A systematic evaluation of Flow Field Flow Fractionation and single-particle ICP-MS to obtain the size distribution of organo-mineral iron oxyhydroxide colloids

Claudia Moens, Nadia Waegeneers, Andreas Fritzsche, Peter Nobels, Erik Smolders

Research output: Contribution to journalArticleAcademicpeer-review

Abstract

Colloidal iron(III)oxyhydroxides (FeOx)are important reactive adsorbents in nature. This study was set up to determine the size of environmentally relevant FeOx colloids with new methods, i.e. Flow Field Flow Fractionation (FlFFF-UV-ICP-MS)and single-particle ICP-MS/MS (sp-ICP-MS)and to compare these with standard approaches, i.e. dynamic light scattering (DLS), nanoparticle tracking analysis (NTA), microscopy (TEM), membrane filtration, centrifugation and dialysis. Seven synthetic nano- and submicron FeOx with different mineralogy and coating were prepared and two soil solutions were included. The FlFFF was optimized for Fe recovery, yielding 70–90%. The FlFFF determines particle size with high resolution in a 1 mM NH 4 HCO 3 (pH 8.3)background and can detect Fe-NOM complexes <5 nm and organo-mineral FeOx particles ranging 5–300 nm. The sp-ICP-MS method had a size detection limit for FeOx of about 32–47 nm. The distribution of hydrodynamic diameters of goethite particles detected with FlFFF, NTA and DLS were similar but the values were twice as large as the Fe cores of particles detected with sp-ICP-MS and TEM. Conventional fractionation by centrifugation and dialysis generally yielded similar fractions as FlFFF but membrane filtration overestimated the large size fractions. Particles formed from Fe(II)oxidation in the presence of NOM showed strikingly smaller organo-mineral Fe-Ox colloids as the NOM/Fe ratio increased. The soil solution obtained with centrifugation of an acid peat was dominated by small (<30 nm)Fe-OM complexes and organo-mineral FeOx colloids whereas that of a mineral pH neutral soil mainly contains larger (30–200 nm)Fe-rich particles. The FlFFF-UV-ICP-MS is recommended for environmental studies of colloidal FeOx since it has a wide size detection range, it fractionates in an environmentally relevant background (1 mM NH 4 HCO 3 )and it has acceptable element recoveries.

Original languageEnglish
Pages (from-to)203-214
JournalJournal of Chromatography A
Volume1599
Early online date15 Apr 2019
DOIs
Publication statusPublished - 16 Aug 2019

Fingerprint

Field Flow Fractionation
Colloids
Fractionation
Minerals
Centrifugation
Flow fields
Soil
Dialysis
Dynamic light scattering
Soils
Nanoparticles
Transmission electron microscopy
Membranes
Recovery
Peat
Mineralogy
Hydrodynamics
Particle Size
Adsorbents
Limit of Detection

Keywords

  • Flow Field Flow Fractionation
  • Multimethod comparison
  • Organo-mineral iron oxyhydroxide colloids
  • Particle size distribution
  • Single-particle inductively coupled plasma-mass spectrometry
  • Triple quadrupole mass spectrometry

Cite this

@article{741635469e7b486e90da9fde62dc804b,
title = "A systematic evaluation of Flow Field Flow Fractionation and single-particle ICP-MS to obtain the size distribution of organo-mineral iron oxyhydroxide colloids",
abstract = "Colloidal iron(III)oxyhydroxides (FeOx)are important reactive adsorbents in nature. This study was set up to determine the size of environmentally relevant FeOx colloids with new methods, i.e. Flow Field Flow Fractionation (FlFFF-UV-ICP-MS)and single-particle ICP-MS/MS (sp-ICP-MS)and to compare these with standard approaches, i.e. dynamic light scattering (DLS), nanoparticle tracking analysis (NTA), microscopy (TEM), membrane filtration, centrifugation and dialysis. Seven synthetic nano- and submicron FeOx with different mineralogy and coating were prepared and two soil solutions were included. The FlFFF was optimized for Fe recovery, yielding 70–90{\%}. The FlFFF determines particle size with high resolution in a 1 mM NH 4 HCO 3 (pH 8.3)background and can detect Fe-NOM complexes <5 nm and organo-mineral FeOx particles ranging 5–300 nm. The sp-ICP-MS method had a size detection limit for FeOx of about 32–47 nm. The distribution of hydrodynamic diameters of goethite particles detected with FlFFF, NTA and DLS were similar but the values were twice as large as the Fe cores of particles detected with sp-ICP-MS and TEM. Conventional fractionation by centrifugation and dialysis generally yielded similar fractions as FlFFF but membrane filtration overestimated the large size fractions. Particles formed from Fe(II)oxidation in the presence of NOM showed strikingly smaller organo-mineral Fe-Ox colloids as the NOM/Fe ratio increased. The soil solution obtained with centrifugation of an acid peat was dominated by small (<30 nm)Fe-OM complexes and organo-mineral FeOx colloids whereas that of a mineral pH neutral soil mainly contains larger (30–200 nm)Fe-rich particles. The FlFFF-UV-ICP-MS is recommended for environmental studies of colloidal FeOx since it has a wide size detection range, it fractionates in an environmentally relevant background (1 mM NH 4 HCO 3 )and it has acceptable element recoveries.",
keywords = "Flow Field Flow Fractionation, Multimethod comparison, Organo-mineral iron oxyhydroxide colloids, Particle size distribution, Single-particle inductively coupled plasma-mass spectrometry, Triple quadrupole mass spectrometry",
author = "Claudia Moens and Nadia Waegeneers and Andreas Fritzsche and Peter Nobels and Erik Smolders",
year = "2019",
month = "8",
day = "16",
doi = "10.1016/j.chroma.2019.04.032",
language = "English",
volume = "1599",
pages = "203--214",
journal = "Journal of Chromatography. A, Including electrophoresis and other separation methods",
issn = "0021-9673",
publisher = "Elsevier",

}

A systematic evaluation of Flow Field Flow Fractionation and single-particle ICP-MS to obtain the size distribution of organo-mineral iron oxyhydroxide colloids. / Moens, Claudia; Waegeneers, Nadia; Fritzsche, Andreas; Nobels, Peter; Smolders, Erik.

In: Journal of Chromatography A, Vol. 1599, 16.08.2019, p. 203-214.

Research output: Contribution to journalArticleAcademicpeer-review

TY - JOUR

T1 - A systematic evaluation of Flow Field Flow Fractionation and single-particle ICP-MS to obtain the size distribution of organo-mineral iron oxyhydroxide colloids

AU - Moens, Claudia

AU - Waegeneers, Nadia

AU - Fritzsche, Andreas

AU - Nobels, Peter

AU - Smolders, Erik

PY - 2019/8/16

Y1 - 2019/8/16

N2 - Colloidal iron(III)oxyhydroxides (FeOx)are important reactive adsorbents in nature. This study was set up to determine the size of environmentally relevant FeOx colloids with new methods, i.e. Flow Field Flow Fractionation (FlFFF-UV-ICP-MS)and single-particle ICP-MS/MS (sp-ICP-MS)and to compare these with standard approaches, i.e. dynamic light scattering (DLS), nanoparticle tracking analysis (NTA), microscopy (TEM), membrane filtration, centrifugation and dialysis. Seven synthetic nano- and submicron FeOx with different mineralogy and coating were prepared and two soil solutions were included. The FlFFF was optimized for Fe recovery, yielding 70–90%. The FlFFF determines particle size with high resolution in a 1 mM NH 4 HCO 3 (pH 8.3)background and can detect Fe-NOM complexes <5 nm and organo-mineral FeOx particles ranging 5–300 nm. The sp-ICP-MS method had a size detection limit for FeOx of about 32–47 nm. The distribution of hydrodynamic diameters of goethite particles detected with FlFFF, NTA and DLS were similar but the values were twice as large as the Fe cores of particles detected with sp-ICP-MS and TEM. Conventional fractionation by centrifugation and dialysis generally yielded similar fractions as FlFFF but membrane filtration overestimated the large size fractions. Particles formed from Fe(II)oxidation in the presence of NOM showed strikingly smaller organo-mineral Fe-Ox colloids as the NOM/Fe ratio increased. The soil solution obtained with centrifugation of an acid peat was dominated by small (<30 nm)Fe-OM complexes and organo-mineral FeOx colloids whereas that of a mineral pH neutral soil mainly contains larger (30–200 nm)Fe-rich particles. The FlFFF-UV-ICP-MS is recommended for environmental studies of colloidal FeOx since it has a wide size detection range, it fractionates in an environmentally relevant background (1 mM NH 4 HCO 3 )and it has acceptable element recoveries.

AB - Colloidal iron(III)oxyhydroxides (FeOx)are important reactive adsorbents in nature. This study was set up to determine the size of environmentally relevant FeOx colloids with new methods, i.e. Flow Field Flow Fractionation (FlFFF-UV-ICP-MS)and single-particle ICP-MS/MS (sp-ICP-MS)and to compare these with standard approaches, i.e. dynamic light scattering (DLS), nanoparticle tracking analysis (NTA), microscopy (TEM), membrane filtration, centrifugation and dialysis. Seven synthetic nano- and submicron FeOx with different mineralogy and coating were prepared and two soil solutions were included. The FlFFF was optimized for Fe recovery, yielding 70–90%. The FlFFF determines particle size with high resolution in a 1 mM NH 4 HCO 3 (pH 8.3)background and can detect Fe-NOM complexes <5 nm and organo-mineral FeOx particles ranging 5–300 nm. The sp-ICP-MS method had a size detection limit for FeOx of about 32–47 nm. The distribution of hydrodynamic diameters of goethite particles detected with FlFFF, NTA and DLS were similar but the values were twice as large as the Fe cores of particles detected with sp-ICP-MS and TEM. Conventional fractionation by centrifugation and dialysis generally yielded similar fractions as FlFFF but membrane filtration overestimated the large size fractions. Particles formed from Fe(II)oxidation in the presence of NOM showed strikingly smaller organo-mineral Fe-Ox colloids as the NOM/Fe ratio increased. The soil solution obtained with centrifugation of an acid peat was dominated by small (<30 nm)Fe-OM complexes and organo-mineral FeOx colloids whereas that of a mineral pH neutral soil mainly contains larger (30–200 nm)Fe-rich particles. The FlFFF-UV-ICP-MS is recommended for environmental studies of colloidal FeOx since it has a wide size detection range, it fractionates in an environmentally relevant background (1 mM NH 4 HCO 3 )and it has acceptable element recoveries.

KW - Flow Field Flow Fractionation

KW - Multimethod comparison

KW - Organo-mineral iron oxyhydroxide colloids

KW - Particle size distribution

KW - Single-particle inductively coupled plasma-mass spectrometry

KW - Triple quadrupole mass spectrometry

U2 - 10.1016/j.chroma.2019.04.032

DO - 10.1016/j.chroma.2019.04.032

M3 - Article

VL - 1599

SP - 203

EP - 214

JO - Journal of Chromatography. A, Including electrophoresis and other separation methods

JF - Journal of Chromatography. A, Including electrophoresis and other separation methods

SN - 0021-9673

ER -