We have developed methods for using in situ electron energy-loss spectroscopy (EELS) to perform quantitative analysis of gas in an environmental transmission electron microscope. Inner-shell EELS was able to successfully determine the composition of gas mixtures with an accuracy of about 15% or better provided that some precautions are taken during the acquisition to account for the extended gas path lengths associated with the reaction cell. The unique valence-loss spectrum associated with many gases allowed simple methodologies to be developed to determine gas composition from the low-loss region of the spectrum from a gas mixture. The advantage of the valence loss approach is that it allows hydrogen to be detected and quantified. EELS allows real-time analysis of the volume of gas inside the reaction cell and can be performed rapidly with typical acquisition times of a few seconds or less. This in situ gas analysis can also be useful for revealing mass transport issues associated with the differential gas diffusion through the system.
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