Zeolite Y has an iconic crystal structure, but more importantly, the hydrogen modification zeolite H-Y is the classic example of a solid acid which is used extensively as a catalyst in the oil industry. This metastable compound cannot be synthesized directly, which creates an opportunity to discuss various preparative strategies with the students, such as the three-stage procedure described here. Stage I concerns the hydrothermal synthesis of zeolite Na-Y, followed by ion-exchange with an ammonium acetate solution to form zeolite NH[subscript 4]-Y, and the latter is subsequently converted to zeolite H-Y by thermolysis. Stages II and III may instead be performed using commercially available zeolites, Na-Y and NH[subscript 4]-Y, respectively, which shifts the learning objectives to structural characterization of zeolites. The characterization of the product and intermediate materials gives the students a practical insight into the applicability and limitations of powder X-ray diffraction, solid-state nuclear magnetic resonance spectroscopy, and thermogravimetric analysis, and how these analytical tools complement each other. These aspects make its synthesis and characterization an ideal practical exercise for an upper-level undergraduate laboratory in inorganic or materials chemistry courses. Moreover, the methods and skills learned during this experiment enable the students to tackle more complex zeolites and related framework materials.