probe Identification and Spin Detection25
- Figure 3.12. Quadruple Resonance HFXY Experiment (WB Probes ≥ 400 Mhz Only!)25
- Figure 3.13. PICS Probe Connector and Spin Rate Monitor Cable on a WB Probe25
- MAS Tubing Connections26
- Figure 3.14. Spin Rate Monitor Cable Connector for 2 Different Types of SB Probes26
- Connections27
  - Wide Bore (WB) Magnet Probes28
  - Figure 3.15. WB DVT Probe MAS Tubing Connections28
  - Figure 3.16. VTN Probe MAS Tubing Connections Note: WVT Probes Are VTN-Type Probes28
  - Figure 3.17. WB Probes: Eject/Insert Connections29
  - Figure 3.18. WB Probes: DVT, Probe Connections for RT and HT Measurements29
  - Standard Bore (SB) Magnet Probes30
  - Figure 3.19. SB VTN Probe MAS Connections30
- Additional Connections for VT Operation31
- Figure 3.20. SB DVT Probe MAS Connections31
- Figure 3.21. WB Probe MAS VTN and WVT, and DVT Probe Connections32
- Figure 3.22. WB Probe MAS DVT Connections33
- Figure 3.23. SB Probe MAS VTN34
- Figure 3.24. SB Probe MAS DVT Connections34
- Figure 3.25. WB Wideline or PE Probes35
- Figure 3.26. WB Wideline or PE Probe Connections35
- Figure 3.27. Low Temperature Heat Exchanger for VTN Probes (Old Style)36
- Figure 3.28. Low Temperature Heat Exchanger for DVT Probes37
- Figure 3.29. Low Temperature Liquid N2 Dewar with DVT Probe/Heat Exchanger38
- Figure 3.30. Bottom View of Low Temperature DVT Probe/Heat Exchanger39
- Figure 3.31. Low Temperature Setup with B-CU X (or B-CU 05)40
- Probe Setup, Operations, Probe Modifiers41
- Setting the Frequency Range of a Wideline (Single Frequency) Probe41
- Figure 3.32. Low Temperature Setup with B-CU X41
- Shifting the Probe Tuning Range42
- Figure 3.33. RF Setup of a Wideline Single Frequency Probe42
- Figure 3.34. Possible Modifiers for Probe Tuning Ranges (400 Mhz and up Only)44
- Figure 3.35. Λ/4 (Low Range) and Λ/2 Mode (High Range), 400 Mhz Probe45
- Figure 3.36. a Λ/4 Only Probe (Left) and a Λ/4 - Λ/2 Probe (Right)46
- Figure 3.37. Without/With Parallel Capacitance to Shift the Tuning Range to Lower Frequency47
- Adding a Frequency Channel to a Probe (WB Probes Only)48
- Figure 3.38. Parallel Coil to Shift the Tuning Range to Higher Frequency48
- Figure 3.39. Mounting a Triple Insert into a Triple Probe49
- Mounting the Probe in the Magnet/Shim Stack50
- EDASP Display: Software Controlled Routing51
- Figure 3.40. Example of a 600 WB NMR Instrument Site51
- Figure 3.41. Short Display, Pulse Routing Only for C/N/H DCP or REDOR Experiment, Observing52
- Figure 3.42. Long Display, Pulse and Receiver Routing53
- Figure 3.43. Pulse on F2, Observe on F1 - Routing54
- Figure 3.44. the Edasp Display for a System with Two Receiver Channels54
4 Basic Setup Procedures55
- General Remarks56
- Setting the Magic Angle on Kbr57
- RF-Routing57
- Figure 4.1. Routing for a Simple One Channel Experiment57
- Setting Acquisition Parameters59
- Figure 4.2. Probe Connections to the Preamplifier59
- Figure 4.3. Pop-Up Window for a New Experiment60
- Figure 4.4. Ased Table with Acquisition Parameters for the Kbr Experiment61
- Figure 4.5. Graphical Pulse Program Display62
- Figure 4.6. Display Example of a Well-Tuned Probe63
- Figure 4.7. Display Example of an Off-Matched and Off-Tuned Probe64
- Figure 4.8. Display Example Where Probe Is Tuned to a Different Frequency64
- Calibrating 1H Pulses on Adamantane65
- Figure 4.9. FID and Spectrum of the 79Br Signal of Kbr Used to Adjust the Magic Angle65
- Figure 4.10. Routing for a Double Resonance Experiment Using High Power Stage for H and X-Nu66
- Figure 4.11. Routing for a Double Resonance Experiment, Changed for Proton Observation67
- Figure 4.12. Proton Spectrum of Adamantane at Moderate Spin Speed68
- Figure 4.13. Setting the Carrier on Resonance69
- Figure 4.14. Expanding the Region of Interest70
- Figure 4.15. Save Display Region to Menu70
- Figure 4.16. the Popt Window71
- Figure 4.17. the Popt Display after Proton P1 Optimization72
- Calibrating 13C Pulses on Adamantane and Shimming the Probe73
- Figure 4.18. Adamantane 13C FID with 50 Msec Aq. Setsh Display74
- Figure 4.19. Adamantane 13C FID with 50 Msec Aq. Setsh with Optimized Z-Shim Value74
- Calibrating Chemical Shifts on Adamantane75
- Setting up for Cross Polarization on Adamantane76
- Figure 4.20. a Cp Pulse Sequence76
- Figure 4.21. Hartmann-Hahn Optimization Profile77
- Figure 4.22. Hartmann-Hahn Optimization Profile Using a Square Proton Contact Pulse78
- Cross Polarization Setup and Optimization for a Real Solid: Glycine79
- Figure 4.23. Display Showing Α-Glycine Taken under Adamantane Conditions, 4 Scans79
- Figure 4.24. Optimization of the Decoupler Offset O2 at Moderate Power, Using Cw Decoupling80
- Figure 4.25. Glycine with Cw Decoupling at 90 Khz RF Field81
- Figure 4.26. Glycine Spectrum with Spinal64 Decoupling at 93 Khz RF Field83
- Table 4.2. Processing Parameters for the Glycine S/N-Test83
- Some Practical Hints for CPMAS Spectroscopy85
- Table 4.3. Reasonable RF-Fields for Max. 2% Duty Cycle85
- Field Setting and Shift Calibration87
- Literature88
5 Decoupling Techniques89
- Heteronuclear Decoupling89
- CW Decoupling89
- TPPM Decoupling90
- Figure 5.1. Optimization of TPPM Decoupling, on Glycine at Natural Abundance90
- SPINAL Decoupling91
- Swept-Frequency-TPPM91
- Decoupling91
- Pi-Pulse Decoupling91
- Homonuclear Decoupling92
- Multiple Pulse NMR: Observing Chemical Shifts of Homonuclear Coupled Nuclei92
- Multiple Pulse Decoupling92
- Transverse Dephasing Optimized Spectroscopy98
- Figure 5.6. Pulse Program for Hahn Echo Sequence98
6 Practical CP/MAS Spectroscopy on Spin 1/2 Nuclei99
- Possible Difficulties99
- Possible Approaches for 13C Samples99
- Possible Approaches for Non-13C Samples101
- Table 6.1. Power Conversion Table101
- Hints, Tricks, Caveats for Multi-Nuclear (CP-)MAS Spectroscopy102
- Setup for Standard Heteronuclear Samples 15N, 29SI, 31P102
7 Basic CP-MAS Experiments105
- Pulse Calibration with CP105
- Figure 7.1. Pulse Program for CP with Flip-Back Pulse105
- Total Sideband Suppression TOSS106
- Table 7.2. Acquisition Parameters106
- Figure 7.2. Pulse Program for CPTOSS107
- Table 7.3. Acquisition Parameters107
- Figure 7.3. Comparison of a CPTOSS and CPMAS Experiment108
- Figure 7.4. CPTOSS243 Experiment on Tyrosine Hcl at 6.5 Khz109
- Seltics110
- Figure 7.5. CPTOSS Experiment on Tyrosine Hcl at 6.5 Khz110
- Figure 7.6. Pulse Program for SELTICS111
- Figure 7.7. SELTICS at 6.5 Khz Sample Rotation on Tyrosine Hcl111
- Figure 7.8. Cholesterylacetate Spectrum Using Sideband Suppression112
- Non-Quaternary Suppression (NQS)113
- Figure 7.9. Block Diagram of the Non-Quaternary Suppression Experiment113
- Table 10.1. Acquisition Parameters113
- Figure 7.10. Glycine 13C CPMAS NQS Experiment with a Dephasing Delay114
- Figure 7.11. Tyrosine 13C CPMAS NQS Experiment with TOSS115
- Spectral Editing Sequences: CPPI, CPPISPI and CPPIRCP116
- Figure 7.12. Block Diagram of the CPPI Experiment116
- Figure 7.13. CPMAS Spectrum of Tyrosine.hcl at 6.5 Khz117
8 Fslg-Hetcor119
- Pulse Sequence Diagram for FSLG HETCOR120
- Figure 8.1. the FSLG Hetcor Experiment120
- Setting up FSLG HETCOR121
- Figure 8.2. the "12121
- Figure 8.3. the Ased Display122
- Table 8.2. Processing Parameters for FSLG-HETCOR (on Tyrosine-Hcl)124
- Results125
- Figure 8.4. FSLG Hetcor Spectrum Tyrosine Hcl125
- Figure 8.5. FSLG Hetcor Spectrum Tyrosine Hcl126
9 Modifications of FSLG HETCOR127
- Carbon Decoupling During Evolution128
- Figure 9.1. Comparison of HETCOR with and Without 13C-Decoupling128
- HETCOR with DUMBO, PMLG or W-PMLG, Using Shapes129
- The Sequence Pmlghet129
- Figure 9.2. HETCOR Using Windowless Phase Ramps130
- Table 9.1. Acquisition Parameters for Pmlg-HETCOR (on Tyrosine-Hcl)130
- W-Pmlghet132
- Table 9.3. Acquisition Parameters for Wpmlg-HETCOR (on Tyrosine-Hcl)132
- Edumbohet133
- Dumbohet134
- Table 9.4. Acquisition Parameters for E-DUMBO-HETCOR (on Tyrosine-Hcl)134
- Table 9.5. Acquisition Parameters for DUMBO-HETCOR (on Tyrosine-Hcl)134
- HETCOR with Cross Polarization under LG Offset135
- Figure 9.3. HETCOR on Tyrosine *Hcl Without (Left) and with LG Contact (1Msec Contact)136
10 Rfdr137
- Experiment138
- Set-Up138
- Figure 10.1. RFDR Pulse Sequence for 2D CPMAS Exchange Experiment138
- Data Acquisition139
- Set-Up 2D Experiment139
- Figure 10.2. the "123" Icon in the Menu Bar of the Data Windows Acquisition Parameter Page139
- Spectral Processing141
- Figure 10.3. 13C Histidine Signal Decay as a Function of the RFDR Mixing Time141
- Figure 10.4. 2D RFDR Spectrum of 13C Fully Labelled Histidine (RFDR Mixing Time 1.85 Ms)142
- BRUKER BIOSPIN User Manual Version142
11 Proton Driven Spin Diffusion (PDSD)143
- Pulse Sequence Diagram145
- Basic Setup145
- Figure 11.1. CPSPINDIFF Pulse Sequence145
- 2D Experiment Setup146
- Acquisition Parameters147
- Figure 11.2. the Acquisition Parameter Window (Eda)147
- Processing Parameters149
- Adjust the Rotational Resonance Condition for DARR/RAD149
- Table 10.2. Processing Parameters149
- Figure 11.3. POPT Result for the Cw Decoupling Power Variation150
- Example Spectra151
- Figure 11.4. 13C CPSPINDIFF of Fully Labeled Tyrosine*Hcl, Spinning at 22 Khz, 4.6 Msec MIX. Up- Per: PDSD, Lower: DARR151
- Figure 11.5. Comparison of DARR/PDSD152
- Figure 11.6. 13C DARR of Fully Labelled Ubiquitine Spinning at 13 Khz153
12 Redor155
- Pulse Sequence157
- Setup157
- Figure 12.1. REDOR Pulse Sequence157
- Data Acquisition159
- Data Processing160
- Figure 12.2. 2D Data Set after "Xf2" Processing160
- Figure 12.3. T1/T2 Relaxation for Further Analysis of the Data Figure and the Analysis Interface161
- Figure 12.4. Saving Data to Continue to the Relaxation Window161
- Figure 12.5. Setting the Correct Analysis Parameter162
- Figure 12.6. Plot of the Normalized Signal Intensity Versus the Evolution Time163
- Figure 12.7. Experimental Data for the Glycine 13C{15N}-REDOR164
- Figure 12.8. Comparison of Experimental Data to a Simulation with Reduced Dipolar Coupling165
- Figure 12.9. Experimental Data with the Corresponding M2 Parabolic Analysis166
- Final Remarks167
13 Super169
- Overview169
