Volatile organic compounds (VOCs) pose an occupational exposure risk due to their commonplace usage across industrial and vocational sectors. With millions of workers annually exposed, monitoring personal VOC exposures becomes an important task. As such, there is a need to improve current monitoring techniques by increasing sensitivity and reducing analysis costs. Recently, our lab developed a novel, preanalytical technique known as photothermal desorption (PTD). PTD uses pulses of high-energy, visible light to thermally desorb analytes from carbonaceous sorbents, with single-walled carbon nanotube buckypapers (BPs) having the best overall performance. To apply this new technology most effectively for chemical analysis, a better understanding of the theoretical framework of the thermal phenomena behind PTD must be gained. The objectives of the present work were 3-fold: measure the thermal response of BPs during irradiation with light; determine the best method for conducting such measurements; and determine the thermal conductivity of BPs. BPs were exposed to four energy densities, produced by light pulses, ranging from 0.28 to 1.33 J/cm2, produced by a xenon flash lamp. The resulting temperature measurements were obtained via fast response thermocouple (T/C) mounted to BPs by three techniques (pressing, adhering, and embedding). Temperature increase measured by T/C using the adhering and pressing techniques resulted in similar values, 29.2 ± 0.8 to 56 ± 3 °C and 29.1 ± 0.9 to 50 ± 5 °C, respectively, while temperature increase measured by embedding the T/C into the BP showed statistically larger increases ranging from 35.2 ± 0.9 to 76 ± 4 °C. Peak BP temperatures for each mounting technique were also compared with the temperatures generated by the light source, which resulted in embedded BPs demonstrating the most temperature conversion among the techniques (74-86%). Based on these results, embedding T/Cs into the BP was concluded to be the best way to measure BP thermal response during PTD. Additionally, the present work modeled BP thermal conductivity using a steady-state comparative technique and found the material's conductivity to be 10.6 ± 0.6 W/m2. The present work's findings will help pave the way for future developments of the PTD method by allowing calculation of the energy density necessary to attain a desired sorbent temperature and providing a means for comparing BP fabrication techniques and evaluating BP suitability for PTD before conducting PTD trials with analytes of interest. Sorbents with greater thermal conductivity are expected to desorb more evenly and withstand higher energy density exposures.