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

Marcell Pálmai, Roland Szalay, Dorota Bartczak, Zoltán Varga, Lívia Naszályi Nagy, Christian Gollwitzer, Michael Krumrey, Heidi Goenaga-Infante

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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.

Original languageEnglish
Pages (from-to)161-165
Number of pages5
JournalJournal of colloid and interface science
Publication statusPublished - May 1 2015



  • Asymmetric flow field-flow fractionation (AF4)
  • ICP-MS
  • SAXS
  • Si-29 silica nanoparticles
  • Si-29 tetraethyl orthosilicate

ASJC Scopus subject areas

  • Electronic, Optical and Magnetic Materials
  • Biomaterials
  • Surfaces, Coatings and Films
  • Colloid and Surface Chemistry

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