Never too Young to Learn

When the SIAS scheme started in 2008, the standard kit included a portable IR spectrometer and a UV-Vis spectrometer. Now, we’ve introduced portable NMR spectrometers into the mix. As well as covering the principles of spectroscopic techniques, our activities primarily use real-life contexts to demonstrate the applications of various techniques.

Modern analytical techniques are a core part of post-16 learning, but high costs of instrumentation and lack of technical support means that most schools do not have access to spectroscopic equipment. SIAS provides access to both the instrumentation and the analytical support through undergraduates and postgraduates at SIAS Host Universities, which not only aids understanding for school students but also provides a glimpse into the kind of practical work that may be included in a university degree.

The feedback received from both students and teachers taking part in this programme indicated clearly that the most valuable improvement would be the introduction of practical hands-on NMR experience. Thanks to funding from the Welsh Government through a National Science Academy grant, we were able to pilot the use of portable NMR spectrometers in 2013 – we now have nine Thermo Scientific picoSpin NMR spectrometers based at SIAS Host Universities across the UK. Students can compare IR with NMR spectroscopy for a range of chemicals, which supports theoretical knowledge and offers students a unique perspective that is currently often only available to PhD students.

NMR spectroscopy is the method of choice for many organic chemists because of its versatility in determining molecular structure, measuring reaction kinetics, monitoring reaction progress and controlling product purity. Students learn that the technique provides a wealth of information on chemical and structural aspects of molecules. We also describe its many applications in process control, whereby the quality of a chemical product, such as petroleum, biodiesel or food and drinks, can be followed by NMR. In situ monitoring and testing of process applications is also possible, as NMR is a non-invasive, non-destructive technique.

Benchtop NMR spectrometers are cryogen-free and our SIAS instruments have a temperature-controlled permanent magnet. They are portable (making them ideal to transport to schools), easy to operate, and affordable. Moreover, they can be set up and ready for use in an acceptable time: approximately one hour for the magnet to warm up, 15 minutes to shim, and only a few minutes for sample acquisition.
The development of benchtop NMR spectrometers has really improved access to this technique for research, undergraduate teaching and most excitingly, in schools. More recent developments in this field seem to be focusing on making this technology even smaller and more portable, whilst increasing resolution to reveal chemical information not available using smaller magnetic fields – that’s exciting to hear.

Feedback from schools has suggested that a portable mass spectrometer would be beneficial for students. The technology already exists, we just need the funding to expand into this area!

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Giants Go Pico

Mark Dixon, NMR product manager in Molecular Spectroscopy at Thermo Fisher Scientific, sheds light on how the NMR market may evolve.

Where are we now?

NMR spectroscopy has been out of reach for so many scientists due to the large cost of entry and subsequent cost of ownership. Previously, to satisfy their need for the unique information that NMR spectra provide, companies and institutions that could not afford to own or run one for themselves have had to use core or external facilities at great monetary and time cost. The affordability and convenience of a benchtop NMR spectrometer makes great sense, and the vast majority of analyses using NMR can be achieved using sub-100 MHz instrumentation. Currently, the organic chemistry education market appears to be the battleground. Various industrial applications are coming to light: food safety, polymers, petrochemicals, and illicit drug analysis, to name a few, but the vast majority of sales today are primarily being made in educational institutions ranging from two-year colleges to four-year degree universities.

Where are we going?

The benchtop NMR field is probably going to split into two distinct markets over time: i) undergraduate teaching and simple industrial applications, in which today’s technology more or less already covers the scope of the needs; and ii) research instrumentation that complements the high-field NMR market. In the latter market, some significant engineering challenges must be overcome before the quality and speed of data collection is up to a standard where a research chemist would use a benchtop NMR instrument for everyday use, only relying on their centralized high-field NMR facility for specialized work.

Where will we be in 10 years?

The next five to ten years will probably see one or more of the smaller players disappear, either by acquisition or for financial reasons; street prices will inevitably come down over time, which may challenge any small business that has high costs or limited reach.

Another component that may drive the uptake of benchtop NMR is any dramatic rise in liquid helium prices due to a predicted drop in supply, which will have a severe effect on the remaining high-field NMR vendors who rely on liquid helium to keep their magnets superconducting. Capabilities of the benchtop instruments themselves should approach those of the current crop of budget-class high-field instruments, but at lower magnetic field strengths.

A new field for portable NMR is likely going to be in process analytical technology. On-line or at-line usage of benchtop NMR in a pilot plant, for example, should be a valuable addition to chemical engineers who currently only use NMR in special situations for troubleshooting. The potential for benchtop NMR in more biochemical or biological applications has not been widely tested or proven yet, but one can see where unique structural information present in NMR spectra would also be of great benefit in those areas.

Spin Snapshot

Tyler England, mechanical engineer at SpinCore Technologies Inc., puts compact NMR in a nutshell.

Market We sell portable NMR devices (the iSpin series). The iSpin-NMR is a complete system console for NMR with spectrometer frequencies from 0 to 100 MHz. The NMR marketplace is growing – we are seeing steadily increasing sales.

Applications Applications are diverse: process control, explosives detection, porous media, solid-state and solution-state NMR for characterization, high-resolution solid-state NMR under MAS (magic angle spinning), wellbore NMR, multi-spectral sensing on autonomous vehicles, medical imaging, quantum computing, optically detected NMR, solid-state physics experiments, nanomagnetism and spintronics – and many others. All of our customers are doing interesting work with NMR. Many of them work with healthcare or academic research applications.

Future Applications for NMR are already widespread – as the technology improves, there is no telling where it can ultimately end up.