A procedure was proposed for decomposing liquid radioactive organic wastes in low-temperature plasma to form solid inorganic products. Thermolysis of two types of extraction systems with heavy fluorinated diluents, proposed for application in radiochemical industry, was studied. The solid and gaseous thermolysis products were completely analyzed. No fluorine-containing organic compounds were detected in the exhaust gases. To prevent formation of corrosive products, a metal cation was added forming insoluble compounds with the decomposition products. A convenient procedure for simultaneous feeding of organic compound and calcium salt in a methanol solution was proposed.