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“150 and More Basic NMR Experiments”

 

Contents / ==> Bugs 

 

Chapter 1 The NMR Spectrometer     

1.1   Principles of an NMR Spectrometer  
1.1.1  The Magnet      
1.1.2  The Spectrometer Console     
1.1.3  The Workstation  
1.1.4  Maintenance   
1.2   Tuning a Probe-Head   
1.2.1  Tuning and Matching with a Reflection Meter    
1.2.2  Tuning and Matching with an R.F. Bridge and an Oscilloscope  
1.2.3  Tuning and Matching with a Wobble Generator 
1.3   The Lock Channel 
1.4   The Art of Shimming  
1.4.1  The Shim Gradients    
1.4.2  The Shimming Procedure  
1.4.3  Gradient Shimming  

 

  • Chapter 2 Determination of the Pulse-Duration   

    Exp. 2.1: Determination of the 90&; 1H Transmitter Pulse-Duration   
    Exp. 2.2: Determination of the 90&; 13C Transmitter Pulse-Duration   
    Exp. 2.3: Determination of the 90&; 1H Decoupler Pulse-Duration    
    Exp. 2.4: The 90&; 1H Pulse with Inverse Spectrometer Configuration   
    Exp. 2.5: The 90&; 13C Decoupler Pulse with Inverse Configuration   
    Exp. 2.6: Composite Pulses        
    Exp. 2.7: Radiation Damping            
    Exp. 2.8: Pulse and Receiver Phases             
    Exp. 2.9: Determination of Radio Frequency Power        
     
  • Chapter 3 Routine NMR Spectroscopy and Standard Tests   

    Exp. 3.1: The Standard 1H NMR Experiment         
    Exp. 3.2: The Standard 13C NMR Experiment      
    Exp. 3.3: The Application of Window Functions   
    Exp. 3.4: Computer-aided Spectral Analysis      
    Exp. 3.5: Line-Shape Test for 1H NMR Spectroscopy   
    Exp. 3.6: Resolution Test for 1H NMR Spectroscopy    
    Exp. 3.7: Sensitivity Test for 1H NMR Spectroscopy      
    Exp. 3.8: Line-Shape Test for 13C NMR Spectroscopy      
    Exp. 3.9  ASTM Sensitivity Test for 13C NMR Spectroscopy     
    Exp. 3.10: Sensitivity Test for 13C NMR Spectroscopy   
    Exp. 3.11: Quadrature Image Test       
    Exp. 3.12: Dynamic Range Test for Signal Amplitudes    
    Exp. 3.13: 13&; Phase Stability Test      
     
  • Chapter 4 Decoupling Techniques    

    Exp. 4.1: Decoupler Calibration for Homonuclear Decoupling  
    Exp. 4.2: Decoupler Calibration for Heteronuclear Decoupling  
    Exp. 4.3: Low Power Calibration for Heteronuclear Decoupling  
    Exp. 4.4: Homonuclear Decoupling    
    Exp. 4.5: Homonuclear Decoupling at Two Frequencies      
    Exp. 4.6: The Homonuclear SPT Experiment      
    Exp. 4.7: The Heteronuclear SPT Experiment       
    Exp. 4.8: 1D Nuclear Overhauser Difference Spectroscopy    
    Exp. 4.9: 1D NOE Spectroscopy with Multiple Selective Irradiation      
    Exp. 4.10: 1H Off-Resonance Decoupled 13C NMR Spectra         
    Exp. 4.11: The Gated 1H-Decoupling Technique   
    Exp. 4.12: The Inverse Gated 1H-Decoupling Technique   
    Exp. 4.13: 1H Single Frequency Decoupling of 13C NMR Spectra    
    Exp. 4.14: 1H Low-Power Decoupling of 13C NMR Spectra   
    Exp. 4.15: Measurement of the Heteronuclear Overhauser Effect    

     
  • Chapter 5 Dynamic NMR Spectroscopy    

    Exp. 5.1: Low Temperature Calibration with Methanol    
    Exp. 5.2: High Temperature Calibration with 1,2-Ethanediol    
    Exp. 5.3: Dynamic 1H NMR Spectroscopy on Dimethylformamide  
    Exp. 5.4: The Saturation Transfer Experiment   
    Exp. 5.5: Measurement of the Rotating Frame Relaxation Time T1r 

