Experimental design is utilized to detect the effect of parameters on the process of hydrogen production. Thanks to experimental design methods, time and money consumption can be decreased. In addition to that, decreasing hazardous solvent and chemical consumption is crucial to the green chemistry approach. Regarding the synthesis of MOFs, solvents like methanol and expensive chemicals like imidazole salt are needed. In addition to that, after MOF synthesis, there are many more steps, like collecting crystals and drying them. Analysis of covariance (ANCOVA) is one of the experimental design tools. ANCOVA is formed from the fusion of two statistical methods, which are analysis of variance (ANOVA) and regression analysis. For this analysis, it is necessary to select one independent variable as a factor. At this time, other independent variables are called covariates. ANCOVA can be applied in various fields like medicine, agriculture, biology, and engineering. For the reaction producing H₂ from NaBH₄ hydrolysis, the researchers used response surface methodology (RSM) and ANOVA. To the best of the authors' knowledge, there is scarce research about the optimization of H₂ production from the NaBH4 hydrolysis reaction with ANCOVA. This study aimed to determine the effect of several parameters (catalyst amount, time, reactant amount) on hydrogen yield from NaBH₄ hydrolysis on several MOFs used in the literature.