Chemical Characterisation and Analysis Facility

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Dynamic reaction monitoring facility

Contacts

For dynamic reaction monitoring enquiries, please contact:

Dr Catherine Lyall
Instrument Specialist (Reaction Monitoring and NMR)
c.l.lyall@bath.ac.uk
+44 (0) 1225 385555

The Dynamic Reaction Monitoring Facility (or DReaM Facility) allows researchers to monitor homogeneous reactions in real-time, under their normal reaction conditions, with a variety of analytical techniques.

As well as kinetic data, the DReaM Facility can also help researchers shed light on reaction intermediates and by-products, allowing a comprehensive picture of all aspects of the reaction in solution to be constructed.

An EPSRC grant was awarded in July 2016 to fund the equipment purchase
 and the Facilty was opened in November 2017 alongside the Reaction Monitoring Symposium.

Until May 2018 significant method development and testing will be undertaken by internal users.

The first call for external proposals for use of the facility between May and October 2018 is now open.

The reaction can be set up in the fume-hood (a Schlenk line and glove box are also available) and the reaction mixture is pumped through flow cells in the NMR spectrometer and the UV spectrometer.

Samples can be taken from the flow pathway and directed to HPLC and/or mass spectrometry analysis. Volatile samples can also be taken from the reaction headspace to a second mass spectrometer.

Equipment

  • Bruker 500 MHz NMR spectrometer with a nitrogen cooled Prodigy cryoprobe. Bruker’s InsightMR flow tube is used to flow the reaction mixture into the NMR spectrometer.
  • Bruker MicrotofQ Mass Spectrometer
  • Agilent 1260 series HPLC
  • OceanOptics UV Spectrometer
  • Hiden Mass Spectrometer for analysis of the headspace volatiles

NMR Spectrometer

nmr-spectrometer-dreamTaking centre stage is the DReaM Facility’s Bruker 500 MHz NMR spectrometer with a nitrogen cooled Prodigy cryoprobe. Bruker’s InsightMR flow tube is used to flow the reaction mixture into the NMR spectrometer, where NMR active species can be detected and quantified. The Prodigy cryoprobe and the flowtube are able to maintain temperatures between -20 °C and 80 °C and pressures up to 10 bar. NMR active nuclei from 15N to 31P, as well as 1H, 2H and 19F, can be observed. A room temperature probe is available for other nuclei if needed, with decreased sensitivity.

Mass Spectrometer

The Facility houses a Bruker MicrOTOF-Q Mass Spectrometer which uses electrospray ionisation time-of-flight (ESI-TOF) as an ionisation technique. This system can be used to obtain accurate mass data for molecules in solution – particularly useful to obtain complementary information for compounds where no (or few) NMR active elements are present. For typical reaction concentrations, samples will need to be diluted to avoid saturating the detector.

HPLC

hplc-dreamThe Facility hosts an Agilent 1260 Infinity II series HPLC with three detection methods:

  • Refractive index (RI) detector
  • Ultra-violet (UV) detector
  • Evaporative light scattering detector (ELSD)

Where samples are compatible with the HPLC columns, samples can be injected from the flow loop into the HPLC. The system also has a manual injector for samples which require work-up in advance of HPLC analysis. Using a chiral HPLC column allows us to investigate enantiomers present in the reaction mixture that can’t be distinguished by NMR. For typical reaction concentrations, samples will need to be diluted to avoid overloading the column.

UV Spectrometer

The flow cell for the OceanOptics UV spectrometer is positioned after the NMR spectrometer in the flow loop but before the reaction mixture returns to the reaction vessel.

Headspace Mass Spectrometer

headspace-mass-spectrometer-dreamWe have a Hiden HPR20 Mass Spectrometer for analysis of the headspace volatiles, using electron ionisation (EI). If your reaction is emitting gaseous by-products in the range of 1-300 AMU, these can be detected. This spectrometer is suitable for reactions up to 30 bar.

Fume hood and glovebox

We have a fume hood with Schlenk line for setting up reactions under inert conditions. If reactions are extremely air-sensitive, there is also an MBRAUN glovebox that can be used as an alternative.

Team

Industrial partners

External users

We welcome users from industry and academia. A call for proposals will be open twice-yearly; in January for Facility time scheduled in the following May-October, and in July for Facility time scheduled in the following November-April.

The first call for external proposals for use of the Dynamic Reaction Monitoring (DReaM) Facility is now open, for Facility time between May and October 2018.

Please read the instrument limitations on this page and download the guidelines for use of the facility before your submit your proposal.

Download and fill in the proposal form and submit your proposal via email to Dr Catherine Lyall before 31 January 2018.

Proposals will be prioritised by the internal and external members of the DReaM Management Board after the deadline.

If you are interested in using the DReaM facility, please email Catherine with any queries and to find out if the facility is suitable for your requirements.

Internal users

Please access our internal wiki pages to find out more about how to apply for time at the DReaM facility or book time for method development experiments.