     
  • Chapter 6 1D Multipulse Sequences     

    Exp. 6.1: Measurement of the Spin-Lattice Relaxation Time T1    
    Exp. 6.2: Measurement of the Spin-Spin Relaxation Time T2   
    Exp. 6.3: 13C NMR Spectra with SEFT 
    Exp. 6.4: 13C NMR Spectra with APT   
    Exp. 6.5: The Basic INEPT Technique   
    Exp. 6.6: INEPT+   
    Exp. 6.7: Refocused INEPT    
    Exp. 6.8: Reverse INEPT    
    Exp. 6.9: DEPT-135     
    Exp. 6.10: Editing 13C NMR Spectra with DEPT      
    Exp. 6.11: Multiplicity Determination with PENDANT   
    Exp. 6.12: 1D-INADEQUATE
    Exp. 6.13: The BIRD Filter  
    Exp. 6.14: TANGO    
    Exp. 6.15: The Heteronuclear Double Quantum Filter   
    Exp. 6.16: Purging with a Spin-Lock Pulse    
    Exp. 6.17: Water Suppression by Presaturation  
    Exp. 6.18: Water Suppression by the Jump and Return Method    

     
  • Chapter 7 NMR Spectroscopy with Selective Pulses     

    Exp. 7.1: Determination of a Shaped 90&; 1H Transmitter Pulse   
    Exp. 7.2: Determination of a Shaped 90&; 1H Decoupler Pulse     
    Exp. 7.3: Determination of a Shaped 90&; 13C Decoupler Pulse   
    Exp. 7.4: Selective Excitation with DANTE  
    Exp. 7.5: SELCOSY 
    Exp. 7.6: SELINCOR: Selective Inverse H,C Correlation via 1J(C,H) 
    Exp. 7.7: SELINQUATE 
    Exp. 7.8: Selective TOCSY  
    Exp. 7.9: INAPT   
    Exp. 7.10: Determination of Long-Range C,H Coupling Constants   
    Exp. 7.11: SELRESOLV 
    Exp. 7.12: SERF     

     
  • Chapter 8 Auxiliary Reagents, Quantitative Determinations,  
              and Reaction Mechanisms
    Exp. 8.1: Signal Separation Using a Lanthanide Shift Reagent  
    Exp. 8.2: Signal Separation of Enantiomers Using a Chiral Shift Reagent  
    Exp. 8.3: Signal Separation of Enantiomers Using a Chiral Solvating Agent 
    Exp. 8.4: Determination of Enantiomeric Purity with Pirkle's Reagent 
    Exp. 8.5: Determination of Enantiomeric Purity by 31P NMR  
    Exp. 8.6: Determination of Absolute Configuration by the Advanced Mosher Method               
    Exp. 8.7: Aromatic Solvent-Induced Shift (ASIS)  
    Exp. 8.8: NMR Spectroscopy of OH-Protons and H/D Exchange  
    Exp. 8.9: Isotope Effects on Chemical Shielding  
    Exp. 8.10: pKa Determination with 13C NMR   
    Exp. 8.11: The Relaxation Reagent Cr(acac)3    
    Exp. 8.12: Determination of Paramagnetic Susceptibility by NMR   
    Exp. 8.13: 1H and 13C NMR of Paramagnetic Compounds   
    Exp. 8.14: The CIDNP Effect  
    Exp. 8.15: Quantitative 1H NMR Spectroscopy: / Determination of the Alcohol Content of Polish Vodka   
    Exp. 8.16: Quantitative 13C NMR Spectroscopy with Inverse Gated 1H-Decoupling        
    Exp. 8.17: NMR Using Liquid-Crystal Solvents                      

     
  • Chapter 9 1D Heteronuclear NMR Spectroscopy   

    Exp. 9.1: 1H-Decoupled 15N NMR Spectra with DEPT     
    Exp. 9.2: 1H-Coupled 15N NMR Spectra with DEPT   
    Exp. 9.3: 19F NMR Spectroscopy    
    Exp. 9.4: 29Si NMR Spectroscopy with DEPT      
    Exp. 9.5: 29Si NMR Spectroscopy with Spin-Lock Polarization   
    Exp. 9.6: 119Sn NMR Spectroscopy  
    Exp. 9.7: 2H NMR Spectroscopy    
    Exp. 9.8: 11B NMR Spectroscopy    
    Exp. 9.9: 17O NMR Spectroscopy with RIDE 
    Exp. 9.10 47/49Ti NMR Spectroscopy with ARING    
     
