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Nanomaterials
Special Issues
Identification and Quantification of Nanomaterials
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Identification and Quantification of Nanomaterials

A special issue of Nanomaterials (ISSN 2079-4991). This special issue belongs to the section "Synthesis, Interfaces and Nanostructures".

Deadline for manuscript submissions: closed (31 August 2023) | Viewed by 16988

Special Issue Editor

Dr. Hubert Rauscher

E-Mail Website
Guest Editor
European Commission Joint Research Centre, Ispra, Italy
Interests: nanomaterials identification and characterisation; advanced materials; nanosafety; definition of nanomaterial; regulatory science; policy support

Special Issue Information

Dear Colleagues,

The identification and quantification of nanomaterials is currently a very active field of research. In view of the numerous ongoing regulatory activities addressing nanomaterials (e.g. amendments of nanospecific provisions in the REACH, Novel Food, Cosmetics and Medical Devices Regulations in Europe, rules and decisions on nanomaterials by US EPA and US FDA) manufacturers and regulators are in urgent need of scientific and technical progress to meet new regulatory requirements for nanomaterials. Identification and quantification of nanomaterials is a key requirement in this context and useful for innovators already in the material development phase to predict classification as nanomaterial (or the contrary) and to anticipate regulatory requirements for the final product. Enforcement laboratories need to be able to assess not only raw materials at the product ingredient level, but they must be able to analyse the final products on the market to identify and quantify the presence of a nanomaterial. Currently, there is an emerging issue with nanoplastics, which poses particular analytical and conceptual challenges. There has been some progress in recent years regarding the identification and quantification of nanomaterials as raw material, but for final products and materials which are difficult to analyse, such as nanoplastics, this is still extremely challenging.


Dr. Hubert Rauscher
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Nanomaterials is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2900 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • nanomaterial identification
  • nanomaterial quantification
  • particle measurement methods (quantitative and qualitative)
  • proxy methods
  • reference materials and standardisation
  • nanomaterials in products, formulations, and in the environment
  • safety of nanomaterials
  • nanoforms
  • nanoplastics
  • advanced nanomaterials

Published Papers (7 papers)

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Research

25 pages, 7478 KiB  
Article
Metrological Protocols for Reaching Reliable and SI-Traceable Size Results for Multi-Modal and Complexly Shaped Reference Nanoparticles
by Nicolas Feltin, Loïc Crouzier, Alexandra Delvallée, Francesco Pellegrino, Valter Maurino, Dorota Bartczak, Heidi Goenaga-Infante, Olivier Taché, Sylvie Marguet, Fabienne Testard, Sébastien Artous, François Saint-Antonin, Christoph Salzmann, Jérôme Deumer, Christian Gollwitzer, Richard Koops, Noham Sebaïhi, Richard Fontanges, Matthias Neuwirth, Detlef Bergmann, Dorothee Hüser, Tobias Klein and Vasile-Dan Hodoroabaadd Show full author list remove Hide full author list
Nanomaterials 2023, 13(6), 993; https://0-doi-org.brum.beds.ac.uk/10.3390/nano13060993 - 09 Mar 2023
Viewed by 1591
Abstract
The study described in this paper was conducted in the framework of the European nPSize project (EMPIR program) with the main objective of proposing new reference certified nanomaterials for the market in order to improve the reliability and traceability of nanoparticle size measurements. [...] Read more.
The study described in this paper was conducted in the framework of the European nPSize project (EMPIR program) with the main objective of proposing new reference certified nanomaterials for the market in order to improve the reliability and traceability of nanoparticle size measurements. For this purpose, bimodal populations as well as complexly shaped nanoparticles (bipyramids, cubes, and rods) were synthesized. An inter-laboratory comparison was organized for comparing the size measurements of the selected nanoparticle samples performed with electron microscopy (TEM, SEM, and TSEM), scanning probe microscopy (AFM), or small-angle X-ray scattering (SAXS). The results demonstrate good consistency of the measured size by the different techniques in cases where special care was taken for sample preparation, instrument calibration, and the clear definition of the measurand. For each characterization method, the calibration process is described and a semi-quantitative table grouping the main error sources is proposed for estimating the uncertainties associated with the measurements. Regarding microscopy-based techniques applied to complexly shaped nanoparticles, data dispersion can be observed when the size measurements are affected by the orientation of the nanoparticles on the substrate. For the most complex materials, hybrid approaches combining several complementary techniques were tested, with the outcome being that the reliability of the size results was improved. Full article
(This article belongs to the Special Issue Identification and Quantification of Nanomaterials)
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16 pages, 5111 KiB  
Article
NanoDefiner Framework and e-Tool Revisited According to the European Commission’s Nanomaterial Definition 2022/C 229/01
by Raphael Brüngel, Johannes Rückert, Philipp Müller, Frank Babick, Christoph M. Friedrich, Antoine Ghanem, Vasile-Dan Hodoroaba, Agnieszka Mech, Stefan Weigel, Wendel Wohlleben and Hubert Rauscher
Nanomaterials 2023, 13(6), 990; https://0-doi-org.brum.beds.ac.uk/10.3390/nano13060990 - 09 Mar 2023
Cited by 1 | Viewed by 1553
Abstract
The new recommended definition of a nanomaterial, 2022/C 229/01, adopted by the European Commission in 2022, will have a considerable impact on European Union legislation addressing chemicals, and therefore tools to implement this new definition are urgently needed. The updated NanoDefiner framework and [...] Read more.
The new recommended definition of a nanomaterial, 2022/C 229/01, adopted by the European Commission in 2022, will have a considerable impact on European Union legislation addressing chemicals, and therefore tools to implement this new definition are urgently needed. The updated NanoDefiner framework and its e-tool implementation presented here are such instruments, which help stakeholders to find out in a straightforward way whether a material is a nanomaterial or not. They are two major outcomes of the NanoDefine project, which is explicitly referred to in the new definition. This work revisits the framework and e-tool, and elaborates necessary adjustments to make these outcomes applicable for the updated recommendation. A broad set of case studies on representative materials confirms the validity of these adjustments. To further foster the sustainability and applicability of the framework and e-tool, measures for the FAIRification of expert knowledge within the e-tool’s knowledge base are elaborated as well. The updated framework and e-tool are now ready to be used in line with the updated recommendation. The presented approach may serve as an example for reviewing existing guidance and tools developed for the previous definition 2011/696/EU, particularly those adopting NanoDefine project outcomes. Full article
(This article belongs to the Special Issue Identification and Quantification of Nanomaterials)
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18 pages, 44412 KiB  
Article
