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Isotopic composition of noble gases and other volatiles (CO2, N2) from minerals of corundum-bearing rocks with isotopically ultralight oxygen from Khitoostrov deposit have been investigated. The studies were conducted on Finesse mass-spectrometry system [1] using step heating in temperature range from 200°C to 1400°C. The following minerals were investigated: corundum, amphibole, garnet, staurolite. For the same samples, differential scanning calorimetry and thermogravimetry curves have been obtained. The first results of the studies show that the low-temperature (less than 400°C) release peaks of carbon dioxide and nitrogen probably represent a laboratory organic contamination. The middle-temperature release peaks (400-800°C) are potentially consistent with decrepitation of fluid inclusions and diffusion of the gases from crystalline lattice of the minerals, and the high-temperature release peaks (900-1400°C) possibly indicate the transformation of mineral structures such as amphibole and staurolite as a result of dehydration. [ABSTRACT FROM AUTHOR]