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Dilute alloys are promising materials for sustainable chemical production; however, their composition and structure affect their performance. Herein, a comprehensive study of the effects of pretreatment conditions on the materials properties of Pd 0.04 Au 0.96 nanoparticles partially embedded in porous silica is related to the activity for catalytic hydrogenation of 1-hexyne to 1-hexene. A combination of in situ characterization and theoretical calculations provide evidence that changes in palladium surface content are induced by treatment in oxygen, hydrogen and carbon monoxide at various temperatures. In turn, there are changes in hydrogenation activity because surface palladium is necessary for H 2 dissociation. These Pd 0.04 Au 0.96 nanoparticles in the porous silica remain structurally intact under many cycles of activation and deactivation and are remarkably resistant to sintering, demonstrating that dilute alloy catalysts are highly dynamic systems that can be tuned and maintained in a active state., (© 2020. The Author(s).)