- Pulse Program170
- Experiment Setup170
- Figure 13.1. Pulse Sequence for 2D CPMAS Exchange Experiment170
- Setup 2D Experiment171
- Figure 13.2. the "123" Icon in the Menu Bar of the Data Windows Acquisition Parameter Page171
- Figure 13.3. the Acquisition Parameter Window (Eda)172
- Data Acquisition173
- Table 11.1. Acquisition Parameters173
- Spectral Processing174
- Figure 13.4. the SUPER Spectrum of Tyrosine Hcl after Processing Using "Xfb175
- Figure 13.5. SUPER Spectrum after Tilting the Spectrum Setting "1 Alpha" = -1176
- Figure 13.6. Various Cross Sections from the Upper 2D Experiment177
14 Symmetry Based Recoupling179
- Pulse Sequence Diagram, Example C7181
- Setup181
- Figure 14.1. C7 SQ-DQ Correlation Experiment181
- Table 14.1. Recommended Probe/Spin Rates for Different Experiments and Magnetic Field182
- Spectrometer Setup for 13C183
- Setup for the Recoupling Experiment183
- Figure 14.2. Optimization of the RF Power Level for DQ Generation/Reconversion on Glycine184
- Figure 14.3. Variation of DQ-Generation/Reconversion Time on a Uniformly 13C Labeled Peptide184
- Setup of the 2D SQ-DQ Correlation Experiment185
- Figure 14.4. PC7 Recoupling Efficiency at a Spinning Speed of 13 Khz185
- Data Acquisition186
- Table 14.2. Acquisition Parameters for DQ-SQ Correlation Experiments Using Symmetry Based Re186
- Spectral Processing188
- 13C Single Quantum Correlation with DQ Mixing189
- Figure 14.5. SC14 2D SQ-DQ Correlation on Tyrosine-Hcl189
- Data Acquisition190
- Spectral Processing191
- Figure 14.6. PC7 2D SQ-SQ Correlation on Tyrosine-Hcl191
15 Pisema193
- Pulse Sequence Diagram194
- Figure 15.1. Pisema Pulse Sequence194
- Setup195
- Table 15.1. Acquisition Parameters197
- Processing198
- Table 15.2. Processing Parameters for the Pisema Experiment198
- Figure 15.2. PISEMA Spectrum of 15N Labeled Acetylated Valine and FID in T1 over 3.008 Ms 64 Data Points199
- Figure 15.3. PISEMA Spectrum of 15N Labeled Kdpf Transmembrane Protein200
16 Relaxation Measurements201
- Describing Relaxation201
- T1 Relaxation Measurements202
- Experimental Methods202
- The CP Inversion Recovery Experiment203
- Figure 16.1. the CPX T1 Pulse Sequence203
- Data Processing205
- Table 16.2. Parameters for 2D Inversion Recovery Experiment205
- Table 16.3. Processing Parameters for CP T1 Relaxation Experiment205
- Figure 16.2. Relaxation of Alpha-Carbon Signal in Glycine207
- The Saturation Recovery Experiment208
- T1P Relaxation Measurements209
- Indirect Relaxation Measurements210
- Indirect Proton T1 Measurements211
17 Basic MQ-MAS213
- Introduction213
- Pulse Sequences213
- Figure 17.1. a 3-Pulse Basic Sequence with Z-Filter214
- Figure 17.2. a 4-Pulse Basic Sequence with Z-Filter214
- Data Acquisition215
- Setting up the Experiment215
- Table 17.1. some Useful Samples for Half-Integer Spin Nuclei216
- Figure 17.3. Comparison of 87Rb MAS Spectra of Rbno3 Excited with Selective and Non-Selective217
- Figure 17.4. Nutation Profiles of Selective and Non-Selective Pulses218
- Figure 17.5. Example for Popt Set-Up for Optimization of P1 and P2219
- Table 17.2. Initial Parameters for Setup219
- Two Dimensional Data Acquisition220
- Figure 17.6. Signal Intensities of 87Rb Resonances in Rbno3 as Function of P1 and P2220
- Table 17.3. F1 Parameters for 2D Acquisition220
- Data Processing222
- Table 17.4. Processing Parameters for 2D FT222
