Reported herein is a multidisciplinary laboratory experiment for advanced undergraduate students that includes elements of material synthesis, in the synthesis of cyclodextrin-containing metal-organic frameworks (CD-MOFs), and environmental chemistry, in the use of these MOFs for pollutant removal. This multiday laboratory experiment starts with the synthesis of cyclodextrin-containing metal-organic frameworks (CD-MOFs) using vapor diffusion crystal growth procedures, followed by the use of the CD-MOFs for a pollutant removal application. Specifically, the CD-MOFs were used for the removal of a methylene blue dye (a common mimic of aromatic pollutants) from an organic solution, with the monitoring of the success of the removal procedures using UV-vis spectroscopy. This experiment was implemented as part of a larger multiday unit, and undergraduate students were particularly engaged with and excited by the CD-MOF synthesis and methylene blue removal experimental modules. As a result, the decision was made to make these two components a stand-alone multidisciplinary laboratory experiment, the results of which are reported herein.