Rutile TiO2 was prepared by microwave calcination of metatitanic acid. A quadratic regression model for the conversion to rutile TiO2 was developed by response surface methodology (RSM), to investigate the effects of the calcination temperature, the calcination time, the sample mass, and their interactions on the conversion rates. Within the scope of the experiments, only the calcination temperature and time had significant effects on the rutile TiO2 conversion. Under the optimized conditions (866โยฐC, 61โmin, 58โg), the predicted rutile TiO2 conversion was 99.91โ%, approaching the actual conversion (99.44โ%). Thus, the optimization by RSM of microwave calcination of metatitanic acid for the preparation of rutile TiO2 is a feasible approach to achieving a more efficient TiO2 production process.