As an outcome of multidiscipline integration, the polymeric surfactant is of growing importance in modern industry and scientific research. However, the instructional introduction on polymeric surfactants is still insufficient in universities nowadays. In order to effectively guide undergraduates to study polymeric surfactant, a new polymeric surfactant, poly(acrylic acid-co-octadecyl acrylate), was designed and synthesized by copolymerization between acrylic acid and octadecyl acrylate. Moreover, its surface activity and rheological performance were also analyzed by contact angle meter, laser scanning confocal microscope, polarizing microscope, and rotary rheometer. Generally, as a combination of the hands-on exercise with theoretical lecture, this laboratory experiment enabled students to understand the key concepts and chemical nature of polymeric surfactants in depth. In addition, the ability to incorporate multidiscipline concepts into the practical issues students must solve was also cultivated by this exercise.