Volatile organic compounds (VOCs) have recently received considerable attention for the analysis and monitoring of different biochemical processes in biological systems such as humans, plants, and microorganisms. The advantage of using VOCs to gather information about a specific process is that they can be extracted using different types of samples, even at low concentrations. Therefore, VOC levels represent the fingerprints of specific biochemical processes. The aim of this work was to develop a sensor based on a photoionization detector (PID) and a zeolite layer, used as an alternative analytic separation technique for the analysis of VOCs. The identification of VOCs occurred through the evaluation of the emissive profile during the thermal desorption phase, using a stainless-steel chamber for analysis. Emission profiles were evaluated using a double exponential mathematical model, which fit well if compared with the physical system, describing both the evaporation and diffusion processes. The results showed that the zeolite layer was selective for propionic acid molecules if compared to succinic acid molecules, showing linear behavior even at low concentrations. The process to define the optimal adsorption time between the propionic acid molecules was performed in the range of 5 to 60 min, followed by a thermal desorption process at 100 °C. An investigation of the relationship between the evaporation and diffusion rates showed that the maximum concentration of detected propionic acid molecules occurred in 15 min. Other analyses were performed to study how the concentration of VOCs depended on the desorption temperature and the volume of the analysis chamber. For this purpose, tests were performed using three analysis chambers with volumes of 25 × 10-6, 50 × 10-6, and 150 × 10-6 m3 at three different desorption temperatures of 20 °C, 50 °C, and 100 °C, respectively. The results demonstrated that the evaporation rate of the VOCs increased rapidly with an increasing temperature, while the diffusion rate remained almost constant and was characterized by a slow decay time. The diffusion ratio increased when using a chamber with a larger volume. These results highlight the capabilities of this alternative technique for VOC analysis, even for samples with low concentrations. The coupling of a zeolite layer and a PID improves the detection selectivity in portable devices, demonstrating the feasibility of extending its use to a wide range of new applications.