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This page is devoted to making life with the NMR spectrometer a little easier to handle. This page will continue to be updated as we also learn new tricks.

Bruker links will be added as TOPSPIN instructions are developed. Use "NMR Guide" on the Bruker computers as an additional resource.

Check out the DCIF Software page for a quick overview of the most commonly used programs in our lab, and try the Chemistry Software and Web Resources page for more general information.

Basic instructions (For 1-dimensional 1H and 13C NMR) can be found here

Considering the incredible number and diversity of chemical instrumentation on the market today it is almost impossible to generalize a page such as this. Unfortunately, many of the tips on these pages are specific to the MIT DCIF. That's not to say that much of this information cannot be useful to a broader audience. We strive to make these tips and guidelines as general as possible. If you know of a way to improve (i.e. better generalize) this page let us know. Thank you for your continuing help.

 

[General Tips] [Solvent Reference Lists] [Experiment Tips and Guides] [Plotting and Printing Tips]
[Instrument Problems and Curiosities] [Sample prep and NMR tube care]

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  General Tips:

  • The first thing you may want to look at is our FAQ (Frequently Asked Questions) sheets. This answers and addresses many of the little problems we encounter on a day to day basis. You can view or download the FAQ sheet: (Varian PDF symbol)(Bruker PDF symbol)
  • Here adobe image is an algorithm for determining the resonances of a 'known' structure.
  • Here adobe image is a helpful algorithm for determining the resonances of an 'unknown' structure.
  • Ever wonder 'Which 2D experiment is best for me?' This useful data sheet may help you in determining which experiment is best for you. This sheet summarizes some of the more common 2D pulse sequences including the information content and pros and cons. Get one here adobe image!
  • Here are some other Academic NMR Facility tutorial / instruction sheets / user guides. These include numerous hardware, software, and experimental tips. I've tried to group them by manufacturer but the is a lot of general information available as well.
NMR Solvent Reference Lists:

Fluorine (19F) lists:
  • The NMR Facility at Indiana University has an extensive list of 19F Chemical Shifts and Coupling Constants. You can find it here.
  • If you prefer your references in .pdf format here is a list from the University of Colorado
  • The NMR periodic table has some good information about Fluorine and other NMR active nuclei
Phosphorous (31P) lists:
  • An extensive Phosphorous NMR reference listing can be found at "The Wired Chemist". The url is here.
  • Another can be found at the University of Indiana. You can get it here

Experiment Guideline Sheets:
(click the acronym to get a description of the experiment)

Basics:

  • Instrument training sheets (covering simple 1D 1H and 13C spectra) are available here.
  • Locking instructions for solvents with multiple types of 2H (CD3OD).
  • Varian Instruction Manuals from the University of Minnesota Chemistry Department NMR Facility. Well thought out and well organized. These are really great!

Observing Nuclei Other than 1H and 13C :

  • Instructions for fluorine and phosphorus acquisition on the Varian 300 adobe image
  • Instructions for running deuterium NMR (Varian 500)

2-D NMR

  • Here is an overview for doing 2D (COSY, ROESY, TOCSY, NOESY, HMBC, HSQC and HMQC) on the Varians adobe image.
  • Instructions to run a TOCSY are here (Varian adobe image) (Bruker adobe image).
    • How to phase a 2D spectrum (Varian).
    • How to plot a 2D spectrum (Varian).
  • Guidelines to perform a ROESY experiment are here (Varian) (Brukeradobe image).
  • How to perform a NOESY experiment can be found here (Varian) (Bruker adobe image).
  • How to run a COSY on the Brukers can be found hereadobe image.
  • Get your HETCOR instructions here (Varian adobe image) (Bruker adobe image).
  • The HMBC instruction sheet is available here (Varian) (Brukeradobe image).
  • The HSQC instruction sheet is available here (Varian adobe image) (Brukeradobe image).
  • The HMQC experiment is described here (Varian adobe image) (Brukeradobe image).
  • Quick tips for running a GCOSY (Varians adobe image).
    • A more detailed description can be found here adobe image.

