Research Instrumentation Facility Resources

• Introduction to NMR - Excellent Hypertext book by Joseph P. Hornak, Ph.D at the Rochester Institute of Technology
• NMR Knowledge Base - From Prof. Kessler's lab, München, Germany, this is a very valuable resource for NMR
• NMR Information server - at the University of Florida 
• NMR Spectroscopy
• NIH Molecular Modeling 
• Larmor Letter (used/wanted equipment)
• SDBS - Searchable spectral database for organic compounds, compiled by the National Institute of Advanced Industrial Science and Technology in Japan.
• AMMRL - Association of Managers of Magnetic Resonance Laboratories
• NMRWiki
• Practical NMR Spectroscopy - Tutorial by Dr. Keith Brown.  An introduction to the mathematical treatment of NMR.
• An Introduction to NMR Spectroscopy, a quick overview of NMR
• NMR Basics
• Triangle Analytical

• Edinburgh
• Emory University
• Iowa State University
• Natl. High Magnet Lab
• Penn State
• Purdue University
• Southern Illinois University 
• U. of California-Berkeley
• U. of California-Davis
• U. of California-San Francisco
• U. of Florida
• U. of Guelph
• U. of Illinois at Chicago
• U. of Illinois-Urbana-Champaign
• U. of Indiana 
• U. of London, Queen Mary & Westfield
• U. of New Mexico
• U North Carolina Chapel Hill
• U. of Pennsylvania
• U. of Colorado Boulder
• U. of Texas Medical Branch (UTMB) at Galveston
• U. of Virginia 
• U. of Washington
• U. of Wisconsin-Madsion
• Wagenigen NMR Center
• Washington U. St. Louis 

• Accelrys
• Acorn NMR
• Advanced Chemistry Development, Inc.
• Bruker USA and Bruker Germany
• Hitachi
• Hypercube 
• Isotec
• JEOL USA 
• Mestrelab
• MR Resources 
• New Era Enterprises
• Numare Spectralab 
• Spectral Data Services 
• Triangle Analytical
• Agilent Instruments
• Wilmad Glass

Sensitivity

• Higher field gives better Signal-to-Noise and better signal dispersion, so 700>600>500>400>300 MHz. Linewidths in Hz are similar whatever the field, so the linewidths in ppm are smaller at the higher field strengths, unless a frequency-dependent line broadening mechanism interferes.
• Probes optimized for a particular nucleus give the best signal to noise ratio (S:N) for that nucleus. The cryoprobes on the 700 MHz are indirect detection probes with the ¹H electronics cooled to reduce thermal noise, and is thus most sensitive to proton. 
• The 300 and 400 MHz have BBO-F probes with automatic tune and match (ATM). A wide range of nuclei are available on these probes. The give better resolution than prior probes due to the ATM and better receivers.

• Availability:  H1 experiments are available on all instruments.
• 1D Proton Experiment 
   
  • Default Parameters 
     
    • ~3 second acquisition time
    • ~2 second relaxation delay
    • Spectral width -4ppm to 16ppm
    • 16 scans
    • Total time: 2 minutes
  • Recommended concentration:  0.1 mM
• Variations on the 1D experiment include: 
   
  • 1D NOE
  • 1D Selective COSY (gradient) though the 2D only takes 4 minutes
  • T1 determination
• 2D COSY - Proton-proton correlation experiment 
   
  • Gives information about pairs of protons that are J-coupled. This usually indicates that the protons are on adjacent carbons, e.g., 3-bonds away (though protons further apart may in some cases be J-coupled).
  • Default Parameters 
     
    • 2 second relaxation delay
    • 1024 complex points in t2 and 128 increments in t1
    • 1 scan per increment
    • Total time: 4 minutes (cosygpsw)
    • Recommended Concentration:  1 mM
  • Variations on COSY 
     
    • DQF-COSY 
       
      • phase-sensitive experiment
      • diagonal peaks are narrower
      • less sensitive
    • TOCSY - total correlation spectroscopy 
       
      • gives correlations for all protons within a spin system
    • NOESY - Proton-proton through-space interactions via NOE 
       
      • Gives information about pairs of protons that are close in space (<5 A apart)
      • Default Parameters 
         
        • 1.5 second relaxation delay
        • 1024 complex points in t2 and 256 increments in t1
        • 2-8 scans per increment
        • Total time: 1 - 5 hours
        • Recommended Concentration:  at least 10 mM
    • ROESY - rotating frame NOE 
       
      • Compounds of molecular weight ~1000-2000
      • Exchange peaks are opposite sign from NOE peaks
    • HMQC - Heteronuclear Multiple Quantum Correlation experiment with DEPT editing
       
      • Gives information about strong proton-carbon J-couplings. A strong proton-carbon J-coupling indicates that the proton is directly bonded to the carbon. This experiment gives information that is identical to HETCORs or HMQCs, which are less sensitive. Additionally, it gives DEPT editing (color encodes – CH and CH₃ versus CH₂).
      • Default Parameters 
         
        • 1.5 second relaxation delay
        • 1024 complex points in t2 and 128 increments in t1
        • 4 scans per increment (hsqcetedgp)
        • Total time: 15 minutes
        • Recommended Concentration:  at least 10 mM
    • HMBC - Heteronuclear Multiple Bond Correlation experiment 
       
      • Gives information about weak proton-carbon J-couplings. A weak proton-carbon J-coupling indicates that the proton is two, three, or four bonds away from the carbon. This experiment gives information about which protons are near to (but not directly bonded to) different carbons. This experiment (in conjunction with the HSQC) can give an enormous amount of information about molecular structure, since the long range proton-carbon correlations can include quaternary carbons, in addition to protonated carbons.
      • Default Parameters 
         
        • 1.5 second relaxation delay
        • 1024 complex points in t2 and 128 increments in t1
        • 4 scans per increment
        • Total time: 25 minutes
        • Recommended Concentration:  at least 20 mM

• H"M"QC - (Change to HSQC) -Heteronuclear "Multiple Quantum" (Change to "Single Quantum") Correlation experiment with DEPT editing
•  
  • Gives information about strong proton-carbon J-couplings. A strong proton-carbon J-coupling indicates that the proton is directly bonded to the carbon. This experiment gives information that is identical to HETCORs or HMQCs, which are less sensitive. Additionally, it gives DEPT editing (color encodes – CH and CH3 versus CH2).
  • Default Parameters
  •  
    • 1.5 second relaxation delay
    • 1024 complex points in t2 and 128 increments in t1
    • 4 scans per increment (hsqcetedgp)
    • Total time: 15 minutes
    • Recommended Concentration: at least 10 mM
• HMBC - Heteronuclear Multiple Bond Correlation experiment
•  
  • Gives information about weak proton-carbon J-couplings. A weak proton-carbon J-coupling indicates that the proton is two, three, or four bonds away from the carbon. This experiment gives information about which protons are near to (but not directly bonded to) different carbons. This experiment (in conjunction with the HSQC) can give an enormous amount of information about molecular structure, since the long range proton-carbon correlations can include quaternary carbons, in addition to protonated carbons.
  • Default Parameters
  •  
    • 1.5 second relaxation delay
    • 1024 complex points in t2 and 128 increments in t1
    • 4 scans per increment
    • Total time: 25 minutes
    • Recommended Concentration: at least 20 mM

• The BBO-F probes will need to be tuned to ³¹P before acquisition with atma. The 600 BBO probe must physically be tuned to ³¹P. Sensitivity is approximately 15 times less than for proton, so adequate Signal-to-Noise for a reasonable length experiment (10 minutes, 256 scans) requires a concentration of > 0.1mM.
• 1D Phosphorus experiment 
   
  • Default Parameters 
     
    • 0.8 second acquisition time with proton decoupling
    • 3.0 second relaxation delay (d1; with NOE enhancement)
    • Spectral width -100ppm to 250ppm
    • 32 scans
    • Total time: ~2 minutes
    • Recommended Concentration:  0.1 mM

The 400 and 300 MHz BBO-F probe is well-suited for direct observe 19F experiments. Tuning these probes to 19F uses the atma command. The 600 MHz NMR with the H/F probe gives the best sensitivity for 19F.

• Sensitivity is approximately the same as for proton, so adequate S/N can be obtained with concentration > 0.1mM.
• 1D Fluorine experiment 
   
  • Default Parameters 
     
    • 0.8 second acquisition time
    • 3.0 second relaxation delay
    • Spectral width 150ppm to -200ppm
    • 16 scans
    • Total time: 3 minutes
    • Recommended Concentration:  0.1mM
  • 1D Fluorine observe, 1H decouple 
     
    • Setup is exactly like direct observe 19F, only F2 is 1H and uses Waltz 16 decoupling.