- Figure 17.7. 2D 87Rb 3QMAS Spectrum of Rbno3223
- Figure 17.8. Comparison of Differently Processed 2D 23Na 3Q MAS Spectra of Na4P2O7224
- Obtaining Information from Spectra225
- Figure 17.9. Calculated Shift Positions Dmq225
- Table 17.5. Values of |R-P| for Various Spins I and Orders P226
- Table 17.6. Chemical Shift Ranges for All MQ Experiments for All Spins I227
- Figure 17.10. 17O MQMAS of Napo3 at 11.7 T (67.8 Mhz) on the Left and 18.8 T (108.4 Mhz) on the228
- Figure 17.11. Slices and Simulations of the 18.8 T 17O MQMAS of Napo3229
- Figure 17.12. Graphical Interpretation of the Spectrum from Figure 17.10230
18 MQ-MAS: Sensitivity Enhancement231
- Split-T1 Experiments and Shifted Echo Acquisition231
- Figure 18.1. Hahn Echo Pulse Sequence and Coherence Transfer Pathway232
- Implementation of DFS into MQMAS Experiments233
- Optimization of the Double Frequency Sweep (DFS)233
- Figure 18.2. Processing of Hahn Echo. Left Is the Shifted Echo233
- Figure 18.3. Four Pulse Sequence and Coherence Transfer Pathway for the 3Q MAS Experiment234
- Figure 18.4. Three Pulse Sequence and Coherence Transfer Pathway234
- Table 18.1. Initial Parameters for the DFS Experiment236
- Figure 18.5. Example for Popt to Set-Up for Optimization of DFS237
- 2D Data Acquisition238
- Figure 18.6. Signal Intensities of 87Rb in Rbno3238
- Table 18.2. Parameters for 2D Data Acquisition of 3-Pulse Shifted Echo Experiment Mp3Qdfs.av239
- Data Processing240
- Table 18.3. Parameters for 2D Data Acquisition of 4-Pulse Z-Filtered Experiment Mp3Qdfsz.av240
- Table 18.4. Processing Parameters241
- Fast Amplitude Modulation - FAM242
- Soft Pulse Added Mixing - SPAM242
- Table 18.5. Parameters for FAM242
- Figure 18.7. Pulse Sequence and Coherence Transfer Pathways for SPAM 3QMAS243
- Table 18.6. Further Parameters for 2D Data Acquisition of SPAM MQMAS Experiment243
19 Stmas245
- Experimental Particularities and Prerequisites245
- Figure 19.1. Principle of 2D Data Sampling in STMAS Experiments245
- Pulse Sequences247
- Figure 19.2. Four-Pulse Sequence and Coherence Transfer Pathway for the Double Quantum Filtered STMAS Experiment with Z-Filter (Stmasdqfz.av)247
- Figure 19.3. Four Pulse Sequence and Coherence Transfer Pathway248
- Experiment Setup249
- Setting up the Experiment249
- Table 19.2. some Useful Samples for some Nuclei with Half Integer Spin249
- Table 19.3. Initial Parameters for the Set-Up of Stmasdfqz.av250
- Two Dimensional Data Acquisition251
- Table 19.4. Initial Parameters for the Set-Up of Stmasdfqe.av251
- Figure 19.4. 87Rb STMAS Spectra of Rbno3252
- Table 19.5. F1 Parameters for the 2D Data Acquisition252
- Data Processing253
- Table 19.6. Processing Parameters for the 2DFT253
20 Double-CP255
- Pulse Sequence Diagram, Double CP (DCP)256
- Double CP Experiment Setup256
- Double CP 2D Experiment Setup256
- Figure 20.1. Pulse Sequence Diagram for 1D (T1=0) and 2D Double CP Experiments256
- Figure 20.2. the Edasp Routing Tables for H-C-N Double CP257
- Channel Setup258
- Figure 20.3. Routing Table for Triple Resonance Setup Change for 15N Pulse Parameter Measurement and CPMAS Optimization258
- Setup of the Double CP Experiment259
- Table 20.1. Recommended Parameters for the DCP Setup260
- Figure 20.4. Shape Tool Display with Ramp Shape from 45 to 55261
- Figure 20.5. Shape Tool Display with a Tangential Shape for Adiabatic Cross Polarization262
