Instrument manufacturer Waters Corporation has teamed up with the University of Surrey to provide students with a practical understanding of a key spectroscopic technique to improve their knowledge and boost their employability, explains Vicky Starkie.
Analytical measurements are key to the continued development of our modern world, but analytical science is often unrepresented within traditional organic, inorganic, physical or applied chemistry courses. With high specificity and sensitivity, mass spectrometry (MS) is ubiquitous in analytical laboratories across industries where it is used to answer fundamental questions, such as: “are these compounds in my sample?” (screening); “how much is in my sample?” [(trace) quantitation]; “what else is in my sample?” (elucidation); and “what is the difference between my sample and another?” (comparison).
Despite MS becoming an established technology in both research and routine environments, academic programmes have not developed at the same pace, leaving undergraduate students with a lack of practical experience.
There are numerous reasons that MS has faced barriers to entry into non-analytical focused laboratory classes. These include cost, specific conditions or programmes required, and complex instrumentation. And in cases where MS is present, the samples are usually not run by the student themselves but are instead handed to a specialist to run. This latter point is critical and can reinforce for undergraduate students the false perception that analytical chemistry is subservient to the taught degree.
However, there are examples of universities who have incorporated MS into their curriculum, to better prepare candidates for industry. The University of Surrey has reported a highhit rate for atmospheric solids analysis probe mass spectrometry (ASAP-MS) in their existing undergraduate organic practicals.
This is described in ‘Atmospheric solids analysis probe mass spectrometry: An easy bolt-on for the synthetic undergraduate teaching laboratory’ by Bingham NM, Wright JS, Mathias SC, Douce D, Sears P, published in Rapid Communications in Mass Spectrometry.
Lead author Dr. Nathaniel Bingham described the purpose as follows: “Our goal was to show how simple to use mass spec can be and complementary to existing organic experiments, without the need to introduce specific mass spec focused practicals. Rather than providing students with mass spec data or sending samples to a technician to run, we can allow students to run the samples themselves and take ownership of their data. Making students aware of how useful mass spec is to an organic chemist is important and showing them that it can be as straight forward as taking an IR spectrum.”
And we can see that this implementation of MS into an undergraduate curriculum is working.
Industry sources said the Surrey students were more employable because they were more industry-ready, co-author Dr Patrick Sears explains.
There are numerous reasons that MS has faced barriers to entry into non-analytical focused laboratory classes. These include cost, specific conditions or programmes required, and complex instrumentation
Sears expands on their methodology “to ensure incorporation into the undergraduate curriculum rather than simply in our dedicated analytical chemistry modules, we needed the MS characterisation to ‘bolt-on’ to existing synthetic practicals, to remove the need to replace current experiments in an already busy schedule”.
For this, the mass spectrometer and technique used needed to be simple, of low cost, and provide rapid results, leading Surrey to implement the Waters RADIAN ASAP Direct Mass Detector.
In the work, they demonstrated the application of the RADIAN ASAP Mass Detector to complement 11 out of 13 existing foundation year and undergraduate (UK Framework for Higher Education Qualifications – FHEQ – level 3–5) organic chemistry experiments in the University of Surrey curriculum.
Mass spectrometry lends itself well to the teaching environment. In its simplest experiment, the RADIAN ASAP Mass Detector can provide a mass-based confirmation of intended product, starting material, and intermediates, within 30 seconds with little to no sample preparation, giving students a clear understanding of what is happening in their synthesis near real-time.
This works with mixtures, as mass spectrometry will separate by mass not chemistry and detects the molecules one at a time. This differs from traditional bulk spectroscopic techniques where mixtures can be quite complicated to interpret due to overlapping responses.
Furthermore, by increasing the cone-voltage of the MS, fragmentation of the molecules can be induced. These fragments can then be used by the student as pieces of the puzzle to elucidate the structure of the parent molecule as the bond breakage is predictable based on bond strengths. Further specificity on these fragments can be gained by looking at the isotope pattern; for example, with an organochlorine compound one would observe two m/z peaks representing 35Cl and 37Cl in a 3:1 ratio reflecting the natural abundance of these two isotopes.
Mass spectrometry complements core analytical skills. For example, extractions of components from materials are a critical part of many industrial workflows. Through the use of the RADIAN ASAP Mass Detector, the students can determine and learn the composition of each extraction (e.g., polar vs non-polar vs acidic and so on) rapidly.
This works with mixtures, as mass spectrometry will separate by mass not chemistry and detects the molecules one at a time. This differs from traditional bulk spectroscopic techniques where mixtures can be quite complicated to interpret due to overlapping responses
Similarly, thin layer chromatography (TLC) remains a commonplace technique. The ASAP probe can be used to transfer the material from the plate into the mass spectrometer, providing mass-based information on each spot, complementing the existing chemical separation.
ASAP-MS can complement a significant majority of the University of Surrey's current organic chemistry undergraduate laboratory curriculum. The simple and rapid sampling technique facilitates its addition to existing experiments as a ‘bolt-on’ technique, without the need to redesign experiments or the curriculum. This could provide important context to common undergraduate experiments and allow students to analyse real mass spectrometry data, in preparation for placements, final year projects, and post-university careers.
The utilisation of mass spectrometry within the undergraduate curriculum has shown promise, and because of the success seen so far Drs Bingham and Sears are now working with Waters to make this material available for the broader community, making it simpler for other institutions to adopt similar programmes.
Vicky Starkie is principal marketing manager – routine mass detection at Waters Corporation and has more than 25 years’ experience in a range of analytical techniques
