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“100 and More Basic NMR Experiments”

ISBN: 3-527-29091-5, VCH, Weinheim , 1996

 Contents and => Known 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 Work-Station
    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
     
  •  Chapter 2 Determination of the Pulse-Length

    Exp. 2.1:    Determination of the 90 1H Transmitter Pulse-Length
    Exp. 2.2:    Determination of the 90 13C Transmitter Pulse-Length
    Exp. 2.3:    Determination of the 90 1H Decoupler Pulse-Length
    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:    Determination of Radiofrequency 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:    Line-Shape Test for 1H NMR Spectroscopy
    Exp. 3.4:    Resolution Test for 1H NMR Spectroscopy
    Exp. 3.5:    Sensitivity Test for 1H NMR Spectroscopy
    Exp. 3.6:    Line-Shape Test for 13C NMR Spectroscopy
    Exp. 3.7:    ASTM Sensitivity Test for 13C NMR Spectroscopy
    Exp. 3.8:    Sensitivity Test for 13C NMR Spectroscopy
    Exp. 3.9:    Quadrature Image Test
    Exp. 3.10:   Dynamic Range Test for Signal Amplitudes
     
  •  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:    The Homonuclear SPT Experiment
    Exp. 4.6:    The Heteronuclear SPT Experiment
    Exp. 4.7:    1D Nuclear Overhauser Difference Spectroscopy
    Exp. 4.8:    1D NOE Spectroscopy with Multiple Selective Irradiation
    Exp. 4.9:    1H Off-Resonance Decoupled 13C NMR Spectra
    Exp. 4.10:   The Gated 1H-Decoupling Technique
    Exp. 4.11:   The Inverse Gated 1H-Decoupling Technique
    Exp. 4.12:   1H Single Frequency Decoupling of 13C NMR Spectra
    Exp. 4.13:   1H Low-Power Decoupling of 13C NMR Spectra
    Exp. 4.14:   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
     
  •  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:    Editing 13C NMR Spectra with SEFT
    Exp. 6.4:    Editing 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:    Editing 13C NMR Spectra with DEPT
    Exp. 6.10:   Editing 13C NMR Spectra with PENDANT
    Exp. 6.11:   1D-INADEQUATE
    Exp. 6.12:   The BIRD Filter
    Exp. 6.13:   TANGO
    Exp. 6.14:   The Heteronuclear Double Quantum Filter
    Exp. 6.15:   Water Suppression by Presaturation
    Exp. 6.16:   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:    Selective COSY
    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 Mechanism

    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:    The Relaxation Reagent Cr(acac)3
    Exp. 8.6:    Quantitative 1H NMR Spectroscopy: Determination of the Alcohol Content of Polish Vodka
    Exp. 8.7:    Quantitative 13C NMR Spectroscopy with Inverse Gated1H-Decoupling
    Exp. 8.8:    Determination of Paramagnetic Susceptibility by NMR
    Exp. 8.9:    The CIDNP Effect
     
  •  Chapter 9 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:    119Sn NMR Spectroscopy
    Exp. 9.6:    2H NMR Spectroscopy
    Exp. 9.7:    11B NMR Spectroscopy
    Exp. 9.8:    17O NMR Spectroscopy with RIDE
     
  •  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:   Double Quantum Filtered COSY with Presaturation
    Exp. 10.8:   C,H Correlation by Polarization Transfer (HETCOR)
    Exp. 10.9:   Long-Range C,H Correlation by Polarization Transfer
    Exp. 10.10:   C,H Correlation via Long-Range Couplings (COLOC)
    Exp. 10.11:   The Basic HMQC Experiment
    Exp. 10.12:   Phase-Sensitive HMQC with BIRD Selection and GARP Decoupling
    Exp. 10.13:   Phase-Sensitive HMBC with BIRD Selection
    Exp. 10.14:   The Basic HSQC Experiment
    Exp. 10.15:   The HOHAHA or TOCSY Experiment
    Exp. 10.16:   The NOESY Experiment
    Exp. 10.17:   The CAMELSPIN or ROESY Experiment
    Exp. 10.18:   The HOESY Experiment
    Exp. 10.19:   2D-INADEQUATE
    Exp. 10.20:   The EXSY Experiment
     
