TY - RPRT A1 - Babick, F. A1 - Mielke, Johannes A1 - Hodoroaba, Vasile-Dan A1 - Weigel, St. A1 - Wohlleben, W. T1 - Critical review manuscript with real-world performance data for counting, ensemble and separating methods including in-build mathematical conversion to number distributions submitted for publication N2 - The content of the paper is the assessment of the performance of (conventional) measurement techniques (MTs)with respect to the classification of disperse materials according to the EC recommendation for a definition of nanomaterial. This performance essentially refers to the accurate assessment of the number weighted median of (the constituent) particles. All data and conclusions are based on the analytical study conducted as real-world performance testing. It comprised different types of MTs (imaging, counting, fractionating, spectroscopic and integral) as well as different types of materials. Beside reference materials with well-defined size distribution the study also included several commercial powders (variation of particle composition, morphology, coating, size range and polydispersity). In order to ensure comparability of measurement results, the participants were guided to use uniform protocols in sample preparation, conducting measurements, data analysis and in reporting results. Corresponding documents have been made public, in order to support the reviewing process of the paper, respectively to ensure the reproducibility of data by other users under the same conditions. The scientific paper relies on a comprehensive set of revised measurement data reported in uniform templates, completely describes the experimental procedures and discusses the MTs’ performance for selected materials in detail. Even more, the study is summarised and evaluated, which leads to recommendations for the use of MTs within a tiered approach of NM characterisation. In addition, the paper critically examines the factors that may affect the outcome of such a comparison among different MTs. KW - Nanomaterial KW - Measurement techniques KW - EC definition of nanomaterial KW - Nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389646 UR - http://www.nanodefine.eu/index.php/downloads/nanodefine-technical-reports UR - http://www.nanodefine.eu/publications/reports/NanoDefine_TechnicalReport_D3.3.pdf SP - D3.3, 1 EP - 72 PB - The NanoDefine Consortium CY - Wageningen, The Netherlands AN - OPUS4-38964 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brüngel, R. A1 - Rückert, J. A1 - Wohlleben, W. A1 - Babick, F. A1 - Ghanem, A. A1 - Gaillard, C. A1 - Mech, A. A1 - Rauscher, H. A1 - Hodoroaba, Vasile-Dan A1 - Weigel, S. A1 - Friedrich, C. M. T1 - NanoDefiner e-Tool: An Implemented Decision Support Framework for Nanomaterial Identification N2 - The European Commission’s recommendation on the definition of nanomaterial (2011/696/EU) established an applicable standard for material categorization. However, manufacturers face regulatory challenges during registration of their products. Reliable categorization is difficult and requires considerable expertise in existing measurement techniques (MTs). Additionally, organizational complexity is increased as different authorities’ registration processes require distinct reporting. The NanoDefine project tackled these obstacles by providing the NanoDefiner e-tool: A decision support expert system for nanomaterial identification in a regulatory context. It providesMT recommendations for categorization of specific materials using a tiered approach (screening/confirmatory), and was constructed with experts from academia and industry to be extensible, interoperable, and adaptable for forthcoming revisions of the nanomaterial definition. An implemented MT-driven material categorization scheme allows detailed description. Its guided workflow is suitable for a variety of user groups. Direct feedback and explanation enable transparent decisions. Expert knowledge is Held in a knowledge base for representation of MT performance criteria and physicochemical particle type properties. Continuous revision ensured data quality and validity. Recommendations were validated by independent case studies on industry-relevant particulate materials. Besides supporting material identification and registration, the free and open-source e-tool may serve as template for other expert systems within the nanoscience domain. KW - EC nanomaterial definition KW - Decision support KW - Expert system KW - Nanomaterial KW - Nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492449 DO - https://doi.org/10.3390/ma12193247 VL - 12 IS - 19 SP - 3247 PB - MDPI CY - Basel, CH AN - OPUS4-49244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Friedrich, C. M. A1 - Weigel, S. A1 - Marvin, H. A1 - Rauscher, H. A1 - Wohlleben, W. A1 - Babick, F. A1 - Löschner, K. A1 - Mech, A. A1 - Brüngel, R. A1 - Hodoroaba, Vasile-Dan A1 - Gilliland, D. A1 - Rasmussen, K. A1 - Ghanem, A. T1 - The NanoDefine Methods Manual N2 - This document is a collection of three JRC Technical Reports that together form the “NanoDefine Methods Manual”, which has been developed within the NanoDefine project ‘Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial’, funded by the European Union’s 7th Framework Programme, under grant agreement 604347. The overall goal of the NanoDefine project was to support the implementation of the European Commission Recommendation on the definition of nanomaterial (2011/696/EU). The project has developed an integrated empirical approach, which allows identifying a material as a nano- or not a nanomaterial according to the EC Recommendation. The NanoDefine Methods Manual consists of three parts: Part 1: The NanoDefiner Framework and Tools, which covers the NanoDefiner framework, general information on measurement methods and performance criteria, and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool. Part 2: Evaluation of Methods, which discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3: Standard Operating Procedures (SOPs), which presents the 23 Standard Operating Procedures developed within the NanoDefine project. In this combined document, these three parts are included as stand-alone reports, each having its own abstract, table of contents, page, table and figure numbering, and references. KW - Nanomaterial KW - Particle size distribution KW - Nanoparticles KW - NanoDefine KW - Nanomaterial classification PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504250 SN - 978-92-76-12335-4 DO - https://doi.org/10.2760/79490 VL - JRC117501 SP - 1 EP - 451 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gaillard, C. A1 - Mech, A. A1 - Wohlleben, W. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Ghanem, A. A1 - Weigel, S. A1 - Rauscher, H. T1 - A technique-driven materials categorisation scheme to support regulatory identification of nanomaterials N2 - Worldwide there is a variety of regulatory provisions addressing nanomaterials. The identification as nanomaterial in a regulatory context often has the consequence that specific legal rules apply. In identifying nanomaterials, and to find out whether nanomaterial-specific provisions apply, the external size of particles is globally used as a criterion. For legal certainty, its assessment for regulatory purposes should be based on measurements and methods that are robust, fit for the purpose and ready to be accepted by different stakeholders and authorities. This should help to assure the safety of nanomaterials and at the same time facilitate their international trading. Therefore, we propose a categorisation scheme which is driven by the capabilities of common characterisation techniques for particle size measurement. Categorising materials according to this scheme takes into account the particle properties that are most important for a determination of their size. The categorisation is exemplified for the specific particle number based size metric of the European Commission's recommendation on the definition of nanomaterial, but it is applicable to other metrics as well. Matching the performance profiles of the measurement techniques with the material property profiles (i) allows selecting the most appropriate size determination technique for every type of material considered, (ii) enables proper identification of nanomaterials, and (iii) has the potential to be accepted by regulators, industry and consumers alike. Having such a scheme in place would facilitate the regulatory assessment of nanomaterials in regional legislation as well as in international relations between different regulatory regions assuring the safe trade of nanomaterials. KW - Nanomaterial KW - Nanoparticles KW - Categorisation scheme KW - EC definition of a nanomaterial KW - Regulatory identification of nanomaterials PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471623 DO - https://doi.org/10.1039/C8NA00175H SN - 2516-0230 SP - 1 EP - 11 PB - The Royal Society of Chemistry AN - OPUS4-47162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Mielke, Johannes A1 - Wohlleben, W. T1 - Measurement and calculation of multimodal material VSSA N2 - In order to ground the debate on the metrics that apply for VSSA determined by adsorption isotherms and to illustrate the consequences of real bimodality for VSSA screening, a bimodal mixture has been selected for systematic investigations. A sample of BaSO4 fine was spiked with 10% g/g of BaSO4 ultrafine. The ultrafine grade is a clear nanomaterial (NM) according to the size criterion with a median Feretmin of 27 nm and the fine grade is clearly a non-NM with a median Feretmin of 249 nm. Because of the number ratio of 300:1, the mixture has to be a NM according to the size criterion. Three independent BET measurements were performed on the mixture by two different labs and resulted in a mean VSSA of 23 m2/cm3 with a standard deviation of 3.3 m2/cm3, which leads to a dminVSSA of 258 nm, and, therefore, would falsely classify the material as a non-NM. This effect was predicted earlier by calculated examples (Roebben et al. 2014) and demonstrates that mixtures of nano- and non-nano multimodal materials very likely lead to false negative classifications. Moreover, the measured VSSA values for the mixture of 23 m²/cm³ are in excellent accord with the value of 24.6 m²/cm³ predicted from the TEM size distributions of the individual materials according to the model described by JRC (Roebben et al. 2014), but are significantly different from the prediction of 309 m²/cm³ obtained from the same TEM size distribution by a particle number weighted approach (Lecloux 2015). The same is true for a 50% g/g mixture. We conclude that the mass-based VSSA approach (Roebben et al. 2014) is equal to the VSSA that is measurable by adsorption isotherms, such as from standardized BET. T2 - NANoREG Technical Meeting on VSSA discussion CY - Schiphol, The Netherlands DA - 26.09.2016 KW - VSSA KW - Nanomaterial KW - Electron microscopy KW - Particle size distribution PY - 2016 AN - OPUS4-38914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Lessons on measurement of nanoparticle size and shape learnt from NanoDefine N2 - The EC Recommendation on the definition of nanomaterial1, based solely on size of the constituent particles, foresees development of harmonised measurement methods ensuring ‘consistent results across materials and over time’. The EU/FP7 large research project NanoDefine (http://www.nanodefine.eu) has been exclusively dedicated to support the implementation of this EC Recommendation for the European Union’s legislation. For the first time, measurement techniques able to determine the size of nanoparticles have been evaluated systematically on a well-defined set of quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. Particularly based on the analytical performance of the measurement techniques as tested on the challenging real-world particulate materials, it was possible to formulate recommendations for use of a new tiered approach consisting of screening and confirmatory techniques. Thus, a consistent framework of guidance for nanomaterial identification