Upon dispersant-assisted exfoliation, pristine carbon nanotubes (CNTs) are divided between the supernatant and precipitate, which makes the determination of dispersant concentration a challenging task. We have developed a thermogravimetric-spectroscopy-based approach to accurately determine the dispersant-assisted CNT (or nanoparticles, in general) concentration in dispersion. A thermogravimetric analysis of the filtered and washed precipitate, that is usually discarded after centrifugation, is used here to accurately calculate the CNT mass in the precipitate and (through mass-balance) its mass in the supernatant. Once the true CNT concentration has been determined, a conventional spectroscopy-based concentration calibration plot is constructed for simple and swift use in further concentration measurements. Such true concentration analysis is crucial for studying the concentration–property relationship.