TY - RPRT A1 - Schmidt, Alexandra A1 - Bresch, Harald A1 - Kämpf, K. A1 - Bachmann, V. A1 - Peters, T. A1 - Kuhlbusch, T. T1 - Development of a specific OECD Test Guideline on Particle Size and Particle Size Distribution of Nanomaterials N2 - In this research project, a new OECD Test Guideline (TG) for the determination of “Particle Size and Particle Size Distributions of Nanomaterials” was developed as the existing OECD TG 110 is considered to be outdated in terms of applicable size range (not covering sizes <200 nm) and methods. By its scope with an applicable size range from 1 to 1000 nm the new Test Guideline (TG PSD) covers the whole nanoscale. The TG PSD is applicable for particulate and fibrous nanomaterials. The prescribed, pairwise measurement of fibre diameter and length in the TG PSD allows for the first time to differen-tiate fibres with regard to their size-dependent hazard properties. Measurement instructions for each included method were validated within two separated interlaboratory comparisons, as a distinction between near spherical particles and fibres when applying the methods has to be made. Besides information on content and structure of the TG PSD, this final report outlines essential steps, considerations and organisational aspects during the development of the TG. Insights into the selec-tion, preparation and prevalidation of test materials used in the interlaboratory comparison are given. Finally, main results of the interlaboratory comparisons and their impacts on the TG PSD are pre-sented. N2 - Im Rahmen des Forschungsprojekts wurde eine neue OECD-Prüfrichtlinie (TG) für die Bestimmung von Partikelgrößen und Partikelgrößenverteilungen von Nanomaterialien entwickelt, da die existie-rende OECD TG 110 zur Bestimmung von Partikelgrößen in Bezug auf den anwendbaren Größenbe-reich und die gegebenen Methoden veraltet ist bzw. den Nanometerbereich < 200 nm nicht abdeckt. Mit ihrem Anwendungsbereich von 1 bis 1000 nm deckt die neue Prüfrichtlinie (TG PSD) die gesamte Nanoskala ab. Die TG PSD ist für partikel- und faserförmige Nanomaterialien anwendbar. Durch die, in der TG PSD vorgeschriebene, paarweise Messung von Faserdurchmesser und -länge ermöglicht diese TG zum ersten Mal Fasern hinsichtlich ihrer größenabhängigen Gefahrstoffeigenschaften zu unter-scheiden. Die Messanweisungen aller enthaltenen Methoden wurden im Rahmen von zwei getrennten Ringversuchen validiert, da bei der Anwendung der Methoden eine Unterscheidung zwischen Parti-keln und Fasern gemacht werden muss. Neben Angaben zum Inhalt und Struktur der TG PSD, befasst sich der vorliegende Abschlussbericht mit den wesentlichen Schritten, Überlegungen und organisatorischen Aspekten bei der Entwicklung der Prüfrichtlinie. Darüber hinaus werden Einblicke in die Auswahl, Vorbereitung und Prävalidierung der im Ringversuch verwendeten Testmaterialien gegeben. Schließlich werden die wichtigsten Ergeb-nisse aus den Ringversuchen und ihre Auswirkungen auf die TG PSD vorgestellt. KW - Nano KW - OECD KW - Particle size distribution KW - Testguideline KW - Nanoparticle PY - 2021 VL - 2021 SP - 1 EP - 47 PB - German Environment Agency CY - Dessau AN - OPUS4-54021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Synthesizing a library of 1000+ reproducible MOFs N2 - While the synthesis of Metal-Organic Framework (MOF) particles can be as easy as adding two solutions together, reproducibly obtaining the same particles, time and time again, is a lot harder. As laboratory-independent reproducibility is a cornerstone of the scientific method, we must put effort into finding and controlling all necessary parameters to achieve this. An open-source Python/EPICS-controlled robotic platform (see picture) was adapted to systematically explore this for a 20 ml MOF synthesis of the Zeolitic Imidazole Framework-8 (ZIF-8) chemistry in methanol. Parameters that were explored included: 1) addition sequence, 2) addition speeds, 3) reaction times, 4) source chemicals, 5) stirring speeds, 6) stirring bar choice, 7) starting concentrations, and 8) workup methodologies. It was found that, by controlling these parameters, highly reproducible syntheses are obtained. Secondly, the variation of these parameters alone led to a dramatic difference in volume-weighted particle size means, which exceeds an order of magnitude as investigated by our in-house X-ray scattering instrument [1]. The syntheses are thoroughly documented in an automated fashion, and the synthesis libraries as well as analyses libraries will become available in batches soon. With this library, it will be possible to extract previously unknown correlations, and other laboratories can produce specific particles by following the exact procedures of the particles of their choice. T2 - 787. WE-Heraeus-Seminar: Accelerated Discovery of New Materials CY - Bad Honnef, Germany DA - 15.05.2023 KW - Metal organic frameworks KW - Automation KW - Lab automation KW - Robotic-supported synthesis KW - Reproducibility KW - Synthesis library KW - X-ray scattering KW - Particle size distribution PY - 2023 AN - OPUS4-57596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fritsch, Tobias T1 - 3D Analysis of Powder for Laser Beam Melting by Synchrotron X-ray CT N2 - Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of complex structures. The quality of the feedstock material receives increasing attention, as it depicts the first part of the L-PBF process chain. The powder quality control in terms of flowability and powder bed packing density is therefore mandatory. In this work, a workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established. Synchrotron computed tomography (CT) was used to correlate the packing density with the particle size and particle shape for three different powder batches. The polydisperse particle size distribution (PSD) was transformed into a statistically equivalent bidisperse PSD. The ratio of the small and large particles helped to understand the powder particle packing density. While the particle shape had a neglectable influence, the particle size distribution was identified as major contributor for the packing density. T2 - AM- Workshop BAM CY - Online meeting DA - 20.04.2021 KW - Additive manufacturing KW - Laser powder bed fusion KW - Powder KW - Particle size distribution KW - Packing density PY - 2021 AN - OPUS4-53477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bennet, Francesca A1 - Hodoroaba, Vasile-Dan T1 - BAM reference data - SEM raw data for the particles size distribution of Al-coated titania nanoparticles (JRCNM62001a and JRCNM62002a) N2 - SEM raw images of Al-coated titania nanoparticles (JRCNM62001 and JRCNM62002a) provided by the JRC repository are provided together with the particle size distribution of the minimum Feret Diameter extracted from the given images. KW - SEM KW - Titania nanoparticles KW - Particle size distribution KW - BAM reference data PY - 2021 DO - https://doi.org/10.5281/zenodo.5007367 PB - Zenodo CY - Geneva AN - OPUS4-52836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Salzmann, Christoph A1 - Pellegrino, Francesco A1 - Hodoroaba, Vasile-Dan T1 - STEM-in-SEM versus SE-InLens-type-SEM as a Reliable Analytical Pair-Tool for Measurement of Nanoparticle Size and Shape Distribution N2 - Following points are addressed in this contribution: Advantages of correlative analysis in electron microscopy; Measurement principle of the different electron microscopy modes used; Presentation of the nanomaterials used for this study; Role of sample preparation; and, with particular description, the Sequence kV-variation with InLens SE & transmission SEM detection of the same field-of-view. KW - Nanoparticles KW - Electron microscopy KW - Metrology KW - Particle size distribution PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.308 VL - 30 IS - Supplement_1 SP - 650 EP - 651 PB - Oxford University Press (OUP) AN - OPUS4-61042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Nanoparticle Populations N2 - Two new projects P15 Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension and P16 Measurement of (relative) number concentration of bimodal silica nanoparticles including deposition from liquid suspension have been started at VAMAS/TWA 34 under the lead of BAM. First results are presented and discussed. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 47th Steering Committee Meeting CY - Turin, Italy DA - 18.10.2022 KW - VAMAS KW - Nanoparticles KW - Inter-laboratory comparison KW - Particle size distribution KW - Nanoparticle concentration PY - 2022 AN - OPUS4-56196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan T1 - Delivering Impact - A new ISO standard on the identification of nanoparticles N2 - Nanoparticles (NPs) are tiny – around 1 to 100 billionths of a meter – and can have different chemistries and behaviours than the same material of larger size. This property has led to advances in a wide range of industries, but it can also confer toxicity. Size measurements are the main way NPs are identified but a lack of standardised methods for identifying ones with complex shapes has hindered evaluation of their potential harm. KW - Nanoparticles KW - Standardisation KW - Particle size distribution KW - nPSize KW - ISO 21363 PY - 2024 UR - https://www.euramet.org/casestudies/casestudiesdetails/news/default-c3b26209e8 SP - 1 EP - 2 PB - EURAMET CY - Braunschweig AN - OPUS4-59626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Other than spherical/monodisperse Towards real world NPs as candidate reference materials for traceable size measurements N2 - By far