According to a method developed by d e B o e r powder samples baked out in vacuo are exposed to iodine vapour which is adsorbed at the powder surface. The amount adsorbed is determined by a simple chemical titration.T h e precautions necessary arid the reproducibility of the observations are discussed in detail. Surface reactions and the effect OF milling in a ball mill can clearly be traced by corresponding changes in the adsorption. 5 1. Zntroducfion. By d e B o e r and collaborators 1 ) the adsorption of iodine vapour in an evacuated system has been used to study the structure: and properties of sublimated layers of CaF,, BaCI., etc. T h e experiments described below were made to investigate whether the same technique could be used to determine the relative surface of powdered substances, this being a measure of particle size.T h e greater part of our observations were made on barium strontium carbonate, a mixed crystal 1 : 1 of BaCO,, and SrCO,, which is used for making oxide coated cathodes. Suspensions of these mixed crystals &re frequently ground in a ball mill before use and we intended to study the variations in particle size due to the milling. Hence this particular choice of material. In the course of the investigation, however. other substances have occasionally been used in order to compare their behaviour with that of BaSr( CO,),.