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

Research output: Contribution to journalArticlepeer-review

11 Scopus citations


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 (US)
Pages (from-to)161-165
Number of pages5
JournalJournal of Colloid And Interface Science
StatePublished - May 1 2015
Externally publishedYes

Bibliographical note

Funding Information:
The authors are greatly indebted to Teréz Kiss for TEM images and Judith Mihály for FTIR experiments. This work was funded by the European Metrology Research Programme (EMRP) under the Joint Research Project NEW03 (NanoChOp). The EMRP is jointly funded by the EMRP participating countries within EURAMET and the European Union.

Publisher Copyright:
© 2015 Elsevier Inc.


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


Dive into the research topics of 'Total synthesis of isotopically enriched Si-29 silica NPs as potential spikes for isotope dilution quantification of natural silica NPs'. Together they form a unique fingerprint.

Cite this