  • Chapter 10 The Second Dimension           

    Exp. 10.1: 2D J-Resolved 1H NMR Spectroscopy   
    Exp. 10.2: 2D J-Resolved 13C NMR Spectroscopy   
    Exp. 10.3: The Basic H,H-COSY Experiment   
    Exp. 10.4: Long-Range COSY  
    Exp. 10.5: Phase-Sensitive COSY  
    Exp. 10.6: Phase-Sensitive COSY-45  
    Exp. 10.7: E.COSY  
    Exp. 10.8: Double Quantum Filtered COSY with Presaturation  
    Exp. 10.9: Fully Coupled C,H Correlation (FUCOUP)   
    Exp. 10.10: C,H Correlation by Polarization Transfer (HETCOR)   
    Exp. 10.11: Long-Range C,H Correlation by Polarization Transfer     
    Exp. 10.12: C,H Correlation via Long-Range Couplings (COLOC)   
    Exp. 10.13: The Basic HMQC Experiment    
    Exp. 10.14: Phase-Sensitive HMQC with BIRD Filter and GARP Decoupling  
    Exp. 10.15: Poor Man's Gradient HMQC  
    Exp. 10.16: Phase-Sensitive HMBC with BIRD Filter   
    Exp. 10.17: The Basic HSQC Experime   
    Exp. 10.18: The HOHAHA or TOCSY Experiment  
    Exp. 10.19: The NOESY Experiment   
    Exp. 10.20: The CAMELSPIN or ROESY Experiment   
    Exp. 10.21: The HOESY Experiment  
    Exp. 10.22: 2D-INADEQUATE  
    Exp. 10.23: The EXSY Experiment   
    Exp. 10.24: X,Y Correlation 

     
  • Chapter 11 1D NMR Spectroscopy with Field Gradients  

    Exp. 11.1: Calibration of Pulsed Field Gradients   
    Exp. 11.2: Gradient Preemphasis   
    Exp. 11.3: Gradient Amplifier Test    
    Exp. 11.4: Determination of Pulsed Field Gradient Ring-Down Delays  
    Exp. 11.5: The Pulsed Gradient Spin-Echo Experiment 
    Exp. 11.6: Excitation Pattern of Selective Pulses  
    Exp. 11.7: The Gradient zz-Filter  
    Exp. 11.8: gs-SELCOSY   
    Exp. 11.9: gs-SELTOCSY 
    Exp. 11.10: DPFGSE-NOE  
    Exp. 11.11: gs-SELINCOR  
    Exp. 11.12: GRECCO   
    Exp. 11.13: WATERGATE    
    Exp. 11.14: Water Supression by Excitation Sculpting     

     
  • Chapter 12 2D NMR Spectroscopy with Field Gradients   

    Exp. 12.1: gs-COSY   
    Exp. 12.2: Phase-Sensitive gs-DQF-COSY   
    Exp. 12.3: gs-HMQC 
    Exp. 12.4: gs-HMBC   
    Exp. 12.5: ACCORD-HMBC    
    Exp. 12.6: Phase-Sensititive gs-HSQC with Sensitivity Enhancement 
    Exp. 12.7: gs-TOCSY   
    Exp. 12.8: gs-HMQC-TOCSY    
    Exp. 12.9: 2Q-HMBC   
    Exp. 12.10: 1H-Detected 2D INEPT-INADEQUATE  
    Exp. 12.11: gs-NOESY   
    Exp. 12.12: gs-HSQC-NOESY   
    Exp. 12.13: gs-HOESY 
    Exp. 12.14: 1H,15N Correlation with gs-HMQC   

     
  • Chapter 13 The Third Dimension       

    Exp. 13.1: 3D HMQC-COSY    
    Exp. 13.2: 3D gs-HSQC-TOCSY    
    Exp. 13.3: 3D H,C,P-Correlation    
    Exp. 13.4: 3D HMBC   

     
  • Chapter 14 Solid-State NMR Spectroscopy  

    Exp. 14.1: Shimming Solid-State Probe-Heads  
    Exp. 14.2: Adjusting the Magic Angle    
    Exp. 14.3: Hartmann-Hahn Matching      
    Exp. 14.4: The Basic CP/MAS Experiment    
    Exp. 14.5: TOSS     
    Exp. 14.6: SELTICS     
    Exp. 14.7: Multiplicity Determination in the Solid-State   

    Appendix 1      
    Instrument Dialects    

    Appendix 2    
    Elementary Product Operator Formalism Rules  

    Glossary and Index     

     

Known Bugs

 

  •  page 267: MgSO4 instead of Mg2SO4
  • page 524: missing phase cycle:
    p1: x, -x
    p2: x, x, -x, -x
    p3, p4: x, y, x, y, -x, -y, -x, -y
    p5: x
    aq: x, -x, -x, x
  • wrong gradient strengths: have to be 0.1 T /m (instead of 0.01 T/m)
    on most pages (434, 437, 440, 447, 450, 453, 457, 460, 465, 478, 482, 486, 490, 494, 498, 502, 507, 510, 514, 521, 529, 539, 547)

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