Nanomaterial application has been recognized as a most important future development for nanomaterial production industries. However, harmful toxic pollutants, especially nanoparticles, could also be produced in the process. Therefore, there is a need to evaluate control technologies by generating monodisperse nanoparticles for experimental purposes. In this research project, atomization and vaporization-condensation technologies were applied to generate solid (NaCl) and liquid (oleic acid) polydisperse particles. A differential mobility analyzer (DMA) was utilized to segregate and produce test nanoparticles. In the generation of polydisperse particles, the geometric standard deviation (GSD) and total number concentration (NC) of NaCl particles segregated from various NaCl(aq) concentration were 1.59−1.89 and 8.47 × 105 − 4.2 × 106 #/cm3. Results show that as NaCl(aq) concentration increases, GSD also increase. However, there is a logarithm relation (y = 2 × 106 Ln(x) + 2 × 106) between NaCl(aq) concentration and NC. For polydisperse oleic acid particles, GSDs and NC of particles segregated from various furnace temperatures are 1.43−1.65 and 7.12 × 105 − 5.35 × 106 #/cm3, respectively. GSDs and NC of oleic acid particles generated from various carrier gas flow are 1.41−1.63 and 7.31×106 − 9.42 × 106 #/cm3, respectively. Furnace temperature and NC are a logarithm relation. Carrier gas flow and NC is a polynomial function. GSD varies as furnace temperature and carrier gas flow increase. Monodisperse nanoparticles were successfully generated from the atomization of 0.5% NaCl(aq) and oleic acid. The GSD, count median diameter (CMD), and total number concentration (NC) NaCl particles segregated from various DMA voltages were 1.04 − 1.08 and 8.33 nm − 128 nm, and 9.89 × 102 − 2.67 × 105 #/cm3, respectively. The GSD, CMD, and total NC of monodisperse oleic acid particles produced from various DMA voltages were 1.04 − 1.06, 8.9 nm − 92.5 nm, and 2.4 × 104 − 7.6 × 105 #/cm3, respectively.