Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods

Dmitri Ciornii; Vasile Dan Hodoroaba; Nizar Benismail; Alina Maltseva; Juan F. Ferrer; Jiamin Wang; Raquel Parra; Ronan Jézéquel; Justine Receveur; Dina Gabriel; Andreas Scheitler; Christa van Oversteeg; Jorg Roosma; Alex van Renesse van Duivenbode; Tim Bulters; Michela Zanella; Alessandro Perini; Federico Benetti; Dora Mehn; Georg Dierkes; Michael Soll; Takahisa Ishimura; Marius Bednarz; Guyu Peng; Lars Hildebrandt; Mathias Peters; Seung Kyu Kim; Jochen Türk; Felix Steinfeld; Jaehak Jung; Sanghee Hong; Eun Ju Kim; Hye Weon Yu; Sven Klockmann; Christoph Krafft; Julia Süssmann; Shan Zou; Alexandra ter Halle; Andrea M. Giovannozzi; Alessio Sacco; Marta Fadda; Mara Putzu; Dong Hoon Im; Nontete Nhlapo; Priscilla Carrillo-Barragán; Natascha Schmidt; Dorte Herzke; Alessio Gomiero; Adrián Jaén-Gil; Damien J.E. Cabanes; Martin Doedt; Vitor Cardoso; Antje Schmitz; Moritz Hawly; Huajuan Mo; Justine Jacquin; Andy Mechlinski; Gbotemi A. Adediran; Jose Andrade; Soledad Muniategui-Lorenzo; Anja Ramsperger; Martin G.J. Löder; Christian Laforsch; Tanja Cirkovic Velickovic; Daniele Fabbri; Irene Coralli; Stefania Federici; Barbara M. Scholz-Böttcher; Jacopo la Nasa; Greta Biale; Cassandra Rauert; Elvis D. Okoffo; Anna Undas; Lihui An; Volker Wachtendorf; Petra Fengler; Korinna Altmann

doi:10.1021/acs.analchem.4c05403

Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods

Dmitri Ciornii, Vasile Dan Hodoroaba, Nizar Benismail, Alina Maltseva, Juan F. Ferrer, Jiamin Wang, Raquel Parra, Ronan Jézéquel, Justine Receveur, Dina Gabriel, Andreas Scheitler, Christa van Oversteeg, Jorg Roosma, Alex van Renesse van Duivenbode, Tim Bulters, Michela Zanella, Alessandro Perini, Federico Benetti, Dora Mehn, Georg DierkesMichael Soll, Takahisa Ishimura, Marius Bednarz, Guyu Peng, Lars Hildebrandt, Mathias Peters, Seung Kyu Kim, Jochen Türk, Felix Steinfeld, Jaehak Jung, Sanghee Hong, Eun Ju Kim, Hye Weon Yu, Sven Klockmann, Christoph Krafft, Julia Süssmann, Shan Zou, Alexandra ter Halle, Andrea M. Giovannozzi, Alessio Sacco, Marta Fadda, Mara Putzu, Dong Hoon Im, Nontete Nhlapo, Priscilla Carrillo-Barragán, Natascha Schmidt, Dorte Herzke, Alessio Gomiero, Adrián Jaén-Gil, Damien J.E. Cabanes, Martin Doedt, Vitor Cardoso, Antje Schmitz, Moritz Hawly, Huajuan Mo, Justine Jacquin, Andy Mechlinski, Gbotemi A. Adediran, Jose Andrade, Soledad Muniategui-Lorenzo, Anja Ramsperger, Martin G.J. Löder, Christian Laforsch, Tanja Cirkovic Velickovic, Daniele Fabbri, Irene Coralli, Stefania Federici, Barbara M. Scholz-Böttcher, Jacopo la Nasa, Greta Biale, Cassandra Rauert, Elvis D. Okoffo, Anna Undas, Lihui An, Volker Wachtendorf, Petra Fengler, Korinna Altmann

Dept. of Civil Engineering

Research output: Contribution to journal › Article › peer-review

1 Scopus citations

Abstract

In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, S_R, in thermo-analytical experiments ranged from 62%-117% (for PE) and 45.9%-62% (for PET). In spectroscopical experiments, the S_R varied between 121% and 129% (for PE) and 64% and 70% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy.

