Air pollution with particulate matter from transport sources is a serious problem in terms of air quality and its impact on human health. The article attempts to test the emitted particles from piston engines in terms of their physical properties and chemical composition. The research test objects were a diesel engine with Euro 5 emission class and a petrol engine, which was a part of the scooter drive system. The conducted research consisted in the analysis of the number, mass, and volume of particles, as well as chemical analysis, using the methods: Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscope with Energy Dispersive Spectroscopy (SEM-EDS), and Evolved gas analysis (EGA). The diesel engine emitted particles in the range of 50–120 nm. With the increase in the engine load, the specific emission of particulate matter increased. In the case of a gasoline engine running without load, the emission of particles smaller than 30 nm was mainly observed. Increasing load of the gasoline engine resulted in an increase in both the concentration of particles and their diameter (average diameter to 90 nm). FTIR analysis showed higher black carbon content in the case of the sample taken from the diesel engine. In order to carry out a more detailed chemical analysis, the EGA and SEM methods were used. On their basis, the chemical composition of particles was presented, and a greater ability to agglomerate of a gasoline engine particles was found.