- Figure 20.6. Double CP Optimization of PL5 in Increments of 0.1 Db263
- Figure 20.7. Double CP Yield, Measured by Comparing CPMAS and DCP Amplitudes of the High Field263
- Setup of the 2D Double CP Experiment264
- 2D Data Acquisition265
- Table 20.2. Recommended Parameters for the DCP 2D Setup265
- Spectral Processing266
- Table 20.3. Recommended Processing Parameters for the DCP 2D266
- Example Spectra267
- Figure 20.8. C-N Correlation Via Double CP in Histidine (Simple Setup Sample). 4Mm Triple H/C/N267
- Figure 20.9. NcαCX Correlation Experiment with 22 Ms DARR Mixing Period for Cα-CX Spin Diffusion on GB1 Protein Run Using an EFREE-Probe268
21 CRAMPS: General271
- Homonuclear Dipolar Interactions271
- Multiple Pulse Sequences271
- W-PMLG and DUMBO272
- Quadrature Detection and Chemical Shift Scaling273
- Figure 21.1. Difference in Amplitude of the Quadrature Channels X and y273
22 Cramps 1D275
- Pulse Sequence Diagram of W-PMLG or DUMBO275
- Figure 22.1. Pulse Sequence Diagram275
- Table 22.1. Phases, RF-Levels, Timings275
- Pulse Shapes for W-PMLG and DUMBO276
- Figure 22.2. PMLG Shape for Wpmlg, Sp1276
- Analog and Digital Sampling Modi277
- Figure 22.3. Shape for DUMBO, Sp1277
- Analog Mode Sampling278
- Digital Mode Sampling278
- Figure 22.4. Analog Sampling Scheme278
- Figure 22.5. Digital Sampling Scheme278
- Setup279
- Parameter Settings for PMLG and DUMBO279
- Table 22.2. PMLG Analog Mode279
- Fine Tuning for Best Resolution281
- Fine Tuning for Minimum Carrier Spike281
- Correcting for Actual Spectral Width281
- Digital Mode Acquisition282
- Examples282
- Figure 22.6. Optimizing Sp1 for Best Resolution282
- Table 22.4. Parameters for Digital Mode282
- Figure 22.7. Optimizing Cnst25 for Minimum Carrier Spike, Optimized at 120°C283
- Figure 22.8. Optimizing P14 for Minimum Carrier Spike, Optimized at 0.6 Μsec283
- Figure 22.9. WPMLG-CRAMPS after Optimization, Digital Acquisition284
23 Modified W-PMLG285
- Pulse Sequence Diagram for Modified W-PMLG285
- Figure 23.1. Pulse Sequence Diagram285
- Pulse Shapes for W-PMLG286
- Setup287
- Parameter Settings for PMLG and DUMBO287
- Fine Tuning for Best Resolution288
- Correcting for Actual Spectral Width288
- Digital Mode Acquisition289
- Table 23.4. Parameters for Digital Mode289
24 Cramps 2D291
- Proton-Proton Shift Correlation (Spin Diffusion)291
- Pulse Sequence Diagram292
- Figure 24.1. Pulse Sequence Diagram292
- Table 24.1. Acquisition Parameters292
- Data Processing293
- Table 11.2. Processing Parameters293
- Table 13.1. Acquisition Parameters293
- Examples294
- Figure 24.2. Setup and Test Spectrum of Alpha-Glycine294
- Table 13.2. Processing Parameters294
- Figure 24.3. Spectrum of Tyrosine-Hydrochloride295
- Proton-Proton DQ-SQ Correlation296
- Figure 24.4. Expansion of the Essential Part of the Spectrum296
- Pulse Sequence Diagram297
- Figure 24.5. Pulse Sequence Diagram297
- Data Processing299
- Examples299
  - Table 24.6. Processing Parameters299
  - Figure 24.6. Glycine, Proton-Proton DQ-SQ Correlation Using WPMLG in both Directions300
  - Figure 24.7. 14.5 Khz W-PMLG/PC7 DQ/SQ Correlation at 600 Mhz with Tyrosine-Hydrochloride301
- Appendix303
  - Form for Laboratory Logbooks303
- Figures309
- Tables315
- Index319

Bruker BioSpin Solid State NMR - Page 103

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