A new method was developed for the preparation of highly monodisperse isotopically enriched Si-29 silica nanoparticles ( 29 Si-silica NPs) with the purpose of using them as spikes for isotope dilution mass spectrometry (IDMS) quantification of silica NPs with natural isotopic distribution. Si-29 tetraethyl orthosilicate ( 29 Si-TEOS), the silica precursor was prepared in two steps starting from elementary silicon-29 pellets. In the first step Si-29 silicon tetrachloride ( 29 SiCl 4 ) was prepared by heating elementary silicon-29 in chlorine gas stream. By using a multistep cooling system and the dilution of the volatile and moisturesensitive 29 SiCl 4 in carbon tetrachloride as inert medium we managed to reduce product loss caused by evaporation. 29 Si-TEOS was obtained by treating 29 SiCl 4 with absolute ethanol.Structural characterisation of 29 Si-TEOS was performed by using 1 H and 13 C nuclear magnetic resonance (NMR) spectroscopy and Fourier-transform infrared (FTIR) spectroscopy. For the NP preparation, a basic amino acid catalysis route was used and the resulting NPs were analysed using transmission electron microscopy (TEM), small angle Xray scattering (SAXS), dynamic light scattering (DLS) and zeta potential measurements.