Integrating Flow Imaging Analysis and Single-Particle ICP-TOFMS for Comprehensive Micro- and Nanoplastic Characterization

Sarah E Szakas; Lyndsey Hendriks; Gunda Koellensperger; Benjamin T Manard

doi:10.1021/acs.analchem.6c02328

Integrating Flow Imaging Analysis and Single-Particle ICP-TOFMS for Comprehensive Micro- and Nanoplastic Characterization

Sarah E Szakas (Corresponding author)
, Lyndsey Hendriks
, Gunda Koellensperger
, Benjamin T Manard (Corresponding author)

Department of Analytical Chemistry

Publications: Contribution to journal › Article › Peer Reviewed

Abstract

Flow imaging analysis (FIA), provides composition-agnostic morphological characterization. These measurements of particle size and shape are valuable to mass-based analysis, such as single particle inductively coupled plasma time-of-flight mass spectrometry (sp-ICP-TOFMS), which provides quantitative data on elements within particles. Using these two methods together enables informed use of geometric assumptions required by sp-ICP-TOFMS, as particle mass is typically converted to a particle diameter using assumed-spherical geometry. To validate this concept, parallel measurements to determine particle diameters were performed by FIA and sp-ICP-TOFMS on four particle suspensions: 300 nm polystyrene Eu-doped nanoparticles, 1 μm Fe-rich beads, 3 μm four element calibration polystyrene beads and 5 μm polystyrene beads. The Fe-particles obtained the highest percent difference from the manufacturer's nominal diameter, as the mean diameter obtained by FIA was overestimated by 21% and sp-ICP-TOFMS underestimated the mean diameter by 20.7%. Two types of particles were selected to test the effect of varying the particle number concentrations (PNC) on sizing accuracy, and both methods accurately sized each particle population at the PNC expected. Single particle analysis of carbon has continued to be a popular research topic, with direct applications to environmental pollutants in terms of nano- and micro- plastics. Real-world plastic particles were studied, and FIA's measured circularity values demonstrated that the particles deviated from spherical geometries, therefore sp-ICP-TOFMS data should be interpreted as mass-based rather than size-based. Combining these techniques enables improved interpretation of particle populations and evaluation of particle sizes.

Original language	English
Pages (from-to)	24200-24214
Number of pages	15
Journal	Analytical Chemistry
Volume	98
Issue number	33
DOIs	https://doi.org/10.1021/acs.analchem.6c02328
Publication status	Published - 25 Aug 2026

Funding

This project partially received funding from FWF Cluster of Excellence COE 17, Circular Bioengineering (Funding DOI: 10.55776/COE17). For open access purposes, the author has applied a CC BY public copyright license to any author accepted manuscript version arising from this submission. This work was supported by the Laboratory Directed Research and Development Program of Oak Ridge National Laboratory, managed by UT-Battelle, LLC, for the United States Department of Energy, under contract DE-AC05-000R22725. This work was funded by the United States National Nuclear Security Administration's (NNSA) Office of Defense Nuclear Nonproliferation Research and Development. The authors would like to also acknowledge Jacquelyn DeMink (ORNL) for the assistance with graphics. The authors thank Ocean Cleanup, in particular Matthias Egger, for providing the ocean-weathered plastic materials used in this study. The authors also acknowledge Maximilian Meyndl and the Core Facility "Interface Characterization" from the Institute of Materials Chemistry and Research, of the University of Vienna, for providing the facilities and equipment required for the cryomilling of the samples.

Funders	Funder number
Thomas Jefferson National Accelerator Facility	DE-AC05-000R22725
Fonds zur Förderung der wissenschaftlichen Forschung (FWF)	10.55776/COE17

Austrian Fields of Science 2012

104002 Analytical chemistry

Access to Document

10.1021/acs.analchem.6c02328

Cite this

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title = "Integrating Flow Imaging Analysis and Single-Particle ICP-TOFMS for Comprehensive Micro- and Nanoplastic Characterization",

abstract = "Flow imaging analysis (FIA), provides composition-agnostic morphological characterization. These measurements of particle size and shape are valuable to mass-based analysis, such as single particle inductively coupled plasma time-of-flight mass spectrometry (sp-ICP-TOFMS), which provides quantitative data on elements within particles. Using these two methods together enables informed use of geometric assumptions required by sp-ICP-TOFMS, as particle mass is typically converted to a particle diameter using assumed-spherical geometry. To validate this concept, parallel measurements to determine particle diameters were performed by FIA and sp-ICP-TOFMS on four particle suspensions: 300 nm polystyrene Eu-doped nanoparticles, 1 μm Fe-rich beads, 3 μm four element calibration polystyrene beads and 5 μm polystyrene beads. The Fe-particles obtained the highest percent difference from the manufacturer's nominal diameter, as the mean diameter obtained by FIA was overestimated by 21\% and sp-ICP-TOFMS underestimated the mean diameter by 20.7\%. Two types of particles were selected to test the effect of varying the particle number concentrations (PNC) on sizing accuracy, and both methods accurately sized each particle population at the PNC expected. Single particle analysis of carbon has continued to be a popular research topic, with direct applications to environmental pollutants in terms of nano- and micro- plastics. Real-world plastic particles were studied, and FIA's measured circularity values demonstrated that the particles deviated from spherical geometries, therefore sp-ICP-TOFMS data should be interpreted as mass-based rather than size-based. Combining these techniques enables improved interpretation of particle populations and evaluation of particle sizes.",

author = "Szakas, \{Sarah E\} and Lyndsey Hendriks and Gunda Koellensperger and Manard, \{Benjamin T\}",

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