Basic- NMR- Experiments

1 150 Basic- NMR-ExperimentsMMO January 2000 Version 2 - DETERMINATION OF THE PULSE-DURATION9 SUMMARY9 Experiment - Determination of the 90 1H Transmitter Pulse Duration9 Experiment - Determination of the 90 13C Transmitter Pulse Duration10 Experiment - Determination of the 90 1H Decoupler Pulse Duration10 Experiment - The 90 1H Pulse with Inverse Spectrometer Configuration11 Experiment - The 90 13C Decoupler Pulse with Inverse Configuration11 Experiment - Composite Pulses12 Experiment - Radiation Damping13 Experiment - Pulse and Receiver Phases13 Experiment - Determination of Radiofrequency Power14 CHAPTER 3 - ROUTINE NMR SPECTROSCOPY AND STANDARD TESTS15 SUMMARY15 Experiment - The Standard 1H NMR Experiment15 Experiment - The Standard 13C NMR Experiment16 Experiment - The Application of Window Functions16 Experiment - Computer-aided Spectral Analysis17 Experiment - Line-Shape Test for 1H NMR Spectroscopy17 Experiment - Resolution Test for 1H NMR Spectroscopy18 Experiment - Sensitivity Test for 1H NMR Spectroscopy18 Experiment - Line-Shape Test for 13C NMR Spectroscopy19 Experiment - ASTM Sensitivity Test for 13C NMR Spectroscopy20 Experiment - Sensitivity Test for 13C NMR Spectroscopy20 Experiment - Quadrature Image Test21 Experiment - Dynamic Range Test for Signal Amplitudes21 Experiment 13 Phase Stability Test22 CHAPTER 4 - DECOUPLING TECHNIQUES23 SUMMARY23 Experiment - Decoupler Calibration for Homonuclear Decoupling23 Experiment.

2 Decoupler Calibration for Heteronuclear Decoupling243 Experiment - Low Power Calibration for Heteronuclear Decoupling25 Experiment - Homonuclear Decoupling25 Experiment - Homonuclear Decoupling at Two Frequencies26 Experiment - The Homonuclear SPT Experiment26 Experiment - The Heteronuclear SPT Experiment27 Experiment - 1D Nuclear Overhauser Difference Spectroscopy27 Experiment - 1D NOE Spectroscopy with Multiple Selective Irradiation28 Experiment - 1H Off-Resonance Decoupled 13C NMR Spectra29 Experiment - The Gated 1H-Decoupling Technique29 Experiment - The Inverse Gated 1H-Decoupling Technique30 Experiment - 1H Single Frequency Decoupling of 13C NMR Spectra30 Experiment - 1H Low Power Decoupling of 13C NMR Spectra31 Experiment - Measurement of the Heteronuclear Overhauser Effect32 CHAPTER 5 - DYNAMIC NMR SPECTROSCOPY33 SUMMARY33 Experiment - Low Temperature Calibration with Methanol33 Experiment - High Temperature Calibration with 1.

3 2-Ethandiol33 Experiment - Dynamic 1H NMR Spectroscopy on Dimethylformamid34 Experiment - The Saturation Transfer Experiment34 Experiment - Measurement of the Rotating Frame Relaxation Time T1p35 CHAPTER 6 - 1D MULTIPULSE SEQUENCES36 SUMMARY36 Experiment - Measurement of the Spin-Lattice Relaxation Time T136 Experiment - Measurement of the Spin-Spin Relaxation Time T237 Experiment - 13C NMR Spectra with SEFT38 Experiment - 13C NMR Spectra with APT38 Experiment - The Basic INEPT Technique39 Experiment - INEPT+40 Experiment - Refocused INEPT40 Experiment - Reverse INEPT41 Experiment - DEPT-13542 Experiment - Editing 13C NMR Spectra with DEPT42 Experiment - Multiplicity Determination with PENDANT43 Experiment - 1D-INADEQUATE44 Experiment - The BIRD Filter45 Experiment - TANGO454 Experiment - The Heteronuclear Double Quantum Filter46 Experiment - Purging with a Spin-Lock Pulse46 Experiment - Water Suppression by Presaturation47 Experiment - Water Suppression by the Jump and Return Method48 CHAPTER 7 - NMR SPECTROSCOPY WITH SELECTIVE PULSES49 SUMMARY49 Experiment - Determination of a Shaped 90o 1H Transmitter Pulse49 Experiment - Determination of a Shaped 90o 1H Decoupler Pulse50 Experiment - Determination of a Shaped 90o 13C Decoupler Pulse50 Experiment - Selective Excitation with DANTE51 Experiment - SELCOSY52 Experiment - SELINCOR.

4 Selective Inverse H,C Correlation via 1J (C,H)52 Experiment - SELINQUATE53 Experiment - Selective TOCSY54 Experiment - INAPT55 Experiment - Determination of Long-Range C,H Coupling Constants56 Experiment - SELRESOLV57 Experiment - SERF57 CHAPTER 8 - AUXILIARY REAGENTS, QUANTITATIVE DETERMINATIONS ANDREACTION MECHANISM59 SUMMARY59 Experiment - Signal Separation Using a Lanthanide Shift Reagent59 Experiment - Signal Separation of Enantiomers Using a Chiral Shift Reagent60 Experiment - Signal Separation of Enantiomers Using a Chiral Solvating Agent60 Experiment - Determination of Enantiomeric Purity with Pirkle s Reagent61 Experiment - Determination of Enantiomeric Purity by 31P NMR61 Experiment - Determination of Absolute Configuration by the Advanced Mosher Method62 Experiment - Aromatic Solvent-Induced Shift (ASIS)

5 62 Experiment - NMR Spectroscopy of OH-Protons and H/D Exchange63 Experiment - Isotope Effects on Chemical Shielding64 Experiment - pKa Determination with 13C NMR64 Experiment - The Relaxation Reagent Cr(acac)365 Experiment - Determination of paramagnetic Susceptibility by NMR65 Experiment - 1H and 13C NMR of paramagnetic Compounds66 Experiment - The CIDNP Effect67 Experiment - Quantitative 1H NMR Spectroscopy: Determination of the Alcohol Content ofPolish Vodka675 Experiment - Quantitative 13C NMR Spectroscopy with Inverse Gated 1H-Decoupling68 Experiment - NMR Using Liquid-Crystal Solvents68 CHAPTER 9 - HETERONUCLEAR NMR SPECROSCOPY70 SUMMARY70 Experiment - 1H-Decoupled 15N NMR Spectra with DEPT70 Experiment - 1H-Coupled 15N NMR Spectra with DEPT71 Experiment - 19F NMR Spectroscopy71 Experiment - 29Si NMR Spectroscopy with DEPT72 Experiment - 29Si NMR Spectroscopy with Spin-Lock Polarization73 Experiment - 119Sn NMR Spectroscopy73 Experiment - 2H NMR Spectroscopy74 Experiment - 11B NMR Spectroscopy74 Experiment - 17O NMR Spectroscopy with RIDE75 Experiment - 47/49Ti NMR Spectroscopy with ARING76 CHAPTER 10 - THE SECOND DIMENSION77

6 SUMMARY77 Experiment - 2D J-Resolved 1H NMR Spectroscopy77 Experiment - 2D J-Resolved 13C NMR Spectroscopy78 Experiment - The Basic H,H-COSY-Experiment79 Experiment - Long-Range COSY79 Experiment - Phase-Sensitive COSY80 Experiment - Phase-Sensitive COSY-4581 Experiment - - Double Quantum Filtered COSY with Presaturation82 Experiment - Fully Coupled C,H Correlation (FUCOUP)83 Experiment - C,H Correlation by Polarization Transfer (HETCOR)84 Experiment - Long-Range C,H Correlation by Polarization Transfer85 Experiment - C,H Correlation via Long-Range Couplings (COLOC)86 Experiment - The Basic HMQC Experiment86 Experiment - Phase-Sensitive HMQC with BIRD Filter and GARP Decoupling87 Experiment - Poor Man s Gradient HMQC88 Experiment - Phase-Sensitive HMBC with BIRD Filter89 Experiment - The Basic HSQC Experiment90 Experiment - The HOHAHA or TOCSY Experiment91 Experiment - The NOESY Experiment92 Experiment - The CAMELSPIN or ROESY Experiment936 Experiment - The HOESY Experiment94 Experiment - 2D-INADEQUATE94 Experiment - The EXSY Experiment95 Experiment - X.

