Metal–organic frameworks (MOFs) have emerged as an important class of porous materials for the flexibility of the combination of inorganic and organic units and their well-characterized structures. The construction of new MOF structures has attracted researchers from various research fields because these crystalline porous materials can be utilized for numerous applications, including gas storage and separation. This chapter describes (i) common techniques for the preparation of MOF materials, (ii) how synthesized MOFs are analyzed to evaluate the materials purity, crystallinity, and porosity, and (iii) in the MOF case studies section, specific procedures showing the same MOF can be produced using different techniques. In addition, recent alternative synthetic procedures including microwave, sonochemical, mechanochemical, electrochemical, and continuous flow synthesis are briefly introduced. In relation to the gas adsorption-related applications, synthetic strategy of MOFs with various morphologies, such as nanoparticles, membranes, monoliths, and pellets, is also discussed.18