A two-component undergraduate laboratory experience has been developed by students in a senior level capstone course. The first component is a 3 h laboratory experience dedicated to the rapid synthesis of a metal−organic framework (MOF) in aqueous solution using readily available reagents and equipment. During the second component, this MOF was characterized via a suite of instruments: powder X-ray diffraction (PXRD), thermal gravimetric analysis (TGA), and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). In addition, quantitative 19F{1H} NMR spectroscopy was utilized to quantify the amount of a polyfluoroalkyl substance, adsorbed from solution. The two 3 h laboratory experiences were subsequently deployed in a foundation level inorganic chemistry course. This two-component, multi-instrument lab experience provides students an opportunity to synthesize a modern porous solid and utilize it in an emerging application of MOF science.