A new approach for the spectroscopic investigation of non-volatile molecular nanoparticles with diameters in the range between 10 and 100 nm is proposed. The nanoparticles are produced in an electrospray with subsequent solvent evaporation. The number size distribution of the generated aerosol is determined with a scanning mobility particle sizer. Fourier transform infrared spectroscopy is used to study the vibrational dynamics of the nanoparticles. As an example, we have investigated sucrose nanoparticles with six different diameters between 36 and 82 nm. From a comparison with different bulk phase spectra. we conclude that sucrose aerosols are formed in a solid amorphous state.