Other Experiments:

Supplemental Techniques:

  • How to calibrate a 90o pulse (Varian adobe image) (Topspin 1.3 adobe image).
  • Bruker VT instructions: Bruker 400 & 401 adobe image .
  • Simple water suppression experiment using PRESAT (Varian adobe image).
  • Water or solvent suppression for the Brukers (Topspin 1.3adobe image) (Topspin 3.1adobe image)
    • Other solvent suppression techniques include BINOM, JUMPRET, and WATERGATE.
    • Selective suppression (or excitation) using shaped pulses (Varian adobe image)
  • How to gradient shim your sample (Varian adobe image) (Bruker 600 adobe image).
    • Homospoil gradient shimming the Varian.
  • Instructions for increasing the number of scans while the acquisition is running, or adding scans to a completed experiment, are here (Varian adobe image)
  • Instructions for queueing experiments in Bruker (setting up multiple experiments at once) can be found hereadobe image

Plotting, Printing & Exporting Tips: (these links are a mix of .pdf files and pop-up windows)

  • Instructions on backing up and transferring data with SecureFx can be found here adobe image. SecureFx can be downloaded here.
  • How can I export my spectrum into a graphics file? (Varian : postscript .ps files) (Topspin 1.3 adobe image :.ps, .pdf, .jpg, .tif & .png files) (Topspin 3.1- use Publish> Save as Pdf)
  • Instructions on how to convert your Varian data to the Bruker format, in order to use Topspin Plot Editor, can be obtained here adobe image.
  • Instructions on how to download and install MNova Lite (AKA MestRec, AKA MestReNova) on your own computer are hereadobe image
  • Instructions on how to convert your Varian & Bruker data to the MNova Lite/Mestrec/MestReNova format can be obtained here adobe image.
  • Instructions on how to plot multiple spectra on one page can be obtained here. (Varian adobe image) (Brukeradobe image)
  • Instructions on how to make a white washed stacked plot can be found here. (Varian adobe image) (Bruker- use instructions above for regular stacked plots)
  • How do I make insets? (Varian) (Bruker: Use Topspin Plot Editor program)
  • Can I import my spectrum into a spreadsheet (Excel, Sigmaplot, Origin, etc)? Check these links. (Varian) (Brukeradobe image).

Instrument Problems and Curiosities? (most of these quick tips will open a small pop-up window)

  • The colors are flashing in the CDE. What's wrong? (Varian)
  • The variable temperature (VT) unit isn't working. What's wrong? (Varian) (Bruker).
  • My sample won't spin. Find out why here.
  • What are Pulsed Field Gradients (PFG's)?
  • Having problems with probe tuning? Check out this excerpt from the October 14th 2002 edition of Varian VNR News. You'll be tuning like a pro in no time!
  • What is the relaxation time? What's the difference between T1 and T2?
  • How do I unlock an experiment that's locked? (Varian)
  • Something is wrong with the spectrometer. ( I can't lock.)
    • Click here to take a graphical tour on how to lock the Varians.
  • My sample won't shim. (Varian and Bruker)
    • If you would like more information on shimming here are a few online resources gathered by Adrienne B. Hoeglund through the AMMRL...
      • A paper by Gerald A. Pearson at the University of Iowa can be found here.
      • A nice little tutorial at the University of Saskatchewan can be found here.
      • And the classic "Shimming Ain't Magic" paper at Acorn NMR Inc. can be found here.
  • Which spectrometer should I use for carbon? Click here.
  • What the heck is apodization?
  • How does 'resolution enhancement' work?
  • What is the Fourier number (fn)?
  • What does the "ADC overflow" error message mean? (Varian)
  • All of my 13C signals are split into multiplets. Click here. These tips are good for both the Bruker and Varian NMR spectrometers.
  • I have integral concerns. What can I do to "improve" my values? (Varian)
  • I need to run my spectra at a higher field to get better resolution. (Not necessarily true.)

NMR Sample Prep and Tube Care:


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