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

doi:10.1016/j.jcis.2014.12.085

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 journal › Article › peer-review

11 Scopus citations

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.

Original language	English (US)
Pages (from-to)	161-165
Number of pages	5
Journal	Journal of Colloid And Interface Science
Volume	445
DOIs	https://doi.org/10.1016/j.jcis.2014.12.085
State	Published - May 1 2015
Externally published	Yes

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.

Keywords

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

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10.1016/j.jcis.2014.12.085

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@article{3a77e37b58fc48eda15feb25ecb03716,

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

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.",

keywords = "Asymmetric flow field-flow fractionation (AF4), ICP-MS, SAXS, Si-29 silica nanoparticles, Si-29 tetraethyl orthosilicate",

author = "Marcell P{\'a}lmai and Roland Szalay and Dorota Bartczak and Zolt{\'a}n Varga and Nagy, {L{\'i}via Nasz{\'a}lyi} and Christian Gollwitzer and Michael Krumrey and Heidi Goenaga-Infante",

note = "Funding Information: The authors are greatly indebted to Ter{\'e}z Kiss for TEM images and Judith Mih{\'a}ly 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: {\textcopyright} 2015 Elsevier Inc.",

year = "2015",

month = may,

day = "1",

doi = "10.1016/j.jcis.2014.12.085",

language = "English (US)",

volume = "445",

pages = "161--165",

journal = "Journal of Colloid And Interface Science",

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T1 - Total synthesis of isotopically enriched Si-29 silica NPs as potential spikes for isotope dilution quantification of natural silica NPs

AU - Pálmai, Marcell

AU - Szalay, Roland

AU - Bartczak, Dorota

AU - Varga, Zoltán

AU - Nagy, Lívia Naszályi

AU - Gollwitzer, Christian

AU - Krumrey, Michael

AU - Goenaga-Infante, Heidi

N1 - 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.

PY - 2015/5/1

Y1 - 2015/5/1

N2 - 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.

AB - 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.

KW - Asymmetric flow field-flow fractionation (AF4)

KW - ICP-MS

KW - SAXS

KW - Si-29 silica nanoparticles

KW - Si-29 tetraethyl orthosilicate

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DO - 10.1016/j.jcis.2014.12.085

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SN - 0021-9797

VL - 445

SP - 161

EP - 165

JO - Journal of Colloid And Interface Science

JF - Journal of Colloid And Interface Science

ER -

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

Abstract

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