TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement N2 - In order to assess new nanomaterials and nanoparticles for potential risks to health and the environment, they need to be well-characterised. The measurement of constituent nanoparticle size, shape, and size distribution are important factors for the risk evaluation process. EMPIR project Improved traceability chain of nanoparticle size measurements (17NRM04, nPSize) is working to assess a range of traceable nanoparticle measurement approaches, including Electron Microscopy (SEM, TEM, STEM-in-SEM), Atomic Force Microscopy and Small Angle X-ray Scattering, and deliver improved calibration methods to users. For the techniques under investigation, physical models of their response to a range of nanoparticle types are developed. Validated reference materials are also used for inter-comparisons of measurement systems, with an evaluation of the associated measurement uncertainty. With project contributions to standards development work, manufacturers will be better placed to assess the human and environmental risks posed by nanomaterials across a whole range of products. T2 - EMPIR nPSize Training Course "Traceable Characterization of Nanoparticles by SAXS" CY - Online meeting DA - 01.02.2021 KW - Nanoparticles KW - Particle size distribution KW - Traceability KW - nPSize KW - SAXS PY - 2021 AN - OPUS4-53883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Feltin, N. A1 - Crouzier, L. A1 - Cios, G. A1 - Tokarski, T. T1 - Correlative imaging analysis of non-spherical nanoparticles N2 - It sounds like being a simple analytical task, it is definitely not. The way toward accurate measurement of the size distribution of nanoparticles (NPs) with complex shape, having a broad size polydispersity, with inhomogeneous chemistry, and with a high degree of agglomeration/aggregation is very challenging for all available analytical methods. Particularly for the NPs with complex shape, the access to the smallest dimension (as e.g. required for regulatory purposes) can be enabled only by using imaging techniques with spatial resolution at the nanoscale. Moreover, the full 3D-chacterisation of the NP shape can be provided either by advanced characterization techniques like 3D-TEM tomography or by correlative analysis, i. e. synergetic/complementary measurement of the same field-of-view of the sample with different probes. Examples of the latter type of analysis are: i) electron microscopy for the lateral dimensions and AFM for the height of the NPs, ii) SEM with STEM-in-SEM (also called T-SEM), iii) Electron Microscopy with TKD (Transmission Kikuchi Diffraction) for determination of the geometrical orientation of crystalline NPs, iv) Raman and SEM for e.g. thickness of graphen flakes, or v) Electron Microscopy for descriptive NP shape and SAXS for the NP concentration, the latter as a NP property able to be measured with higher and higher accuracy. For all these types of measurement, reference NPs are necessary for the validation of the measured size. Particularly non-spherical reference NPs are still missing. Examples of such new reference NPs as characterized by the correlative analyses enumerated above will be presented in detail in the contribution. T2 - 2021 Fall Meeting of the European Materials Research Society (E-MRS) CY - Online meeting DA - 20.9.2021 KW - Nanoparticles KW - Transmission Kikuchi Diffraction (TKD) KW - Correlative imaging KW - Electron microscopy KW - AFM KW - TiO2 KW - VAMAS PY - 2021 UR - https://www.european-mrs.com/meetings/2021-fall-meeting AN - OPUS4-53367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Kuchenbecker, Petra A1 - Hodoroaba, Vasile-Dan A1 - Rabe, Torsten T1 - Comparative study of suitable preparation methods to evaluate irregular shaped, polydisperse nanoparticles by scanning electron microscopy (SEM). N2 - Reliable characterization of materials at the nanoscale regarding their physio-chemical properties is a challenging task, which is important when utilizing and designing nanoscale materials. Nanoscale materials pose a potential toxicological hazard to the environment and the human body. For this reason, the European Commission amended the REACH Regulation in 2018 to govern the classification of nanomaterials, relying on number-based distribution of the particle size. Suitable methods exist for the granulometric characterization of monodisperse and ideally shaped nanoparticles. However, the evaluation of commercially available nanoscale powders is problematic. These powders tend to agglomerate, show a wide particle size distribution and are of irregular particle shape. Zinc oxide, aluminum oxide and cerium oxide with particle sizes less than 100 nm were selected for the studies and different preparation methods were used comparatively. First, the nanoparticles were dispersed in different dispersants and prepared on TEM-supported copper grids. Furthermore, individual powders were deposited on carbon-based self-adhesive pads. In addition, the samples were embedded by hot mounting and then ground and polished. The prepared samples were investigated by scanning electron microscopy (including the transmission mode STEM-in-SEM) and Dynamic Light scattering. The software package ImageJ was used to segment the SEM images and obtain the particle sizes and shapes and finally the number-based particles size distribution with size expressed as various descriptors. T2 - Ceramics 2021 CY - Online meeting DA - 19.04.2021 KW - Nanoparticles KW - Preparation KW - Characterization PY - 2021 AN - OPUS4-53272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - VAMAS TWA 37 - Quantitative Microstructural Analysis & Liaison with ISO/TC 202 Microbeam Analysis, Liaison with ISO N2 - The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. Further, a short overview of the VAMAS areas of activities is given where Germany is involved. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 46th Steering Committee Meeting CY - Online meeting DA - 08.09.2021 KW - VAMAS KW - Nanoparticles KW - Standardisation KW - Inter-laboratory comparison KW - ISO/TC 202 KW - ISO/TC 229 KW - ISO/TC 201 KW - Microstructure KW - EBSD PY - 2021 UR - http://www.vamas.org/twa/ AN - OPUS4-53237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Hörenz, Christoph A1 - Pellegrino, F. A1 - Maurino, V. A1 - Durand, B. A1 - Taché, O. T1 - Nanoparticle size, shape, and concentration measurement at once – two VAMAS pre-standardization projects ready to start N2 - A case study on the TEM analysis of the size and shape distribution of TiO2 bipyramidal nanoparticles prepared on TEM grids was included in the recently published ISO standard ISO 21363. It was agreed to organize at a later stage a second inter-lab comparison with the nanoparticles distributed to the participants as a liquid suspension. Protocols for uniform nanoparticle deposition on suited supports developed and optimized within the EMPIR nPSize project are also prepared to be distributed. For this, we have chosen the VAMAS platform (www.vamas.org) which offers an excellent international infrastructure of laboratories with high competence in nanoparticle measurement. The VAMAS technical working area dedicated to nanoparticle measurement is TWA 34 ‘Nanoparticle populations’. For this type of nanoparticles, the size and shape distributions are the primary parameters to be reported. Due to the good deposition protocols developed, an automated image analysis is enabled (in contrast to the manual analysis of irregular TiO2 nanoparticles. In parallel with the TiO2 nanoparticle exercise, two spherical SiO2 nanoparticle samples with bi-modal size distributions (nominal relative number concentrations of 1:1 and 10:1) are prepared for a second VAMAS inter-lab comparison. Here, the nanoparticle concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations of the two modes. For the absolute nanoparticle concentration to be measured by imaging methods it is necessary to control the volume of the liquid suspension deposited on the substrate and to obtain such a homogeneous nanoparticle deposition on the substrate which allows to count (or extrapolate) all the deposited particles. KW - Electron microscopy KW - Inter-laboratory comparison KW - Nanoparticles KW - SiO2 KW - TiO2 KW - VAMAS PY - 2021 DO - https://doi.org/10.1017/S1431927621008126 VL - 27 IS - Suppl. 1 SP - 2250 EP - 2251 PB - Cambridge University Press AN - OPUS4-53124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strommer, Bettina A1 - Böhning, Martin A1 - Schulze, Dietmar A1 - Schartel, Bernhard T1 - Natural Rubber Nanocomposites via Optimized Latex Premixing and Conventional Technical Processing N2 - Creation of highly functional materials and replacement of high amounts of conventional fillers are driving forces for the development of nanocomposites. Besides the type and properties of nanoparticles, their dispersing in the elastomeric matrix and the stability of this dispersion through all processing steps are the main factors for the resulting performance of the produced material. Therefore, a preparation chain via latex premixing to a highly filled masterbatch, followed by conventional technical processing is to be developed. Three types of carbon-based particles are characterized as such (SEM, Raman Spectroscopy, BET specific surface area) and in combination with natural rubber, as nanocomposites (TEM. Hardness, Abrasion resistance, Compression set, Cone calorimetry). All of the studied particles lead to an improvement in the investigated mechanical properties, the extent of reinforcement depends strongly on the specific surface of the particle interacting with the elastomeric matrix in combination with their shape. T2 - DKG Elastomer Symposium CY - Online meeting DA - 28.06.2021 KW - Processing KW - Elastomers KW - Nanocomposites KW - Graphene KW - Nanoparticles KW - Latex KW - Natural rubber PY - 2021 AN - OPUS4-53106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Hörenz, Christoph A1 - Pellegrino, F. A1 - Maurino, V. A1 - Durande, B. A1 - Taché, O. T1 - Nanoparticle size, shape, and concentration measurement at once – two VAMAS pre-standardization projects ready to start N2 - A case study on the TEM analysis of the size and shape distribution of TiO2 bipyramidal nanoparticles prepared on TEM grids was included in the recently published ISO standard ISO 21363. It was agreed to organize at a later stage a second inter-lab comparison with the nanoparticles distributed to the participants as a liquid suspension. Protocols for uniform nanoparticle deposition on suited supports developed and optimized within the EMPIR nPSize project are also prepared to be distributed. For this, we have chosen the VAMAS platform (www.vamas.org) which offers an excellent international infrastructure of laboratories with high competence in nanoparticle measurement. The VAMAS technical working area dedicated to nanoparticle measurement is TWA 34 ‘Nanoparticle populations’. For this type of nanoparticles, the size and shape distributions are the primary parameters to be reported. Due to the good deposition protocols developed, an automated image analysis is enabled (in contrast to the manual analysis of irregular TiO2 nanoparticles. In parallel with the TiO2 nanoparticle exercise, two spherical SiO2 nanoparticle samples with bi-modal size distributions (nominal relative number concentrations of 1:1 and 10:1) are prepared for a second VAMAS inter-lab comparison. Here, the nanoparticle concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations of the two modes. For the absolute nanoparticle concentration to be measured by imaging methods it is necessary to control the volume of the liquid suspension deposited on the substrate and to obtain such a homogeneous nanoparticle deposition on the substrate which allows to count (or extrapolate) all the deposited particles. T2 - Microscopy and Microanalysis 2021 CY - Online meeting DA - 01.08.2021 KW - Nanoparticles KW - Electron microscopy KW - VAMAS KW - Inter-laboratory comparison KW - TiO2 KW - SiO2 PY - 2021 AN - OPUS4-53065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennet, Francesca A1 - Burr, L. A1 - Schmid, D. A1 - Hodoroaba, Vasile-Dan T1 - Towards a method for quantitative evaluation of nanoparticle from suspensions via microarray printing and SEM analysis N2 - As part of the development of a library of accurate and efficient methods for measurement of nanoparticle properties, we develop and optimize a method for the efficient analysis of nanoparticle size distribution from suspensions via microprinting and digital analysis of electron microscopy (SEM and TEM) images, with the ultimate aim of automated quantitative concentration analysis (calculated from drop volume). A series of different nanoparticle suspensions (gold, latex, and SiO2 in varying sizes and concentrations) were printed onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 nanoparticles/mL and imaged with SEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee-ring effect. KW - Nanoparticles KW - Particle size distribution KW - Electron microscopy KW - Microarray printing KW - Sample preparation KW - Nanoparticle concentration PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528455 DO - https://doi.org/10.1088/1742-6596/1953/1/012002 VL - 1953 SP - 012002 PB - IOP Publishing AN - OPUS4-52845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Hörenz, Christoph A1 - Mansfeld, Ulrich A1 - Pellegrino, F. A1 - Maurino, V. A1 - Marguet, S. A1 - Testard, F. A1 - Taché, O. A1 - Bartczak, D. A1 - Nunez, S. A1 - Abad Alvaro, I. A1 - Goenaga-Infante, H. 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 A1 - Schmitt, M. 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 - GEN A1 - Hodoroaba, Vasile-Dan A1 - Hörenz, Christoph T1 - Improving nanoparticle size measurement accuracy for safety assessment N2 - Nanomaterials and nanoparticles are finding applications across a wide range of technology sectors, from medicine and food to transportation and construction. In order to assess these new materials for potential risks to health and the environment, they need to be well-characterised. The measurement of constituent nanoparticle size, shape, and size distribution are important factors for the risk evaluation process. EMPIR project Improved traceability chain of nanoparticle size measurements (17NRM04, nPSize) is working to assess a range of traceable nanoparticle measurement approaches, including Scanning Electron Microscopy (also in Transmission Mode), Atomic Force Microscopy and Small Angle X-ray Scattering, and deliver improved calibration methods to users. For the techniques under investigation, physical models of their response to a range of nanoparticle types are developed. Validated reference materials will also be used for an inter-comparison of measurement systems, with an evaluation of the associated measurement uncertainty. With project contributions to standards development work, manufacturers will be better placed to assess the human and environmental risks posed by nanomaterials across a whole range of products. KW - Nanoparticles KW - Particle size distribution KW - Traceability KW - Electron microscopy KW - AFM KW - SAXS PY - 2021 UR - https://www.euramet.org/?L=0&news=40%3A1159 SP - 1 PB - EURAMET e.V. CY - Braunschweig AN - OPUS4-52129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Minimum Requirements for Nanomaterial Data - Examples with Electron Microscopy and Energy-Dispersive X-Ray Spectroscopy N2 - In dem Vortrag werden, anhand ausgewählten Beispielen aus der Elektronenmikroskopie und EDX-Elementanalyse, die minimalen Anforderungen an Referenzdaten für zuverlässige und reproduzierbare Ergebnisse (z.B. Partikelgrößenverteilung, Elementzusammensetzung) bei der Charakterisierung von Nanomaterialien vorgestellt und diskutiert. N2 - Based on practical examples of analysis with Electron Microscopy and Energy-Dispersive X-ray Spectroscopy, the minimum information requirements for reliable and reproducible nanomaterial characterization data such as particle size and shape distribution and elemental analysis are presented and discussed. T2 - nano@BAM-Workshop Digitalisierung in der Nanosicherheit CY - Online meeting DA - 04.12.2020 KW - Nanoparticles KW - Electron microscopy KW - EDX KW - Reference data KW - Reproducibility KW - Standardisation PY - 2020 AN - OPUS4-51775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rühle, Bastian A1 - Hodoroaba, Vasile-Dan T1 - Towards Automated Electron Microscopy Image Segmentation for Nanoparticles of Complex Shape by Convolutional Neural Networks N2 - In this contribution different ways are explored with the aim to generate suitable training data for ‘non-ideal’ samples using various approaches, e.g., computer-generated images or unsupervised learning algorithms such as generative adversarial networks (GANs). We used these data to train simple CNNs to produce segmentation masks of SEM images and tested the trained networks on real SEM images of complex nanoparticle samples. The novel use of CNN for the automated analysis of the size of nanoparticles of complex shape and with a high degree of agglomeration has proved to be a promising tool for the evaluation of particle size distribution on a large number of constituent particles. Further development and validation of the preliminary model, respectively larger training and validation data sets are necessary. KW - Nanoparticles KW - Convolutional neural networks KW - Image segmentation KW - Electron microscopy KW - Automatisation PY - 2020 DO - https://doi.org/10.1017/S1431927620017262 VL - 26 IS - S2 SP - 1188 EP - 1189 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Cios, G. A1 - Tokarski, T. A1 - Mansfeld, Ulrich A1 - Ortel, Erik A1 - Mielke, Johannes A1 - Pellegrino, F. A1 - Maurino, V. T1 - Towards 3D Understanding of Non-spherical Nanoparticles by Transmission Kikuchi Diffraction (TKD) for Improved Particle Size Distribution by Electron Microscopy N2 - In this paper one refined approach is applied to determine the exact orientation of bipyramidal TiO2 nanoparticles prepared with good dispersion as almost isolated particles on a carbon TEM grid. The advantages of the recently developed high-throughput Transmission Kikuchi Diffraction (TKD) are used to identify quickly and reliably the geometrical orientation of the crystalline TiO2 nanoparticle bipyramids (anatase) on a statistically relevant number of particles. KW - Nanoparticles KW - Transmission Kikuchi Diffraction (TKD) KW - Electron microscopy KW - TiO2 KW - 3D PY - 2020 DO - https://doi.org/10.1017/S1431927620013999 VL - 26 IS - S2 SP - 260 EP - 261 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hörenz, Christoph A1 - Tache, O. A1 - Bartczak, D. A1 - Nunez, S. A1 - Abad Alvaro, I. A1 - Goenaga-Infante, H. A1 - Hodoroaba, Vasile-Dan T1 - A Study on the Analysis of Particle Size Distribution for Bimodal Model Nanoparticles by Electron Microscopy N2 - The present study addresses the capability of measurement of relative particle number concentration by scanning electron microscopy for model bimodal silica and gold samples prepared in the frame of the European research project “nPSize - Improved traceability chain of nanoparticle size measurements” as candidate reference nanoparticles. KW - Nanoparticles KW - Particle size distribution KW - Bimodal size distribution KW - Traceability PY - 2020 DO - https://doi.org/10.1017/S1431927620021054 VL - 26 IS - S2 SP - 2282 EP - 2283 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph A1 - Pellegrino, F. A1 - Maurino, V. A1 - Taché, O. A1 - Bartczak, D. A1 - Cuello Nuñez, S. A1 - Abad Álvaro, I. A1 - Goenaga Infante, H. A1 - Hodoroaba, Vasile-Dan T1 - Improved Sample Preparation for the Analysis of Nanoparticles by Electron Microscopy N2 - In this work, we present various promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded number ratios resembling the nominal number ratios. The reliable measurement of the NP concentration of polydisperse samples by electron microscopy, even if relative, is new and of special relevance because up to now only the size of the particles, i.e. the abscissa of the PSD, can be measured reliably. T2 - NANOSAFE 2020 CY - Online meeting DA - 16.11.2020 KW - Nanoparticles KW - Particle size distribution KW - Electron microscopy KW - Bimodal KW - SiO2 KW - Gold PY - 2020 AN - OPUS4-51714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Improved Sample Preparation for the Analysis of Nanoparticles by Electron Microscopy N2 - Various promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM are presented. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded number ratios resembling the nominal number ratios. The reliable measurement of the NP concentration of polydisperse samples by electron microscopy, even if relative, is new and of special relevance because up to now only the size of the particles, i.e. the abscissa of the PSD, can be measured reliably. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - Particle size distribution KW - Sample peparation KW - Electron microscopy PY - 2020 AN - OPUS4-51716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bennet, Francesca A1 - Burr, L. A1 - Schmid, D. A1 - Hodoroaba, Vasile-Dan T1 - Towards a method for quantitative evaluation of nanoparticles in suspension via Microprinting and SEM analysis N2 - A series of different nanoparticle suspensions (Gold, Latex, and SiO2 in varying concentrations) were microprinted onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 NP/mL and imaged with SEM and TSEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee ring effect. T2 - nanoSAFE 2020 CY - Online meeting DA - 16.11.2020 KW - Nanoparticles KW - Microprinting KW - Image analysis PY - 2020 AN - OPUS4-51699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria A1 - Kulla, Hannes A1 - Prinz, Carsten A1 - Bienert, Ralf A1 - Marquardt, Julien A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska T1 - Synthesis of Bimetallic Nickel Nanoparticles as Catalysts for the Sabatier Reaction N2 - Nanoparticles (NP) have become important materials for a variety of chemical technologies. The enhance surface-area-to-volume ratio of NPs is very high, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni nanoparticles were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the catalytically active sites are accessible. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - Joint Polish-German Crystallographic Meeting CY - Wroclaw, Poland DA - 24.02.2020 KW - Nanoparticles KW - Synthesis KW - Catalysis PY - 2020 AN - OPUS4-51663 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 - Outcomes for the Strategy/Metrology Groups of ISO/TC 229 Nanotechnologies N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, VAMAS inter-laboratory comparisons) to be standardized and implemented in accredited analytical laboratories is discussed. Complementation and/or filling gaps of published and ongoing standardisation projects on size, shape and number concentration measurements under ISO/TC 229/JWG 2 are offered. T2 - Annual Meeting of ISO/TC 229 Nanotechnologies - Strategy and Metrology Groups CY - Online meeting DA - 06.11.2020 KW - Nanoparticles KW - Size KW - nPSize KW - Inter-laboratory comparison KW - ISO/TC 229 KW - VAMAS PY - 2020 AN - OPUS4-51544 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; nPSize offer after 2 Ys N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, VAMAS inter-laboratory comparisons) to be standardized and implemented in accredited analytical laboratories is discussed. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - Size KW - Shape KW - Traceability KW - EMPIR KW - Reference materials KW - VAMAS PY - 2020 AN - OPUS4-51477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Feltin, N. T1 - Hybrid metrology for microscopy of nanoparticles N2 - This presentation is structured in two parts: i) Hybrid metrology by combining SEM with AFM (N. Feltin) and ii) hybridization and corelative microscopy by SEM, STEM-in-SEM, TEM, EDS, Auger Electron Microscopy, TKD and more (D. Hodoroaba). The first part is focused on the metrological part of the hybrid measurement SEM-AFM, the second part offers some further possibilities of correlative microscopy of nanoparticles based on practical examples. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - SEM KW - AFM KW - Metrology KW - Particle size distribution KW - Correlative imaging KW - STEM-in-SEM (TSEM) PY - 2020 AN - OPUS4-51476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hahn, Marc Benjamin T1 - TOPAS cell model with nanoparticles N2 - These files contain cell models for TOPAS/Geant4 and the inclusion of nano particles in particle scattering simulations. A simple spherical cell with nanoparticles can be generated in a fast manner. The user has the option to include the following organelles: nucleus, mitochondria, cell membrane. Additionally nanoparticles can be included in the cytosol and at the surface of the nucleus and/or the mitochondria. The C++ classes in this repository extend the functionality of the TOPAS (http://www.topasmc.org/) Monte-Carlo program, which is itself a wrapper of the Geant4 MCS Toolkit (http://geant4.org). The sourcecode together with examples and scorers are provided. "If you use this extension please cite the following literature: Hahn, M.B., Zutta Villate, J.M. "Combined cell and nanoparticle models for TOPAS to study radiation dose enhancement in cell organelles." Sci Rep 11, 6721 (2021). https://doi.org/10.1038/s41598-021-85964-2 " KW - Monte-Carlo simulation KW - MCS KW - Geant4 KW - TOPAS KW - TOPAS-nBio KW - Dosimetry KW - Nanoparticles KW - Nanoparticle KW - AuNP KW - Gold KW - Microdosimetry KW - Targeted nanoparticle KW - Simulation KW - Particle scattering KW - Cell KW - Nucleus KW - Mitochondria KW - Cancer therapy KW - Radiation therapy PY - 2020 UR - https://github.com/BAMresearch/TOPAS-CellModels UR - https://github.com/MarcBHahn/TOPAS-CellModels DO - https://doi.org/10.26272/opus4-51150 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Usmani, Shirin M. A1 - Plarre, Rüdiger A1 - Hübert, Thomas A1 - Kemnitz, E. ED - Richter, K. ED - Van de Kulien, J.-W. T1 - Termite resistance of pine wood treated with nano metal fluorides N2 - Fluorides are well-known as wood preservatives. One of the limitations of fluoride-based wood preservatives is their high leachability. Alternative to current fluoride salts such as NaF used in wood protection are low water-soluble fluorides. However, impregnation of low water-soluble fluorides into wood poses a challenge. To address this challenge, low water-soluble fluorides like calcium fluoride (CaF2) and magnesium fluoride (MgF2) were synthesized as nanoparticles via the fluorolytic sol−gel synthesis and then impregnated into wood specimens. In this study, the toxicity of nano metal fluorides was assessed by termite mortality, mass loss and visual analysis of treated specimens after eight weeks of exposure to termites, Coptotermes formosanus. Nano metal fluorides with sol concentrations of 0.5 M and higher were found to be effective against termites resulting in 100% termite mortality and significantly inhibited termite feeding. Among the formulations tested, the least damage was found for specimens treated with combinations of CaF2 and MgF2 with an average mass loss less than 1% and visual rating of “1”. These results demonstrate the efficacy of low water-soluble nano metal fluorides to protect wood from termite attack. KW - Holzschutzmittel KW - Nanoparticles KW - Fluorides KW - Termites PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514325 DO - https://doi.org/10.1007/s00107-020-01522-z VL - 78 SP - 493 EP - 499 PB - Springer CY - Berlin AN - OPUS4-51432 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 after 2Ys? 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. T2 - 28th Meeting of CEN/TC 352 Nanotechnologies CY - Online meeting DA - 16.10.2020 KW - Nanoparticles KW - CEN/TC 352 Nanotechnologies KW - Particle size distribution KW - Traceability PY - 2020 AN - OPUS4-51437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan T1 - 2020 Microscopy Today Micrograph Awards N2 - Gold nanocubes with a monodispersed size distribution (edge = 55 nm) deposited on a silicon wafer. These tiny uniform cubes were produced as reference nanoparticles within the EMPIR project nPSize - Improved traceability chain of nanoparticle size measurements. SEM image acquired at 10 kV with an in-lens secondary electron detector. Image colored in ImageJ using LUT “Orange hot.” Published in Microscopy and Microanalysis 25(S2) (2019) 2328. KW - Nanoparticles KW - Au-nanocubes KW - Reference materials KW - Electron microscopy PY - 2020 DO - https://doi.org/10.1017/S1551929520001339 VL - 28 IS - 5 SP - 14 EP - 15 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan T1 - Gold nanocubes with monodispersed size distribution (SEM SE) N2 - Gold nanocubes with a monodispersed size distribution (edge = 55 nm) deposited on a silicon wafer. These tiny uniform cubes were produced as reference nanoparticles in the frame of the European project nPSize - Improved traceability chain of nanoparticle size measurements. SEM Image acquired at 10 kV with an in-lens secondary electron detector. Image colored in ImageJ using LUT “Orange hot.” Published in Microscopy and Microanalysis 25(S2) (2019) 2328. KW - Nanoparticles KW - Nanocubes KW - Electron microscopy KW - Reference materials PY - 2020 DO - https://doi.org/10.1017/S1551929520001157 VL - 28 IS - 4 SP - 12 EP - 12 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Cios, G. A1 - Tokarski, T. A1 - Mansfeld, Ulrich A1 - Ortel, Erik A1 - Mielke, Johannes A1 - Pellegrino, F. A1 - Maurino, V. T1 - Towards 3D understanding of non spherical nanoparticles by Transmission Kikuchi Diffraction (TKD) for improved particle size distribution by electron microscopy N2 - In this paper one refined approach is applied to determine the exact orientation of bipyramidal TiO2 nanoparticles prepared with good dispersion as almost isolated particles on a carbon TEM grid. The advantages of the recently developed high-throughput Transmission Kikuchi Diffraction (TKD) are used to identify quickly and reliably the geometrical orientation of the crystalline TiO2 nanoparticle bipyramids (anatase) on a statistically relevant number of particles. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Transmission Kikuchi Diffraction (TKD) KW - TiO2 KW - 3D KW - Electron microscopy PY - 2020 AN - OPUS4-51113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Rühle, Bastian T1 - Towards automated electron microscopy image segmentation for nanoparticles of complex shape by convolutional neural networks N2 - In this contribution different ways are explored with the aim to generate suitable training data for ‘non-ideal’ samples using various approaches, e.g., computer-generated images or unsupervised learning algorithms such as generative adversarial networks (GANs). We used these data to train simple CNNs to produce segmentation masks of SEM images and tested the trained networks on real SEM images of complex nanoparticle samples. The novel use of CNN for the automated analysis of the size of nanoparticles of complex shape and with a high degree of agglomeration has proved to be a promising tool for the evaluation of particle size distribution on a large number of constituent particles. Further development and validation of the preliminary model, respectively larger training and validation data sets are necessary. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Automatisation KW - Image segmentation KW - Convolutional neural networks KW - Electron microscopy PY - 2020 AN - OPUS4-51114 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Hörenz, Christoph A1 - Durande, B. A1 - Taché, O. A1 - Bartczak, D. A1 - Cuello-Nuñez, S. A1 - Ábad-Alvaro, I. A1 - Goenaga-Infante, H. T1 - Analysis of Particle Size Distribution for Bimodal Model Nanoparticles by Scanning Electron Microscopy N2 - The present study addresses the capability of measurement of relative particle number concentration by scanning electron microscopy for model bimodal silica and gold samples prepared in the frame of the European research project “nPSize - Improved traceability chain of nanoparticle size measurements” as candidate reference nanoparticles. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Silica KW - Gold KW - Electron microscopy KW - Particle size distribution PY - 2020 AN - OPUS4-51112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Preparation of Nanoparticulate Samples for Electron Microscopy N2 - This presentation addresses the importance of proper sample preparation to obtain suitable samples for electron microscopic measurements. The objective as well as the requirements are discussed. Further, different sample deposition methods for various types of nanoparticulate samples are shown. T2 - nPSize Web Conference CY - Online meeting DA - 23.07.2020 KW - Nanoparticles KW - Electron microscopy KW - Sample preparation KW - Particle size distribution KW - Particle number concentration PY - 2020 AN - OPUS4-51047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Benettoni, P. A1 - Stryhanyuk, H. A1 - Wagner, S. A1 - Hachenberger, Y. A1 - Jungnickel, H. A1 - Tentschert, J. T1 - Analytical and Characterisation Excellence in nanomaterial risk assessment: A tiered approach Task2.5 N2 - The final results of Task 2.5 "Optimization of sample preparation for characterization of ENPs using TOF-SIMS under real-life conditions (a.) UfZ: polymer template; b.) BAM: pressing of pellets)" were presented. T2 - ACEnano General Meeting CY - Amsterdam, The Netherlands DA - 05.03.2020 KW - Nanoparticles KW - ToF-SIMS KW - Preparation PY - 2020 AN - OPUS4-50572 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 - GEN A1 - Mech, A. A1 - Rauscher, H. A1 - Rasmussen, K. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Ghanem, A. A1 - Wohlleben, W. A1 - Marvin, H. A1 - Brüngel, R. A1 - Friedrich, C. M. A1 - Löschner, K. A1 - Gilliland, D. T1 - The NanoDefine Methods Manual - Part 3: Standard Operating Procedures (SOPs) N2 - The present series of reports, the NanoDefine Methods Manual, 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'1 funded by the European Union's 7th Framework Programme, under grant agreement 604347. In 2011 the European Commission (EC) published the recommendation (2011/696/EU) for a definition of the term 'nanomaterial'1, the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices. The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano or non-nano material according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by: - addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all - developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies. Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the D50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context. The NanoDefine Methods Manual consists of the following three parts:  Part 1: The NanoDefiner Framework and Tools  Part 2: Evaluation of Methods  Part 3: Standard Operating Procedures (SOPs) Part 1 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 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project. The current document is part 3. KW - Nanomaterial KW - Nanoparticles KW - Particle size distribution KW - NanoDefine KW - Standard Operation Procedures KW - Nanomaterial classification KW - SOP PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503710 SN - 978-92-76-11955-5 DO - https://doi.org/10.2760/02910 SN - 1831-9424 VL - JRC117501 SP - 1 EP - 215 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mech, A. A1 - Rauscher, H. A1 - Rasmussen, K. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Ghanem, A. A1 - Wohlleben, W. A1 - Marvin, H. A1 - Brüngel, R. A1 - Friedrich, C. M. T1 - The NanoDefine Methods Manual - Part 2: Evaluation of methods N2 - The present series of reports, the NanoDefine Methods Manual, 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. In 2011 the European Commission (EC) published a recommendation for a definition of the term 'nanomaterial', the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes1. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices. The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano- or not a nanomaterial according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by: - addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all stakeholders (authorities, policy makers, commercial firms), - developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies. Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the x50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context. The NanoDefine Methods Manual consists of the following three parts:  Part 1: The NanoDefiner Framework and Tools  Part 2: Evaluation of Methods  Part 3: Standard Operating Procedures (SOPs) Part 1 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 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project. The current document is part 2. KW - Nanomaterial KW - Nanoparticles KW - NanoDefine KW - Particle size distribution KW - Nanomaterial classification PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503708 SN - 978-92-76-11953-1 DO - https://doi.org/10.2760/071877 SN - 1831-9424 VL - JRC117501 SP - 1 EP - 133 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mech, A. A1 - Rauscher, H. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Wohlleben, W. A1 - Marvin, H. A1 - Weigel, S. A1 - Brüngel, R. A1 - Friedrich, C. M. T1 - The NanoDefine Methods Manual - Part 1: The NanoDefiner Framework and Tools N2 - The present series of reports, the NanoDefine Methods Manual, 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. In 2011 the European Commission (EC) published a recommendation for a definition of the term 'nanomaterial', the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes1. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices. The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano- or not a nanomaterial according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by: - addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all stakeholders (authorities, policy makers, commercial firms), - developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies. Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the x50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context. The NanoDefine Methods Manual consists of the following three parts:  Part 1: The NanoDefiner Framework and Tools  Part 2: Evaluation of Methods  Part 3: Standard Operating Procedures (SOPs) Part 1 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 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project. The current document is part 1. KW - Nanomaterial KW - Nanoparticles KW - NanoDefine KW - Nanoparticle size distribution KW - Nanomaterial classification KW - Framework KW - Tools PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503699 SN - 978-92-76-11950-0 DO - https://doi.org/10.2760/55181 SN - 1831-9424 SP - 1 EP - 89 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, C. A1 - Marguet, S. A1 - Maurino, V. A1 - Hodoroaba, Vasile-Dan T1 - Computation of scattering curves for particles with arbitrary shapes using Debye’s formula N2 - Small-angle scattering data from particle dispersions with narrow size distributions are usually analysed by fitting a model function to the data, which is composed of a monodisperse form factor with a size distribution and, optionally, a structure factor. For common particle shapes like solid spheres, core-shell particles, ellipsoids or rods, the form factor can be computed analytically, and several software packages are readily available which provide a compilation of form factors.1,2 Recently, highly monodisperse nanoparticles with a variety of shapes have been synthesized, e.g. cubes and bipyramids3,4 with lightly capped edges, for which analytic form factors are harder to derive. We compute an approximation to the scattering curve of arbitrary shapes by filling the shape with a quasi-random distribution of point scatterers and using Debye’s formula to get the overall scattering curve. The highly optimized debyer code is used to perform an efficient evaluation of Debye’s formula,5 which can perform the evaluation of 500,000 point scatterers in two minutes on commodity hardware. Moderate polydispersity is handled by interpolating the computed scattering curve over q from a master curve. In this way, the code is fast enough to perform data fitting of particle ensembles with moderate polydispersity for arbitrary shapes to experimental data. This work was partly funded by the 17NRM04 nPSize project of the EMPIR programme co-financed by the EMPIR participating states and by the European Union’s Horizon 2020 research and innovation programme. T2 - 17th Nordic Workshop on Scattering from Soft Matter CY - Linköping, Sweden DA - 14.01.2020 KW - X-ray scattering KW - Nanoparticles KW - Particle shape KW - Modelling KW - Form factor PY - 2020 UR - http://nssm2020.se/ AN - OPUS4-50368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Characterization of nanoparticles - Measurement processes for nanoparticles N2 - Characterization of Nanoparticles: Measurement Processes for Nanoparticles surveys this fast growing field, including established methods for the physical and chemical characterization of nanoparticles. The book focuses on sample preparation issues (including potential pitfalls), with measurement procedures described in detail. In addition, the book explores data reduction, including the quantitative evaluation of the final result and its uncertainty of measurement. The results of published inter-laboratory comparisons are referred to, along with the availability of reference materials necessary for instrument calibration and method validation. The application of these methods are illustrated with practical examples on what is routine and what remains a challenge. In addition, this book summarizes promising methods still under development and analyzes the need for complementary methods to enhance the quality of nanoparticle characterization with solutions already in operation. KW - Nanoparticles KW - Characterization method KW - Sample preparation KW - Inter-laboratory comparison KW - Standardisation KW - Measurement uncertainty KW - Case studies PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/C2017-0-00312-9 SP - 1 EP - 566 PB - Elsevier CY - Amsterdam AN - OPUS4-50284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria A1 - Bienert, Ralf A1 - Prinz, Carsten A1 - Emmerling, Franziska T1 - Synthesis of bimetallic nickel nanoparticles as catalysts for the Sabatier reaction N2 - Nanoparticles (NPs) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - Adlershofer Forschungsforum 2019 CY - Berlin, Germany DA - 11.11.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria A1 - Bienert, Ralf A1 - Prinz, Carsten A1 - Emmerling, Franziska T1 - Synthesis of bimetallic nickel nanoparticles for catalysis N2 - We present the synthesis of monodisperse monometallic Ni nanoparticles (NPs) and bimetallic NiCu respectively NiCo NPs. The NPs were investigated using SAXS, STEM, EDX, and XANES, showing that the NPs are size tunable and stable while the surface is not entirely covered. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4. T2 - 11th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 04.12.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria A1 - Bienert, Ralf A1 - Prinz, Carsten A1 - Emmerling, Franziska T1 - Synthesis of bimetallic nickel nanoparticles as catalysts for the Sabatier reaction N2 - Nanoparticles (NP) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - 31. Tag der Chemie 2019 CY - Berlin, Germany DA - 11.07.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang A1 - Müller, Anja A1 - Heinrich, Thomas A1 - Kunz, Valentin A1 - Nymark, P. A1 - Radnik, Jörg T1 - Chemical characterization of nanoparticles by PCA-assisted ToF-SIMS: a) Core-shell character, b) transformation and c) grouping studies N2 - This talk was given within the scope of the SIMS-22 conference in October 2019 in Kyoto (Japan). It deals with the surface analytical investigation of nanoparticles by PCS-assisted ToF-SIMS. This technique is applicable to core-shell nanoparticles, in order to distinguish a complete encapsulation from an incomplete encapsulation of the core by the shell material. Furthermore, the depletion process of organic nanoparticle coatings caused by UV-weathering is investigated. Finally, the significance of grouping studies for nanomaterials research and risk assessment is demonstrated. T2 - The 22nd International Conference on Secondary Ion Mass Spectrometry (SIMS-22) CY - Kyoto, Japan DA - 20.10.2019 KW - Nanoparticles KW - ToF-SIMS KW - Principal component analysis (PCA) PY - 2019 AN - OPUS4-50075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Mansfeld, Ulrich A1 - Hörenz, Christoph A1 - Pellegrino, F. A1 - Maurino, V. A1 - Marguet, S. A1 - Testard, F. A1 - Tache, O. A1 - Bartczak, D. A1 - Goenaga-Infante, H. 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 - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Yamamoto, K. A1 - Grulke, E. A. A1 - Maurino, V. ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. 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. In the TEM micrograph the particles tracked manually according to the measurement protocol. 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 CY - Berlin, Germany DA - 14.05.2018 KW - Titanium dioxide KW - Nanoparticles KW - Shape-controlled KW - Electron microscopy PY - 2019 SN - 978-3-95606-440-1 DO - https://doi.org/https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - F-61 SP - 245 EP - 255 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grauel, Bettina A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Haase, M. A1 - Homann, C. T1 - Progress report NaYF4:Yb,Er upconversion nanoparticles: determination of energy loss processes for the systematic enhancement of the luminescence efficiency N2 - A report on the progress of the PhD work on upconversion nanoparticles is given, showing lifetimes and quantum yields of single- and co-doped Yb,Er nanocrystals with and without inert shell. T2 - Arbeitsgruppenseminar Prof. Oliver Benson CY - Berlin, Germany DA - 23.10.2019 KW - Upconversion KW - Spectroscopy KW - Nanoparticles KW - Lifetime PY - 2019 AN - OPUS4-49754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike A1 - Drescher, D. A1 - Büchner, T. A1 - Müller, L. A1 - Wanka, Antje A1 - Hösl, S. A1 - Ascher, Lena A1 - Cruz-Alonso, M. A1 - Pisonero, J. A1 - Kneipp, J. A1 - Jakubowski, Norbert T1 - Imaging of biological samples by LA-ICP-MS N2 - In recent years, elemental imaging of biological samples like tissue thin sections using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining more and more importance. Improvements concerning spatial resolution as well as signal-to-background ratio due to low-dispersion sample chambers make LA-ICP-MS also interesting for single cell analysis. To evaluate the interaction of nanoparticles (NPs) with cells LA-ICP-MS was applied for the imaging of individual cells. Our findings show, that NP aggregates can be localized within cellular compartments. The uptake efficiency depends strongly on the physico-chemical properties of the nanostructures (size, chemical composition, surface modification), as well as on the incubation conditions (concentration, time). Moreover, LA-ICP-MS is increasingly becoming an important complementary technique in bioanalysis by using element-tagging strategies to determine biomolecules indirectly. Based on the specific binding between antibodies and their corresponding antigens, proteins and peptides can be detected in tissue or cells using tagged antibodies. As artificial tags metal chelates loaded with lanthanides, polymer-based elemental tags or metal-containing nanoparticles can be used. Thereby LA-ICP-MS is a sensitive detection tool for multiplexed immuno-histochemistry of tissue and cell samples. Our results demonstrate the potential of LA-ICP-MS to investigate the distribution of naturally occurring elements, administered agents as well as biomolecules by using metal-tagged antibodies. T2 - Workshop on tandem LIBS/LA-ICP-MS 2019 CY - Berlin, Germany DA - 18.11.2019 KW - Laser ablation KW - ICP-MS KW - Nanoparticles KW - Imaging PY - 2019 AN - OPUS4-49704 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian A1 - Nirmalananthan-Budau, Nithiya A1 - Roloff, Alexander A1 - Resch-Genger, Ute T1 - Surface Functional Group Quantification on Micro- and Nanoparticles N2 - Organic and inorganic micro- and nanoparticles are increasingly used as drug carriers, fluorescent sensors, and multimodal labels in the life and material sciences. Typically, these applications require further functionalization of the particles with, e.g., antifouling ligands, targeting bioligands, stimuli-responjsive caps, or sensor molecules. Besides serving as an anchor point for subsequent functionalization, the surface chemistry of these particles also fundamentally influences their interaction with the surrounding medium and can have a significant effect on colloidal stability, particle uptake, biodistribution, and particle toxicity in biological systems. Moreover, functional groups enable size control and tuning of the surface during the synthesis of particle systems. For these reasons, a precise knowledge of the chemical nature, the total number of surface groups, and the number of groups on the particle surface that are accessible for further functionalization is highly important. In this contribution, we will will discuss the advantages and limitiations of different approaches to quantify the amount of commonly used surface functional groups such as amino,[1,2] carboxy,[1,2] and aldehyde groups.[3] Preferably, the quantification is carried out using sensitive and fast photometric or fluorometric assays, which can be read out with simple, inexpensive instrumentation and can be validated by complimentary analytic techniques such as ICP-OES and quantitative NMR. T2 - NANAX Hamburg CY - Hamburg, Germany DA - 16.09.2019 KW - Microparticles KW - Nanoparticles KW - Quantitative Analysis KW - Surface KW - Funtional Groups PY - 2019 AN - OPUS4-49616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Mansfeld, Ulrich A1 - Pellegrino, F. A1 - Maurino, V. A1 - Marguet, S. A1 - Testard, F. A1 - Tache, O. A1 - Bartczak, D. T1 - New reference material candidates for traceable size measurement of non-spherical nanoparticles N2 - New model nanoparticles with well-controlled shape were synthesized within the EMPIR project nPSize - Improved traceability chain of nanoparticle size measurements. Their systematic characterization takes place by the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering. Following reference nanoparticle candidates are under investigation with respect to their homogeneity and stability: titania nanoplatelets (10-15 nm x 50-100 nm), titania bipyramides (~60 nm x 40 nm), titania acicular particles (100 nm x 15-20 nm; aspect ratio 5.5/6), gold nanorods (~10 nm x 30 nm), and gold nanocubes (~55 nm x 55 nm x 55 nm). T2 - HyMET Workshop on optical surface analysis methods for nanostructured layers CY - Berlin, Germany DA - 10.10.2019 KW - Nanoparticles KW - Reference materials KW - Traceability KW - Particle size distribution PY - 2019 AN - OPUS4-49285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Mansfeld, Ulrich A1 - Pellegrino, F. A1 - Maurino, V. A1 - Marguet, S. A1 - Testard, F. A1 - Tache, O. A1 - Bartzcak, D. T1 - New reference material candidates for traceable size measurement of nonspherical nanoparticles 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. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Nanoparticles KW - Size distribution KW - Electron microscopy KW - Certified reference materials KW - Traceability PY - 2019 AN - OPUS4-49227 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. A1 - Thünemann, Andreas T1 - In-situ SAXS/WAXS investigation of zinc oxide nanotube formation N2 - Zinc oxide nanostructures possess optical properties that are dependent on particle shape and size. Here, we report on the synthesis of elongated zinc oxide tubes via the in-situ aggregation of spherical particles. Using a custom-built, lab-based instrument, x-ray scattering can be investigated over more than three decades in scattering vector q, allowing for a complete investigation from atomic distances up to larger-than-nano structures. For this study, the hydrolytic synthesis of stearate stabilized zinc oxide nanostructures in tetrahydrofuran was performed and the reaction mixture was continuously fed through the SAXS/WAXS apparatus by means of a peristaltic pump. For comparison to nanospheres, oleate-functionalized zinc oxide particles were synthesized in a microwave-assisted fashion, and depending on reaction temperature, sphere radii could be adjusted between 2.6 and 3.8 nm, changing the optical and crystal lattice properties. The evaluation of the in-situ measurements showed that at the beginning of the synthesis of the stearate-stabilized zinc oxide, similar, spherical particles are formed as in the oleate-based synthesis. In contrast, as the reaction progresses, the stearate-capped particles aggregate into elongated rods with radii of a few nanometres, which eventually form the nanotubes. These have radii of 30-50 nm and lengths of several hundred nanometres. Nevertheless, these structures still possess optical properties like the ultra-small zinc oxide spheres, i.e. a bright, yellow fluorescence. Therefore, we assume that the originally formed, ultra-small spheres, are still present within the tube structure, but separated by stearate, and thus determine their fluorescence properties. T2 - SAXS excites CY - Graz, Austria DA - 24.09.2019 KW - SAXS KW - Zinc oxide KW - Nanoparticles PY - 2019 AN - OPUS4-49135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mansfeld, Ulrich A1 - Pellegrino, F. A1 - Maurino, V. A1 - Marguet, S. A1 - Testard, F. A1 - Tache, O. A1 - Hodoroaba, Vasile-Dan T1 - Towards accurate analysis of particle size distribution for non-spherically shaped nanoparticles as quality control materials N2 - Most industrial nanoparticles have non-spherical shapes and also possess polydisperse size distributions, and due to their agglomeration/ aggregation state are difficult (or even impossible) to be addressed individually. Further, driven by regulatory purposes related to the identification of a material as a nanomaterial, the accurate measurement of the smallest dimension of a (nano)particulate material makes the analysis even more complex. In the first phase of the EU Project nPSize - Improved traceability chain of nanoparticle size measurements (https://www.bam.de/Content/DE/Projekte/laufend/nPSize/npsize.html), the efforts are focused on synthesis of nanoparticles of well-defined, non-spherical shape. Following candidates of reference materials (CRM) with certifiable particle size (distribution) are under characterization with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-60 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). KW - Nanoparticles KW - Imaging KW - Non-spherical KW - Reference material KW - Particle size distribution PY - 2019 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/towards-accurate-analysis-of-particle-size-distribution-for-nonspherically-shaped-nanoparticles-as-quality-control-materials/CD48E9298865410124E22837D8CF73A0 DO - https://doi.org/10.1017/S1431927619012376 SN - 1431-9276 SN - 1435-8115 VL - 25 IS - Suppl. 2 SP - 2328 EP - 2329 PB - Cambridge University Press AN - OPUS4-48856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Mansfeld, Ulrich A1 - Pellegrino, F. A1 - Maurino, V. A1 - Marguet, S. A1 - Testard, F. A1 - Tache, O. T1 - Towards accurate analysis of particle size distribution for non-spherically shaped nanoparticles as quality control materials N2 - Measurement of nanoparticle size (distribution) becomes a challenging analytical problem when non-spherical nanoparticles must be accurately measured. Most industrial nanoparticles have not only non-spherical shapes but also possess polydisperse size distributions, and due to their agglomeration/aggregation state are difficult (or even impossible) to be addressed individually. Moreover, driven by regulatory purposes related to the identification of a material as a nanomaterial, the accurate measurement of the smallest dimension of a (nano)particulate material makes the analysis even more complex. In the first phase of the EU Project nPSize - Improved traceability chain of nanoparticle size measurements (https://www.bam.de/Content/DE/Projekte/laufend/nPSize/npsize.html), the efforts are focused on synthesis of nanoparticles of well-defined, non-spherical shape. Following candidates of reference materials (CRM) with certifiable particle size (distribution) are under characterization with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-60 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). T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - Nanoparticles KW - Reference materials KW - Traceability KW - Non-spherical shape KW - Titanium dioxide PY - 2019 AN - OPUS4-48671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Quantitative microstructural analysis - VAMAS/TWA 37 N2 - The 44th Meeting of the Versailles Project on Advanced Materials and Standards (VAMAS) Steering Committee has just taken place at NIST in Boulder (CO, USA). BAM participates with significant contributions in Technical Working Areas on nanoparticle and surface chemistry characterization, but also has positioned itself to new global material challenges and trends in the developement of advanced materials and their characterization, such as thermal properties, self-healing materials, and micro- and nanoplastic. T2 - Annual Meeting of the Versailles Project on Advanced Materials and Standards (VAMAS) Steering Committee CY - Boulder, CO, USA DA - 22.05.2019 KW - VAMAS KW - Nanoparticles KW - Microbeam analysis KW - Advanced materials PY - 2019 AN - OPUS4-48184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Schroeder, Barbara A1 - Le Xuan, Hoa A1 - Völzke, Jule L. A1 - Weller, Michael G. T1 - Preactivation crosslinking – An efficient method for the oriented immobilization of antibodies N2 - Crosslinking of proteins for their irreversible immobilization on surfaces is a proven and popular method. However, many protocols lead to random orientation and the formation of undefined or even inactive by-products. Most concepts to obtain a more targeted conjugation or immobilization requires the recombinant modification of at least one binding partner, which is often impractical or prohibitively expensive. Here a novel method is presented, which is based on the chemical preactivation of Protein A or G with selected conventional crosslinkers. In a second step, the antibody is added, which is subsequently crosslinked in the Fc part. This leads to an oriented and covalent immobilization of the immunoglobulin with a very high yield. Protocols for Protein A and Protein G with murine and human IgG are presented. This method may be useful for the preparation of columns for affinity chromatography, immunoprecipitation, antibodies conjugated to magnetic particles, permanent and oriented immobilization of antibodies in biosensor systems, microarrays, microtitration plates or any other system, where the loss of antibodies needs to be avoided, and maximum binding capacity is desired. This method is directly applicable even to antibodies in crude cell culture supernatants, raw sera or protein-stabilized antibody preparations without any purification nor enrichment of the IgG. This new method delivered much higher signals as a traditional method and, hence, seems to be preferable in many applications. KW - Antibody coating KW - Proximity-enhanced reaction KW - Immunoglobulins KW - IgG KW - Protein G KW - Protein A KW - Immunoprecipitation KW - Immunocapture KW - Stabilization KW - Biosensor KW - Biochip KW - Microarray KW - ELISA KW - Immunoassay KW - Immunosensor KW - Crosslinker KW - Nanoparticles KW - Click chemistry KW - Herceptin KW - Trastuzumab PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-478797 DO - https://doi.org/10.20944/preprints201904.0205.v1 SN - 2310-287X SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-47879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rohner, C. A1 - Braun, Ulrike A1 - Schlögl, R. A1 - Lunkenbein, T. T1 - Electron beam induced amorphisation of polypropylene particles N2 - Untersuchung von Polypropylen Nanopartikeln mittels REM. Es wird die Hypothese aufgestellt, dass mit der Paarverteilungsfunktion auf den Alterunszustand geschlossen werden kann. N2 - Analysis of polypropylene nanoparticles with scanning elektron spectroscopy (SEM). The poster describes the hypothesis that the pair distribution function determined by SEM can be used to deduce the state of polymer age. T2 - Microscopy characterisation of organic-inorganic interfaces 2019 CY - Berlin, Germany DA - 07.03.2019 KW - Nanopartikel KW - Mikroplastik-Analytik KW - Paarverteilungsfunktion KW - Pair distribution function KW - Nanoparticles KW - Microplastic analysis PY - 2019 AN - OPUS4-47890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra A1 - Hodoroaba, Vasile-Dan T1 - Considerations for nanomaterial identification of powders using volume-specific surface area method N2 - The EC’s 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. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming. For most measurement methods for particle size determination it is necessary to initially disperse the particles in a suitable liquid. However, as the particle size decreases, the adhesion forces increase strongly, making it more difficult to deagglomerate the particles and to assess accurately the result of this process. Therefore, the success of the deagglomeration process substantially determines the measurement uncertainty and hence, the comparability between different methods. Many common methods such as dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS) or ultrasound attenuation spectroscopy (US) can give good comparable results for the size of nanoparticles, if they are properly separated and stabilized (e.g. in reference suspensions). In order to avoid the use of hardly available and expensive methods such as SEM / TEM for all powders, an agglomeration-tolerant screening method is useful. One of the measurement methods well suited to probe the size of particulate powder is the determination of the 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 nano- or non-nanomaterial. The identification of a nanomaterial by VSSA method is accepted by the EU recommendation. However, the application of the VSSA method was associated also with some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions, but also with the degree of sphericity of the particles. For particles containing micro-pores or having a microporous coating, false positive results are induced. Furthermore, broad particle size distributions made necessary to additionally correct the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach was tested in relation with SEM and TEM measurements. The introduction of a correction term for deviations from sphericity and further additions improved the applicability of VSSA as a screening method. T2 - Partec CY - Nuremberg, Germany DA - 09.04.2019 KW - VSSA KW - Nanoparticles PY - 2019 AN - OPUS4-47874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Surface and Microbeam Analytical Methods @BAM N2 - An overview of the activities in the field of surface and microbeam analysis at BAM-6.1 is given with focus on physico-chemical characterization at the nanoscale. Ideas of potential joint activities are presented: structural and chemical analysis of graphene, deposition techniques for nanoparticles, EBSD on steel for a broader range of methods, instruments and types of steel, soft X-ray Analysis of low-Z materials, analysis of mesoporous thin films, etc. T2 - BAM-IFW Workshop CY - Dresden, Germany DA - 28.03.2019 KW - PC characterisation KW - Nanoscale KW - Nanoparticles PY - 2019 AN - OPUS4-47860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steinhoff, U. A1 - Hodoroaba, Vasile-Dan T1 - EMPIR Erläuterung der Fördermaßnahme und Beispiele aus der Nanotechnologie N2 - Das EMPIR-Förderprogramm wird kurz erläutert und laufende Projekte aus der Nanotechnologie werden vorgestellt. Der Schwerpunkt liegt auf Standardisierungsprojekten, die gemeinsam mit ISO/TC 229 'Nanotechnologies' und CEN/TC 352 'Nanotechnologies' zu neuen Normen führen sollten. Als Beispiel für laufende Nanotechnologie-Projekte mit Koordination aus Deutschland werden MagNaStand (PTB) und nPSize (BAM) gegeben. T2 - Treffen des Normungsausschusses NA 062-08-17 AA Nanotechnologien CY - KIT, Karlsruhe, Germany DA - 07.03.2019 KW - EMPIR KW - Nanoparticles KW - Reference materials KW - Particle size distribution KW - Traceability KW - Standardisation PY - 2019 AN - OPUS4-47859 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kunz, Valentin T1 - Surface chemical transformations of nanoparticles N2 - Nanomaterials are a relatively new class of materials for which a regulatory framework still has to be established and regulators require comprehensive datasets of well characterized nanomaterials for the implementation. Especially information about the surface chemistry of nanoparticles is crucial, since it largely determines their biological and environmental fate. How the surface chemistry changes under relevant ageing conditions is of particular interest, because exposure will normally occur not to the pristine material but to a nanoform that underwent some kind of transformation. In this talk, first a short overview about the contributions of division 6.1 to multiple European-funded projects will be presented, in which surface analytical techniques are used to improve the physical-chemical characterization of nanomaterials. Secondly, a study investigating the surface-chemical transformations of a representative set of titanium dioxide nanoparticles is discussed in more detail. The ageing has partly been performed at the BAM division 7.5, and the surface chemistry was analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS). By analyzing the complex mass spectra with principal component analysis (PCA), it was possible to identify even subtle changes that occur upon ageing. T2 - Abteilungsseminar CY - BAM, Berlin, Germany DA - 25.2.2019 KW - Nanoparticles KW - Surface Chemistry KW - Ageing KW - Titanium Dioxide KW - ToF-SIMS PY - 2019 AN - OPUS4-47444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Müller, Anja T1 - Introduction to photoelectronspectroscopy N2 - A short introduction to XPS/ESCA with the focus on nanoparticles and the preparation of such particles for the measurements T2 - Meeting of ACE Nano CY - Berlin, Germany DA - 18.02.2019 KW - ESCA/XPS KW - Nanoparticles KW - Preparation PY - 2019 AN - OPUS4-47437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Arakawa, Akihiro A1 - Jakubowski, Norbert A1 - Flemig, Sabine A1 - Köllensperger, G. A1 - Rusz, M. A1 - Iwahata, D. A1 - Traub, Heike A1 - Hirata, T. T1 - LA-ICP-MS study of Ag nanoparticle transport in a three-dimensional in vitro model N2 - We have applied laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) with subcellular resolution as an elemental mass microscope to investigate the distributions of Ag nanoparticles (NP) in a 3-dimentional multicellular spheroid (MCS) model. The production of MCS has been optimized by changing the seeding cell number (500 to 40,000 cells) and the growth period (1 to 10 days). Incubations of MCS with Ag nanoparticle suspensions were performed with a concentration of 5 µg mL-1 for 24 hours. Thin-sections of the Eosin stained MCS were analysed by elemental mass microscopy using LA-ICP-MS to image distributions of 109Ag, 31P, 63Cu, 66Zn and 79Br. A calibration using NP suspensions was applied to convert the measured Ag intensity into the number of particles being present in each measurement pixel. The numbers of NP determined ranged from 30 up to 4,000 particles in an enrichment zone. The particle distribution was clearly correlated to 31P, 66Zn and 79Br and was localized in an outer rim of proliferating cells (confirmed by DAPI) with a width of about two-single cell diameters. For the highest seeding cell number NPs were only detected in this outer rim, whereas small molecules as for instance 79Br and 109Ag ions were detected in the core of the MCS as well. Aniline blue staining demonstrated that this outer rim was rich in collagen structures in which fibroblast cells were embedded and a thin-membrane was visible which separated the core from the biological active cell layer functioning as biological barriers for NP transport. In this presentation, we will show the possibility using this 3-dimensional model for toxicological and medical applications. T2 - European Winter Conference on Plasma Spectrochemistry EWCPS-2019 CY - Pau, France DA - 03.02.2019 KW - Laser ablation KW - ICP-MS KW - Nanoparticles KW - Cell KW - Multicellular spheroid PY - 2019 AN - OPUS4-47374 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 - Kjaervik, Marit A1 - Dietrich, P. A1 - Thissen, A. A1 - Schwibbert, Karin A1 - Defedov, A. A1 - Wöll, C. A1 - Unger, Wolfgang T1 - Exploring the capabilities of NAP-XPS: Application to metal-organic frameworks, nanoparticles and biofilms N2 - Near-ambient pressure XPS makes it possible to characterise samples not compatible to ultra-high vacuum, and enables the study of liquid-solid, gas-liquid and gas-solid interfaces. NAP-XPS meas-urements of biofilms, suspended nanoparticles and metal-organic frameworks were performed with EnviroESCA developed by SPECS. An interesting application is surface characterisation of biofilms, which are bacterial communities embedded in a self-produced polysaccharide matrix. Various model systems ranging from pure polysaccharides of alginate to biofilms harvested directly from the growth medium have been char-acterised in humid conditions[1]. NAP-XPS also makes it possible to characterise nanoparticles in solution. Silver nanoparticles in aqueous solution were characterised and the Ag 3d-spectrum compared to spectra obtained of dried nanoparticles in UHV-conditions[2]. The binding energy of the Ag 3d-core level peak was shifted by 0,6 eV towards higher binding energy for suspended nanoparticles compared to the dried sample measured in UHV. This can be assigned to a change in surface potential at the water-nanoparticle interface. Metal-organic frameworks (MOFs) are suitable materials for gas storage of small molecules due to their nanoporous, crystalline structure. However, instability in humidity remains an issue for many types of MOFs. XPS-measurements of the MOF-structure HKUST-1 were performed in various NAP-conditions to assess the stability of the sample and its interaction with the gas molecules as water, methanol and pyridine. T2 - 5th AP-XPS Workshop CY - Berlin, Germany DA - 11.12.18 KW - Biofilms KW - E. coli KW - NAP-XPS KW - Metal organic frameworks KW - Nanoparticles PY - 2018 AN - OPUS4-47060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kunz, Valentin A1 - Kjaervik, Marit A1 - Müller, Anja A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang T1 - How to meet new challenges in advanced nanoparticle analytics N2 - Three current research projects performed at BAM’s Division for Surface Analysis and Interfacial Chemistry are presented that tackle important challenges with regard to the characterization of nanomaterials: 1) The characterization at ambient pressure, 2) the investigation of core-shell nanoparticles, and 3) the characterization of non-spherical particles by electron microscopy. 1) Surface analytical techniques such as Photoelectron Spectroscopy (XPS) or Secondary Ion Mass Spectrometry (SIMS) typically require measurements in ultra-high vacuum. However, for many applications (e.g. catalysis and nanotoxicology) it is important to know the surface chemical properties of nanomaterials at ambient conditions. Therefore, near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) was used to investigate nanoparticles in suspension. The used instrumental set-up allows to directly insert nanoparticle suspensions into the analysis chamber and to measure without prior sample preparation. Compared to dry reference samples measured under high-vacuum, a shift towards higher binding energies was observed for silver nanoparticles in water, indicating a change of surface potential at the water-nanoparticle interface. 2) To determine the dimensions of core-shell nanoparticles (shell thickness, core and total diameter), scanning transmission X-ray microscopy (STXM) was used. The analyzed model system consists of a polytetrafluorethylene (PTFE) core surrounded by a polystyrene (PS) shell, providing a strong X-ray absorption contrast at the C K-edge and a well-defined interface. The introduced STXM‐based methodology yields particle dimensions in agreement with scanning electron microscopy (SEM) results and provides additional information such as the position of the particle core, which cannot be extracted from a SEM micrograph. 3) The accurate measurement of size distributions of non-spherically shaped nanoparticles (representing most of the industrial nanoparticulate materials) is a challenging analytical task. High-resolution electron microscopy (TEM and SEM) is best suited to access the shape of individual nanoparticles. To fill the gap between ideal, monodisperse particles of spherical shape and complex real-world samples, BAM has started the work to develop reference nanoparticles of controlled shape, such as TiO2 platelets, bipyramids, and elongated particles. Results of a recent ISO inter-laboratory comparison will be shown with emphasis on the measurement parameters, descriptors and data analysis. T2 - NanoSafe Conference 2018 CY - Grenoble, France DA - 5.11.2018 KW - Nanoparticles PY - 2018 AN - OPUS4-46730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Donėlienė1, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. T1 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid N2 - A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. T2 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - Nanoparticles KW - Titanium oxide KW - Laser ablation in liquid KW - Electron microscopy KW - XRD PY - 2018 AN - OPUS4-46502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Verhassel, A. A1 - Shinde, S. A1 - Kimani, Martha Wamaitha A1 - Guedes, I. A1 - Sellegren, B. A1 - Rurack, Knut A1 - Tuomela, J. A1 - Härkönen, P. T1 - Application of novel tumor cell glycan-specific nanoprobes for detecting and targeting breast and prostate cancer N2 - Glycosylation is a post-translational modification that is involved in the regulation of many biological processes. The glycosylation pattern in cancer cells differs from that in normal cells. One of the main alterations that has been observed in several cancers is the increase of sialic acids at the end of the glycan. The increase of sialic acids and other alterations affect development and progression of tumors and are found to play an important role in cancer invasiveness and metastasis. Molecularly imprinted polymers (MIPs) are synthetic recognition elements that show high selectivity and affinity for their targets. These polymers show promising applications in detection methods for cancer cells. In this study newly synthesized MIPs, labelled with a nitrobenzoxadiazole (NBD) fluorophore, are investigated for their specificity and utility in the detection of cancer cell-related sialic acids. T2 - Biomarkers – methods and technologies CY - Malmö, Sweden DA - 25.10.2018 KW - Nanoparticles KW - MIPs KW - Cancer PY - 2018 AN - OPUS4-46490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - LA-ICP-MS for the analysis of nanoparticles in cells N2 - Many current nanomaterials can serve as contrast agents in cellular or tissue imaging, drug delivery vehicles or therapeutics, whereas others can cause toxic effects. In order to evaluate nano-bio interactions, the number of nanoparticles (NPs) inside cells as well as their localisation within cellular substructures is of particular interest. The cellular uptake depends on the primary characteristics of the NPs (e.g. size, shape, surface coating) and on the cell type. Laser ablation inductively coupled plasma mass spectrometry (LA‑ICP‑MS) is more and more used to study the NP pathway from uptake, via intracellular processing up to cell division. High-spatial resolution laser ablation at single cell level is achieved using novel low-dispersion LA chambers and by careful optimisation of laser energy, ablation frequency and scan speed at small laser spot sizes down to 1 µm. Different examples from BAM, Division 1.1 and cooperation partners using LA-ICP-MS to localize and quantify metal-containing nanoparticles are shown. The results demonstrate the potential of LA-ICP-MS providing insight into NP uptake, intracellular distribution and cell-to-cell variation. T2 - 13. Symposium "Massensprektrometrische Verfahren der Elementspurenanalyse" + 26. ICP-MS Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Laser ablation KW - Cells KW - Nanoparticles KW - Imaging PY - 2018 AN - OPUS4-46440 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 measurements - Is a liaison to CEN/TC 352 nanotechnologies useful? N2 - The main objectives of the new EMPIR project nPSize are to establish EU capability of traceable measurement of NP size and shape, lower uncertainties of NP size measurement by developement of new nano-CRMs, new models (physical and machine learning), 3D method combination, and also by new ISO and CEN standards on accurate NP size measurement and guidance and knowledge transfer. The envisaged outcomes of the project will be presented and their suitability will be discussed to be taken over as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies. T2 - Joint Working Groups and 24th CEN/TC 352 Nanotechnologies Meetings CY - DIN, Berlin, Germany DA - 09.10.2018 KW - Nanoparticles KW - Size KW - Particle size distribution KW - Particle shape KW - Traceability KW - Standardisation KW - CEN/TC 352 Nanotechnologies PY - 2018 AN - OPUS4-46252 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Overview on the most advanced and suitable NanoDefine measurement methods 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. T2 - VCI-NanoDefine Follow-up Meeting CY - VCI, Frankfurt am Main, Germany DA - 25.09.2018 KW - Nanoparticles KW - Nanomaterial KW - EC definition of nanomaterial KW - Nanoparticle size distribution PY - 2018 AN - OPUS4-46251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Schneider, Markus A1 - Schäpe, Kaija A1 - Unger, Wolfgang A1 - Stockmann, Jörg M. T1 - Classification of engineered Titania nanomaterials via surface analysis using principal component analysis (PCA) assisted Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) N2 - Due to the growing number of engineered nanomaterials (NM) the need for a reliable risk assessment for these materials is today bigger than ever before. Especially the nanomaterial’s surface or shell directly interacts with its environment and therefore is a crucial factor for NM’ toxicity or functionality. Especially, titania is one of the NM with the greatest technological importance. It is used for a large number of applications and can be found in food, cosmetics, glasses, mirrors, paints to mention only a few. In 2012, experts estimate[d] the annual European nano-titania production or utilization at an amount of more than 10,000 t. Great progress has been achieved in the area of NM investigation and characterization during the past decade. A variety of publications provide information about technological innovation as well as hazard potential, which means the potential risk on human health and ecosystems. However, enhanced data harmonization and well-defined standards for nanomaterial analysis, could significantly improve the reliability of such studies which often suffers from varying methods, parameters and sample preparations. To develop a suitable approach for the NM’s risk assessment, the ACEnano project aims at establishing a toolbox of verified methods. The size of this well-structured European project allows to handle even those big challenges like data harmonization and standardization. Due to its powerful combination of superior surface sensitivity and lateral resolution down to the Nano regime, ToF-SIMS could become one of these toolbox methods. Supported by multivariate data analysis such as principal component analysis (PCA), the method can be used for sub-classification of nanomaterial families using slight differences in surface chemistry. Here, we show a PCA supported classification of titania nanoparticles from various sources (NIST, JRC, BAM) with ToF-SIMS. Parameters like size, shell, pre-preparation and crystal system cause variance in the data and allow us to distinguish the species from each other. Moreover, this variance in the data also occurs and can be used for investigation when we compare our measurements of particle ensembles with those of grown titania films. The carefully selected and refined peaks allow a reasonable particle categorization and further a reliable allocation of blank feeds, which introduces a promising approach for NM characterization in the context of NM risk assessment. T2 - SIMS-Europe CY - Münster, Germany DA - 16.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS KW - PCA KW - Titania PY - 2018 AN - OPUS4-46250 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, Katja A1 - Unger, Wolfgang T1 - Chemical characterisation and classification of (Core-Shell) nanoparticles using PCA assisted ToF-SIMS 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 and their growing use in everyday life. 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’ behaviour. 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 layers and thus gives us an idea of possible interactions involved. Supported by multivariate data analysis such as principal component analysis (PCA), the method can also be used for sub-classification of different materials using slight differences in surface chemistry. Here, we present data of 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. Principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. This is achieved by measurement of a statistically relevant set of samples for every particle sample. We acquired surface spectra under static SIMS conditions with Bi32+ and analysed the resulting spectra by PCA. The carefully selected and refined peaks allow a reasonable categorization and further a reliable allocation of blank feeds. In detail, the fluorine containing, organic fragments are an indication for a heterogeneous shell that has errors. Furthermore, results on Au nanoparticles with and without an antibody shell are presented. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - SIMS-Europe CY - Münster, Germany DA - 16.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS KW - PCA KW - Titania KW - Core-Shell PY - 2018 AN - OPUS4-46249 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Müller, Anja A1 - Unger, Wolfgang T1 - Chemical characterisation of (core-shell) nanoparticles using PCA assisted 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 layers 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, results on Au nanoparticles with and without an antibody shell are presented. 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 - 3rd NanoSafety Forum for Young Scientists CY - Valetta, Malta DA - 08.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS PY - 2018 AN - OPUS4-46248 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Yamamoto, K. A1 - Grulke, E. A. T1 - Size and shape distribution of bipyramidal TiO2 nanoparticles by transmission electron microscopy – an inter-laboratory comparison 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. KW - Nanoparticles KW - Electron microscopy KW - Titanium oxide KW - Particle size distribution PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/size-and-shape-distribution-of-bipyramidal-tich-nanoparticles-by-transmission-electron-microscopy-an-interlaboratory-comparison/9E2FA0C716DB5F881E3032D014DFD52B DO - https://doi.org/10.1017/S1431927618009017 SN - 1431-9276 SN - 1435-8115 VL - 24 IS - S1 (August 2018) SP - 1706 EP - 1707 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-46005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donėlienė, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. A1 - Hodoroaba, Vasile-Dan T1 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid N2 - A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. KW - Laser ablation in liquid KW - Nanoparticles KW - Titanium oxide KW - Particle morphology PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/electron-microscopy-and-xray-diffraction-analysis-of-titanium-oxide-nanoparticles-synthesized-by-pulsed-laser-ablation-in-liquid/AE368446FAC70E08C514F9AEABFD131B DO - https://doi.org/10.1017/S1431927618009030 VL - 24 IS - S1 (August) SP - 1710 EP - 1711 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-45949 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 - Size and shape distribution of bipyramidal TiO2 nanoparticles by TEM - An inter-laboratory comparison 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 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - Nanoparticles KW - Electron microscopy KW - ISO KW - Nanotechnology PY - 2018 AN - OPUS4-45750 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maurino, V. A1 - Hodoroaba, Vasile-Dan A1 - Pellutiè, L. A1 - Pellegrino, F. A1 - Ortel, Erik A1 - Isopescu, R. T1 - Synthesis of Shape controlled TiO2 N2 - Titanium dioxide is one of the most studied metal oxides due to its chemical, surface, electronic and (photo)catalytic properties, providing this material of multisectorial applications ranging from healthcare, photocatalysis, smart materials with self cleaning and self sterilizing properties and solar energy harvesting. However it is difficult to correlate the functional properties of TiO2 nanomaterials to the properties at single nanoparticle level due to the high polydispersity in shape, size and surface features of the currently available TiO2 nanoparticles (NPs). Although intensive experimental and theoretical studies have been conducted on the reactivity of different surfaces of metal oxides such as TiO2 much less attention is paid on the dependence of functional properties, like photocatalytic activity, dye adsorption, open circuit potential and fill factor in dye sensitized solar cells, on crystal facets in different orientations. One of the goal of SETNanoMetro project was the development of design rules to tune crystal facets of TiO2 NPs in order to optimize and control functional properties. In the present work we have developed a series of design rules in order to obtain sets of anatase TiO2 NPs with low polydispersity and to tune their shape and size by hydrothermal processing of Ti(IV)-Triethanolamine complex in presence of different shape controllers. Through a careful experimental design, a predictive soft model was developed. The model is able to predict the synthesis outcome allowing to tune the shape factor from 5 (prisms) to 1.5 (bipyramids) to 0.2 (platelets). This allows to control the main crystal facets exposed ranging from (100) to (001). Due to the dependence of functional properties of nanomaterials on shape distribution and not only size, the availability of NPs sets with uniform and well defined and tunable shapes can be of paramount relevance in order to produce reference nanomaterials for shape measurement. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Anatase KW - Shape control KW - Hydrothermal synthesis KW - Nanoparticles PY - 2018 AN - OPUS4-45634 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 - Resch-Genger, Ute A1 - Nirmalananthan-Budau, Nithiya A1 - Moser, Marko A1 - Geißler, Daniel T1 - Simple and Validated 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 - NanoWorkshop 2018 CY - Berlin, Germany DA - 14.05.2018 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 - OPUS4-45179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya A1 - Moser, Marko A1 - Behnke, Thomas A1 - Geißler, Daniel A1 - Resch-Genger, Ute T1 - Multimodal cleavable reporters for the optical quantification of functional groups on nano- and microparticles N2 - Polymer nanoparticles (NPs) are of increasing importance for a wide range of applications in the material and life sciences. This includes their application as carriers for e.g., analyte-responsive ligands for DNA sequencing platforms, drugs as well as dye molecules for use as multichromophoric reporters for signal enhancement in optical assays or the fabrication of nanosensors and targeted probes in bioimaging studies. All these applications require surface functionalization of the particles with e.g., ligands, sensor dyes, or analyte recognition moieties like biomolecules, and subsequently, the knowledge of the chemical nature and total number of surface groups as well as the number of groups accessible for coupling reactions. Particularly attractive for the latter are optically active reporters together with sensitive and fast optical assays, which can be read out with simple, inexpensive instrumentation. We assessed a variety of conventional and newly developed colorimetric and fluorometric labels for optical surface group analysis, utilizing e.g., changes in intensity and/or color for signal generation. Moreover, novel cleavable and multimodal reporters were developed which consist of a reactive group, a cleavable linker, and an optically active moiety, chosen to contain also heteroatoms for straightforward method validation by elemental analysis, ICP-OES, ICP-MS or NMR. In contrast to conventional labels measured bound at the particle surface, which can favor signal distortions by scattering and encoding dyes, cleavable reporters can be detected colorimetrically or fluorometrically both attached at the particle surface and after quantitative cleavage of the linker in the transparent supernatant after particle removal e.g., by centrifugation. Here, we present first results obtained for the optical quantification of carboxylic and amino groups on a series of self-made polystyrene NPs with different types of labels and compare their potential and drawbacks for surface group analysis. T2 - NanoWorkshop 2018 CY - Berlin, Germany DA - 14.05.2018 KW - Optical assays KW - Cleavable probes KW - Conventional dyes KW - Nanoparticles PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-45177 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 - 16th Czech-Slovak Spectroscopic Conference CY - Luhacovice, Czech Republic DA - 27.05.2018 KW - Single cell analysis KW - ICP-MS KW - Nanoparticles PY - 2018 AN - OPUS4-45161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 -