Hot-stage microscopy - Direct Analysis in Real-time mass spectrometry (HDM) as a novel tool for monitoring thermally-driven reactions on a small scale

Abstract

There is a requirement for reliable real-time analytical tools for reaction monitoring to optimise chemical syntheses. We have developed a new technique which combines thermal analysis, digital microscopy and chemical identification using ambient ionisation mass spectrometry. We term this hot-stage microscopy-Direct Analysis in Real-Time mass spectrometry (HDM). The technique provides optical data as a function of temperature coupled with chemical characterisation of evolved species, including reactants, intermediates and products throughout the course of a reaction.In addition, only a few milligrams of sample are required with analyte detection down to the nanogram range. We demonstrate the benefits of HDM using a series of solventfree reactions. Our results confirm the suitability of the technique as the reactions studied follow the same pathways as published previously. The accurate temperature control achieved with HDM could also be used to assess the optimum temperature at which thermally-driven reactions can proceed efficiently.

Applications of ambient ionization mass spectrometry in 2020: An annual review

“…Masuda and Kobayashi similarly employed DART‐MS, this time for the rapid monitoring of direct‐type hydroxymethylation and Mukaiyama‐type hydroxymethylation reactions, achieving quantification using an isotope‐labeled internal standard 131 . Finally, Ashton et al applied DART‐MS to study thermally‐driven chemical reactions 132 . The method combined a heated stage onto which a few milligrams of the material was placed and heated in a linear fashion, with DART monitoring changes throughout the process.…”

“… 131 Finally, Ashton et al applied DART‐MS to study thermally‐driven chemical reactions. 132 The method combined a heated stage onto which a few milligrams of the material was placed and heated in a linear fashion, with DART monitoring changes throughout the process. As a result, small‐scale thermally driven reactions could be monitored in real time.…”