The study of the “Volcanic Sublimates” observed at the orifice of active volcanoes are important to know the process of the differentiation of the magmatic emanation. So-called “Volcanic Sublimates” are, however, not always true sublimate from the magmatic emanation, but include products of reactions among volcanic gases, surface water and surrounding rocks. In a previous paper, one of the present authors reported that small amounts of fluorine and chlorine deposited on the surface of a silica-glass tube on heating the samples of igneous rocks above 800℃, and that sodium and ammonium ions were found by qualitative tests. The result suggests that a detail study on the sublimates formed in the experiments mentioned above will give exact informations about the sublimate directly derived from the magmatic emanation. In the present study, 30~50g. of finely powdered samples of volcanic rocks were heated at 1000℃ in the silica-glass tube which is evacuated to 10-1~10-2mmHg excluding water vapor. The sublimates deposited on the silica-glass tube were devided into several fractions with 100℃ intervals. Water soluble halogens and alkalis were determined in each fractions. Qualitative tests were also done to examine if there were some other compounds sublimed from the rock.