TY - RPRT A1 - Kunath, K. A1 - Lüth, Peter A1 - Schmidt, Martin A1 - Simon, K. A1 - Uhlig, S. T1 - Evaluation of the interlaboratory test 2010-2011 on the method DIN EN15188:2007 'Determination of the spontaneous ignition behaviour of dust accumulations' N2 - For the classification and safe handling and use of the chemicals, special standardized testing proce-dures have been developed and are used world-wide. Safety experts must be able to fully rely on the precise execution of the respective laboratory tests and assessments. In this context interlaboratory tests (round robin tests, interlaboratory comparisons / intercomparisons) are a crucial element of a laboratory's quality system. Participation in interlaboratory tests is explicitly recommended by the standard ISO/IEC 17025. The present document reports on the results of the interlaboratory test 2010/2011 on the test method DIN EN 15188:2007 “Determination of the spontaneous ignition behaviour of dust accumulations” [1] which was organized by the Center for Quality Assurance for Testing of Dangerous Goods and Haz-ardous Substances. The test method DIN EN 15188:2007 is applied to characterize the self-ignition behaviour of combus-tible dusts. The experimental basis for describing the self-ignition behaviour of a given dust is the de-termination of the self-ignition temperatures (TSI) of differently-sized volumes of the dust sample by isoperibolic hot storage experiments (storage at constant oven temperatures) in commercially availa-ble ovens. The results thus measured reflect the dependence of self-ignition temperatures upon dust volume [1]. Several internal investigations and interlaboratory comparisons in the past have shown significant differences between the lab-specific results of hot storage tests. Figure 2-1 shows the Pseudo-Arrhenius plot of hot storage tests of eight different laboratories (Round Robin Test 2002, BAM). The dust under this investigation was Lycopodium powder (spores). The par-ticipants of this interlaboratory test used different laboratory ovens (size, ventilation) as well as differ-ent sample baskets (shape, mesh size, single- and double-walled). Figure 2-1 shows clearly that this test failed to produce reasonable reproducibility of the TSI between the different laboratories. As possible reasons for the deviations have been identified lab-specific dif-ferences, e.g.: - oven ventilation (enforced, natural convection), - oven size, - sample baskets, - radiation effects, - measuring precision (temperature difference between tests with ignition and no ignition), - minimum sample size. To reduce the differences between the labs it was necessary to ameliorate the testing method and to improve the execution of the method by the lab. From there, the installation of an inner chamber into the laboratory oven was suggested as experimental set-up in EN 15188:2007 to provide more repro-ducible test conditions. The aappropriateness of this set-up has not been verified yet. The current interlaboratory test 2010-2011 focuses on the use of a special mesh wire screen and spe-cial volumes of the sample baskets (cubes) to normalise/harmonise the test conditions in the different labs. In preparation for the interlaboratory test a joint program between Syngenta and BAM has been initiated in 2009. As a result of these investigations a modified set-up ( chapter 3) has been identi-fied to be probably more appropriate than the suggested set-up in DIN EN-15188:2007. Due to the time-consuming test procedure and to optimize the workflow for the laboratories this in-terlaboratory test should be performed stepwise as a multi-level test ( chapter 5.4) on one typical test sample. KW - Interlaboratory test KW - Self-ignition KW - Spontaneous ignition PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-282978 SN - 978-3-9815748-4-5 IS - Final Report SP - 1 EP - 113 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-28297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thomas, Hans-Martin A1 - Junger, M. A1 - Hintze, H. A1 - Krull, R. A1 - Rühe, S. T1 - Pioneering inspection of railroad rails with eddy currents N2 - Using a rail-inspection train, the Deutsche Bahn's system of railroads is continuously checked for traffic-induced defects. Until now, only ultrasonic inspection was used. In addition, eddy-current inspection could successfully and efficiently be used to detect and evaluate certain surface cracks - so-called head checks. There have already been reports about laboratory tests which proved the general suitability of this test method [1,2]. The next step - described here - consisted of practical trials under real-life conditions. A test system which is able to fulfil the strict requirements (test speeds of up to 100 km/h, complex probe guidance, suppression of electrical and mechanical interference, recording of data, filtering and evaluation of data) was developed. As part of the rail-inspection train and as a manual system, this inspection system was successfully tested on the Deutsche Bahn's system of railroads under real-life conditions. T2 - 15th World Conference on Non-Destructive Testing (WCNDT) CY - Roma, Italy DA - 2000-10-15 KW - Schienenprüfung PY - 2000 UR - http://www.ndt.net/article/wcndt00/papers/idn796/idn796.htm SN - 1435-4934 VL - 5 IS - 11 SP - 1 EP - 6(?) PB - NDT.net CY - Kirchwald AN - OPUS4-1010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thomas, Hans-Martin A1 - Krull, R. A1 - Rühe, S. T1 - Prüfung und Analyse von Oberflächenanrissen an verlegten Eisenbahnschienen mit Wirbelstrom T2 - Querschnittseminar. ZfP zur Anlagenüberwachung ; Seminar ZfP zur Anlagenüberwachung CY - Berlin, Deutschland DA - 2000-11-06 KW - Schienenprüfung KW - Wirbelstromprüfung PY - 2000 SN - 3-931381-33-1 N1 - Serientitel: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. – Series title: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. IS - 74 SP - 31 EP - 38 PB - DGZfP CY - Berlin AN - OPUS4-1011 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Thomas, Hans-Martin A1 - Junger, M. A1 - Krull, R. A1 - Rühe, S. T1 - Erste Erfahrungen beim Einsatz der Wirbelstromprüfung an Eisenbahnschienen N2 - Das Streckennetz der Deutschen Bahn wird mit Hilfe eines Schienenprüfzuges ständig auf betriebsbedingte Schädigungen überwacht. Bisher wurde hier ausschließlich das Ultraschallprüfverfahren eingesetzt. In Ergänzung dazu könnte die Wirbelstromprüfung für den Nachweis und die Bewertung spezieller Oberflächenrisse - sog. Head Checks - erfolgreich und wirtschaftlich sinnvoll eingesetzt werden. Über Laboruntersuchungen, die die grundsätzliche Eignung dieser Prüftechnik zeigten, wurde bereits berichtet. Der nächste Entwicklungsschritt besteht in der praktischen Erprobung unter realen Einsatzbedingungen. Hierbei stellen die hohen Prüfgeschwindigkeiten von bis zu 28 m/s (entsprechend 100 km/h Fahrgeschwindigkeit des Prüfzuges) eine besondere Herausforderung dar. Es gibt zahlreiche Probleme zu bewältigen. Diese betreffen beispielsweise die Sondenführung, die Signalfilterung, die Datenerfassung und die Unterdrückung von Störeinflüssen. Über erste Erfahrungen wird berichtet. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2000 CY - Innsbruck, Österreich DA - 2000-05-29 KW - Schienenprüfzug KW - Head checks PY - 2000 UR - http://www.ndt.net/abstract/dgzfp00/data/61.htm SN - 3-931381-32-3 VL - 73-1 IS - 2 SP - 617 EP - 624 PB - DGZfP CY - Berlin AN - OPUS4-1107 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mielentz, Frank A1 - Milmann, Boris A1 - Krause, Martin A1 - Müller, W. A1 - Crail, S. T1 - Zerstörungsfreie Risscharakterisierung in Betonbauteilen mit Ultraschall N2 - Die Risstiefenbestimmung in Festen Fahrbahnen ist hinsichtlich der Dauerhaftigkeit der Konstruktion von wesentlichem Interesse. Im Rahmen eines gemeinsamen Forschungsvorhabens mit der DB AG wurden aus der Literatur bekannte Ansätze bewertet und darauf aufbauend ein Verfahren zur bildgebenden Rissdarstellung entwickelt. Rissüberbrückende Bewehrung sowie Kontaktstellen zwischen den Rissflanken wirken als Schallbrücken und erschweren die Risscharakterisierung, wie bei einem Einsatz an einer Betriebserprobungsstrecke festgestellt wurde. Ein aus der Literatur bekanntes Verfahren der einfachen Laufzeitmessung erwies sich für die Tiefenbestimmung von realen verunreinigten Rissen als ungeeignet. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen CY - Leipzig, Germany DA - 25.10.2001 PY - 2001 VL - 76-CD SP - 1 EP - 10 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-1188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thomas, Hans-Martin A1 - Pohl, Rainer A1 - Rühe, S. A1 - Krull, R. T1 - Weiterentwicklung der Wirbelstromhandprüftechnik für Schienenfehler T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2001 CY - Berlin, Deutschland DA - 2001-05-21 PY - 2001 UR - http://www.ndt.net/article/dgzfp01/papers/p35/p35.htm N1 - Serientitel: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. – Series title: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. IS - 75-CD, CD-ROM PB - DGZfP CY - Berlin AN - OPUS4-1305 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Thomas, Hans-Martin A1 - Pohl, Rainer A1 - Krull, R. A1 - Hintze, H. A1 - Rühe, S. T1 - Erfahrungen beim Einsatz der Wirbelstromprüfung an Schienen N2 - Kurzfassung Es wurde eine Prüftechnologie basierend auf dem Wirbelstromverfahren entwickelt, mit der es möglich ist, oberflächennahe Fehler in Schienen zu detektieren und zu bewerten. Die bisherigen Untersuchungen haben gezeigt, dass Fahrkantenfehler (Head Checks) mit Risstiefen bis zu 10 mm bewertet werden können. Darüber hinaus werden weitere Inhomogenitäten und Fehler wie z. B. Schleuderstellen, Belgrospi's und Squats detektiert. Für die Anwendung der Prüftechnologie kommen 4 Anwendungsgebiete in Frage: Ausrüstung von Schienenprüfzügen, Manuelle Schienenprüfung, Ausrüstung von Schienenschleifzügen, Ausrüstung von stationären Schienenprüfständen. Die Prüftechnik befindet sich zur Zeit in der Erprobungsphase. Der Schienenprüfzug der Deutschen Bahn AG wird in Kürze mit einem achtkanaligen Prüfsystem ausgerüstet. Ebenfalls im Erprobungseinsatz befindet sich ein Handprüfsystem zur manuellen Schienenprüfung. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2002 CY - Weimar, Deutschland DA - 2002-05-06 PY - 2002 UR - http://www.ndt.net/article/dgzfp02/papers/v36/v36.htm SN - 3-931381-39-0 N1 - Serientitel: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. – Series title: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. IS - 80-CD PB - DGZfP CY - Berlin AN - OPUS4-1391 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thomas, Hans-Martin A1 - Pohl, Rainer A1 - Krull, R. A1 - Hintze, H. A1 - Luke, M. A1 - Rühe, S. A1 - Junger, M. T1 - Einsatz der Wirbelstromprüfung zur Detektion von Head Checks an Fahrkanten von Schienen PY - 2002 SN - 0941-0821 IS - 2 SP - 46 EP - 49 PB - Verl. Stahleisen CY - Düsseldorf AN - OPUS4-1405 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Babutzka, Martin A1 - Valet, Svenja A1 - Kotula, Stefan A1 - Burkert, Andreas A1 - Gümmer, K. A1 - Bender, S. A1 - Huckshold, M. T1 - Normentwurf für ein Prüfverfahren zur Bestimmung von Deckschichtwiderständen an Zinküberzügen mittels gelartiger Elektrolyte N2 - Das Grundproblem der heute verfügbaren und normativ geregelten Prüfverfahren für Zinküberzüge besteht neben den realitätsfernen Prüfbedingungen vor allem in der subjektiv geprägten Auswertung der Prüfergebnisse. Die systematische Betrachtung der Entwicklungen der letzten Jahre zeigt, dass die üblichen Verfahren den aktuellen Anforderungen damit schon vom Ansatz her nicht gerecht werden können und auch die bisher betriebene, fortlaufende Variation und Anpassung von Prüfbedingungen keinen grundlegend neuen Lösungsansatz bieten können. Ein solcher ergibt sich nur, wenn die Zinküberzüge hinsichtlich der kinetischen Eigenschaften der Deckschichtbildung und -auflösung umfassend beschrieben werden können, was nur durch den Einsatz elektrochemischer Untersuchungsmethoden mittels Gelelektrolyten möglich ist. Aus diesem Grund wurde im Verbundforschungsvorhaben GELELEK auf der Basis elektrochemischer Methoden unter Verwendung eines Gelelektrolyten ein Normenvorschlag für eine Prüfnorm erarbeitet und zur Normungsreife geführt, welcher den Anforderungen an ein Messsystem für Feldanwendungen entspricht. Im Verbundforschungsvorhaben GELELEK wurde eine gezielte Kombination von Laboruntersuchungen mit Untersuchungen im Feld und Bauteilen unter realen Einsatzbedingungen angestrebt. Randbedingungen für eine gesicherte Messung von atmosphärisch bewitterten Zinküberzügen unter Einsatz von Gelelektrolyten wurden erarbeitet und im Normenvorschlag festgeschrieben. Darüber hinaus wurde ein mobiles Messgerät für Messungen mit Gelelektrolyten an realen Bauteilen entwickelt. Nach Abschluss des Forschungsvorhabens steht Industrievertretern und Prüfinstituten ein wissenschaftlich gesichertes Messverfahren basierend auf Kennwerten zur Verfügung, um Zinküberzüge und deren momentane Schutzwirkung unter praxisrelevanten Bedingungen einschätzen und normativ geregelt prüfen zu können. Der vorliegende Forschungsbericht gibt einen Überblick über die Motivation zur Durchführung des Forschungsvorhabens, wichtige Arbeitsschritte, Details zur entwickelten Prüfmethode sowie Einsatzmöglichkeiten für Prüfinstitute und Unternehmen. KW - Normung KW - Zink KW - Korrosion KW - Deckschichtbildung KW - Atmosphärische Korrosion KW - Korrosionsprüfung PY - 2022 UR - https://www.gav-verzinken.de/forschung/wissenspool SP - 1 EP - 24 AN - OPUS4-54947 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Thomas, Hans-Martin A1 - Rühe, S. A1 - v. Hornhardt, A. A1 - Krull, R. T1 - Wirbelstrom-Handprüfsystem für Eisenbahnschienen N2 - Besonders in beweglichen Weichenteilen, wie z.B. Zungen und beweglichen Herzstückspitzen ist die Detektion von Rissen, die zum Bruch des Bauteils führen können, von außerordentlicher Bedeutung. Wegen der komplizierten geometrischen Randbedingungen muß der Schienenprüfzug hier seinen Prüfkopfträger anheben. Aus diesem Grund werden diese Bereiche regelmäßig durch eine manuelle Ultraschallprüfung überwacht. Da auch sehr kleine Anrisse im Oberflächenbereich interessant sind, soll das bereits vorhandene Prüfverfahren durch ein Wirbelstrom-Handprüfsystem so erweitert werden, daß eine sichere Detektion in den gefährdeten Bereichen möglich ist. Aufbau und Wirkungsweise des Wirbelstrom-Handprüfsystems werden erläutert. KW - Wirbelstrom-Handprüfsystem KW - Eisenbahnschienen PY - 2000 UR - http://www.ndt.net/abstract/dgzfp00/data/96.htm SN - 3-931381-32-3 VL - 73-2 IS - 2 SP - 883 EP - 889 PB - DGZfP CY - Berlin AN - OPUS4-879 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüth, Peter A1 - Uhlig, S. A1 - Frost, K. A1 - Malow, Marcus A1 - Michael-Schulz, Heike A1 - Schmidt, Martin A1 - Zakel, Sabine T1 - CEQAT-DGHS interlaboratory tests for chemical safety: Validation of laboratory test methods by determining the measurement uncertainty and probability of incorrect classification including so-called “Shark profiles” N2 - Laboratory test results are of vital importance for correctly classifying and labelling chemicals as “hazardous” as defined in the UN Globally Harmonized System (GHS) / EC CLP Regulation or as “dangerous goods” as defined in the UN Recommendations on the Transport of Dangerous Goods. Interlaboratory tests play a decisive role in assessing the reliability of laboratory test results. Interlaboratory tests performed over the last 10 years have examined different laboratory test methods. After analysing the results of these interlaboratory tests, the following conclusions can be drawn: 1. There is a need for improvement and validation for all laboratory test methods examined. 