A three-tiered experiment for undergraduate Instrumental Analysis students is presented in which students characterize the solid-state thermal behavior of an active pharmaceutical ingredient (acetaminophen) and excipient (a-lactose hydrate) using differential scanning calorimetry, thermogravimetric analysis, and thermal microscopy. Students are required to perform qualitative and quantitative analysis, incorporating data from the three thermal analysis techniques to successfully interpret melting, decomposition, and dehydration thermal transitions. Students use thermal analysis software to determine transition temperatures and enthalpies of transitions, and use stoichiometric calculations to calculate the water of hydration.