An undergraduate practical exercise has been designed to provide hands-on, instrument-based experience of advanced characterization techniques. A research experience approach is taken, centered around the concept of solid-state polymorphism, which requires a detailed knowledge of molecular and crystal structure to be gained by advanced analytical techniques normally considered as the preserve of a research facility. Powder and single crystal diffraction techniques are primarily required and implemented via the unique approach of the students themselves using benchtop instruments dedicated to teaching, as opposed to more complex and difficult to access research instruments. Furthermore, the manual instructions for performing the practical are delivered via an adapted Electronic Laboratory Notebook system where, for each specific aspect of the practical, students note their intentions, actions, observations, and inferences. Assessors can access the notebooks and provide targeted online feedback for each individual section. Evaluation of the approach is based on interviews and surveys with the first cohort of 65 students that performed the practical.