2. To avoid any discrepancy concerning the classification and labelling of chemicals, the use of validated laboratory test methods should be state of the art, with the results accompanied by the measurement uncertainty and (if applicable) the probability of incorrect classification. This paper addresses the probability of correct/incorrect classification (for example, as dangerous goods) on the basis of the measurement deviation obtained from interlaboratory tests performed by the Centre for quality assurance for testing of dangerous goods and hazardous substances (CEQAT-DGHS) to validate laboratory test methods. This paper outlines typical results (e.g. so-called “Shark profiles” – the probability of incorrect classification as a function of the true value estimated from interlaboratory test data) as well as general conclusions and steps to be taken to guarantee that laboratory test results are fit for purpose and of high quality. T2 - 13th International Symposium on Hazards, Prevention and Mitigation of Industrial Explosions (ISHPMIE 2020) CY - Brunswick, Germany DA - 27.07.2020 KW - Dangerous goods KW - Hazardous substances KW - Interlaboratory test KW - Test method KW - Validation KW - Quality assurance KW - Measurement uncertainty KW - Incorrect classification KW - Shark profiles PY - 2021 DO - https://doi.org/10.1016/j.jlp.2021.104532 SN - 0950-4230/ VL - 72 SP - 104532 PB - Elsevier Ltd. AN - OPUS4-52751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Anker, Andy S. A1 - Aspuru-Guzik, Alán A1 - Ben Mahmoud, Chiheb A1 - Bennett, Sophie A1 - Briling, Ksenia R. A1 - Changiarath, Arya A1 - Chong, Sanggyu A1 - Collins, Christopher M. A1 - Cooper, Andrew I. A1 - Crusius, Daniel A1 - Darmawan, Kevion K. A1 - Das, Basita A1 - David, Nicholas A1 - Day, Graeme M. A1 - Deringer, Volker L. A1 - Duarte, Fernanda A1 - Eardley-Brunt, Annabel A1 - Evans, Matthew L. A1 - Evans, Rob A1 - Fairlamb, Ian A1 - Franklin, Barnabas A. A1 - Frey, Jeremy A1 - Ganose, Alex M. A1 - Goulding, Mark A1 - Hafizi, Roohollah A1 - Hakkennes, Matthijs A1 - Hickey, Niamh A1 - James, Gillian A1 - Jelfs, Kim E. A1 - Kalikadien, Adarsh V. A1 - Kapil, Venkat A1 - Koczor-Benda, Zsuzsanna A1 - Krammer, Ferdinand A1 - Kulik, Heather J. A1 - Kumar, Vishank A1 - Kuttner, Christian A1 - Lam, Erwin A1 - Lou, Yuchen A1 - Mante, Eltjo A1 - Martin, Jennie A1 - Mroz, Austin M. A1 - Nematiaram, Tahereh A1 - Pare, Charles W. P. A1 - Patra, Sarbani A1 - Proudfoot, James A1 - Ruscic, Branko A1 - Ryder, Matthew R. A1 - Sakaushi, Ken A1 - Saßmannshausen, Jörg A1 - Savoie, Brett M. A1 - Schneider, Nadine A1 - Schwaller, Philippe A1 - Skjelstad, Bastian Bjerkem A1 - Sun, Wenhao A1 - Szczypiński, Filip T. A1 - Torrisi, Steven A1 - Ueltzen, Katharina A1 - Vishnoi, Shubham A1 - Walsh, Aron A1 - Wang, Xinwei A1 - Wilson, Chloe A1 - Wu, Ruiqi A1 - Zeitler, Jakob T1 - Discovering structure–property correlations: General discussion N2 - This article is a discussion of the paper "Web-BO: Towards increased accessibility of Bayesian optimisation (BO) for chemistry" by Austin M. Mroz, Piotr N. Toka, Ehecatl Antonio del Río Chanona and Kim E. Jelfs (Faraday discussions, 2025, 256, 221-234). KW - Materials design KW - Machine learning KW - Automation KW - Materials discovery PY - 2025 DO - https://doi.org/10.1039/d4fd90062f SN - 1359-6640 SN - 1364-5498 VL - 256 IS - Themed collection: Data-driven discovery in the chemical sciences SP - 373 EP - 412 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-62208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Yue A1 - Martin, A. A1 - Wolf, G.-U. A1 - Rabe, S. A1 - Worzala, H. A1 - Lücke, B. A1 - Meisel, M. A1 - Witke, Klaus T1 - Structural transformations of VOHPO4.1/2H2O in the Presence of Ammonia KW - Vanadium KW - Ammoniak KW - Phosphat KW - Phyrophosphorsäure PY - 1996 SN - 0897-4756 SN - 1520-5002 VL - 8 IS - 5 SP - 1135 EP - 1140 PB - American Chemical Society CY - Washington, DC AN - OPUS4-684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Thomas, Hans-Martin A1 - Pohl, Rainer A1 - Rühe, S. T1 - Automatische Auswertung von Wirbelstrombildern N2 - Die Wirbelstromprüftechnik ist eine hochempfindliche Prüfmethode, mit der kleinste Materialschäden in metallischen Prüfkörpern nachgewiesen werden können. Die Prüfung kann berührungslos und bei sehr hohen Prüfgeschwindigkeiten durchgeführt werden. Dies sind beste Voraussetzungen für den Einsatz in automatischen Produktionsanlagen. Die Wirbelstromprüfung kann vielfach direkt in die Produktionslinie von Halbzeugen integriert werden. Zur Abdeckung der gewünschten Prüffläche werden je nach geforderter Prüfempfindlichkeit Durchlaufsensoren, Anordnungen von mehreren Tastsonden oder rotierende Sensoren eingesetzt. Die Entscheidung über das Vorhandensein einer unzulässigen Inhomogenität wird durch das Überschreiten einer festgelegten Signalschwelle festgestellt, wonach eine Aussortierung ausgelöst werden kann. Dieses einfache Kriterium versagt jedoch, wenn durch das Prüfteil Anzeigen hervorgerufen werden, die nach ihrer Herkunft unterschieden werden müssen. Beispielsweise könnte eine Prüfaufgabe so gestellt sein, daß in einem Prüfteil Poren geduldet werden, während rißartige Inhomogenitäten unzulässig sind. Anhand von Beispielen wird gezeigt, wie durch den Einsatz von speziellen Computeralgorithmen an flächenhaft gewonnenen Wirbelstrombildern eine Unterscheidung der Anzeigentypen durchgeführt werden kann. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 1999 CY - Celle, Deutschland DA - 1999-05-10 KW - Wirbelstrombilder PY - 1999 UR - http://www.ndt.net/abstract/dgzfp99/data/17.htm SN - 3-931381-27-7 VL - 1 IS - 68 SP - 163 EP - 171 PB - DGZfP CY - Berlin AN - OPUS4-833 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Liehr, Sascha A1 - Wander, Lukas A1 - Bornemann-Pfeiffer, Martin A1 - Müller, S. A1 - Maiwald, Michael A1 - Kowarik, Stefan T1 - Artificial neural networks for quantitative online NMR spectroscopy N2 - Industry 4.0 is all about interconnectivity, sensor-enhanced process control, and data-driven systems. Process analytical technology (PAT) such as online nuclear magnetic resonance (NMR) spectroscopy is gaining in importance, as it increasingly contributes to automation and digitalization in production. In many cases up to now, however, a classical evaluation of process data and their transformation into knowledge is not possible or not economical due to the insufficiently large datasets available. When developing an automated method applicable in process control, sometimes only the basic data of a limited number of batch tests from typical product and process development campaigns are available. However, these datasets are not large enough for training machine-supported procedures. In this work, to overcome this limitation, a new procedure was developed, which allows physically motivated multiplication of the available reference data in order to obtain a sufficiently large dataset for training machine learning algorithms. The underlying example chemical synthesis was measured and analyzed with both application-relevant low-field NMR and high-field NMR spectroscopy as reference method. Artificial neural networks (ANNs) have the potential to infer valuable process information already from relatively limited input data. However, in order to predict the concentration at complex conditions (many reactants and wide concentration ranges), larger ANNs and, therefore, a larger Training dataset are required. We demonstrate that a moderately complex problem with four reactants can be addressed using ANNs in combination with the presented PAT method (low-field NMR) and with the proposed approach to generate meaningful training data. KW - Online NMR spectroscopy KW - Real-time process monitoring KW - Artificial neural networks KW - Automation KW - Process industry PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507508 DO - https://doi.org/10.1007/s00216-020-02687-5 SN - 1618-2642 VL - 412 IS - 18 SP - 4447 EP - 4459 PB - Springer CY - Berlin AN - OPUS4-50750 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kern, Simon A1 - Liehr, Sascha A1 - Wander, Lukas A1 - Bornemann-Pfeiffer, Martin A1 - Müller, S. A1 - Maiwald, Michael A1 - Kowarik, Stefan T1 - Training data of quantitative online NMR spectroscopy for artificial neural networks N2 - Data set of low-field NMR spectra of continuous synthesis of nitro-4’-methyldiphenylamine (MNDPA). 1H spectra (43 MHz) were recorded as single scans. Two different approaches for the generation of artificial neural networks training data for the prediction of reactant concentrations were used: (i) Training data based on combinations of measured pure component spectra and (ii) Training data based on a spectral model. Synthetic low-field NMR spectra First 4 columns in MAT-files represent component areas of each reactant within the synthetic mixture spectrum. Xi (“pure component spectra dataset”) Xii (“spectral model dataset”) Experimental low-field NMR spectra from MNDPA-Synthesis This data set represents low-field NMR-spectra recorded during continuous synthesis of nitro-4’-methyldiphenylamine (MNDPA). Reference values from high-field NMR results are included. KW - NMR spectroscopy KW - Real-time process monitoring KW - Artificial neural networks KW - Online NMR spectroscopy KW - Automation KW - Process industry PY - 2020 DO - https://doi.org/10.5281/zenodo.3677139 PB - Zenodo CY - Geneva AN - OPUS4-50456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gruskovà, J. A1 - Martin, G. A1 - Kresten, O. A1 - Mitthoff, F. A1 - Kaska, K. A1 - Hofmann, C. A1 - Kreuzer, W. A1 - Phelps, M. A1 - Boydston, K. A1 - Easton Jr., R. L. A1 - Knox, K. T. A1 - Kelbe, D. A1 - Kasotakis, D. A1 - Christens-Barry, W. A. A1 - Stewart, D. A1 - Rabin, Ira A1 - Hahn, Oliver A1 - Glaser, L. A1 - Garrevoet, J. A1 - Shevchuk, I. A1 - Klumpp, S. A1 - Deckers, D. A1 - Buck, J. ED - Cronier, M. ED - Mondrain, B. T1 - Insights-into-the-Digital-Recovery-of-the-Scythica-Vindobonesia N2 - The Scythica Vindobonensia, the new fragments on Gothic incursions into Roman provinces in the Balkans in the middle of the third century AD that were revealed some years ago in a Greek palimpsest at the Austrian National Library in Vienna (ÖNB), are commonly considered as one of the most important additions of the last decades to the corpus of texts from classical Antiquity. Tere is a high degree of confdence among scholars in supposing that the fragments come from the lost work Scythica written in Greek by the third-century historian P. Herennius Dexippus (Δέξιππος) of Athens. The new fragments have hence also been called Dexippus Vindobonensis. In his Scythica, Dexippus recorded wars of the Romans with the Goths (and other tribes) whom he called Scythians. The work had been hitherto known only from excerpts and quotes by later authors. Eight pages of a Byzantine manuscript copy of the ancient text have survived hidden underneath the visible surface of the last four parchment folios of the Vienna manuscript Historicus graecus 73, f. 192r -195v4. The copy is written in a Greek calligraphic minuscule which has been estimated by palaeographers to be of the middle or the second half of the eleventh century. In the thirteenth century, the text (on each of the eight pages arranged in one column, with 30 lines per page) was washed of the parchment and the valuable material made from animal skin was re-used for Christian texts. The new writing largely covered the faded remnants of the original text. It thus became hidden from the human eye for more than seven hundred years. Its discovery by Jana Grusková, a classical philologist specialized in the transmission of Greek texts, resulted from a systematic review of all Greek palimpsests kept at the Austrian National Library in Vienna at the beginning of the twenty-first century and a detailed examination of the four folios in 2007-20097. KW - Scythica Vindobonensia, KW - Gothic incursions KW - A Greek palimpsest KW - Antiquity KW - Byzantine manuscript KW - Vienna manuscript PY - 2020 SN - 978-2-916716-81-7 SN - 0577-1471 VL - 2020 IS - 24/1 SP - 945 EP - 967 PB - Association des Amis du Centre d’Histoire et Civilisation de Byzance CY - Paris ET - 1 AN - OPUS4-53843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Martin A1 - Herter, Jürgen A1 - Droste, Bernhard A1 - Hartwig, S. T1 - Compressive behaviour of axially loaded spruce wood under large deformations at different strain rates N2 - Impact limiting components of packages for the transport of radioactivematerials are often designed as wood filled steel constructions. Wood absorbs major part of the impact energy in order to minimise the impact load acting upon the containment. Dynamic impact experiments with wood filled impact limiters showed different crushing mechanisms for axially loaded wood depending on their lateral constraint. Tests on spruce wood samples (Picea abies) were performed in order to clarify the influence of strain rate from static to 30 s-1 on a) compression strength, b) stress at a global strain level of 50%, and c) energy absorption capacity at 50% deformation, including statistical evaluation of the results. Results were as follows: strain rate increase led to significantly higher compression strength, stress and strain energy at a strain level of 50%. Lateral strain restriction had no effect on compression strength; it had a significant effect on stress and strain energy at strain level of 50%. Therefore, the definition of a general yield curve for wood under large deformations is not possible, the yield curve has to be chosen taking into account lateral constraints. KW - Compression KW - Wood KW - Spruce KW - Picea abies KW - Impact PY - 2011 DO - https://doi.org/10.1007/s00107-010-0442-x SN - 0018-3768 VL - 69 IS - 3 SP - 345 EP - 357 PB - Springer CY - Berlin ; Heidelberg AN - OPUS4-22980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - König, S. A1 - Diersch, R. A1 - Lührmann, A. A1 - Müller, Karsten A1 - Neumann, Martin A1 - Quercetti, Thomas A1 - Droste, Bernhard T1 - Full-Scale Drop Testing of the CONSTOR®, V/TC Package Program, and Preliminary Results KW - Drop test KW - Package KW - Spent fuel cask KW - Transport PY - 2005 SN - 0893-6188 VL - 33 IS - 3 SP - 4 EP - 10 PB - Institute of Nuclear Materials Management CY - Northbrook, Ill. AN - OPUS4-12269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - König, S. A1 - Diersch, R. A1 - Lührmann, A. A1 - Müller, Karsten A1 - Neumann, Martin A1 - Quercetti, Thomas A1 - Droste, Bernhard T1 - Full-scale Drop Testing of the CONSTOR V/TC Package - Program and Preliminary Results KW - Fallversuche KW - Transportbehälter für radioaktive Stoffe PY - 2005 SN - 0893-6188 VL - 33 IS - 3 SP - 4 EP - 10 PB - Institute of Nuclear Materials Management CY - Northbrook, Ill. AN - OPUS4-6875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arppe, Riika A1 - Hyppänen, I. A1 - Perälä, N. A1 - Peltomaa, R. A1 - Kaiser, Martin A1 - Würth, Christian A1 - Christ, S. A1 - Resch-Genger, Ute A1 - Schäferling, Michael A1 - