TY - CONF A1 - Robertson, Daniela A1 - Schröder, Hartmut A1 - Böhning, Martin A1 - Brummermann, K. A1 - Kaundinya, I. A1 - Saathoff, F. T1 - Test method for the assessment of the service life of polymeric geosynthetic barriers (GBR-P) for road tunnels N2 - This paper is dealing with a systematic investigation to evaluate the testing method “autoclave test” for the assessment of the oxidative durability of polyolefin-based GBR-P products applied in road tunnel construction. The aim was to derive suitable exposure conditions and criteria for a practical testing procedure with regard to service lifetimes up to 100 years. The screening test (index test) according to DIN EN ISO 13438 developed in the BAM was applied in extended form and amended by a basic characterization, as well as complementary analyses, following autoclave exposure. The time dependency of some of the products and the so called lifetime parameter of one product were investigated and compared with the results of conventional oven tests. Based on the results of the research program some conclusions and practical outlooks were concluded. T2 - Euro GEO 5 - 5th European geosynthetics congress CY - Valencia, Spain DA - 16.09.2012 KW - Durability KW - Oxidation KW - Acceleration ageing KW - GBR-P PY - 2012 SN - 978-0415-64340-5 VL - 1 IS - Topic: Transport SP - 150 EP - 154 AN - OPUS4-27312 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Werrel, Martin A1 - Deubel, Jan A1 - Krüger, Simone A1 - Hofmann-Böllinghaus, Anja A1 - Antonatus, E. A1 - Krause, U. A1 - Duerler, F. T1 - Use and benefit of a controlled-atmosphere cone calorimeter N2 - A controlled-atmosphere cone calorimeter that is built by modifying the Standard apparatus with the addition of a controlled-atmosphere chamber offers a time- and cost-saving approach for reaction-to-fire testing in vitiation- and ventilation-controlled atmospheres. Due to the design of the added enclosure no mechanical changes on cone calorimeter’s Standard ductwork are required. This offers some advantages but also important limitations. The design has an open connection between the outlet of the added enclosure and the cone calorimeter’s exhaust hood. Therefore, sufficient ambient air from the laboratory surroundings is drawn into the System to introduce effects which have the potential to affect test results significantly. A procedure which is is suitable to consider physical effects of the ambient air on the calculation of the heat release rate is presented as well as initial results of an application towards toxic potency assessment. Signs for Chemical effects of the ambient air such as post reactions are shown but subject of an ongoing work. T2 - Fire and materials 2013 - 13th International conference and exhibition CY - San Francisco, CA, USA DA - 28.01.2013 KW - Controlled-atmosphere cone calorimeter KW - Heat release rate KW - Oxygen consumption KW - Smoke toxicity PY - 2013 SP - 273 EP - 286 PB - Interscience Communications CY - London, UK AN - OPUS4-27707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roters, F. A1 - Aslam, A. A1 - Bai, Y. A1 - Büschelberger, M. A1 - Bulert, K. A1 - Butz, A. A1 - Hickel, Tilmann A1 - Jogi, T. A1 - Klitschke, S. A1 - Martin, M. A1 - Meyer, L.-P. A1 - Morand, L. A1 - Nahshon, Y. A1 - Radtke, N. A1 - Saikia, Ujjal A1 - Trondl, A. A1 - Wessel, A. A1 - Zierep, P. A1 - Helm, D. T1 - StahlDigital: Ontology-Based Workflows for the Steel Industry N2 - The innovative strength of the steel industry is based on the mastery of microstructure–property relationships. Digital workflows can largely contribute to this aim by making the complexity of workflows reproducible and their execution user independent. In this work, the tools and workflows developed in the project StahlDigital as part of the German MaterialDigital initiative are presented and application examples are provided. A steel ontology builds the foundation for data collection and storage as well as for the semantic description of experimental and simulation data processing workflows. A dataspace powered by the Dataspace Management System (DSMS) digitally represents such workflows and manages data along them in a Findable, Accessible, Interoperable, Reusable manner aiming to derive new knowledge. Experimental data processed via DSMS can be further evaluated and used as input for simulation workflows. The simulations included in such workflows are run by the workflow system pyiron, which has been semantically extended in StahlDigital for this purpose. KW - Steel KW - Rolling KW - Multiscale simulation KW - Ontology KW - Workflow PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627187 DO - https://doi.org/10.1002/adem.202402148 SN - 1527-2648 SP - 1 EP - 13 PB - Wiley VHC-Verlag AN - OPUS4-62718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Schäfers, F. A1 - Adam, Christian T1 - Chemical state of chromium, sulfur, and iron in sewage sludge ash based phosphorus fertilizers N2 - As an essential element of all life forms, phosphorus (P) is vital to the fertilizer industry. With decreasing quantity and quality of phosphate rock resources, recycling P-fertilizers from wastewater is of increasing interest. The P-fertilizer products of a recently developed thermochemical process for P recovery from sewage sludge ash (SSA) were investigated by chromium, sulfur, and iron K-edge X-ray near-edge structure (XANES) spectroscopy. This paper focuses the formation and prevention of toxic chromium(VI) and toxic sulfides during the thermochemical processes. Reducing conditions prevent the oxidation of chromium(III) in the SSA to toxic chromium(VI). Sulfides formed under the reducing conditions are nontoxic iron sulfides. Hematite (Fe2O3) present in the SSA is reduced to magnetite (Fe3O4). A gentle post-treatment at 400 °C under oxidizing conditions converts the iron sulfides into plant-available iron sulfates. This oxidative post-treatment does not form undesired chromium(VI) compounds. KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Phosphorus recovery KW - Sewage sludge ash KW - Chromium KW - Sulfur KW - Iron PY - 2015 DO - https://doi.org/10.1021/acssuschemeng.5b00678 SN - 2168-0485 VL - 3 IS - 10 SP - 2376 EP - 2380 PB - ACS Publ. CY - Washington, DC AN - OPUS4-34166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lilensten, L. A1 - Provost, K. A1 - Perrière, L. A1 - Fonda, E. A1 - Couzinié, J. A1 - Amman, F. A1 - Radtke, Martin A1 - Dirras, G. A1 - Guillot, I. T1 - Experimental investigation of the local environment and lattice distortion in refractory medium entropy alloys N2 - EXAFS analysis of pure elements, binary and ternary equiatomic refractory alloys within the Nb-Zr-Ti-Hf- Ta system is performed at the Nb and Zr K-edges to analyze the evolution of the chemical local environ- ment and the lattice distortion. A good mixing of the elements is found at the atomic scale. For some compounds, a distribution of distances between the central atom and its neighbors suggests a distortion of the structure. Finally, analysis of the Debye-Waller parameters shows some correlation with the lat- tice distortion parameter δ², and allows to quantify experimentally the static disorder in medium entropy alloys. KW - BAMline KW - Refractory alloys KW - EXAFS KW - Debye-Waller parameter PY - 2022 DO - https://doi.org/10.1016/j.scriptamat.2022.114532 SN - 1359-6462 VL - 211 SP - 1 EP - 6 PB - Elsevier Ltd. AN - OPUS4-55287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grengg, C. A1 - Koraimann, G. A1 - Ukrainczyk, N. A1 - Rudic, O. A1 - Luschnig, S. A1 - Gluth, Gregor A1 - Radtke, Martin A1 - Dietzel, M. A1 - Mittermayr, F. T1 - Cu- and Zn-doped alkali activated mortar – Properties and durability in (bio)chemically aggressive wastewater environments N2 - Metakaolin-based alkali activated mortars (AAM) - with and without CuSO4·5H2O and ZnO addition (mass ratio Mn+/solid binder 0.08% to 1.7%) - were casted and exposed within an extensive long-term field campaign over the period of 20 months to a sewer basin, strongly affected by biogenic acid corrosion. (Un-)exposed AAM were tested regarding their physicochemical and microstructural properties, bioreceptivity and overall durability. Metal addition led to a retarding effect during alkali-activation reaction, as well as to an increase in open porosity of up to 3.0% and corresponding lower compressive strength of up to 10.9%. Reduced microbial colonization and diversity were observed on AAM with Cu, while Zn addition led to increased biodiversity. We propose that the observed higher durability of Cu-doped AAM is due to antibacterial effects and associated reduction of biogenic acid production, superseding overall negative effects of metal-dosage on physical material properties. Observed lower durability of Zn-doped AAM was related to combined negative physicochemical and microbial effects. KW - Microbially induced corrosion KW - Alkali-activated materials KW - Biogenic acid corrosion KW - Biogene Schwefelsäurekorrosion KW - MIC PY - 2021 DO - https://doi.org/10.1016/j.cemconres.2021.106541 SN - 0008-8846 VL - 149 SP - 1 EP - 15 PB - Elsevier CY - Oxford AN - OPUS4-53070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nowak, S.H. A1 - Bjeoumikhov, A. A1 - Von Borany, J. A1 - Buchriegler, J. A1 - Munnik, F. A1 - Petric, M. A1 - Renno, A.D. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Strüder, L. A1 - Wedell, R. A1 - Ziegenrücker, R. T1 - Examples of XRF and PIXE imaging with few microns resolution using SLcam® a color X-ray camera N2 - We present results of recent development of the color X-ray camera, type SLcam®, allowing detection of X-ray images with few microns resolution. Such spectral resolution is achieved with the use of high-quality polycapillary optics combined with sub-pixel resolution. Imaging of Siemens star resolution test chart reveals that the resolution limit of SLcam® can go down to nearly 5µm. Several real sample examples of measurements carried out at the laboratory, synchrotron, and particle-induced X-ray emission beamlines are shown. This is the first time SLcam® is used as particle-induced X-ray emission detector. KW - X-ray KW - Color X-ray camera KW - CXC KW - Synchrotron radiation KW - BESSY KW - BAMline PY - 2015 DO - https://doi.org/10.1002/xrs.2590 SN - 0049-8246 VL - 44 IS - 3 SP - 135 EP - 140 PB - Wiley & Sons, Ltd. CY - Chichester AN - OPUS4-33170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zier, M. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Radtke, Martin A1 - Munnik, F. T1 - Accurate stopping power determination of 15N ions for hydrogen depth profiling by a combination of ion beams and synchrotron radiation N2 - Hydrogen analysis is of particular importance in thin film technology and it is often necessary to obtain a depth profile. The method with the best depth resolution is NRA using the 6385 keV resonance of the 1H(15N,αγ)12C nuclear reaction. The correct quantification of the depth and concentration scales in the measured hydrogen profiles relies on accurate stopping power values. We present a method to deduce these values from a combination of two techniques: NRA and X-ray reflectometry (XRR). This method is applied to the determination of the stopping power of ~6.4 MeV 15N ions in H-containing amorphous Si-layers (a-Si:H). Density-independent stopping powers at different H concentrations are determined by combining the results from NRA and XRR with an overall uncertainty of 3.3%, showing good agreement with SRIM values. This work shows exemplary the methodology for future evaluation of stopping powers for quality assurance in NRA. KW - Nuclear reaction analysis KW - Hydrogen depth profiling KW - Stopping cross section KW - Linear energy transfer KW - Synchrotron radiation KW - XRR PY - 2012 DO - https://doi.org/10.1016/j.nimb.2011.07.027 SN - 0168-583X SN - 1872-9584 VL - 273 SP - 18 EP - 21 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-25722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabral, A.R. A1 - Radtke, Martin A1 - Munnik, F. A1 - Lehmann, B. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Tupinambá, M. A1 - Kwitko-Ribeiro, R. T1 - Iodine in alluvial platinum-palladium nuggets: evidence for biogenic precious-metal fixation N2 - Synchrotron radiation-induced X-ray fluorescence (SR-XRF) spectrometry was applied to determine iodine concentrations in alluvial Pt–Pd aggregates with delicate morphological features from Córrego Bom Sucesso, Minas Gerais, Brazil. The millimetre-sized botryoidal and rod-shaped grains of alluvial Pt–Pd–Hg intermetallic compounds have surprisingly high concentrations of iodine, in the range from 10 to ~ 120 μg/g. Because iodine is a strongly biophile element, known to be enriched in peatlands and plant remains in soils by microbial activity, its concentration in the Pt–Pd nuggets suggests biogenic precious-metal fixation in the aqueous alluvial milieu. Biogenic and inorganic processes, such as bioreduction and electrochemical metal accretion, could mutually have contributed to the growth of nanoparticles, formed on organic templates, to millimetric Pt–Pd nuggets. KW - Lodine KW - Pt-Pd nuggets KW - Córrego Bom Sucesso KW - Minas Gerais KW - Brazil PY - 2011 DO - https://doi.org/10.1016/j.chemgeo.2010.12.003 SN - 0009-2541 SN - 1872-6836 VL - 281 IS - 1-2 SP - 125 EP - 132 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-23174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fiedler Bremer, C. A1 - Scholz, R. A1 - Myslicki, S. A1 - Starke, P. A1 - Boller, C. A1 - Walther, F. A1 - Krause, Martin T1 - NDT-based characteriazation of timber and vulcanized fiber for civil infrastructure N2 - The paper addresses beech wood as well as vulcanized fiber and discusses the results obtained when using acoustic emission and thermography as non-destructive testing techniques along tensile and load increase fatigue tests to characterize the wooden material’s behavior under increasing fatigue loads to get enhanced information regarding the fatigue behavior of both materials. Reference is mainly made to the materials’ anisotropic and microstructural behavior and what implications this has with respect to the materials’ strength. The influence of moisture is discussed, as well as parameters that may deserve monitoring in the sense of structural health monitoring to be applied in timber structures in general. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Ermüdung KW - Belastungsversuch KW - Thermographie KW - ZfP KW - Timber PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-346377 UR - https://www.ndt.net/?id=18419 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 11 PB - NDT.net CY - Kirchwald AN - OPUS4-34637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pogány, A. A1 - Balslev-Harder, D. A1 - Braban, Ch. F. A1 - Cassidy, N. A1 - Ebert, V. A1 - Ferracci, V. A1 - Hieta, T. A1 - Leuenberger, D. A1 - Martin, N. A. A1 - Pascale, C. A1 - Peltola, J. A1 - Persijn, S. A1 - Tiebe, Carlo A1 - Twigg, M. M. A1 - Vaittinen, Olavi A1 - van Wijk, J. A1 - Wirtz, K. A1 - Niederhauser, B. T1 - A metrological approach to improve accuracy and reliability of ammonia measurements in ambient air N2 - The environmental impacts of ammonia (NH3) in ambient air have become more evident in the recent decades, leading to intensifying research in this field. A number of novel analytical techniques and monitoring instruments have been developed, and the quality and availability of reference gas mixtures used for the calibration of measuring instruments has also increased significantly. However, recent inter-comparison measurements show significant discrepancies, indicating that the majority of the newly developed devices and reference materials require further thorough validation. There is a clear need for more intensive metrological research focusing on quality assurance, intercomparability and validations. MetNH3 (Metrology for ammonia in ambient air) is a three-year project within the framework of the European Metrology Research Programme (EMRP), which aims to bring metrological traceability to ambient ammonia measurements in the 0.5–500 nmol mol−1 amount fraction range. This is addressed by working in three areas: (1) improving accuracy and stability of static and dynamic reference gas mixtures, (2) developing an optical transfer standard and (3) establishing the link between high-accuracy metrological standards and field measurements. In this article we describe the concept, aims and first results of the project. KW - Ammonia in ambient air KW - Traceability KW - Reference gas standards KW - Optical transfer standard KW - Validation and testing infrastructure PY - 2016 DO - https://doi.org/10.1088/0957-0233/27/11/115012 SN - 0957-0233 VL - 27 IS - 11 SP - 115012 EP - 115026 PB - IOP Publishing Ltd. AN - OPUS4-39130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ordavo, I. A1 - Ihle, S. A1 - Arkadiev, V. A1 - Scharf, Oliver A1 - Soltau, H. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, S. A1 - Buzanich, Günter A1 - Gubzhokov, R. A1 - Günther, A. A1 - Hartmann, R. A1 - Holl, P. A1 - Kimmel, N. A1 - Kühbacher, M. A1 - Lang, M. A1 - Langhoff, N. A1 - Liebel, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Schaller, G. A1 - Schopper, F. A1 - Strüder, L. A1 - Thamm, C. A1 - Wedell, R. T1 - A new pnCCD-based color X-ray camera for fast spatial and energy-resolved measurements N2 - We present a new high resolution X-ray imager based on a pnCCD detector and a polycapillary optics. The properties of the pnCCD like high quantum efficiency, high energy resolution and radiation hardness are maintained, while color corrected polycapillary lenses are used to direct the fluorescence photons from every spot on a sample to a corresponding pixel on the detector. The camera is sensitive to photons from 3 to 40 keV with still 30% quantum efficiency at 20 keV. The pnCCD is operated in split frame mode allowing a high frame rate of 400 Hz with an energy resolution of 152 eV for Mn Kα (5.9 keV) at 450 kcps. In single-photon counting mode (SPC), the time, energy and position of every fluorescence photon is recorded for every frame. A dedicated software enables the visualization of the elements distribution in real time without the need of post-processing the data. A description of the key components including detector, X-ray optics and camera is given. First experiments show the capability of the camera to perform fast full-field X-Ray Fluorescence (FF-XRF) for element analysis. The imaging performance with a magnifying optics (3×) has also been successfully tested. KW - X-ray CCD camera KW - pnCCD KW - Fast X-ray imaging KW - XRF KW - Full-field X-ray fluorescence KW - Elemental analysis KW - High quantum efficiency KW - High energy resolution KW - Polycapillary optics PY - 2011 DO - https://doi.org/10.1016/j.nima.2011.05.080 SN - 0168-9002 SN - 0167-5087 VL - 654 SP - 250 EP - 257 PB - North-Holland CY - Amsterdam AN - OPUS4-24370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kanngießer, B. A1 - Malzer, W. A1 - Fuentes Rodriguez, A. A1 - Reiche, I. A1 - Voigt, F. A1 - Radtke, Martin T1 - 3D micro X-ray fluorescence spectroscopy - combining elemental analysis with chemical speciation PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=495 SN - 0179-4159 SP - 495 EP - 497 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3513 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Calligaro, T. A1 - Radtke, Martin A1 - Reiche, I. A1 - Riesemeier, Heinrich T1 - Fingerprinting ancient gold by measuring Pt with spatially resolved high energy Sy-XRF N2 - Trace elements of ancient gold such as Pt, give fundamental information on the circulation of the metal in the past. In the case of objects from the cultural heritage, the determination of trace elements requires non-destructive point analysis in general. These conditions and the need of good detection limits restrain the number of applicable analytical techniques. After the development of a PIXE set-up with a selective Cu or Zn filter of 75 µm and of a PIXE-XRF set-up using a primary target of As, we tested the possibilities of spatially resolved Sy-XRF to determine Pt in gold alloys. With a Zn filter, PIXE showed a detection limit of 1000 ppm in gold while PIXE-XRF lowers this detection limit down to 80 ppm. This last value being constrained by the resonant Raman effect produced on gold. In order to improve the detection limit of Pt keeping the non-destructiveness and access to point analysis, we developed an analytical protocol for XRF with synchrotron radiation at BESSY II, using the BAMline set-up. The L-lines of Pt were excited by a beam of energy above and below 11.564 keV and measured using a Si(Li) detector with a 50 µm Cu filter. A µ-beam of 100–250 µm2 was used according to the size of the sample. The determination of the Pt content in the samples was carried out by Monte-Carlo simulation and subtraction of Au and Pt spectra obtained on pure standards. The limit of detection for Pt of 20 ppm was determined by using certified standards. The detection limits of a small set of other characteristic elements of gold were also measured using an incident energy of 33 keV. KW - PIXE-XRF KW - Sy-XRF KW - Pt KW - Ancient gold KW - Fingerprinting PY - 2005 DO - https://doi.org/10.1016/j.nimb.2005.06.150 SN - 0168-583X SN - 1872-9584 VL - 240 IS - 1-2 SP - 505 EP - 511 PB - Elsevier CY - Amsterdam AN - OPUS4-14236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Radtke, Martin A1 - Reiche, I. A1 - Riesemeier, Heinrich A1 - Strub, Erik T1 - Analysis of trace elements in gold alloys by SR-XRF at high energy at the BAMline N2 - Measuring in a non-destructive way the characteristic trace elements of the metal allows following the circulation of gold in the past. The aim of this work is to probe the possibilities of X-ray fluorescence with high energy synchrotron radiation (SR-XRF) at the BAMline at BESSY II to determine the concentration of Pt in ancient gold alloys. A HP-Ge detector was used to measure the Pt K-lines excited with an incident energy of 79.5 keV. Data processing was done by subtraction of a Pt free gold standard spectrum from the spectrum of the sample. Depending on the sample composition, the MDL ranges between 40 and 90 ppm. The first results obtained for a small set of gold alloys of different thickness, size and composition showed that high energy SR-XRF is a significant method for the non-destructive determination of Pt in gold. KW - SR-XRF KW - Gold KW - Provenancing KW - Trace elements PY - 2008 DO - https://doi.org/10.1016/j.nimb.2008.03.008 SN - 0168-583X SN - 1872-9584 VL - 266 IS - 10 SP - 2334 EP - 2338 PB - Elsevier CY - Amsterdam AN - OPUS4-17735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodrigues, M. A1 - Cappa, F. A1 - Schreiner, M. A1 - Ferloni, P. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Woytek, B. A1 - Alram, M. T1 - Further metallurgical analyses on silver coins of Trajan (AD 98-117) N2 - Within an interdisciplinary project, preliminary results of which were published in 2007, a group of 65 silver coins (denarii) of Trajan, evenly distributed over the entire span of his reign (2nd to 6th consulate), as well as 3 coins from the reign of his predecessor, the emperor Nerva (AD 96–98), had been acquired on the coin market. These pieces could be cross-sectioned in order to carry out analyses. Measurements were performed with µ-XRF and µ-SRXRF to check the fineness of the denarius alloy as well as to investigate if the coins of the different consulates showed distinct traits concerning the main impurities which could suggest a change of ore sources. Furthermore, it was examined whether the influx of precious metals into the Roman treasury after Trajan's Dacian campaigns (AD 101/102 and 105/106) could have had any repercussions on the composition of the denarius alloy; comparative data was provided by the analysis of nine imitations of Roman Republican denarii presumably struck in Dacia. Documentation of the cross-sections was performed with SEM/EDX in order to clarify details concerning the specific microstructure of the coins. An enrichment of Ag of approx. 100 to 200 µm in the near surface regions of most of the coins could be observed, which is due to corrosion effects. Previous metallographic analyses done by several scholars had been inadequate to clarify the central numismatic and economic questions. With the presented analyses, it was possible to correct the results of the earlier research and to provide, for the first time, a secure basis of data for the investigation of the development of the silver alloy used for denarii in Trajan's reign. PY - 2011 DO - https://doi.org/10.1039/c0ja00252f SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 5 SP - 873 EP - 1100 PB - Royal Society of Chemistry CY - London AN - OPUS4-23623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nowak, S.H. A1 - Bjeoumikhov, A. A1 - Von Borany, J. A1 - Buchriegler, J. A1 - Munnik, F. A1 - Petric, M. A1 - Radtke, Martin A1 - Renno, A.D. A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Wedell, R. T1 - Sub-pixel resolution with a color X-ray camera N2 - The color X-ray camera SLcam® is a full-field, single photon detector providing scanning-free, energy and spatially resolved X-ray imaging. Spatial resolution is achieved with the use of polycapillary optics guiding X-ray photons from small regions on a sample to distinct energy dispersive pixels on a charged-coupled device detector. Applying sub-pixel resolution, signals from individual capillary channels can be distinguished. Therefore, the SLcam® spatial resolution, which is normally limited to the pixel size of the charge-coupled device, can be improved to the size of individual polycapillary channels. In this work a new approach to a sub-pixel resolution algorithm comprising photon events also from the pixel centers is proposed. The details of the employed numerical method and several sub-pixel resolution examples are presented and discussed. KW - Color X-ray camera KW - Sub pixel analysis PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-334948 DO - https://doi.org/10.1039/c5ja00028a SN - 0267-9477 SN - 1364-5544 SP - 1890 EP - 1897 PB - Royal Society of Chemistry CY - London AN - OPUS4-33494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Fischer, M. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - Inca figurines from the Ethnologisches Museum in Berlin: an analytical study of some typical and atypical productions N2 - Fourteen hollow and one cast anthropomorphic and zoomorphic figurines produced in Incan times for ritual offerings from the Ethnologisches Museum in Berlin were selected to investigate the technologies and alloys used for their fabrication with portable optical microscopy and non-destructive XRF elemental analysis. This group of gold and silver figurines includes typical specimens of the Inca production, such as the four silver figurines from the Island Coati in Lake Titicaca and the two gold figurines from Pachacamac, as well as specimens that are seldom present in collections, which makes them atypical. In addition to the tall figurines with atypical hair or standing pose, one bicolour figurine half silver, half gold) and another with coloured inlays were included in this study for comparison. The large majority of the silver specimens are made from very high quality alloys and the gold figurines are made from alloys containing low copper contents and silver ranging from 30wt% to 52wt%. KW - Gold KW - pXRF KW - Inca PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-436015 DO - https://doi.org/10.4000/bifea.8232 SN - 0303-7495 VL - 46 IS - 1 SP - 221 EP - 251 PB - Institut Français d'Études Andines AN - OPUS4-43601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de O. Primo, J. A1 - Horsth, D.F. A1 - de S. Correa, J. A1 - Das, A. A1 - Bittencourt, C. A1 - Umek, P. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Yusenko, Kirill A1 - Zanetta, C. A1 - Anaissi, F.J. T1 - Synthesis and Characterization of Ag/ZnO Nanoparticles for Bacteria Disinfection in Water N2 - n this study, two green synthesis routes were used for the synthesis of Ag/ZnO nanoparticles, using cassava starch as a simple and low-cost effective fuel and Aloe vera as a reducing and stabilizing agent. The Ag/ZnO nanoparticles were characterized and used for bacterial dis- infection of lake water contaminated with Escherichia coli (E. coli). Characterization indicated the formation of a face-centered cubic structure of metallic silver nanoparticles with no insertion of Ag into the ZnO hexagonal wurtzite structure. Physicochemical and bacteriological analyses described in “Standard Methods for the Examination of Water and Wastewater” were used to evaluate the efficiency of the treatment. In comparison to pure ZnO, the synthesized Ag/ZnO nanoparticles showed high efficiencies against Escherichia coli (E. coli) and general coliforms present in the lake water. These pathogens were absent after treatment using Ag/ZnO nanoparticles. The results indicate that Ag/ZnO nanoparticles synthesized via green chemistry are a promising candidate for the treatment of wastewaters contaminated by bacteria, due to their facile preparation, low-cost synthesis,and disinfection efficiency. KW - Synchrotron KW - BAMline PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562440 DO - https://doi.org/10.3390/nano12101764 SN - 2079-4991 VL - 12 IS - 10 SP - 1 EP - 18 PB - MDPI CY - Basel AN - OPUS4-56244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Förste, F. A1 - Bauer, L. A1 - Streeck, C. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Kadow, D. A1 - Keil, C. A1 - Mantouvalou, I. T1 - Quantitative Analysis and 2D/3D Elemental Imaging of Cocoa Beans Using X‑ray Fluorescence Techniques N2 - As an important raw material for the confectionery industry, the cocoa bean (Theobroma cacao L.) has to meet certain legal requirements in terms of food safety and maximum contaminant levels in order to enter the cocoa market. Understanding the enrichment and distribution of essential minerals but also toxic metals is of utmost importance for improving the nutritional quality of this economically important raw food material. We present three X-ray fluorescence (XRF) techniques for elemental bio-imaging of intact cocoa beans and one additional XRF technique for quantitative analysis of cocoa pellets. The interrelation of all the methods presented gives a detailed picture of the content and 3D-resolved distribution of elements in complete cocoa beans for the first time. KW - BAMline KW - Synchrotron KW - XRF KW - CXC KW - Cocoa PY - 2023 DO - https://doi.org/10.1021/acs.analchem.2c05370 VL - 95 SP - 5627 EP - 5635 PB - ACS Publications AN - OPUS4-57832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grengg, C. A1 - Gluth, Gregor A1 - Mittermayr, F. A1 - Ukrainczyk, N. A1 - Bertmer, M. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Leis, A. A1 - Dietzel, M. T1 - Deterioration mechanism of alkali-activated materials in sulfuric acid and the influence of Cu: A micro-to-nano structural, elemental and stable isotopic multi-proxy study N2 - In this study, a multi-proxy approach combining 29Si, 27Al and 1H MAS-NMR, FEG-EPMA, XANES at the Cu K-edge and XRD analytics with hydrochemical tools such as ICP-OES analyses, oxygen-isotope signatures, and thermodynamic modelling was applied to K-silicate-activated metakaolin specimens - with and without CuSO4·5H2O addition - exposed to sulfuric acid at pH = 2 for 35 days. The results revealed a multistage deterioration mechanism governed by (i) acid diffusion, (ii) leaching of K-A-S-H, (iii) microstructural damage related to precipitation of expansive (K,Ca,Al)-sulfate-hydrate phases (iv) complete dissolution of the K-A-S-H framework, (v) and formation of silica gel in the outermost corroded regions. Copper ions were mainly located in layered spertiniite-chrysocolla-like phases in the as-cured materials. The results demonstrate an overall negative effect of Cu addition on chemical material durability, implying that the reported higher durability of Cu-doped AAM in biocorrosion environments can be best explained by bacteriostatic effects. KW - Alkali-activated materials KW - Acid resistance KW - Microbially induced corrosion KW - MIC PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520567 DO - https://doi.org/10.1016/j.cemconres.2021.106373 SN - 0008-8846 VL - 142 SP - 1 EP - 15 PB - Elsevier CY - Oxford AN - OPUS4-52056 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gomes, Bruna F. A1 - Prokop, Martin A1 - Bystron, Tomas A1 - Loukrakpam, Rameshwori A1 - Melke, Julia A1 - Lobo, Carlos M. S. A1 - Fink, Michael A1 - Zhu, Mengshu A1 - Voloshina, Elena A1 - Kutter, Maximilian A1 - Hoffmann, Hendrik A1 - Yusenko, Kirill V. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Röder, Bettina A1 - Bouzek, Karel A1 - Paulus, Beate A1 - Roth, Christina T1 - Following Adsorbed Intermediates on a Platinum Gas Diffusion Electrode in H3PO3-Containing Electrolytes Using In Situ X-ray Absorption Spectroscopy N2 - One of the challenges of high-temperature polymer electrolyte membrane fuel cells is the poisoning of the Pt catalystwith H3PO4. H3PO4 is imbibed into the routinely used polybenzimidazole-based membranes, which facilitate Proton conductivity in the temperature range of 120−200 °C. However, when leached out of the membrane by water produced during operation, H3PO4 adsorbs on the Pt catalyst surface, blocking the active sites and hindering the oxygen reduction reaction (ORR). The reduction of H3PO4 to H3PO3, which occurs at the anode due to a combination of a low potential and the presence of gaseous H2, has been investigated as an additional important contributing factor to the observed poisoning effect. H3PO3 has an affinity toward adsorption on Pt surfaces even greater than that of H2PO4 −. In this work, we investigated the poisoning effect of both H3PO3 and H3PO4 using a half-cell setup with a gas diffusion electrode under ambient conditions. By means of in situ X-ray absorption spectroscopy, it was possible to follow the signature of different species adsorbed on the Pt nanoparticle catalyst (H, O, H2PO4 −, and H3PO3) at different potentials under ORR conditions in various electrolytes (HClO4, H3PO4, and H3PO3). It was found that H3PO3 adsorbs in a pyramidal configuration P(OH)3 through a Pt−P bond. The competition between H3PO4 and H3PO3 adsorption was studied, which should allow for a better understanding of the catalyst poisoning mechanism and thus assist in the development of strategies to mitigate this phenomenon in the future by minimizing H3PO3 generation by, for example, improved catalyst design or adapted operation conditions or changes in the electrolyte composition. KW - H3PO4 life cycle KW - XAS KW - In situ coupling KW - High-temperature fuel cells KW - H3PO3, KW - Δμ XANES PY - 2022 DO - https://doi.org/10.1021/acscatal.2c02630 SN - 2155-5435 VL - 12 IS - 18 SP - 11472 EP - 11484 PB - American Chemical Society (ACS) AN - OPUS4-64733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Nowak, S. H. A1 - Petric, M. A1 - Buchriegler, J. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, Z. A1 - von Borany, J. A1 - Munnik, F. A1 - Radtke, Martin A1 - Renno, A. D. A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Tilgner, J. A1 - Wedell, R. T1 - Road to micron resolution with a color X-ray camera - Polycapillary optics characterization N2 - In a color X-ray camera spatial resolution is achieved by means of a polycapillary optic conducting X-ray photons from small regions on a sample to distinct energy dispersive pixels on a CCD matrix. At present, the resolution limit of color X-ray camera systems can go down to several microns and is mainly restricted by Pixel dimensions. The recent development of an efficient subpixel resolution algorithm allows a release from pixel size, limiting the resolution only to the quality of theoptics. In this work polycapillary properties that influence the spatial resolution are systematized and assessed both theoretically and experimentally. It is demonstrated that with the current technological Level reaching one micron resolution is challenging, but possible. KW - Color X-ray camera KW - Polycapillary optics PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404404 DO - https://doi.org/10.48550/arXiv.1705.08939 SN - 2331-8422 SP - 1 EP - 11 PB - Cornell University CY - Ithaca, NY AN - OPUS4-40440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - C. Pardo Pérez, L. A1 - Arndt, A. A1 - Stojkovikj, S. A1 - Y. Ahmet, I. A1 - T. Arens,, J. A1 - Dattila, F. A1 - Wendt, R. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Davies, V. A1 - Höflich, K. A1 - Köhnen, E. A1 - Tockhorn, P. A1 - Golnak, R. A1 - Xiao, J. A1 - Schuck, G. A1 - Wollgarten, M. A1 - López, N. A1 - T. Mayer, M. T1 - Determining Structure-Activity Relationships in Oxide Derived CuSn Catalysts During CO2 Electroreduction Using X-Ray Spectroscopy N2 - The development of earth-abundant catalysts for selective electrochemical CO2 conversion is a central challenge. Cu-Sn bimetallic catalysts can yield selective CO2 reduction toward either CO or formate. This study presents oxide-derived Cu-Sn catalysts tunable for either product and seeks to understand the synergetic effects between Cu and Sn causing these selectivity trends. The materials undergo significant transformations under CO2 reduction conditions, and their dynamic bulk and surface structures are revealed by correlating observations from multiple methods—X-ray absorption spectroscopy for in situ study, and quasi in situ X-ray photoelectron spectroscopy for surface sensitivity. For both types of catalysts, Cu transforms to metallic Cu0 under reaction conditions. However, the Sn speciation and content differ significantly between the catalyst types: the CO-selective catalysts exhibit a surface Sn content of 13 at. % predominantly present as oxidized Sn, while the formate-selective catalysts display an Sn content of ≈70 at. % consisting of both metallic Sn0 and Sn oxide species. Density functional theory simulations suggest that Snδ+ sites weaken CO adsorption, thereby enhancing CO selectivity, while Sn0 sites hinder H adsorption and promote formate production. This study reveals the complex dependence of catalyst structure, composition, and speciation with electrochemical bias in bimetallic Cu catalysts. KW - Electrochemical CO2 conversion KW - Cu catalysts KW - X-ray absorption spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547116 DO - https://doi.org/10.1002/aenm.202103328 SN - 1614-6832 VL - 12 IS - 5 SP - 2103328 PB - Wiley-VCH GmbH AN - OPUS4-54711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Cakir, Cafer Tufan A1 - Radtke, Martin A1 - Haider, M. Bilal A1 - Emmerling, Franziska A1 - F. M. Oliveira, P. A1 - Michalchuk, Adam T1 - Dispersive x-ray absorption spectroscopy for time-resolved in situ monitoring of mechanochemical reactions N2 - X-ray absorption spectroscopy (XAS) provides a unique, atom-specific tool to probe the electronic structure of solids. By surmounting long-held limitations of powder-based XAS using a dynamically averaged powder in a Resonant Acoustic Mixer (RAM), we demonstrate how time-resolved in situ (TRIS) XAS provides unprecedented detail of mechanochemical synthesis. The use of a custom-designed dispersive XAS (DXAS) setup allows us to increase the time resolution over existing fluorescence measurements from ∼15 min to 2 s for a complete absorption spectrum. Hence, we here establish TRIS-XAS as a viable method for studying mechanochemical reactions and sampling reaction kinetics. The generality of our approach is demonstrated through RAM-induced (i) bottom-up Au nanoparticle mechanosynthesis and (ii) the synthesis of a prototypical metal organic framework, ZIF-8. Moreover, we demonstrate that our approach also works with the addition of a stainless steel milling ball, opening the door to using TRIS-DXAS for following conventional ball milling reactions. We expect that our TRIS-DXAS approach will become an essential part of the mechanochemical tool box. KW - In situ studies KW - Dipsersive XAS KW - Mechanochemistry KW - Time-resolved PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567659 DO - https://doi.org/10.1063/5.0130673 SN - 1089-7690 VL - 157 IS - 21 SP - 1 EP - 12 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-56765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martin-Sanchez, Pedro Maria A1 - Miller, A. Z. A1 - Garcia-Sanchez, A. M. A1 - Martin-Sanchez, Pedro Maria A1 - F.C. Pereira, M. A1 - Afonso, M. J. A1 - Saiz-Jimenez, C. A1 - Spangenberg, J. E. A1 - Jurado, V. A1 - Dionísio, A. A1 - Chaminé, H. I. A1 - Hermosin, B. T1 - Origin of abundant moonmilk deposits in a subsurface granitic environment N2 - Subsurface granitic environments are scarce and poorly investigated. A multi-disciplinary approach was used to characterize the abundant moonmilk deposits and associated microbial communities coating the granite walls of the 16th Century Paranhos spring water tunnel in Porto city (north-west Portugal). It is possible that this study is the first record of moonmilk in an urban subsurface granitic environment. The morphology and texture, mineralogical composition, stable isotope composition and microbial diversity of moonmilk deposits have been studied to infer the processes of moonmilk formation. These whitish secondary mineral deposits are composed of very fine needle fibre calcite crystals with different morphologies and density. Calcified filaments of fungal hyphae or bacteria were distinguished by field emission scanning electron microscopy. Stable isotope analysis revealed a meteoric origin of the needle fibre calcite, with an important contribution of atmospheric CO2, soil respiration and HCO3 − from weathering of Ca-bearing minerals. The DNA-based analyses revealed the presence of micro-organisms related to urban contamination, including Actinobacteria, mainly represented by Pseudonocardia hispaniensis, Thaumarchaeota and Ascomycota, dominated by Cladosporium. This microbial composition is consistent with groundwater pollution and contamination sources of the overlying urban area, including garages, petrol stations and wastewater pipeline leakage, showing that the Paranhos tunnel is greatly perturbed by anthropogenic activities. Whether the identified micro-organisms are involved in the formation of the needle fibre calcite or not is difficult to demonstrate, but this study evidenced both abiotic and biogenic genesis for the calcite moonmilk in this subsurface granitic environment. KW - Biomineralization KW - Carbonate precipitation KW - Granite KW - Moonmilk KW - Needle fibre calcite PY - 2017 UR - https://onlinelibrary.wiley.com/doi/full/10.1111/sed.12431 DO - https://doi.org/10.1111/sed.12431 SN - 1365-3091 VL - 65 IS - 2 SP - 1482 EP - 1503 PB - Wiley AN - OPUS4-43622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vigna, L. A1 - Gottschalk, Martin A1 - Cacocciola, N. A1 - Verna, A. A1 - Marasso, S. L. A1 - Seeger, Stefan A1 - Pirri, C.F. A1 - Cocuzza, M. T1 - Flexible and reusable parylene C mask technology for applications in cascade impactor air quality monitoring systems N2 - The development of traceable new methodologies to quantify elemental air pollutants in particulate matter (PM) supports modernization of methods used in air quality monitoring networks in Europe. In the framework of the EURAMET EMPIR AEROMET II project, the combination of cascade impactor aerosol sampling and total reflection X-ray fluorescence elemental spectroscopy (TXRF) was investigated. This technique requires a traceable calibration based on reference samples. This paper describes a new, simple and effective method to produce such reference samples using flexible, reusable, and low-cost parylene C shadow masks, fabricated by photolithographic steps. These shadow masks can be used to produce reference samples that mimic the Dekati cascade impactor’s deposition patterns by applying as-prepared micro stencils to 30 mm acrylic substrates and evaporating a reference material (Ti) in arrangements of thin circular dots. The highly flexible direct patterning of acrylic discs with reference material, otherwise impossible with conventional photolithography, allows multiple reusing of the same micro stencils. The aspect ratios of the dots could be repeated with an error less than 4 %. A first set of standard reference samples for the 13 stages of the Dekati cascade impactor was produced and preliminary TXRF measurements of the deposited Ti masses were performed. The centricity of the deposition patterns turned out to be an important parameter for the quality of the TXRF results. The parylene mask technology for the production of reference samples turns out to be a promising new approach for the traceable calibration of TXRF spectrometers for the quantification of element concentrations in environmental aerosol samples but, due to its great versatility, it could be used for several other micropatterning applications on conventional and unconventional substrates. KW - AEROMET II KW - Aerosol KW - Parylene C KW - Reference samples KW - Flexible shadow masks KW - Cascade impactor KW - Air quality monitoring KW - Micropatterning KW - Mask fabrication KW - Elemental aerosol analysis KW - TXRF PY - 2022 DO - https://doi.org/10.1016/j.mne.2022.100108 SN - 2590-0072 VL - 14 SP - 1 EP - 19 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-54252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Reiche, I. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Guerra, M.F. T1 - Beyond the Great Wall: Gold of the silk roads and the first empire of the Steppes N2 - Fingerprinting ancient gold work requires the use of nondestructive techniques with high spatial resolution (down to 25 µm) and good detection limits (micrograms per gram level). In this work experimental setups and protocols for synchrotron radiation induced X-ray fluorescence (SRXRF) at the BAMline of the Berlin electron storage ring company for synchrotron radiation (BESSY) in Berlin for the measurement of characteristic trace elements of gold are compared considering the difficulties, shown in previous works, connected to the quantification of Pt. The best experimental conditions and calculation methods were achieved by using an excitation energy of 11.58 keV, a silicon drift chamber detector (SDD) detector, and pure element reference standards. A detection limit of 3 µg/g has been reached. This newly developed method was successfully applied to provenancing the Xiongnu gold from the Gol Mod necropolis, excavated under the aegis of the United Nations Educational, Scientific and Cultural Organization (UNESCO). The composition of the base alloys and the presence of Pt and Sn showed that, contrary to what is expected, the gold foils from the first powerful empire of the steppes along the Great Wall were produced with alluvial gold from local placer deposits located in Zaamar, Boroo, and in the Selenga River. KW - Synchrotron radiation KW - X-ray fluorescence KW - Limit of detection KW - Platinum KW - Silicon drift detector KW - SR-microXRF KW - Elemental imaging KW - Gold PY - 2013 DO - https://doi.org/10.1021/ac3025416 SN - 0003-2700 SN - 1520-6882 VL - 85 IS - 3 SP - 1650 EP - 1656 PB - American Chemical Society CY - Washington, DC AN - OPUS4-30224 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guilherme, A. A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Coroado, J. A1 - Dos Santos, J.M.F. A1 - Carvalho, M.L. T1 - Synchrotron micro-XRF with compound refractive lenses (CRLs) for tracing key elements on Portuguese glazed ceramics N2 - Several glazed ceramic fragments (XVIth to XVIIIth centuries) from two production centers in Portugal (Coimbra and Lisbon) were the object of this study. The ones from Coimbra comprise two sets of samples: faiences and tiles. The ones from Lisbon are only tiles (azulejos, in Portuguese). The three main divisions of such pieces are the ceramic support (body), glaze and surface decoration. The system decoration/glaze is not easy to investigate, due to the high heterogeneity resulting from the mixing procedures and firing temperatures used. Moreover, the ability of the pigment to diffuse into the base glaze varies depending on the composition of both the pigment and the glaze in terms of fusibility. In order to raster these effects, high resolution techniques are required. In this work, synchrotron micro-X-ray fluorescence (µ-XRF) analysis was performed to monitor the profiles of the characteristic elements from the colors used and the glaze in well prepared cross-sections of the samples. Key elements are: Co for blue, Mn for purple, Cu for green, Sb for yellow, Pb for the glaze and Fe for the body. The major difference observed is that faiences have glaze thicknesses between 150 and 200 µm and tiles have glaze thicknesses between 350 and 400 µm. Furthermore, in faiences all the pigments except the yellow ones are well dispersed into the glassy matrix, while in tiles, all of them are just partially diffused throughout the glaze. However, differences between the tiles from Coimbra and Lisbon were observed. In the samples from Lisbon, a higher intake from the pigment throughout the glaze is observed. KW - Synchrotron micro-XRF KW - Compound refractive lenses (CRLs) KW - Portuguese glazed ceramics PY - 2012 DO - https://doi.org/10.1039/c2ja30030c SN - 0267-9477 SN - 1364-5544 VL - 27 IS - 6 SP - 966 EP - 974 PB - Royal Society of Chemistry CY - London AN - OPUS4-26789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tissot, I. A1 - Troalen, L.G. A1 - Manso, M. A1 - Ponting, M. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Barreiros, M. A. A1 - Shaw, I. A1 - Carvalho, M.L. A1 - Guerra, M.F. T1 - A multi-analytical approach to gold in Ancient Egypt: Studies on provenance and corrosion N2 - Recent results from a three-year multi-disciplinary project on Ancient Egyptian gold jewellery revealed that items of jewellery from the Middle Kingdom to the New Kingdom were manufactured using a variety of alluvial gold alloys. These alloys cover a wide range of colours and the majority contain Platinum Group Elements inclusions. However, in all the gold foils analysed, these inclusions were found to be absent. In this work a selection of gilded wood and leather items and gold foil fragments, all from the excavations by John Garstang at Abydos (primarily from Middle Kingdom graves), were examined using Scanning Electron Microscopy-Energy Disperse Spectroscopy (SEM-EDS), X-Ray Fluorescence (µXRF), Particle Induced X-Ray Emission (µPIXE) and Double Dispersive X-Ray Fluorescence (D²XRF). The work allowed us to characterise the composition of the base-alloys and also to reveal the presence of Pt at trace levels, confirming the use of alluvial gold deposits. Corrosion products were also investigated in the foils where surface tarnish was visually observed. Results showed that the differences in the colour of corrosion observed for the foils are related not only to the thickness of the corrosion layer but also to a multi-layer structure containing the various corrosion products. KW - Gold KW - Egypt KW - PGE KW - Provenance KW - Corrosion KW - muXRF KW - muPIXE KW - D2XRF KW - SEM-EDS PY - 2015 DO - https://doi.org/10.1016/j.sab.2015.03.012 SN - 0584-8547 SN - 0038-6987 VL - 108 SP - 75 EP - 82 PB - Elsevier CY - Amsterdam AN - OPUS4-33155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Buzanich, Günter A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Scharf, O. A1 - Scholz, Philipp A1 - Guerra, M.F. T1 - Double Dispersive X-Ray Fluorescence (D2XRF) based on an Energy Dispersive pnCCD detector for the detection of platinum in gold N2 - With the aim of improving limits of detection (LOD) of trace elements in a matrix with adjacent fluorescence energies, a simple double dispersive X-ray fluorescence detection system (D2XRF) was constructed to operate at the beamlines BAMline and the mySpot @ BESSY II. This system is based on the combination of a crystal analyzer with an energy resolving single photon counting pnCCD. Without further collimators, the efficient suppression of the background by the pnCCD and the good energy resolution of the crystal results in improved LOD. In first order reflections, an energy resolution of 13 eV for Cu Kα was reached, and an energy range of 1 keV was covered in one shot. This new system was applied to the detection of platinum (Pt) in gold leaves with a LOD of 0.9 mg/kg, which is the lowest attained by totally non-destructive methods nowadays. The presence of Pt in gilded objects from Abydos and Byzantine mosaics provides vital information, as it indicates the alluvial origin of the gold for these examples. KW - Platinum Wavelength dispersive D2XRF KW - Gold Synchrotron XRF PY - 2016 DO - https://doi.org/10.1016/j.microc.2015.10.039 VL - 125 SP - 56 EP - 61 PB - Elsevier Science CY - Amsterdam AN - OPUS4-35777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M.F. A1 - Neri, E. A1 - Radtke, Martin T1 - Gold leaf tesserae: tracing the origins of gold using synchrotron-based techniques N2 - To gain insight into the possible origin of the gold used in the production of tesserae containing gold leaf less than 0.5 μm thick placed between two layers of glass, we propose a non-destructive synchrotron radiation (SR) XRF protocol based on sequential analysis under optimised analytical conditions. Using this protocol, trace element analysis is achieved with detection limits of 1–6 mg/kg. As Pt and Au have adjacent fluorescence energies, we tested the most challenging situation, when Pt is present in very low concentrations in gold. Data obtained by double-dispersive XRF (D2XRF) and μXRF for fourth–ninth-century mosaics decorating nine Eastern and Western religious buildings show that the Eastern and Western tesserae are made from different alloys. However, these alloys are identical to those used to make gold leaf for gilding, because plastic deformation requires the use of gold alloys with high ductility and malleability. Although trace element composition of gold used in the concerned period is only available for coins, by comparing the amounts of Pt contained in the tesserae and in the coins we show that Roman tesserae are made from Roman gold, as described in the documentary sources. We observe for the Byzantine period the use of a Byzantine gold and of gold supposedly from different stages of recycling, and we suggest the use of Umayyad and Abbasid gold for the production of Islamic tesserae. KW - Gold KW - XRF KW - Synchrotron KW - BAMline KW - D2XRF KW - Tesserae PY - 2023 DO - https://doi.org/10.1140/epjp/s13360-022-03638-y SN - 2190-5444 VL - 138 IS - 2 SP - 1 EP - 15 AN - OPUS4-57208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Berger, Achim A1 - Calligaro, T. A1 - Duval, A. A1 - Görner, Wolf A1 - Guerra, M.-F. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Reiche, I. A1 - Riesemeier, Heinrich A1 - Roth, M. T1 - Study of Ag and Au based historical and archaeological objects by high energy Sy-XRF KW - Synchrotron KW - XRF analysis KW - Drawings KW - Archaeometry KW - Gold KW - Röntgenfluoreszenzanalyse KW - RFA KW - Zeichnungen KW - Archäometrie KW - Albrecht Dürer KW - gold PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=544 SN - 0179-4159 SP - 544 EP - 546 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Guerra, M.F. A1 - Martinón-Torres, M. A1 - Lemasson, Q. A1 - Moignard, B. A1 - Pacheco, C. A1 - Pichon, L. A1 - Macdonald, L. A1 - Hess, M. A1 - Tissot, I. ED - Guerra, M. F. ED - Martinón-Torres, M. ED - Quirke, S. T1 - Analytical approaches to Egyptian goldwork N2 - The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail. KW - Gold KW - Synchrotron KW - D2XRF KW - Egypt PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586039 DO - https://doi.org/10.17863/CAM.99681 SP - 131 EP - 191 AN - OPUS4-58603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -