NMR Facility

Department of Chemistry University of Oxford

The CRL NMR facilities provide research support for Organic Chemistry, Inorganic Chemistry and Chemical Biology in the Chemistry Department. These services may also be made available to other departments in the University by special arrangement. Use of the facilities is explained briefly below and is covered in the introductory NMR training session that all users of the facilities must attend.

  

Safety Statement

 

 

There are specific safety hazards associated with use of the NMR instruments that relate primarily to the presence of intense stray magnetic fields in the vicinity of the instruments which may affect or interfere with:

-heart pacemakers
-medical implants
-magnetic bank or ID cards
-watches (non-LCD)

As a consequence, specific rules exist regarding access to the NMR laboratories:

-Anyone with a heart pacemaker must not go beyond the magnetic field hazard warning signs posted in the CRL and will not be allowed access to any NMR laboratory.
-Anyone with a medical implant must seek approval from the Director of NMR Spectroscopy before entering any NMR laboratory or making direct use of any NMR spectrometer.
-No laboratory coats are to be worn in the NMR laboratories.
-No metal objects are to be taken into NMR laboratories.

Anyone wishing to make use of any of the NMR spectrometers MUST undergo the appropriate training session with a member of the NMR staff before using the instruments (see below).  This includes the open-access automated spectrometers. 

Organic Chemistry and Chemical Biology Facilities

Use of the NMR facilities

 The research facilities make use of nine solution NMR spectrometers and operate on four levels:

  1. "Open Access" automated spectrometers: these are available to all research workers at all times and provide routine 1D and 2D NMR characterisation based on 1H, 13C, 19F and 31P NMR (see experiment list). The spectrometers are located on the ground and first floors. Instruments available are: Bruker DPX200, AVF400 and AVG400. In addition, the DPX300 spectrometer located in the Dyson Perrins Laboratory is available to use out of Teaching Lab. hours (the instrument must be booked for use).
  2. "Hands-On" spectrometers: these may be used by trained chemists who wish to acquire their own NMR data, including multinuclear NMR and variable temperature studies. The spectrometers are located in the basement NMR lab. Instruments available are: Bruker AVB400, AVB500 and AVX500
  3. Submission Service: This is a service operated by the NMR staff who undertake analysis of samples submitted by research workers. The work typically involves more complex experiments and/or low sample masses. The Service is based in the basement NMR lab and uses: Bruker AVB500, AVC500 and AVX500
  4. Research Projects: These are projects involve the NMR staff (and research students) through longer-term and more complex investigations typically in collaboration with research groups within Chemistry. Most work uses the Bruker 500,600 and 700 MHz spectrometers.

The usual procedure for using the facilities is as follows:

1) Initial spectra for characterisation purposes should be collected on one of the open access spectrometers at 200 or 400 MHz. A brief training session is provided by the NMR staff to demonstrate their operation (contact Maria for this training). You should first collect a basic 1H 1D spectrum of your compound to check its structure and the sample integrity and quality (see guidance on Sample Preparation). You may then need to collect further experiments on the open-access instruments to characterise the molecule, provided the sample is of sufficient quality. You should not collect all available experiments on a sample of unknown quality as these may waste instrument time; always assess the 1H spectrum first.

A document summarising available experiments is available.

The data collected may be sufficient for your needs; if not you may use the hands-on instruments or submit to the NMR service.

2) If you wish to be trained to use the hands-on instruments and thus be able to execute NMR experiments yourself, you should first discuss these requirements with your group supervisor. If they agree you should be trained, please email Tim to explain your needs and make arrangements for training. Initial training is provided on the AVB400  spectrometer and must be given by a member of the NMR staff; you will be asked to undergo training even if you have hands-on experience from elsewhere, but this will be tailored accordingly. Each instrument has an associated booking scheme which will explained as part of the training session. The AVB400  is available for use at all times whereas the AVX500 is shared with the NMR service and has more restricted access.

3) Submissions to the NMR Service are made through the submission point located in the basement (high-field) NMR lab. This requires that you:

provide a sample ready for analysis

  • complete a sample submission form
  • make an entry in the electronic submission list for every sample to be analysed.
  • You must also provide a 1H NMR spectrum of the submitted sample wherever possible (such as from the open access instruments) demonstrating it is of suitable quality for further NMR analysis. If you require advice on the most appropriate experiments etc, please consult either Tim or Barbara who would be happy to advise. Completed samples and their spectra are returned to your research group trays at the submission point in the basement lab. (there is also a submission fridge for unstable or more volatile samples). See also the NMR service page.

4) If you have a need for more detailed or longer term NMR projects please discuss these with Tim in the first instance.

Data from all our spectrometers can be downloaded for local storage and for off-line processing. The current status of the open-access instruments is also viewable on the web and allows you to see whether your experiments have been completed; see the Automation History Lists on the download page.

Inorganic Chemistry Facilities

The Inorganic facilities provide both open access and hands-on instrumentation, but do not provide a formal submission service. These instruments (two Bruker AVIII 400 MHz and one Bruker AVIII 500 MHz) are found on the second floor and in the basement NMR lab. Please contact Nick if you wish to be trained to use these instruments.