College chemistry faculties might not have considered including isothermal titration calorimetry (ITC) in their majors' curriculum because experimental data from this instrumental method are often analyzed via automation (software). However, the software-based data analysis can be replaced with a spreadsheet-based analysis that is readily accessible to undergraduate students. This article describes a three-phase study (three lab periods) of cation-hexametaphosphate complexation via ITC, including the asymptote method by which students perform their own ITC data analysis, to demonstrate how ITC experiments can provide students with critical thinking opportunities comparable to other data-analysis-intensive physical-analytical experiments.