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The aluminosilicate zeolite ZSM–5 (MFI) offers Lewis acid sites confined to regular straight-channel pores with specific micropore volumes greater than 0.1 cm³/g. Cu and Zn were introduced to synthesized frameworks using ion exchange procedures. Diffuse reflectance UV-vis and energy dissipative x-ray (EDX) spectroscopies confirm that Brønsted acids were exchanged for metallic counter-ions in the synthesized framework. In situ UV-vis spectroscopy was used to characterize the oxidative stability of the ions, and in situ DRIFTS confirmed characteristic nitric oxide binding. The conversion and selectivity of the NO oxidation reaction are compared between the two metal-exchanged zeolites and a reference, H–ZSM–5.