Abstract: | Maturation provides whisky with a mild and smooth texture by removing the irritating alcoholic flavor. However, the precise mechanism by which the whisky flavor is improved through the maturation process remains unknown. In this study, we performed mesoscopic structural measurements—dynamic light scattering (DLS) and small‐angle X‐ray scattering (SAXS)—to elucidate the relationship between the liquid structure and flavor maturation of whiskies. Both techniques detected two scattering components corresponding to the clusters formed by the extractives from oak casks during maturation, which are not present in the new make (freshly distilled whisky). Analyzing the scattering profiles revealed that only the small clusters increase in concentration during maturation. It is concluded the small cluster component is crucial for obtaining flavorful whiskies, while the large cluster component, whose concentration is independent of the maturation time, is related to the alcoholic irritation of the whiskies, as demonstrated by the sonication test. |