Nanomaterial Characterization in Complex Media—Guidance and Application
by Yves Uwe Hachenberger, Daniel Rosenkranz, Charlotte Kromer, Benjamin Christoph Krause, Nadine Dreiack, Fabian Lukas Kriegel, Ekaterina Koz’menko, Harald Jungnickel, Jutta Tentschert, Frank Stefan Bierkandt, Peter Laux, Ulrich Panne and Andreas Luch
Nanomaterials 2023, 13(5), 922; https://0-doi-org.brum.beds.ac.uk/10.3390/nano13050922 - 02 Mar 2023
Cited by 3 | Viewed by 1447
Abstract
A broad range of inorganic nanoparticles (NPs) and their dissolved ions possess a possible toxicological risk for human health and the environment. Reliable and robust measurements of dissolution effects may be influenced by the sample matrix, which challenges the analytical method of choice. [...] Read more.
A broad range of inorganic nanoparticles (NPs) and their dissolved ions possess a possible toxicological risk for human health and the environment. Reliable and robust measurements of dissolution effects may be influenced by the sample matrix, which challenges the analytical method of choice. In this study, CuO NPs were investigated in several dissolution experiments. Two analytical techniques (dynamic light scattering (DLS) and inductively-coupled plasma mass spectrometry (ICP-MS)) were used to characterize NPs (size distribution curves) time-dependently in different complex matrices (e.g., artificial lung lining fluids and cell culture media). The advantages and challenges of each analytical approach are evaluated and discussed. Additionally, a direct-injection single particle (DI sp)ICP-MS technique for assessing the size distribution curve of the dissolved particles was developed and evaluated. The DI technique provides a sensitive response even at low concentrations without any dilution of the complex sample matrix. These experiments were further enhanced with an automated data evaluation procedure to objectively distinguish between ionic and NP events. With this approach, a fast and reproducible determination of inorganic NPs and ionic backgrounds can be achieved. This study can serve as guidance when choosing the optimal analytical method for NP characterization and for the determination of the origin of an adverse effect in NP toxicity. Full article
(This article belongs to the Special Issue Identification and Quantification of Nanomaterials)
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11 pages, 43589 KiB  
Article
Isolation of Exosomes from Human Serum Using Gold-Nanoparticle-Coated Silicon Surface
by Krishna Thej Pammi Guru, Nusrat Praween and Palash Kumar Basu
Nanomaterials 2023, 13(3), 387; https://0-doi-org.brum.beds.ac.uk/10.3390/nano13030387 - 18 Jan 2023
Cited by 4 | Viewed by 1824
Abstract
Exosomes, whose mean diameter ranges from 20 nm to 200 nm, are cell-secreted vesicles and are abundant in most biological fluids, such as blood, urine, tears, sweat, breast milk, etc. Exosomal size variations and their composition can be attributed to several factors, such [...] Read more.
Exosomes, whose mean diameter ranges from 20 nm to 200 nm, are cell-secreted vesicles and are abundant in most biological fluids, such as blood, urine, tears, sweat, breast milk, etc. Exosomal size variations and their composition can be attributed to several factors, such as age, gender and disease conditions of the individual. Existing techniques, such as ultracentrifugation and density gradient ultracentrifugation, for exosome isolation are instrument-dependent, time-consuming and lack specificity. In the present work, a gold-nanoparticle (GNP)-coated silicon (Si) wafer, functionalized with polyethylene glycol (PEG) was used for conjugation with anti-CD63 antibody via EDC NHS chemistry and incubated with serum to immobilize the exosomes on the Si surface. The surface-immobilized exosomes were eluted and quantified by a nanoparticle tracking analyzer (NTA). It was observed that an increase in GNP density on the Si wafer increases the size range and total number of exosomes that are being isolated. Western blotting performed for proteins such as HSP 70 and calnexin confirmed the immobilization and elution of exosomes. The proposed technique can be used as an alternative to existing techniques, as it has several benefits such as reusability of the Si surface for several isolations, minimal instrumental requirement, isolation of exosomes in two hours and compatibility with the microfluidic platform, making the technique suitable for real-time application. The proposed method could be useful in isolating a specific subrange of exosomes by altering the size of the GNP used for coating the Si wafer. Full article
(This article belongs to the Special Issue Identification and Quantification of Nanomaterials)
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20 pages, 3590 KiB  
Article
Counting Small Particles in Electron Microscopy Images—Proposal for Rules and Their Application in Practice
by Harald Bresch, Vasile-Dan Hodoroaba, Alexandra Schmidt, Kirsten Rasmussen and Hubert Rauscher
Nanomaterials 2022, 12(13), 2238; https://0-doi-org.brum.beds.ac.uk/10.3390/nano12132238 - 29 Jun 2022
Cited by 9 | Viewed by 2788
Abstract
Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count [...] Read more.
Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials. Full article
(This article belongs to the Special Issue Identification and Quantification of Nanomaterials)
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32 pages, 7400 KiB  
Article
Determination of the Transport Efficiency in spICP-MS Analysis Using Conventional Sample Introduction Systems: An Interlaboratory Comparison Study
by Otmar Geiss, Ivana Bianchi, Guillaume Bucher, Eveline Verleysen, Frédéric Brassinne, Jan Mast, Katrin Loeschner, Lucas Givelet, Francesco Cubadda, Francesca Ferraris, Andrea Raggi, Francesca Iacoponi, Ruud Peters, Anna Undas, Alexandra Müller, Ann-Katrin Meinhardt, Birgit Hetzer, Volker Gräf, Antonio R. Montoro Bustos and Josefa Barrero-Moreno
Nanomaterials 2022, 12(4), 725; https://0-doi-org.brum.beds.ac.uk/10.3390/nano12040725 - 21 Feb 2022
Cited by 15 | Viewed by 3436
Abstract
In single particle inductively coupled plasma mass spectrometry (spICP-MS), the transport efficiency is fundamental for the correct determination of both particle number concentration and size. In the present study, transport efficiency was systematically determined on three different days with six carefully characterised gold [...] Read more.
In single particle inductively coupled plasma mass spectrometry (spICP-MS), the transport efficiency is fundamental for the correct determination of both particle number concentration and size. In the present study, transport efficiency was systematically determined on three different days with six carefully characterised gold nanoparticle (AuNP) suspensions and in seven European and US expert laboratories using different ICP-MS instruments and spICP-MS software. Both particle size—(TES)—and particle frequency—(TEF)—methods were applied. The resulting transport efficiencies did not deviate much under ideal conditions. The TEF method however systematically resulted in lower transport efficiencies. The extent of this difference (0–300% rel. difference) depended largely on the choice and storage conditions of the nanoparticle suspensions used for the determination. The TES method is recommended when the principal measurement objective is particle size. If the main aim of the measurement is the determination of the particle number concentration, the TEF approach could be preferred as it might better account for particle losses in the sample introduction system. Full article
(This article belongs to the Special Issue Identification and Quantification of Nanomaterials)
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18 pages, 7787 KiB  
Article
Correlative Analysis of the Dimensional Properties of Bipyramidal Titania Nanoparticles by Complementing Electron Microscopy with Other Methods
by Loïc Crouzier, Nicolas Feltin, Alexandra Delvallée, Francesco Pellegrino, Valter Maurino, Grzegorz Cios, Tomasz Tokarski, Christoph Salzmann, Jérôme Deumer, Christian Gollwitzer and Vasile-Dan Hodoroaba
Nanomaterials 2021, 11(12), 3359; https://0-doi-org.brum.beds.ac.uk/10.3390/nano11123359 - 10 Dec 2021
Cited by 6 | Viewed by 2487
Abstract
In this paper, the accurate determination of the size and size distribution of bipyramidal anatase nanoparticles (NPs) after deposition as single particles on a silicon substrate by correlative Scanning Electron Microscopy (SEM) with Atomic Force Microscopy (AFM) analysis is described as a new [...] Read more.
In this paper, the accurate determination of the size and size distribution of bipyramidal anatase nanoparticles (NPs) after deposition as single particles on a silicon substrate by correlative Scanning Electron Microscopy (SEM) with Atomic Force Microscopy (AFM) analysis is described as a new measurement procedure for metrological purposes. The knowledge of the exact orientation of the NPs is a crucial step in extracting the real 3D dimensions of the particles. Two approaches are proposed to determine the geometrical orientation of individual nano-bipyramides: (i) AFM profiling along the long bipyramid axis and (ii) stage tilting followed by SEM imaging. Furthermore, a recently developed method, Transmission Kikuchi Diffraction (TKD), which needs preparation of the crystalline NPs on electron-transparent substrates such as TEM grids, has been tested with respect to its capability of identifying the geometrical orientation of the individual NPs. With the NPs prepared homogeneously on a TEM grid, the transmission mode in a SEM, i.e., STEM-in-SEM (or T-SEM), can be also applied to extract accurate projection dimensions of the nanoparticles from the same sample area as that analysed by SEM, TKD and possibly AFM. Finally, Small Angle X-ray Scattering (SAXS) can be used as an ensemble technique able to measure the NPs in liquid suspension and, with ab-initio knowledge of the NP shape from the descriptive imaging techniques, to provide traceable NP size distribution and particle concentration. Full article
(This article belongs to the Special Issue Identification and Quantification of Nanomaterials)
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