according to the EC Definition has been issued in form of the NanoDefiner e-tool (https://labs.inf.fh-dortmund.de/NanoDefiner), with a transparent decision flow scheme and an extensive user manual. Selected examples of analysis and classification as nano-/non-nanomaterials will be given, highlighting the limits of applicability of the available measurement techniques in dependence on sample properties. On some recent relevant developments in sample preparation – as a crucial part for an accurate analysis - will be also reported. T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Nanoparticles KW - Nanomaterial KW - Particle size distribution KW - EU definition of nanomaterial PY - 2018 AN - OPUS4-44804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of nanoparticle size and shape distribution – Current situation and outlook N2 - The EC Recommendation on the definition of nanomaterial, based solely on size of the constituent particles, foresees development of harmonised measurement methods ensuring ‘consistent results across materials and over time’. The EU/FP7 research project NanoDefine has been exclusively dedicated to support the implementation of this EC Recommendation for the European Union’s legislation. For the first time, measurement techniques able to determine the size of nanoparticles have been evaluated systematically on a well-defined set of quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. Particularly based on the analytical performance of the measurement techniques as tested on the challenging real-world particulate materials, it was possible to formulate recommendations for use of a new tiered approach consisting of screening and confirmatory techniques. Thus, a consistent framework of guidance for nanomaterial identification according to the EC Definition has been issued in form of the NanoDefiner e-tool, with a transparent decision flow scheme and an extensive user manual. Selected examples of analysis and classification as nano-/non-nanomaterials will be given, highlighting the limits of applicability of the available measurement techniques in dependence on sample properties. On some recent relevant developments in sample preparation – as a crucial part for an accurate analysis - will be also reported. Further, ISO/TC 229 ‘Nanotechnologies’ activities aiming at establishing accurate TEM and SEM measurement of NP size and shape as robust, traceable, standard procedures are highlighted. With participation of BAM, study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated or shape-controlled titania nano-powder for which size and shape distribution of primary particles must be measured accurately. T2 - Symposium Preparation, Characterization and Processing of Nano and Submicron Powders CY - Berlin, Germany DA - 14.06.2018 KW - Nanoparticles KW - Nanomaterial KW - EC definition KW - Nanoparticle size distribution PY - 2018 AN - OPUS4-45191 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Mielke, Johannes A1 - Babick, F. A1 - Ullmann, C. T1 - Evaluation of particle sizing techniques for the implementation of the EC definition of a nanomaterial N2 - Many techniques are available for measuring particle size distribution. For ideal materials (spherical particles, well dispersed) it is possible to evaluate the Performance of These methods. The performance of the analytical instrumentation for the purpose of classifying materials according to EC Definition is unknown. In this work the performance of commercially available particle sizing techniques on representative NanoDefine set of real-world testing materials (RTM) and quality control materials (QCM) for the implementation of the Definition is evaluated. T2 - 4. Sitzung des wissenschaftlichen Beirats zum Themefeld Umwelt der BAM CY - BAM, Berlin, Germany DA - 13.04.2018 KW - Nanoparticles KW - Nanomaterial KW - Characterization methods KW - EU definition KW - Nanodefine PY - 2018 AN - OPUS4-44693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Wohlleben, W. A1 - Mielke, Johannes A1 - Rauscher, H. T1 - Volume specific surface area (VSSA) by BET as a reliable metric for (nano)particle size analysis for powders N2 - We discuss the role of the volume specific surface area (VSSA) as determined from the specific surface area measured by the (extended) Brunauer-Emmett-Teller (BET) technique, in the identification process of powdered nano- and non-nanomaterials in line with the EU definition of nanomaterial. Results obtained in the NanoDefine project demonstrate that under appropriate conditions, VSSA can be used as proxy to the number-based particle size distribution. The extent of agreement between nano/non-nano classification by electron microscopy (EM) and classification by VSSA is investigated systematically on a large set of diverse particulate substances, representing most of the cases expected in regulatory practice. Thus, parameters such as particle shape, size polydispersity/multi-modality, and particle (inner or coating) porosity are evaluated. Based on these results, we derive a tiered screening strategy for powders, involving the use of VSSA for the purpose of implementing the definition of nanomaterial, and recommend it for inclusion in a technical guidance for the implementation of the definition. T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Nanoparticles KW - Nanomaterial KW - Particle size distribution KW - BET KW - VSSA PY - 2018 AN - OPUS4-44801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Aktivitäten der BAM im EU-Projekt NanoDefine N2 - Die Präsentation gibt einen Überblick über die Aktivitäten der BAM im EU-Projekt 'NanoDefine'. Verknüpfungen zur Entwicklung von nano-Referenzmaterialien, ISO- und VAMAS-Aktivitäten und anderen nano-Projekten werden vorausschauend diskutiert. T2 - Expertenaustausch zum Thema ‘Nanosicherheit’ zwischen BMU, BMWi und BAM CY - Berlin, Germany DA - 01.06.2018 KW - Nanomaterial KW - ISO KW - NanoDefine KW - EU-Definition KW - Nanopartikel PY - 2018 AN - OPUS4-45078 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -