Bruker BioSpin Solid State NMR - 20.2 Double CP Experiment Setup; 20.2.1 Double CP 2 D Experiment Setup

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256 (327) BRUKER BIOSPIN User Manual Version 002

Double-CP

Pulse Sequence Diagram, Double CP (DCP) 20.1

Figure 20.1. Pulse sequence diagram for 1D (t

=0) and 2D double CP experi-

ments.

Double CP Experiment Setup 20.2

Double CP 2D Experiment Setup 20.2.1

1. Prepare your probe for triple resonance applications H/C/N

2. Load a sample of glycine,

N and C

,-C

(or only C

C labelled. Make sure

the sample is α-glycine, you will get nowhere with γ-glycine, since the proton

1ρ

is very short and CP just does not work with high efficiency. Rotate at 11

kHz. The sample may be fully labelled or diluted with natural abundance gly

cine. A restricted volume rotor is preferred. If a different spin rate is used, a dif-

ferent shape must be generated for the second CP step.

= 1, 3 φ

= 0 + States-TPPI (t

) φ

= 0 0 0 0 1 1 1 1

2 2 2 2 3 3 3 3

rec

=0 2 2 0 3 1 1 3

2 0 0 2 1 3 3 1

= 0 0 0 0 2 2 2 2

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 - 20.2 Double CP Experiment Setup; 20.2.1 Double CP 2 D Experiment Setup

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