most of the current nanoparticle (NP) research is dealing with (quasi-) spherical and/or monodisperse particles. However, many NPs used in industrial applications are rather aspherical and polydisperse. This inhomogeneity considerably hampers their characterization and, particularly, the accurate determination of the nanoparticle size. In order to overcome this problem and to promote the availability of standardized size measurement methods, it is crucial to develop and establish (candidate) reference materials with inhomogeneous size (distribution), aspherical shape as well as agglomerated or aggregated particles. Therefore, a new set of NPs including Au-, SiO2 , and TiO2-particles is investigated. The range of properties comprises polydisperse spherical, bimodal spherical, rod-like, acicular, bipyramidal, sheet-like as well as cubic NPs. With respect to a good traceability of the measurements, size and size distributions of the candidate reference materials are determined using microscopic methods like scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning electron microscopy in transmission mode (STEM-in-SEM), atomic force microscopy (AFM) as well as small angle X-ray scattering (SAXS) as an ensemble technique. The development of protocols for sample preparation is of particular importance to obtain a homogeneous dispersion of the NPs on a substrate. Further, approaches for signal modelling for all the methods above are being developed. The initiation of two VAMAS (www.vamas.org/twa34/index.html) inter-laboratory comparisons on bipyramidal titania and bimodal silica with different modal concentration ratios will be also highlighted. T2 - E-MRS Spring Meeting 2021 CY - Online meeting DA - 31.05.2021 KW - Nanoparticles KW - Particle size distribution KW - Imaging KW - Traceability KW - Reference material PY - 2021 AN - OPUS4-52764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement; What nPSize can offer to CEN/TC 352? N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, inter-laboratory comparisons) as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies are discussed. E.g. the first technical report of nPSize on full algorithm sequences for nanoparticle detection and size measurement as developed on both a physical basis (SEM, TSEM, AFM and SAXS) and by machine learning is put at disposal. T2 - 29th Meeting of CEN/TC 352 Nanotechnologies CY - Online meeting DA - 25.03.2021 KW - Nanoparticles KW - Electron microscopy KW - CEN/TC 352 Nanotechnologies KW - Particle size distribution KW - Modelling KW - Machine learning PY - 2021 AN - OPUS4-52464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Challenges in Traceable Size Measurement of Non-Spherical, Non-Monodisperse Nanoparticles - nPSize N2 - Size measurement of nanoparticles (NP) becomes a challenging analytical problem when non-spherical shapes must be traceably measured. However, most industrial NPs have irregular shapes and broad size distribution making it often more complex to follow European regulatory to identify a material as a nanomaterial according to which accurate measurement of the smallest dimension and its size Distribution is necessary. The European research project nPSize - Improved traceability chain of nanoparticle size measurements aims to fill this gap by developing potential non-spherical reference nanoparticles, measurement procedures and physical modelling to improve the traceability chain, comparability and compatibility for NP size measurements between different methods. Therefore, new model NP with well-controlled shape has been synthesized and are supposed to be systematically characterized using the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering. Following NP candidates are under investigation with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-100 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). In addition, sample preparation procedures as well as measurement analysis procedures with evaluation of appropriate measurands and descriptors for each material class and method are being developed to support standardization. To underpin the traceability of the size measurement of nonspherical NP, physical modelling of the signals in e.g. electron microscopy techniques will be used and in combination, the implementation of machine learning is aimed to facilitate measurement Analysis procedures, especially regarding the accurate thresholding/segmentation of the NPs.zeige mehr T2 - Nanoparticle Reference Materials - Production and Cerification Training Course CY - London, UK DA - 10.12.2019 KW - Nanoparticles KW - Traceability KW - Particle size distribution KW - Electron microscopy KW - Reference materials KW - Non-spherical shape PY - 2019 AN - OPUS4-50040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -