Biodiesel is an alternative fuel to gasoline due to its environmental and economical benefits. Glycerol is the main by-product of the biodiesel production by transesterification of vegetable oil with methanol or ethanol. The esterification of glycerol with acetic acid can be a good choice for utilization of by-product glycerol. In this work esterification of glycerol with acetic acid was performed in liquid phase autoclave batch reactor in the presence of Smopex-101. Complete glycerol conversion was achieved in the reaction studies even at room temperatures. Effects of reaction temperatures and initial reactant molar ratios on the glycerol conversions and product selectivity were also investigated. The maximum diacetin (77 %) and triacetin (23 %) selectivities were achieved at 363 K and glycerol/acetic acid; 1/12 molar ratio. Acetylation reactions were performed with acetyl chloride in the presence of Smopex-101 in order to increase triacetin selectivity. 66 % triacetin selectivity was achieved in acetylation reaction studies in a period of 1200 minutes at room temperature.