TY - CONF A1 - Kuchenbecker, Petra A1 - Hodoroaba, Vasile-Dan A1 - Lindemann, Franziska A1 - Gemeinert, Marion A1 - Wohlleben, W. T1 - Advanced screening method using volume-specific surface area (VSSA) for nanomaterial classification of powders N2 - The EU recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. Within the European Project NanoDefine (www.nanodefine.eu) a two-tier approach has been developed, whereby firstly a screening method is applied for the rough classification as a nanomaterial or non-nanomaterial, and for borderline cases a confirmatory method (imaging methods or field flow fractionation) must be considered. One of the measurement methods well suited to particulate powder is the determination of volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nanomaterial or non-nanomaterial. The correct identification of a nanomaterial by VSSA method (positive test) is accepted by the EU recommendation. However, the application of the VSSA method is associated also by some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape. For particles containing micro-pores or having a microporous coating, false positive results will be produced. Furthermore, broad particle size distributions – as typically for ceramic materials – as well as multi-modal size distributions make necessary to adjust the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach will be tested (in relation with SEM and TEM measurements) in order to expand the actual knowledge and improve the method. T2 - Jahrestagung der Deutschen Keramischen Gesellschaft mit Symposium Hochleistungskeramik CY - München, Germany DA - 10.04.2018 KW - VSSA KW - Nanoparticles PY - 2018 AN - OPUS4-45097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Yamamoto, K. A1 - Grulke, E. A. A1 - Maurino, V. T1 - Shape controlled TiO2 nanoparticles as candidates for nano-CRM’s – an ISO case study N2 - Extraction of true, 3D shape (and size) of non-spherical nanoparticles (NPs) is associated with errors by conventional 2D electron microscopy using projection images. Significant efforts within the ISO technical committee TC 229 ‘Nanotechnologies’ are aimed at establishing accurate TEM and SEM measurement of NP size and shape as robust, standard procedures. Study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated titania nano-powder for which size and shape distribution of primary crystallites of irregular shape must be measured accurately. To be noticed is e. g. the fact that the measurement procedure allows only manual selection of the particles clearly distinguishable for analysis as well as manual definition of the contour of the imaged NPs. An inter-laboratory exercise on titania NPs (pure anatase, grown by hydrothermal synthesis) of well-defined non-spherical shape, i.e. bipyramidal has been recently started within ISO/TC 229 under similar conditions as for the irregular shaped titania. Overlapped particles were allowed to be considered, as long as they are clearly distinguishable. One decisive NP selection criterion was to analyze only those NPs with a roundness value below 0.7, i.e. the NPs laying on the support foil and, hence, with projection areas clearly deviating from perfect circles (R=1). The overall evaluation (for 15 labs) of the size descriptors (area, Feret, minFeret, perimeter) and shape descriptors (aspect ratio, roundness, compactness, extent) by analysis of variance is just to be finished and included in ISO/WD 21363 Nanotechnologies -- Protocol for particle size distribution by transmission electron microscopy. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Titanium oxide KW - Nanoparticles KW - Shape-controlled KW - Electron microscopy KW - Reference material PY - 2018 AN - OPUS4-44996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Bosse, H. T1 - Improved traceability chain of nanoparticle size measurements – the new EMPIR project nPSize N2 - Coming as response to the needs expressed by The European Commission mandating CEN, CENELEC and ETSI to develop European standards for methods that can characterize reliably manufactured nanomaterials, a new European metrology research project ‘nPSize - Improved traceability chain of nanoparticle size measurements’ has received funding for the next three years. The project will develop methods, reference materials and modelling to improve the traceability chain, comparability and compatibility for nanoparticle size measurements to support standardization. nPSize has selected only those nanoparticle sizing techniques which are able to provide traceable results: electron microscopy (SEM, TSEM and TEM), AFM and SAXS. Metrologists from national metrological or designated institutes (PTB, LNE, LGC, VSL, SMD and BAM) will work together with scientists with know-how in development of new nano reference nanoparticles (CEA, University of Turin, LGC, BAM) and with experts in advanced data processing, e.g. by machine learning (POLLEN). With the support of DIN, the project outcomes will be channelized to standardization bodies such as ISO/TC 229 ‘Nanotechnologies’/JWG 2 ‘Nanoparticle Measurement and Characterization’ (SEM, TSEM and TEM), CEN/TC 352 ‘Nanotechnologies’ (SEM, TSEM and TEM), ISO/TC 201/SC 9 (AFM), ISO/TC 24/SC 4 (SAXS). Three technical work packages will ensure input for impact to standardization community, nanoparticle manufacturers, instrument manufacturers, and (accredited) service laboratories: - WP1 Performance and traceability of characterization methods - WP2 Reference materials - Preparation and Characterization - WP3 Modelling and development of measurement procedures Well-defined non-spherical nanoparticles shapes such as cubes, platelets, bipyramids, rods/acicular will be developed, with mono- and polydisperse size distribution, as well as with accurate particle number concentration (by SAXS and isotopically enrichment for ICP-MS). Physical modelling of the signal for TSEM, SEM, 3D-AFM and SAXS will be used to feed machine learning modeling from a-priori measurement data. Further, data fusion will be developed for hybrid sizing techniques: SEM with TSEM/TEM, SEM/TSEM with AFM, SEM/TSEM with SAXS with the final aim of improving the true shape and size of non-spherical nanoparticles by a better estimation of the measurement uncertainties. In the second half-time of the project dedicated workshops (focused on method improvement and reference materials development) will be organized to disseminate the gained knowledge to end-users. Further, a data library with relevant tagged measurement data is planned to be organized and made publicly available. Inter-laboratory comparisons based on the newly developed multi-modal nano reference materials will be organized preferably within VAMAS/TWA 34 ‘Nanoparticle populations’. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Nanoparticles KW - Size KW - Shape KW - Traceable size PY - 2018 AN - OPUS4-44995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Mielke, Johannes A1 - Dohányosová, P. A1 - Müller, P. A1 - López-Vidal, S. T1 - Controlled electrospray deposition of nanoparticles for improved analysis by electron microscopy N2 - Of many experimental techniques for measuring particle sizes and size distributions, electron microscopy (EM) is considered as the gold standard, especially in the nano range (1–100 nm). Furthermore, high-resolution X-ray spectroscopy (EDX) in conjunction with EM can be applied to individual NPs. Preparation of an EM sample for generic particulate materials is a difficult task. Usually, the particles in a suspension are deposited on a support. However, this procedure includes the drying of larger solvent amounts on the substrate itself, and this can affect the spatial distribution of the deposited particles. One possibility to overcome this is the use of an electrospray system, where the suspension of particles is sprayed onto the substrate in charged droplets that are so small that they either dry off on the substrate immediately without affecting the position of particles, or even already during their flight time to the substrate. Additionally, the charging of particles minimizes agglomeration and aggregation, maximizing the collection of the EM grids. The prototype of an electrospray deposition system from RAMEM under its trademark IONER (www.ioner.eu) was tested. Electrospray is theoretically described since a long time, but no dedicated commercial instruments are available for the preparation of TEM grids yet, apart from electrostatic deposition of aerosols. Several materials have been sprayed onto TEM grids and the resulting particle distributions were evaluated. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles (suited to automatic analysis). The project has received funding from the European Union’s Seventh Programme for research, technological development and demonstration under grant agreement No 604347. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Nanoparticles KW - Electrospray KW - Electron microscopy PY - 2018 AN - OPUS4-44994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - XPS at BAM - Some insights into our activities N2 - Some examples will be given showing the application of XPS in different fields, like polymers, nanoparticles, solar cells and inorganic thin films. T2 - Besuch beim GFZ Potsdam CY - Potsdam, Germany DA - 18.05.2018 KW - XPS KW - Surface analytics KW - Nanoparticles KW - Polymers KW - Solar cells PY - 2018 AN - OPUS4-44981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert A1 - Müller, L. A1 - Traub, Heike A1 - Esteban-Fernández, D. A1 - Panne, Ulrich A1 - Wanka, Antje A1 - Kneipp, J. T1 - Method development for metal detection at cellular levels by ICP-MS N2 - An overview about different analytical approaches will be presented of how to detect metals in individual biological cells by use of ICP-MS. For this purpose, we are using different sample introduction systems for ICP-MS for detection, imaging and quantification of metals at cellular levels. By use of laser ablation, we have studied the up-take by and distribution of nanoparticles in single cells. Recently we have developed staining techniques to measure protein and DNA content of cells and identifying the cell status by immunoassays using metal-tagging of antibodies. New research based on cell arrays will be shortly discussed. Using pneumatic nebulization and microdroplet generation, we have also studied the up-take of nanoparticles and toxic metals as well as essential elements in single cells using different ICP-MS mass spectrometric concepts (sector field instrument, triple-quad instrument, time of flight (CyTOF) instrument). The different ICP-MS based methods will be compared concerning their analytical figures of merit and their strengths and weaknesses will be evaluated. T2 - Projektmeeting CY - Bremen, Germany DA - 18.04.2018 KW - Single cell ICP-MS KW - LA-ICP-MS with cellular resolution KW - Nanoparticles PY - 2018 AN - OPUS4-44851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya A1 - Moser, Marko A1 - Geißler, Daniel A1 - Behnke, Thomas A1 - Resch-Genger, Ute T1 - Multimodal cleavable reporters vs conventional labels for optical quantification of amino and carboxy groups on nanomaterials and microparticles N2 - Carboxy, amino, and thiol groups play a critical role in a variety of physiological and biological processes and are frequently used for bioconjugation reactions. Moreover, they enable size control and tuning of the surface during the synthesis of particle systems. Especially, thiols have a high binding affinity to noble metals and semiconductors (SC). Thus, simple, inexpensive, robust, and fast methods for the quantification of surface groups and the monitoring of reactions involving ligands are of considerable importance for the characterization of modified or stabilized nanomaterials including polymers. We studied the potential of the Ellman’s assay, recently used for the quantification of thiol ligands on SC nanocrystals by us1 and the 4-aldrithiol assay for the determination of thiol groups in molecular systems and on polymeric, noble and SC nanomaterials. The results were validated with ICP-OES and reaction mechanisms of both methods were studied photometrically and with ESI-TOF-MS. The investigation of the reaction mechanisms of both methods revealed the influence of different thiols on the stoichiometry of the reactions2, yielding different mixed disulfides and the thiol-specific products spectroscopically detected. The used methods can quantify freely accessible surface groups on nanoparticles, e.g., modified polystyrene nanoparticles. For thiol ligands coordinatively bound to surface atoms of, e.g., noble or SC nanomaterials, depending on the strength of the thiol-surface bonds, particle dissolution prior to assay performance can be necessary. We could demonstrate the reliability of the Ellman’s and aldrithiol assay for the quantification of surface groups on nanomaterials by ICP-OES and derived assay-specific requirements and limitations. Generally, it is strongly recommended to carefully control assay performance for new samples, components, and sample ingredients to timely identify possible interferences distorting quantification. T2 - BAM-BfR Seminar 2018 CY - Berlin, Germany DA - 15.02.2018 KW - Surface functionalization KW - Nanoparticles KW - Surface chemistry KW - Multimodal reporters PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Nirmalananthan-Budau, Nithiya A1 - Moser, Marko A1 - Geißler, Daniel A1 - Behnke, Thomas A1 - Schneider, Ralf T1 - Simple and Versatile Methods for Quantifying Functional Groups, Ligands, and Biomolecules on Nanomaterials N2 - Many applications of nanomaterials in the life sciences require the controlled functionalization of these materials with ligands like polyethylene glycol (PEG) and/or biomolecules such as peptides, proteins, and DNA. This enables to tune their hydrophilicity and biocompatibility, minimize unspecific interactions, improve biofunctionalization efficiencies, and enhance blood circulation times. Moreover, it is the ultimate prerequisite for their use as reporters in assays or the design of targeted optial probes for bioimaging. At the core of these functionalization strategies are reliable and validated methods for surface group and ligand quantification that can be preferably performed with routine laboratory instrumentation, require only small amounts of substances, and are suitable for many different types of nanomaterials. We present here versatile and simple concepts for the quantification of common functional groups, ligands, and biomolecules on different types of organic and inorganic nano-materials, using different types of optical reporters and method validation with the aid of multimodal reporters, method comparisons, and mass balances. T2 - INNANOPART open day CY - London, UK DA - 24.04.2018 KW - Surface functionalization KW - Nanoparticles KW - Surface chemistry KW - Multimodal reporters PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44849 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 A1 - Mielke, Johannes A1 - Dohányosová, P. A1 - Müller, P. A1 - López-Vidal, S. T1 - Controlled deposition of nanoparticles by electrospray for improved analysis by imaging techniques N2 - Of many experimental techniques for measuring particle sizes and size distributions, electron microscopy (EM) is still considered as the gold standard, especially in the nano range (1–100 nm). Furthermore, high-resolution X-ray spectroscopy (EDX) in conjunction with EM can be applied to individual NPs. Preparation of an EM sample for generic particulate materials is a difficult task. Usually the particles in a suspension are deposited on a support. However, this procedure includes the drying of larger solvent amounts on the substrate itself, and this can affect the spatial distribution of the deposited particles. One possibility to overcome this is the use of an electrospray system, where the suspension of particles is sprayed onto the substrate in charged droplets that are so small that they either dry off on the substrate immediately without affecting the position of particles, or even already during their flight time to the substrate. Additionally, the charging of particles minimizes agglomeration and aggregation, maximizing the collection of the EM grids. The prototype of an electrospray deposition system from RAMEM under its trademark IONER (www.ioner.eu) was tested. Electrospray is theoretically described since a long time, but no dedicated commercial instruments are available for the preparation of TEM grids yet, apart from electrostatic deposition of aerosols.2 Several materials have been sprayed onto TEM grids and the resulting particle distributions were evaluated. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles (suited to automatic analysis). T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Electrospray deposition KW - Nanoparticles KW - Electron microscopy PY - 2018 AN - OPUS4-44802 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 - Jakubowski, Norbert A1 - Müller, L. A1 - Traub, Heike A1 - Esteban-Fernández, D. A1 - Panne, Ulrich A1 - Wanka, Antje A1 - Schellenberger, E. A1 - Theuring, F. A1 - Kneipp, J. T1 - Method development for metal detection at cellular levels by ICP-MS N2 - An overview about different analytical approaches will be presented of how to detect metals in individual biological cells by use of ICP-MS. For this purpose, we are using different sample introduction systems for ICP-MS for detection, imaging and quantification of metals at cellular levels. By use of laser ablation, we have studied the up-take by and distribution of nanoparticles in single cells. Recently we have developed staining techniques to measure protein and DNA content of cells and identifying the cell status by immunoassays using metal-tagging of antibodies. New research based on cell arrays will be shortly discussed. Using pneumatic nebulization and microdroplet generation, we have also studied the up-take of nanoparticles and toxic metals as well as essential elements in single cells using different ICP-MS mass spectrometric concepts (sector field instrument, triple-quad instrument, time of flight (CyTOF) instrument). The different ICP-MS based methods will be compared concerning their analytical figures of merit and their strengths and weaknesses will be evaluated. T2 - ACS Annual Meeting CY - New Orleans, LA, USA DA - 18.03.2018 KW - Single cell ICP-MS KW - LA-ICP-MS with cellular resolution KW - Nanoparticles PY - 2018 AN - OPUS4-44799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Müller, Anja A1 - Schneider, Markus A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Chemical Analysis of Core-Shell Nanoparticles using ToF-SIMS and XPS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behavior. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layer and thus gives us an idea of the interactions involved. Here, we present initial data on the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Furthermore, principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - XPS KW - ToF-SIMS KW - Nanoparticles PY - 2018 AN - OPUS4-44795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Sparnacci, K. A1 - Unger, Wolfgang A1 - Schneider, Markus A1 - Müller, Anja T1 - Chemical Analysis of Core-Shell Nanoparticles using ToF-SIMS and XPS N2 - The analysis of nanomaterials is current an important task - especially in case of risk assessment, as the properties of these material class are not well understood currently. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surfaces chemical composition has to be investigated to get a better understanding and prediction of the nanomaterials' behavior. ToF-SIMS has proven as a powerful tool to determine said chemical composition. Its superior surface sensitivity allows us to study mainly the utmost atomic layer and therefore gives us an idea of the interactions involved. Here, we show first result from the validation of the method for the analysis of polystyrene and gold nanoparticles. ToF-SIMS will be compared to other methods like XPS, T-SEM or REM. Furthermore, principle component analysis (PCA) will be used to detect the influence of different sample preparation performed by an innovative microfluidic device. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - XPS KW - ToF-SIMS KW - Nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - nPSize - Improved traceability chain of nanoparticle size measurements N2 - The overall objective of project Improved traceability chain of nanoparticle size measurements is to improve the traceability chain for nanoparticle size measurements. The main impact will be achieved by manifold contributions to standard documents for CEN/TC 352 “Nanotechnologies”, which directly addresses the research needs of CEN, CENELEC and ETSI mandated by EC to develop standards for methods and reference materials to accurately measure the size and size distribution of nanoparticles. This will take place in collaboration with ISO/TC229 ‘Nanotechnologies’, ISO/TC24/SC4 ‘Particle characterization’ and ISO/TC201 ‘Surface analysis’/ SC9 ‘Scanning probe microscopy’. T2 - 4. Sitzung des wissenschaftlichen Beirats zum Themefeld Umwelt der BAM CY - BAM, Berlin, Germany DA - 13.04.2018 KW - Nanoparticles KW - Nanoparticle size KW - Traceability KW - Standardization PY - 2018 AN - OPUS4-44695 LA - eng 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 - Müller, Anja A1 - Schneider, Markus A1 - Heinrich, Thomas T1 - Surface chemical analysis of engineered nanoparticles by means of transmission x-ray microscopy and mass spectrometry N2 - PTFE/PS core-shell-nanoparticles were characterised by STXM, T-SEM, and ToF-SIMS. Shell-thicknesses were calculated and compared. Preliminary results from ToF-SIMS showed the capabilities of this method. T2 - BAM-BfR Seminar CY - Berlin, Germany DA - 15.02.2018 KW - STXM KW - NEXAFS KW - ToF-SIMS KW - SEM KW - Nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44181 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mielke, Johannes A1 - Babick, F. A1 - Uusimäki, T. A1 - Müller, P. A1 - Verleysen, E. A1 - Hodoroaba, Vasile-Dan T1 - Evaluation of electron microscopy techniques for the purpose of classification of nanomaterials N2 - One current and much-debated topic in the characterization of nanomaterials (NM) is the implementation of the recently introduced recommendation on a definition of a nanomaterial by the European Commission. All currently available sizing techniques able to address nanoparticles were systematically evaluated. It was demonstrated that particle sizing techniques like: analytical centrifugation, particle tracking analysis, single-particle inductively coupled plasma mass-spectrometry, differential electrical mobility analysis, dynamic light scattering, small angle X-ray scattering, ultrasonic attenuation spectrometry, but also gas Adsorption analysis based on the BET-method can be applied for a screening classification. However, the quality of the results depends on the individual material to be classified. For well-dispersed, nearly spherical (nano)particles most of the sizing techniques can be applied in a quick and reliable way. In contrast, the classification of most real-world materials is a challenging task, mainly due to non-spherical particle shape, large polydispersity or strong agglomeration/ aggregation of the particles. In the present study it was shown that these issues can be resolved in most cases by electron microscopy as a confirmatory classification technique. Electron microscopy techniques such as TEM, STEM, SEM or TSEM transmission in SEM) are capable of assessing the size of individual nanoparticles accurately (see Figures 1 and 2). Nevertheless the challenging aspect is sample preparation from powder or liquid form on the substrate, so that a homogeneous distribution of well-separated (deagglomerated) particles is attained. The systematic study in this work shows examples where the extraction of the critical, smallest particle dimension - as the decisive particle parameter for the classification as a NM - is possible by analysing the sample after its simple, dry preparation. The consequences of additional typical issues like loss of information due to Screening of smaller particles by larger ones or the (in)ability to access the constituent particles in aggregates are discussed. T2 - European Microscopy Congress emc 2016 CY - Lyon, France DA - 28.08.2016 KW - Nanomaterial classification KW - Nanoparticles KW - Electron microscopy PY - 2016 SN - 9783527808465 DO - https://doi.org/10.1002/9783527808465.EMC2016.5767 SP - 13 EP - 14 PB - Wiley-VCH AN - OPUS4-44087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reuther, R. A1 - Marvin, H. A1 - Müller, P. A1 - Löschner, K. A1 - Hodoroaba, Vasile-Dan A1 - Stintz, M. A1 - Kammer, F. v. d. A1 - Köber, R. A1 - Rauscher, H. T1 - A new tiered analytical approach and e-Tool for material classification to support the implementation of the EU Nano-Definition N2 - The EC recommendation for the definition of nanomaterial [2011/696/EU] requires the quantitative size determination of constituent particles in samples down to 1 nm. Accordingly, a material is a nanomaterial if 50 % or more of the particles are in the size range 1-100 nm. The fact that engineered nanomaterials already exist in many industrial and consumer products challenges the development of measurement methods to reliably identify, characterize and quantify their occurrence as substance and in various matrices. The EU FP7 NanoDefine project [www.nanodefine.eu] has addressed this challenge by developing a robust, readily implementable and cost-effective measurement strategy to obtain quantitative particle size distributions and to distinguish between nano and non-nano materials according to the EU definition. Based on a comprehensive evaluation of existing methodologies and intra- and inter-lab comparisons, validated measurement methods and instrument calibration procedures have been established to reliably measure the size of particles within 1-100 nm, and beyond, including different shapes, coatings and chemical compositions in industrial materials and consumer products. Case studies prove their applicability for various sectors, including food, pigments and cosmetics. Main outcome is the establishment of an integrated tiered approach including rapid screening (tier 1) and confirmatory methods (tier 2), and a user manual to guide end-users, such as manufacturers, in selecting appropriate methods. Another main product is the “NanoDefiner” e-Tool allowing the standardised / semi-automated selection of appropriate methods for material classification according to the EU definition. Results also contribute to standardization efforts, such as CEN TC 352 or ISO TC 229. T2 - EuroNanoForum 2017 CY - Valletta, Malta DA - 21.06.2017 KW - Nanomaterial classification KW - Nanoparticles KW - EC definition of nanomaterial KW - Tiered approach PY - 2017 UR - http://euronanoforum2017.eu/ AN - OPUS4-43993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, R. A1 - Hodoroaba, Vasile-Dan T1 - SEM or TEM for the characterization of nanoparticles? N2 - Scanning Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM) ? This is a question, nowadays discussed in EM labs of research and industry involved in the characterization and metrology of nanoparticles. The Scanning principle is adapted to TEM, the Transmission mode is adapted to Ultra High Resolution SEM. Can modern SEM replace TEM, reach atomic resolution even without Cs corrector or nm lateral resolution for energydispersive X-ray spectroscopy (EDX)? Due to the development of a New Cold Field Emission (NCFE) electron source Hitachi SEMs SU9000 and SU8200 can deliver routinely sub-nm image resolution and EDX mappings at very high count rates and a lateral EDX resolution of a few nm. A TiO2 sample provided by BAM was analysed at 30kV using low kV STEM – simultaneously with the Through-the-lens (TTL) SE detector, the Bright Field transmitted and Dark Field transmitted signals. By this method a pixel precise information of the particles surface using SE, its chemical nature using DF-STEM and its crystalline structure using Bright Field signal is given in one 40sec scan. The advantage of this observation mode compared to Ultra Low Voltage imaging is outlined. T2 - Microscopy Conference 2017 CY - Lausanne, Switzerland DA - 21.08.2017 KW - SEM KW - TEM KW - Nanoparticles PY - 2017 UR - http://www.mc2017.ch/ AN - OPUS4-43890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -