Thermal decomposition of dried crystalline powder obtained from titanium(IV) bis(acetylacetonate) diisopropoxide (75 % solution in 2-propanol) (1) was monitored by simultaneous TG/DTA, EGA-FTIR and EGA-MS measurements and the results were compared with those of amorphous powder obtained by gelling of acetylacetonate-modified titanium(IV) tetra-isopropoxide at molar ratio of 1:2 in boiling 2-methoxyethanol (2). Thermal degradation of 1 in the temperature range of 25–700¡ãC consists of 5 steps with a total mass loss of 62.5 % . EGA by FTIR and MS revealed the release of H2O below 120¡ãC; followed by an intensive evolution of acetylacetone around 245¡ãC. The release of acetone and acetic acid occurs up to 270¡ãC and that of CO and CO2 up to 530¡ãC.