TY - JOUR A1 - Schmidt, Birgit Angelika A1 - Ziemann, M. A A1 - Pentzien, Simone A1 - Gabsch, T. A1 - Koch, W. A1 - Krüger, Jörg T1 - Technical analysis of a Central Asian wall painting detached from a Buddhist cave temple on the northern Silk Road N2 - A great number of Central Asian wall paintings, archeological materials, architectural fragments, and textiles, as well as painting fragments on silk and paper, make up the so called Turfan Collection at the Asian Art Museum in Berlin. The largest part of the collection comes from the Kucha region, a very important cultural center in the third to ninth centuries. Between 1902 and 1914, four German expeditions traveled along the northern Silk Road. During these expeditions, wall paintings were detached from their original settings in Buddhist cave complexes. This paper reports a technical study of a wall painting, existing in eight fragments, from the Buddhist cave no. 40 (Ritterhöhle). Its original painted surface is soot blackened and largely illegible. Grünwedel, leader of the first and third expeditions, described the almost complete destruction of the rediscovered temple complex and evidence of fire damage. The aim of this case study is to identify the materials used for the wall paintings. Furthermore, soot deposits as well as materials from conservation interventions were of interest. Non-invasive analyses were preferred but a limited number of samples were taken to provide more precise information on the painting technique. By employing optical and scanning electron microscopy, energy dispersive X-ray spectroscopy, micro X-ray fluorescence spectroscopy, X-ray diffraction analysis, and Raman spectroscopy, a layer sequence of earthen render, a ground layer made of gypsum, and a paint layer containing a variety of inorganic pigments were identified. KW - Wall paintings KW - Central Asia KW - Silk Road KW - Pigments KW - Microscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-357297 DO - https://doi.org/10.1179/2047058414Y.0000000152 VL - 61 IS - 2 SP - 113 EP - 122 PB - Routledge Taylor & Francis Group CY - London AN - OPUS4-35729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Salge, T. A1 - Mielke, Johannes A1 - Ortel, Erik A1 - Schmidt, R. T1 - Characterisation of nanoparticles by means of high-resolution SEM/EDS in transmission mode N2 - Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass – thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS. T2 - European Microbeam Analysis Society’s 14th European Workshop on Modern Developments and Applications in Microbeam Analysis (EMAS 2015) CY - Portorož, Slovenia DA - 03.05.2015 KW - High-resolution KW - SEM KW - T-SEM KW - EDX KW - Nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355628 UR - http://iopscience.iop.org/article/10.1088/1757-899X/109/1/012006 DO - https://doi.org/10.1088/1757-899X/109/1/012006 SN - 1757-899X VL - 109 SP - 012006-1 EP - 012006-12 PB - IOP Publishing Ltd CY - Bristol, UK AN - OPUS4-35562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald A1 - Schmidt, Alexandra A1 - Bachmann, V. A1 - Kämpf, K. A1 - Kuhlbusch, T. A1 - Schwirn, K. A1 - Völker, D. ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. T1 - OECD Test Guideline on particle size and size distribution of manufactured nanomaterials N2 - The properties of nanomaterials are influenced not only by their chemical composition but also by physical properties (such as size, geometry and crystal structure). For the reliable determination and assessment of behaviour and effects of nanomaterials as well as for the determination of the exposure of humans and environment a comprehensive physical-chemical characterization of nanomaterials is essential. This is an important prerequisite to identify them as nanomaterials and to interpret and compare test results and - in future – to forecast interaction and effects of nanomaterials. In 2006, the OECD launched a sponsorship program for the testing of nanomaterials in which 11 nanomaterials were thoroughly investigated using a variety of methods. The aim of the project was, among other things, to find out where problems occur and where there are gaps in the measurement and test procedures and where are changes required. An important outcome of the sponsorship program was the finding that the OECD Test Guidelines should in several cases be extended to the specific needs in testing of nanomaterials. The existing standardized test methods of the OECD for physical-chemical characterization have not been developed for nanomaterials in particular. A high demand for an extension of the test guidelines was identified. Germany complied with the OECD's request in 2017 and has agreed to extend the “Test Guideline on Particle Size Distribution / Fiber Length and Diameter Distributions Test Guideline” for Manufactured Nanomaterials (MN). UBA commissioned BAM and BAuA with the preparation of the Test Guideline. The aim of the project is the development of a harmonized test protocol for a valid and reproducible determination of particle size and size distribution which is one of the most relevant physical-chemical properties for MNs. Different measuring methods provide different results for the size distribution of the particles. This is caused by the different measuring principles of the methods. Each method measures a specific parameter that ultimately determines particle size. First, the measured quantity differs for each method (Scattered light intensity, 2D image / projection, electric mobility, etc.). Second, the calculated diameters of the MN may differ (Feret Diameter, Area Projection, Mobility Diameter, Aerodynamic Diameter, Hydrodynamic Diameter). Third, a measuring method provides a size distribution which is measured either mass-based, surface-based or number-based. A conversion between the results requires additional parameters and thus possibly increases the measurement error. In addition to the technical differences, the individual parameters are strongly influenced by the structure and material of the nanoparticles. For example, a surface functionalization can lead to very different results in the size distribution. The suitability of measurement methods differs with the material of the MN. As a result, two very different results can be measured for the particle size distribution using two different methods, which are nevertheless both correct. Several large projects in recent years therefore concluded that nanomaterials should be characterized by at least two complementary method. Imaging techniques are regarded as one of these methods for the characterization, the complementary methods are supposed to be statistical methods. The different results for the size distribution of nanomaterials become problematic for the registration of new MN. A comparable and reproducible size distribution is a prerequisite for a standardized registration. In the future, the particle size distribution in the EU will also decide on the classification of a substance as a nanomaterial or as a non-nanomaterial. Especially in borderline cases, a standardized and comparable measurement methodology is therefore essential. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - OECD KW - Guideline KW - Particle size distribution KW - Nano KW - Prüfrichtlinie PY - 2019 SN - 978-3-95606-440-1 DO - https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - F-61 SP - 125 EP - 132 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kämpf, K. A1 - Bachmann, V. A1 - Bresch, Harald A1 - Schmidt, Alexandra A1 - Kuhlbusch, T. A1 - Schwirn, K. A1 - Völker, D. ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. T1 - OECD Test Guideline on particle size and particle size distribution of manufactured nanomaterials: simultaneous measurement of length and diameter of fibers N2 - The new OECD test guideline will address the following four main steps in the determination of the length and width distributions of fibers: sample preparation, image acquisition, data evaluation and uncertainty analysis. As the sample preparation has to be optimized for each material, general quality criteria will be given in the protocol. For full visibility of a fiber the appropriate resolution has to be chosen. In the data evaluation the length and diameter of each fiber will be determined concurrently to allow for application of different regulatory definitions. The quality of the results critically depends on the sample preparation as well as the data evaluation. In this step the classification rules have to be formulated and followed accurately in order to optimize reproducibility of the method. The SOP will be validated in an international round robin test, which is planned for 2018/2019. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - OECD KW - Nano KW - Guideline KW - Particle size distributuion KW - Prüfrichtlinie PY - 2019 SN - 978-3-95606-440-1 DO - https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - F-61 SP - 302 EP - 302 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schwirn, K. A1 - Völker, D. A1 - Ahtianinen, J. A1 - Schmidt, Alexandra A1 - Bresch, Harald A1 - Kämpf, K. A1 - Bachmann, V. A1 - Kuhlbusch, T. ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. T1 - OECD Test Guidelines development for chemicals safety assessment of nanomaterials N2 - The OECD test guidelines (TGs) for testing chemicals have been widely used for regulatory purposes all over the world since the establishment of the Mutual Acceptance of Data (MAD) principle in 1984. This MAD principle ensures that, if a chemical is tested under the Good Laboratory Practice (GLP) conditions accordingly to an OECD TG, the data should be accepted in all OECD countries. The TGs have been developed, harmonized, internationally validated (round robin tests) and adopted by OECD countries to be used for the physical-chemical characterisation, fate estimation, and hazard identification for risk assessment of various chemicals. In addition to the TGs, OECD Guidance Documents (GDs) usually provide guidance on how to use TGs and how to interpret the results. These GDs do not have to be fully experimentally validated, and hence they are not under MAD, but they are based on relevant published scientific research. But are the existing TGs and the related GDs applicable and adequate for the regulatory testing of nanomaterials? In general, for nanomaterials it is accepted that most of the "endpoints" or more precisely measurement variables are applicable. However, for some endpoints new or amended TGs are needed. In addition, several GDs are needed to give more precise advice on the test performance in order to gain regulatory relevant data on nanomaterials. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - OECD KW - Nano KW - Guideline KW - Nanomaterials KW - Prüfrichtlinie PY - 2019 SN - 978-3-95606-440-1 DO - https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - F-61 SP - 279 EP - 279 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49515 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulz, K. A1 - Schmack, R. A1 - Klemm, H. W. A1 - Kabelitz, Anke A1 - Schmidt, T. A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - Mechanism and kinetics of hematite crystallization in air: Linking bulk and surface models via mesoporous films with defined nanostructure N2 - Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sampleaveraged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of Information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., Domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent Domain growth that terminates only upon complete transformation. A Johnson−Mehl−Avrami−Kolmogorov model describes the kinetics over a wide temperature range. The derived understanding enables the first synthesis of ferrihydrite films with ordered mesoporosity and quantitative control over the films’ hematite and ferrihydrite content. KW - Iron oxide KW - Crystallization KW - Mesoporous films KW - Nanostructure PY - 2017 DO - https://doi.org/10.1021/acs.chemmater.6b05185 SN - 0897-4756 SN - 1520-5002 VL - 29 IS - 4 SP - 1724 EP - 1734 AN - OPUS4-39690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sprachmann, J. A1 - Wachsmuth, T. A1 - Bhosale, M. A1 - Burmeister, D. A1 - Smales, Glen Jacob A1 - Schmidt, M. A1 - Kochovski, Z. A1 - Grabicki, N. A1 - Wessling, R. A1 - List-Kratochvil, E. J. W. A1 - Esser, B. A1 - Dumele, O. T1 - Antiaromatic Covalent Organic Frameworks Based on Dibenzopentalenes N2 - Despite their inherent instability, 4n π systems have recently received significant attention due to their unique optical and electronic properties. In dibenzopentalene (DBP), benzanellation stabilizes the highly antiaromatic pentalene core, without compromising its amphoteric redox behavior or small HOMO−LUMO energy gap. However, incorporating such molecules in organic devices as discrete small molecules or amorphous polymers can limit the performance (e.g., due to solubility in the battery electrolyte solution or low internal surface area). Covalent organic frameworks (COFs), on the contrary, are highly ordered, porous, and crystalline materials that can provide a platform to align molecules with specific properties in a well-defined, ordered environment. We synthesized the first antiaromatic framework materials and obtained a series of three highly crystalline and porous COFs based on DBP. Potential applications of such antiaromatic bulk materials were explored: COF films show a conductivity of 4 × 10−8 S cm−1 upon doping and exhibit photoconductivity upon irradiation with visible light. Application as positive electrode materials in Li-organic batteries demonstrates a significant enhancement of performance when the antiaromaticity of the DBP unit in the COF is exploited in its redox activity with a discharge capacity of 26 mA h g−1 at a potential of 3.9 V vs. Li/Li+ . This work showcases antiaromaticity as a new design principle for functional framework materials. KW - SAXS KW - MOUSE KW - Covalent Organic Frameworks KW - Batteries PY - 2023 DO - https://doi.org/10.1021/jacs.2c10501 SP - 1 EP - 12 PB - ACS Publications AN - OPUS4-56958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Maiwald, Michael A1 - Bassler, M. A1 - Deilmann, M. A1 - Ens, W. A1 - Frenzel, F. A1 - Gerlach, M. A1 - Großmann, J. A1 - Grümbel, F. A1 - Heisterkamp, M. A1 - Kaiser, U. A1 - Lambrecht, A. A1 - Ohlenkamp, R. A1 - Pötter, T. A1 - Pyka, P. A1 - Roos, E. A1 - Schmidt, A. A1 - Schünemann, U. A1 - Theuer, M. A1 - Tukle, A. A1 - Weber, N. T1 - Technologie-Roadmap „Prozess-Sensoren 2027+“ N2 - Die Technologie-Roadmap „Prozess-Sensoren 2027+“ ist eine Weiterentwicklung vorgängiger Technologie-Roadmaps. Im Zentrum dieser Roadmaps stehen Sensoren zur Erfassung von physikalischen und chemischen Messgrößen mittels spezifischer und unspezifischer Messverfahren, die zur Steuerung und dem besseren Verständnis von Prozessen dienen. Die Roadmap fasst die gemeinsame Technologie- und Marktsicht von Anwendern, Herstellern und Forschungseinrichtungen im Bereich Prozess-Sensorik in der verfahrenstechnischen Industrie zusammen. Sie beschreibt die wesentlichen Trends im Bereich Prozess-Sensorik und künftige Handlungsbedarfe für Hersteller, Anwender sowie für Einrichtungen der Forschung und Lehre. Für die aktuellen und zukünftigen Anforderungen an Prozess-Sensoren werden 19 Thesen formuliert. Die Thesen basieren auf den Thesen der vorangegangenen Roadmaps, wobei die aus heutiger Sicht erforderlichen Anpassungen, Ergänzungen und teilweise auch Streichungen vorgenommen wurden. Die Thesen sind in 5 Themencluster eingeordnet. Digitalisierung und Nachhaltigkeit sind übergreifende Kernthemen der künftigen Entwicklung. KW - Technologie-Roadmap Prozess-Sensoren KW - Prozessindustrie KW - Prozessanalytik KW - Sensorik KW - Digitalisierung KW - NAMUR PY - 2021 SP - 1 EP - 63 AN - OPUS4-53741 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Gogates, G. A1 - Eberhard, H. A1 - Pedersen, P. L. A1 - Ellison, S. A1 - Schmidt, Anita A1 - Abrantes da Costa, M. E. A1 - Holmgren, M. A1 - Tasic, T. A1 - Hald, J. T1 - Guidance for the Management of Computers and Software in Laboratories with Reference to ISO/IEC 17025:2005 N2 - This guideline is intended to be used as an aid to laboratories when they are managing the use of software and computers with respect to the requirements of ISO/IEC 17025. The working group consisted of representatives from accreditation bodies and conformity assessment operators, specifically laboratory organisations, but also included certification bodies, inspection bodies and metrology institutes. KW - Software KW - Laboratory KW - ISO/IEC 17025 PY - 2006 UR - http://www.eurolab.org/documents/2-2006.pdf VL - 2/2006 SP - 1 EP - 31 PB - EUROLAB CY - Paris AN - OPUS4-35414 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haist, M. A1 - Link, J. A1 - Nicia, D. A1 - Leinitz, Sarah A1 - Baumert, C. A1 - von Bronk, T. A1 - Cotardo, D. A1 - Eslami Pirharati, M. A1 - Fataei, S. A1 - Garrecht, H. A1 - Gehlen, C. A1 - Hauschildt, I. A1 - Ivanova, I. A1 - Jesinghausen, S. A1 - Klein, C. A1 - Krauss, H.-W. A1 - Lohaus, L. A1 - Lowke, D. A1 - Mazanec, O. A1 - Pawelczyk, S. A1 - Pott, U. A1 - Radebe, N. W. A1 - Riedmiller, J. J. A1 - Schmid, H.-J. A1 - Schmidt, Wolfram A1 - Secrieru, E. A1 - Stephan, D. A1 - Thiedeitz, M. A1 - Wilhelm, M. A1 - Mechtcherine, V. T1 - Interlaboratory study on rheological properties of cement pastes and reference substances: comparability of measurements performed with different rheometers and measurement geometries N2 - This paper presents the results of an interlaboratory study of the rheological properties of cement paste and ultrasound gel as reference substance. The goal was to quantify the comparability and reproducibility of measurements of the Bingham parameters yield stress and plastic viscosity when measured on one specific paste composition and one particular ultrasound gel in different laboratories using different rheometers and measurement geometries. The procedures for both in preparing the cement paste and carrying out the rheological measurements on cement paste and ultrasound gel were carefully defined for all of the study’s participants. Different conversion schemes for comparing the results obtained with the different measurement setups are presented here and critically discussed. The procedure proposed in this paper ensured a reasonable comparability of the results with a coefficient of variation for the yield stress of 27% and for the plastic viscosity of 24%, despite the individual measurement series’ having been performed in different labs with different rheometers and measurement geometries. KW - Rheometry KW - Rheology KW - Interlaboratory test KW - Test setup KW - Testing procedure KW - Cement paste KW - Ultrasound gel PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511220 DO - https://doi.org/10.1617/s11527-020-01477-w SN - 1871-6873 VL - 53 IS - 4 SP - 92 PB - Rilem AN - OPUS4-51122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -