Reported herein is a chemistry experiment integrating polymer chemistry and instrumental analysis for the juniors majoring in chemistry. This experiment has a different scheduling framework than traditional experiments with a fixed lab period and schedule. The students arrange their experiment flexibly and individually. Styrene maleic anhydride copolymer (SMA) was used to stabilize hexadecanol emulsion, followed by microencapsulation through in situ polymerization of formaldehyde-melamine. The obtained microcapsules are characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC), and gas chromatography (GC). This experiment enables the students to understand the concepts of polymeric surfactant, condensation reaction, and in situ polymerization. Furthermore, this experiment is beneficial to cultivate their practical ability of handling modern instruments. The flexibility and versatility significantly enhance the applicability of this experiment and the likelihood of widespread adaptation.