Original language	English
Pages (from-to)	8719-8728
Number of pages	10
Journal	Analytical Chemistry
Volume	97
Issue number	16
DOIs	https://doi.org/10.1021/acs.analchem.4c05403
State	Published - 29 Apr 2025

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10.1021/acs.analchem.4c05403

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Ciornii, D., Hodoroaba, V. D., Benismail, N., Maltseva, A., Ferrer, J. F., Wang, J., Parra, R., Jézéquel, R., Receveur, J., Gabriel, D., Scheitler, A., van Oversteeg, C., Roosma, J., van Renesse van Duivenbode, A., Bulters, T., Zanella, M., Perini, A., Benetti, F., Mehn, D., ... Altmann, K. (2025). Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods. Analytical Chemistry, 97(16), 8719-8728. https://doi.org/10.1021/acs.analchem.4c05403

@article{33dcabe9d7ad4bdab734b8ca48037d0c,

title = "Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods",

abstract = "In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, SR, in thermo-analytical experiments ranged from 62\%-117\% (for PE) and 45.9\%-62\% (for PET). In spectroscopical experiments, the SR varied between 121\% and 129\% (for PE) and 64\% and 70\% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy.",

author = "Dmitri Ciornii and Hodoroaba, \{Vasile Dan\} and Nizar Benismail and Alina Maltseva and Ferrer, \{Juan F.\} and Jiamin Wang and Raquel Parra and Ronan J{\'e}z{\'e}quel and Justine Receveur and Dina Gabriel and Andreas Scheitler and \{van Oversteeg\}, Christa and Jorg Roosma and \{van Renesse van Duivenbode\}, Alex and Tim Bulters and Michela Zanella and Alessandro Perini and Federico Benetti and Dora Mehn and Georg Dierkes and Michael Soll and Takahisa Ishimura and Marius Bednarz and Guyu Peng and Lars Hildebrandt and Mathias Peters and Kim, \{Seung Kyu\} and Jochen T{\"u}rk and Felix Steinfeld and Jaehak Jung and Sanghee Hong and Kim, \{Eun Ju\} and Yu, \{Hye Weon\} and Sven Klockmann and Christoph Krafft and Julia S{\"u}ssmann and Shan Zou and \{ter Halle\}, Alexandra and Giovannozzi, \{Andrea M.\} and Alessio Sacco and Marta Fadda and Mara Putzu and Im, \{Dong Hoon\} and Nontete Nhlapo and Priscilla Carrillo-Barrag{\'a}n and Natascha Schmidt and Dorte Herzke and Alessio Gomiero and Adri{\'a}n Ja{\'e}n-Gil and Cabanes, \{Damien J.E.\} and Martin Doedt and Vitor Cardoso and Antje Schmitz and Moritz Hawly and Huajuan Mo and Justine Jacquin and Andy Mechlinski and Adediran, \{Gbotemi A.\} and Jose Andrade and Soledad Muniategui-Lorenzo and Anja Ramsperger and L{\"o}der, \{Martin G.J.\} and Christian Laforsch and \{Cirkovic Velickovic\}, Tanja and Daniele Fabbri and Irene Coralli and Stefania Federici and Scholz-B{\"o}ttcher, \{Barbara M.\} and \{la Nasa\}, Jacopo and Greta Biale and Cassandra Rauert and Okoffo, \{Elvis D.\} and Anna Undas and Lihui An and Volker Wachtendorf and Petra Fengler and Korinna Altmann",

note = "Publisher Copyright: {\textcopyright} 2025 The Authors. Published by American Chemical Society.",

year = "2025",

month = apr,

day = "29",

doi = "10.1021/acs.analchem.4c05403",

language = "English",

volume = "97",

pages = "8719--8728",

journal = "Analytical Chemistry",

issn = "0003-2700",

number = "16",

}

Ciornii, D, Hodoroaba, VD, Benismail, N, Maltseva, A, Ferrer, JF, Wang, J, Parra, R, Jézéquel, R, Receveur, J, Gabriel, D, Scheitler, A, van Oversteeg, C, Roosma, J, van Renesse van Duivenbode, A, Bulters, T, Zanella, M, Perini, A, Benetti, F, Mehn, D, Dierkes, G, Soll, M, Ishimura, T, Bednarz, M, Peng, G, Hildebrandt, L, Peters, M, Kim, SK, Türk, J, Steinfeld, F, Jung, J, Hong, S, Kim, EJ, Yu, HW, Klockmann, S, Krafft, C, Süssmann, J, Zou, S, ter Halle, A, Giovannozzi, AM, Sacco, A, Fadda, M, Putzu, M, Im, DH, Nhlapo, N, Carrillo-Barragán, P, Schmidt, N, Herzke, D, Gomiero, A, Jaén-Gil, A, Cabanes, DJE, Doedt, M, Cardoso, V, Schmitz, A, Hawly, M, Mo, H, Jacquin, J, Mechlinski, A, Adediran, GA, Andrade, J, Muniategui-Lorenzo, S, Ramsperger, A, Löder, MGJ, Laforsch, C, Cirkovic Velickovic, T, Fabbri, D, Coralli, I, Federici, S, Scholz-Böttcher, BM, la Nasa, J, Biale, G, Rauert, C, Okoffo, ED, Undas, A, An, L, Wachtendorf, V, Fengler, P & Altmann, K 2025, 'Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods', Analytical Chemistry, vol. 97, no. 16, pp. 8719-8728. https://doi.org/10.1021/acs.analchem.4c05403

