• Structure Elucidation

    1D and 2D experiments

Listing Row

Monday, June 8, 2015
Monday, June 8, 2015
  • Training

    To schedule a training please sign up in micores and request training through that site, if you encounter any problems please email Larisa Yeomans at yeomans@umich.edu

    Make sure you set aside 2 hours of your time for training.  In the basic training you will learn to run 1D experiments 1H, 13C, and one of the most useful 2D experiment HSQC. Following the data acquisition you will be trained on data processing using Mestrenova.  The NMR laboratory has 2 perpetual licenses at your disposal.

  • Sample Preparation

    Make sure that you have a decent quality NMR tube and that your deuterated solvents from an open bottle are not too old.  Deuterated solvents tend to absorb water with time after opening. Common deuterated NMR solvents include CDCl3, methanol-d4, acetone-d6,  DMSO-d6, D2O, etc...  

    DMSO-d6 is a great solvent for NMR but you won´t be able to recover your sample, that is why I recommend you try to run your sample on a solvent that is easy to remove once you are done.

    Great results will be obtained if your use 5-25mg of your compound and dissolve it in 600-700 uL of deuterated solvent.   Lower volumes require longer shimming.  

    NMR Tube care:

    You should contact scientific glassblower Roy Wentz  (734)763-6357 at the Glass Shop 3416 in Chemistry, and purchase an NMR cleaning apparatus with your shortcode (~$80 as of 2018).  It really speeds up the cleaning process.   

    Once they are clean, lay them flat on a piece of aluminum foil and let them dry in the oven (the oven should be set around 80-100 celsius)  for a couple hours.

    Make sure you don´t leave the clean tubes in the oven for extended periods of time since that can compromise their shape.   A warped tube will give you crappy looking spectra.   

     

     

  • Reserve time to use the instruments

    The instruments can be reserved by scheduling equipment time after you have logged in into micores for the NMR lab.

    Once you are trained you will be granted acces to reserve instrument time for the 400MHz and the 500MHz. 

    COLLEGE OF PHARMACY GRADUATE STUDENTS  AND RESEARCH STAFF HAVE RESERVATION PRIORITY

    The 400MHz can be reserved up to an hour from 8:00am-7:00pm during the week and after that you can reserve freely for overnight runs.  You can reserve for as long as you need to over the weekend.

    The 500MHz can be reserved freely.

     

     

  • Sample Service

    We also offer the services of sample service, in that case you can bring your sample prepared or we can prepare it for you. At the end you will get your raw data, and NMR processed spectra in a pdf format. If you want to submit a service request please log in into micores and submit your request.

  • Fees

    Hands on:

    400 MHz
    University of Michigan Investigators - $13 per hour
    External Users - $60 per hour

    500 MHz
    University of Michigan Investigators - $18 per hour
    External Users - $70 per hour

     

    Consulting rate

    Internal- $60 per hour

    External- $80 per hour

     

    If Spectroscopist Performs the Experiments:

    $31 in addition to hourly fee for machine usage