A paradigm shift in low-field NMR spectroscopy for industrial process monitoring, control, and optimisation

We are all familiar with the concept of travel, and visiting York from Glasgow is conceptually a trial matter. When we reflect on this process, however, there are lots of potential questions we might ask about the mode of transport, the route and the potential to get lost.
A similar range of questions could be asked about chemical reactions. We select starting materials and seek to transform them into products. The route we choose is equally complex. Now, however, the participants are much smaller and very special methods are needed to view them. Furthermore, with an optimal solution we get the most product from the least starting material using the least amount of energy and other resources as possible. If think of a reaction that is undertaken on the 1,000,000 tonne scale it is also clearly vital to minimise waste.
In Chemistry, there is a very special and often expensive method called nuclear magnetic resonance spectroscopy (NMR) that allows us to take pictures of the participants as they travel from starting materials to products. This methods is normally very insensitive and hence very expensive large magnets are required. If we want to use this technology to deliver clean and efficient chemistry on an industrial scale we need to find a way to work with smaller lower cost magnets, ideally using the Earth's magnetic field. In this project we aim to develop a new method using such low-magnetic field NMR devices to follow the route taken by molecules during their conversion into high value products in both laboratory and industrial settings. We will use a special form of hydrogen gas, known as parahydrogen to increase the sensitivity of the NMR measurement to a level that will allow to achieve this goal. Parahydrogen was actually the fuel of the space shuttle and one might view it here as acting like a molecular microscope whilst at the same time removing (filtering) any unwanted signals from spectators to the reaction of interest. We will build-up our understanding of the reactions route by taking our NMR pictures which contains precise information about the identity of the participants (molecules) at different times after the start of the reaction. This means that we will monitor the same process several times in order to produce the necessary molecular level picture that will ultimately allow us to optimise our chosen reaction. The enhanced level of information that will be provided by our new device will enable scientists and industrialists to develop and optimise reactions in a way that was previously impossible and hence contribute more positively to society.

The project is of relevance to areas of strategic importance as identified by the research councils (critical (c) to supportive (s)): analytical science (c), catalysis (c), chemical reaction dynamics and mechanisms (c), chemical structure (c), computational and theoretical chemistry (s), sensors and instrumentation (c) and synthetic coordination chemistry (c). Its unprecedented approach will see the power of NMR used to provide valuable insights that have relevance to both environmental sustainability (via catalysis) and UK Plc.
It is the opportunity to improve existing processes and to also develop new manufacturing processes, e.g. novel intensified and continuous, through laboratory and plant scale measurements that will secure cost-savings and efficiency gains. This will be achieved in conjunction with the CPI, which is the process element of the UK government funded 'High Value Manufacturing Catapult' network. CPI works with academics and SMEs to translate a broad range of technologies in industrial biotechnology, smart chemistry, anaerobic digestion, sustainable engineering and biologics manufacture. In addition, engagement with members of CPACT, who represent a broad spectrum of industrial interest, will maximise the utilisation of the new technology. Julian Morris of Morris Associates, in his capacity as CPACT Technical Director, will provide a key link between academia and industry to ensure dissemination of the research and promotion of the technology within industry. A steering group will be set-up, which will be chaired by an industrial representative, to ensure that the technology developed meets the needs for manufacturing across a range of sectors. Company representatives will attend project meetings, provide input on design criteria and help with benchmarking of the prototype technology. In the second route to economic impact, this project offers the opportunity to support the UK supply chain in advanced instrumentation and research equipment. This would be achieved through the development of novel instrumentation by formal collaboration with either Bruker-BioSpin, Oxford Instruments or Magritek Limited.
Our chosen approach using parahydrogen is unique and will serve as a model from which to work to revolutionise the potential of NMR to study reactions. There has been a huge research investment in the development of hyperpolarisation methods aligned to healthcare in both the USA and Europe over the last decade; York has world leading expertise here and spin-offs into this area are expected. The potential for this work to manifest itself directly in health in the future is therefore not unrealistic.
The applicants have substantial previous experience in collaborating with commercial companies and have attracted recent support through industrial CASE awards. Support for patent protection, IP management and commercialisation is provided by our Universities Research and Enterprise Offices. Once any patent protection issues have been resolved, the results obtained will be presented at national and international conferences and during visits to universities and industrial research centres. The investigators will seek further collaborations with potential users of the technology. They will attend relevant conferences and have given invited/keynote lectures at such conferences. Most importantly, the results will be published as communications in leading international journals, followed by full papers, which include further studies. The investigators will develop their webpages to disseminate and showcase the results obtained and, if appropriate, will work with the Departmental and University press officers. In addition to communicating with other researchers in the field, it is very important to inform the public. The applicants have published general science articles and given public lectures. We will extend these and related outreach activities.