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Interfacial solar vapor generation has recently drawn much attention because of its high solar-to-vapor generation efficiency. Here we introduce the basic experimental procedures and analysis for undergraduates to perform such an experiment to catch up with the cutting-edge research wave. Interfacial solar vapor generation employs an interfacial solar vapor generator to localize the solar harvest and the vapor generation process at the air–water interface. In the experiment, three commonly seen black materials, namely, a black trash bag, carbon fabric, and black packing polyester, are used as the basic starting materials for the construction of solar vapor generators. The light absorption properties are measured with UV–vis spectroscopy, and the solar vapor generation efficiencies are obtained using the data collected with an electronic balance and thermometers. Overall, this experiment aims to introduce undergraduate students in chemistry, environmental science, textiles, geoscience, materials science, or engineering to a cutting-edge technology in solar energy conversion, environmental protection, and clean water access.