The scope of the study involves identifying the optimal means to effectively use the electrospinning technique to obtain pumice-containing nanofibers. Nanofiber containing pumice in a solution was electrospun to obtain smooth, cylindrical, bead-free, and ultrafine nanomaterials. The study also analyzed the molecular [Fourier transform infrared spectroscopy (FTIR)], thermal [differential scanning calorimetry (DSC)], zeta potential, size, polydispersity index [dynamic light scattering (DLS)], and surface [scanning electron microscope (SEM)] parameters of the pumice-containing nanofibers having JP6 (applied voltage: 6 kV) and JP12 (12 kV) properties. While the distance (10 cm), flow rate (0.8 mL/h), and other parameters of the electrospinning process were fixed, two different voltages were applied to obtain the pumice-containing nanofiber. The average diameter of the nanoencapsulated pumice produced at 6 kV was defined as 98.6 nm in gelatin nanomats with 31.8 nm. The average diameter of the nanocapsule pumice produced under a 12 kV voltage was found to be 85.8 nm, and the average diameter of the nanomats (non–nanoencapsulated) was 35.2 nm. The average zeta potential values of the pumice-containing nanofiber were also determined in the nanosize range. The JP6 and JP12 PDI values were determined as 0.165 and 0.566, respectively. Peaks characteristic of pumices as defined in the literature were observed in the FTIR results, while DSC analysis results revealed strong endo- and exothermic peaks. As a result of this study, it has been proved that pumice can be reduced to nanosize with the electrospinning technique and it is nanoencapsulated in nanofiber. When the obtained pumice-containing nanofiber was examined, it was determined that the surface area of the nanofiber was large and resistant to thermal heat.