Solution State NMR

The solution-state NMR facilities are located in A73/A74 Faraday Building and are used for both research and teaching.

The instruments are run in open access mode 24/7, but users must have suitable training before being allowed access to the NMR suites, so contact Dr Geoffrey Akien beforehand. Trained undergraduates can access the space by themselves from 9 am-5 pm, Monday to Friday, but must be supervised outside of these hours.

During peak hours (Monday to Friday, 8 am-6 pm) the maximum time allowed per experiment is 15 minutes, although users may have more than one experiment per sample. To maintain responsive access for others, the "Priority" ability is enabled for all users. At busy times of the year, the peak/off-peak timings may change to maximise throughput of samples.

Liquid nitrogen fills are generally carried out every Monday morning, but one instrument will always be available for immediate use. Liquid helium fills take place approximately every 5-6 months, and users will be advised by email when these take place, and if there are any other scheduled interruptions. A list of activity is also maintained on the Chemistry Booking System.

Current status and bookings

The regular status pages are synchronised with the live pages every five minutes, but the live ones are updated by the spectrometers as soon as something happens.

Note that the "live" direct links to the spectrometer pages will work only if you've got your credentials properly setup to access the LUNA filestore, and if you right-click, select "Copy link address", and copy and paste it into a new tab. It unfortunately won't work if you just click on the link directly, but once you've got a bookmark setup than everything should Just Work.

IconWeb needs to be specially configured on a per-user basis - ask Geoff if this is something you might be interested in.

Research - Bruker AVANCE III 400

The Bruker AVANCE III 400 (NanoBay v1) is fitted with a 5 mm 1H-X broadband observe (BBFO, 109Ag-19F) RT probe, and is currently equipped with a 60-position SampleXpress autosampler. The instrument is currently controlled with TopSpin 3.6.5 on Windows 10. It is primarily intended for research use, but from time to time it is also used for undergraduate teaching.

Owing to the higher sensitivity of the 400 compared to the 300, several of the longer experiments (e.g. carbon, HMBC) have versions appended with the ".fast" suffix so that they will run in less than 15 minutes each and so fit within daytime limits. Note that these will only give good-quality spectra if your sample is concentrated enough - 10-20 mg in 0.6 ml solvent is a reasonable concentration to use for this.

A wide variety of experiments are configured to run in automation, but if there's something missing just ask.

  • 1H - qualitative and quantitative
  • 1H with automated single and multiple solvent suppression
  • DOSY
  • 13C and DEPT135
  • COSY
  • Edited HSQC
  • HMBC, H2BC
  • A variety of experiments up to 75 °C in day-to-day automation, and up to 150 °C with special permissions.
  • Support for a variety of X-nuclei including 2H, 7Li, 10B, 11B, 14N, 15N, 19F, 23Na, 27Al, 29Si, 31P, 33S, 45Sc, 77Se, 89Y, 95Mo, 97Mo 111Cd, 113Cd, 119Sn, 121Sb, 123Sb, 127I, 133Cs, 195Pt. For most spin-1/2 nuclei experiments 1H,X-HMBC 2D spectra are also available, and usually the better choice.

The standard temperature is 298.0 K and is calibrated using 1H and the standard Bruker 99.8% D MeOH-d4 reference sample. For high-temperature experiments, the standard corrections are not quite correct - we have ethylene glycol calibration data to deal with this.

For low-temperature experiments, we need to replace the normal VT gas with a liquid nitrogen evaporator, so these must be run out of automation and discussed with Geoffrey Akien.

The maximum temperature possible for the BBFO probe is 150 °C, but for safety and various experimental reasons, anything above 75 °C requires permission and training.

Bruker AVANCE III 400

Teaching - Bruker Fourier 300

The Bruker Fourier 300 (MHz) instrument is fitted with a 5 mm 1H/13C-observe probe (DUL/ES) currently equipped with a 16-position SampleXpress Lite autosampler. The instrument is controlled using TopSpin 3.2pl7 on Windows 10. The primary use of this is for teaching, but research samples can be run on this at any time.

Currently configured experiments in automation:

  • 1H - qualitative and quantitative
  • 13C and DEPT135
  • COSY
  • Edited HSQC, HMBC

The sensitivity of the 300 is about half of the 400, so there are no pre-configured ".fast" versions of experiments. However, parameters can still be manually adjusted to fit into the 15 minute daytime limits if necessary.

Owing to differences between the 300 and the 400, the 300 is not recommended for use with deuterated solvents with more than one peak, with the exception of MeOH-d4 and toluene-d8 which have workarounds in place. The instrument is capable of VT up to 65 °C, but for various different reasons this is not available in automation. This is similarly the case for 1D 2H experiments.

Burker Fourier 300

Also available for communal use are:

  • Specialist solvents and additives
  • Coaxial inserts for external referencing
  • Amberised tubes for light-sensitive samples
  • Screw-cap and "Young's"-type tubes for air-sensitive samples
  • 3 mm tubes and suitable spinners
  • 5 mm Shigemi tubes for small samples, matched for either CDCl3 or D2O (both normal and "advanced")
  • FEP tube liners for corrosive samples
  • Aluminium NMR tube heating block with thermocouple well for use with stirrer hotplates
  • Butane torch for flame-sealing tubes
  • Heat guns
  • Ultrasonic bath
  • Vortexer
  • Mini centrifuge
  • Hand centrifuge for NMR tubes
  • Eppendorf mechanical pipettes and tips for dispensing 0.5 μl to 5 ml
  • Small dewar for pre-cooling of NMR tubes

If there's something that we don't have that you think would be worthwhile for the Department, let us know and we can look into buying it in for communal use.