X‐ray studies of samples made of sucrose, glucose, and acetylsalicylic acid were made to determine if the latter is in solid solution with the sugars. The main constituent of the samples was sucrose and the amounts of acetylsalicylic acid varied from one and a half to twenty per cent. The samples were prepared by melting and heating the sugar combinations to 160°C, removing essentially all the water and allowing to cool. The acetylsalicylic acid was then incorporated in one set of samples at 140°C and in another at a temperature between 110–115°C, that is, both above and below the melting point (133–5°C) of the compound. The former samples were far more hygroscopic than the latter, but in neither case did the acetylsalicylic acid seem to form a solid solution with the rest of the constituents.