7 Y Correlation96 CHAPTER 11 - NMR SPECTROSCOPY WITH PULSED FIELD GRADIENTS98 SUMMARY98 Experiment - Calibration of Pulsed Field Gradients98 Experiment - Gradient Preemphasis99 Experiment - Gradient Amplifier Test99 Experiment - Determination of Pulsed Field Gradient Ring-Down Delays100 Experiment - The Pulsed Gradient Spin-Echo Experiment100 Experiment - Excitation Pattern of Selective Pulses101 Experiment - The Gradient zz-Filter102 Experiment - gs-SELCOSY102 Experiment - gs-SELTOCSY103 Experiment - DPFGSE-NOE104 Experiment - gs-SELINCOR105 Experiment - GRECCO106 Experiment - WATERGATE106 Experiment - Water Suppression by Excitation Sculpting107 CHAPTER 12 - 2D NMR SPECTROSCOPY WITH FIELD GRADIENTS108 SUMMARY108 Experiment - gs-COSY108 Experiment - Phase-Sensitive gs-DQF-COSY109 Experiment - gs-HMQC110 Experiment - gs-HMBC110 Experiment - ACCORD-HMBC111 Experiment - Phase-Sensitive gs-HSQC with Sensitivity Enhancement112 Experiment - gs-TOCSY113 Experiment - gs-HMQC-TOCSY114 Experiment - 2Q-HMBC115 Experiment - Gradient-Selected 1H-Detected 2D INEPT-INADEQUATE116 Experiment - gs-NOESY117 Experiment - gs-HSQC-NOESY118 Experiment - gs-HOESY119 Experiment - 1H, 15N Correlation with gs-HMQC1197 CHAPTER 13 - THE THIRD DIMENSION121 SUMMARY121 Experiment - 3D HMQC-COSY121 Experiment - 3D gs-HSQC-TOCSY122 Experiment - 3D H,C.

8 P-Correlation122 Experiment - 3D HMBC123 CHAPTER 14 - SOLID-STATE NMR SPECTROSCOPY124 SUMMARY124 Experiment - Shimming Solid-State Probe-Heads124 Experiment Adjusting the Magic Angle125 Experiment - Hartmann-Hahn Matching126 Experiment The Basic CP/MAS Experiment127 Experiment - TOSS127 Experiment - SELTICS128 Experiment - Multiplicity Determination in the Solid-State1298,QWURGXFWLRQHere you will find some information about the Bruker pulse programs andparameters, which are needed to repeat the Experiments shown in thebook: 150 and More Basic NMR Experiments written by S. Braun, , S. Berger, VCH Weinheim, you will find the experiment number, followed by the Bruker pulseprogram, the settings of the different channels and a list of the acquisitionand processing number of the chapters are identically with the number of thechapters in the book contains a lot of very interesting Experiments .

9 If you want torepeat such Experiments with a BRUKER Avance instrument you needthe pulse program and the parameters belonging to the pulse needed parameters are sometimes different or more then mentionedin the book. BRUKER has its own nomenclature for the parameters,which is different from the book. For example the 90 transmitter pulse isalways P1, D2 is a delay depending on the coupling constant (1/2 J) andso is possible that the needed pulse program isn t yet in your library, in thatcase send me an e-mail: 2- Determination of the Pulse-DurationSummaryExperimentPulse of the 90 1 HTransmitter of the 90 13 CTransmitter of the 90 1 HDecoupler 90 1H Pulse with InverseSpectrometer 90 13C Decoupler Pulsewith Inverse and Receiver of RadiofrequencyPowerExperiment Determination of the 90 1H Transmitter Pulse Durationpulse program:zg01D-sequence, using p0 for any flip angle.

10 Result is a routine proton of the needed channels:F1:1HF2:offAcquisition parametersPL1 : F1 channel - high power level for 1 Htransmitter pulse, here 3dB was usedP0 : F1 channel - 1H transmitter pulse, to bevaried, 1 usec as initial value andincrease by 2 usecD1 : 30 sec - relaxation delayTD :4 KSW : 500 HzO1 : on resonance of CHCl3 signalNS :1RG : receiver gain for correct ADC inputProcessing parametersSI :2 KBC_mod :quadWDW :EMLB :1 HzFT :fourier transformationphase correction :adjust the phase of thefirst spectrum to pureabsorption and for all otherexperiments use the samevalues for the phasecorrection (PK)baseline correction :ABSplot :use XWINPLOT10 Experiment Determination of the 90 13C Transmitter Pulse Durationpulse program:zg0dc1D-sequence with F2 decoupling, using p0 for any flip angle.