Total synthesis of isotopically enriched Si-29 silica NPs as potential spikes for isotope dilution quantification of natural silica NPs

Pálmai, Marcell and Szalay, Roland and Bartczak, Dorota and Varga, Zoltán and Naszályi Nagy, Lívia and Gollwitzer, Christian and Krumrey, Michael and Goenaga-Infante, Heidi (2015) Total synthesis of isotopically enriched Si-29 silica NPs as potential spikes for isotope dilution quantification of natural silica NPs. Journal of Colloid and Interface Science, 445 (1). pp. 161-165. ISSN 0021-9797

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Abstract

A new method was developed for the preparation of highly monodisperse isotopically enriched Si-29 silica nanoparticles (29Si-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 (29Si-TEOS), the silica precursor was prepared in two steps starting from elementary silicon-29 pellets. In the first step Si-29 silicon tetrachloride (29SiCl4) was prepared by heating elementary silicon-29 in chlorine gas stream. By using a multistep cooling system and the dilution of the volatile and moisture-sensitive 29SiCl4 in carbon tetrachloride as inert medium we managed to reduce product loss caused by evaporation. 29Si-TEOS was obtained by treating 29SiCl4 with absolute ethanol. Structural characterisation of 29Si-TEOS was performed by using 1H and 13C 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 X-ray scattering (SAXS), dynamic light scattering (DLS) and zeta potential measurements. Finally, the feasibility of using enriched NPs for on-line field-flow fractionation coupled with multi-angle light scattering and inductively coupled plasma mass spectrometry (FFF/MALS/ICP-MS) has been demonstrated.

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