In this study, microcapsules containing different contents of different kinds of fragrances and with a regular spherical shape, 2,0–8,0 µm diameter, were synthesized in various core:shell ratios. Mint and cuir fragrances were successfully encapsulated in poly(urea-formaldehyde) (PUF) shell via in-situ polymerization. This was confirmed by optical microscope, scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FTIR) studies. By observation from thermogravimetric analysis (TGA), it was found a relation between thermal gravimetric curves and the amount of fragrance encapsulated, which was later contrasted by ultraviolet-visible spectroscopy. In this way, comparatively, the yield percentage values can be quantitatively defined with a sufficient degree of accuracy by TGA method