Time-resolved photoluminescence spectroscopy (TRPS) shows potential as a sensitive, nondestructive, high throughput, label-free laser-based spectroscopy technique capable of analysing low concentrations of organic species adsorbed on and within zeolite pores. Here we report the results from a study that uses TRPS to characterise photoluminescence (PL) arising from synthesised chabazite framework zeolites at three different stages of the detemplation process (from an uncalcined, partially calcined, and calcined zeolite). Temporal resolution was used to demonstrate the steric confinement effects of OSDA within a zeolite framework and therefore to establish a signature region for determining the presence of the template. Gated spectra comparisons between an uncalcined and a partially calcined zeolite demonstrated the presence of template alongside the proliferation of template-derived combustion products. An analysis of lifetime values demonstrated the ability for TRPS to track depletion of OSDA and establish a characteristic PL spectrum for a clean zeolite. The sensitivity of the technique is high enough to reveal that there is still residual organic material remaining in a zeolite even after an extended thermal detemplation process.