  •  Chapter 11 NMR Spectroscopy with Pulsed Field Gradients

    Exp. 11.1:   Calibration of Pulsed Field Gradients
    Exp. 11.2:   The Pulsed Gradient Spin-Echo Experiment
    Exp. 11.3:   Gradient-Selected H,H-COSY
    Exp. 11.4:   Gradient-Selected Phase-Sensitive DQF COSY
    Exp. 11.5:   Gradient-Selected HMQC
    Exp. 11.6:   Gradient-Selected HMBC
    Exp. 11.7:   Phase-Sensitive Gradient-Selected HSQC
    Exp. 11.8:   Gradient-Selected TOCSY
    Exp. 11.9:   Gradient-Selected HMQC-TOCSY
    Exp. 11.10:   Gradient-Selected 1H-Detected 2D INEPT-INADEQUATE
    Exp. 11.11:   Gradient-Selected SELINCOR
    Exp. 11.12:   GRECCO
    Exp. 11.13:   WATERGATE
     
  •  Chapter 12 The Third Dimension

    Exp. 12.1:   3D HMQC-COSY
    Exp. 12.2:   3D Gradient-Selected HSQC-TOCSY
    Exp. 12.3:   3D H,C,P-Correlation


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Known Bugs:

  • page 3, line 4 from bottom: change "ms" into "microseconds"!
     
  • page 56: Correct citation of Günthers Book in ref [1] see page 34, ref [4]
     
  • page 155 second line: change to "p2, p4: 180 "
     
  • page 158, line 8 from bottom: change "C-3" into "C-4"
     
  • page 167, phase cycle for acquisition shoud read x, -x,-x, x, -x, x, x, -x
     
  • page 173: change phase program for p2 to " -x, -x, x, x, -y, -y, y, y" and for aq to “ x,x, -x, -x, y, y, -y, -y"
     
  • page 196: change in parameter list d2 to "1/[4J(C.,C)]"
     
  • page 210: add in parameter list "p4: 90 13C decoupler pulse"
     
  • page 237: In ref. [1] change publication year from "1958" into "1959"
     
  • page 270: first line of pulse phases: change "p4" into "p5"
     
  • page 272, line 4 from top: change "independent" into "dependent"
     
  • page 289 and page 292: phase cycle for p2, change to x, -x, x, -x, y, -y, y, -y
     
  • page 295: phase cycle for p4, change to y, -x, -y, x, -x, -y, x, y
     
  • page 351, line 6 from top: change "have not diffused" into "have diffused"
     
  • page 375, line 2 from top change "IH" into IH with superscript minus
     
  • page 399: parameter list: d2: change 1/[2J(C,H) into 1/[4J(C,H)]
         increment for t2 evolution: change 1/[2sw2] into 1/sw2
     
  • page 403: change time requirements into 6h
         add as second sentence: "Use appropriate pass and stop r.f. filters
         in all three channels"

         parameter list: d2: change 145 Hz into 160 Hz increment for t2

         evolution 1/[2sw2] into 1/[4sw2]

         add: "preacquisition delay as short as possible"
     
  • page 406: 7th column, first row: add for Jeol instrument: "Alpha", "Lambda"
            
         7th column, second row:add for Jeol Computer: "VAX Alpha AXP"
     
  • page 407: parameter "pulse width": change the Jeol entry "Pwx" into "PWx"
            
         parameter "delay": change the Jeol entry "Pix" into "PIx"
            
         parameter "preacquisition delay": change the Varian entry "pad" into "rof2"
     
  • page 408: second row of table: remove the Varian entries "ni"


 Some of these errors have been corrected in the first reprint. Many thanks
 to all collegues who pointed our attention to these problems.
 



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