UiO-66 particles were synthesized under various synthesis conditions to study the adsorption of carbon dioxide for hydrogen purification. For the purpose, the design and analysis of experiments was performed using statistical design of experiment method. As the synthesis time, temperature and acetic acid amount increased, the crystallinity of UiO-66 particles increased. Especially, the amount of acetic acid was confirmed as an important factor in determining the crystallinity of the particles. The specific surface area of the particles measured by the nitrogen adsorption method also showed a similar tendency. Using the general factor analysis in the experimental design method, the main effects and interactions of major factors were analyzed. In addition, the carbon dioxide adsorption capacity was predicted using a nonlinear regression method. Then, the adsorption performance was shown through surface and contour maps for all ranges.