TY - JOUR

T1 - Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods

AU - Ciornii, Dmitri

AU - Hodoroaba, Vasile Dan

AU - Benismail, Nizar

AU - Maltseva, Alina

AU - Ferrer, Juan F.

AU - Wang, Jiamin

AU - Parra, Raquel

AU - Jézéquel, Ronan

AU - Receveur, Justine

AU - Gabriel, Dina

AU - Scheitler, Andreas

AU - van Oversteeg, Christa

AU - Roosma, Jorg

AU - van Renesse van Duivenbode, Alex

AU - Bulters, Tim

AU - Zanella, Michela

AU - Perini, Alessandro

AU - Benetti, Federico

AU - Mehn, Dora

AU - Dierkes, Georg

AU - Soll, Michael

AU - Ishimura, Takahisa

AU - Bednarz, Marius

AU - Peng, Guyu

AU - Hildebrandt, Lars

AU - Peters, Mathias

AU - Kim, Seung Kyu

AU - Türk, Jochen

AU - Steinfeld, Felix

AU - Jung, Jaehak

AU - Hong, Sanghee

AU - Kim, Eun Ju

AU - Yu, Hye Weon

AU - Klockmann, Sven

AU - Krafft, Christoph

AU - Süssmann, Julia

AU - Zou, Shan

AU - ter Halle, Alexandra

AU - Giovannozzi, Andrea M.

AU - Sacco, Alessio

AU - Fadda, Marta

AU - Putzu, Mara

AU - Im, Dong Hoon

AU - Nhlapo, Nontete

AU - Carrillo-Barragán, Priscilla

AU - Schmidt, Natascha

AU - Herzke, Dorte

AU - Gomiero, Alessio

AU - Jaén-Gil, Adrián

AU - Cabanes, Damien J.E.

AU - Doedt, Martin

AU - Cardoso, Vitor

AU - Schmitz, Antje

AU - Hawly, Moritz

AU - Mo, Huajuan

AU - Jacquin, Justine

AU - Mechlinski, Andy

AU - Adediran, Gbotemi A.

AU - Andrade, Jose

AU - Muniategui-Lorenzo, Soledad

AU - Ramsperger, Anja

AU - Löder, Martin G.J.

AU - Laforsch, Christian

AU - Cirkovic Velickovic, Tanja

AU - Fabbri, Daniele

AU - Coralli, Irene

AU - Federici, Stefania

AU - Scholz-Böttcher, Barbara M.

AU - la Nasa, Jacopo

AU - Biale, Greta

AU - Rauert, Cassandra

AU - Okoffo, Elvis D.

AU - Undas, Anna

AU - An, Lihui

AU - Wachtendorf, Volker

AU - Fengler, Petra

AU - Altmann, Korinna

PY - 2025/4/29

Y1 - 2025/4/29

N2 - In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, SR, in thermo-analytical experiments ranged from 62%-117% (for PE) and 45.9%-62% (for PET). In spectroscopical experiments, the SR varied between 121% and 129% (for PE) and 64% and 70% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy.

AB - In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, SR, in thermo-analytical experiments ranged from 62%-117% (for PE) and 45.9%-62% (for PET). In spectroscopical experiments, the SR varied between 121% and 129% (for PE) and 64% and 70% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy.

UR - http://www.scopus.com/inward/record.url?scp=105003927407&partnerID=8YFLogxK

U2 - 10.1021/acs.analchem.4c05403

DO - 10.1021/acs.analchem.4c05403

M3 - Article

AN - SCOPUS:105003927407

SN - 0003-2700

VL - 97

SP - 8719

EP - 8728

JO - Analytical Chemistry

JF - Analytical Chemistry

IS - 16

ER -

Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods

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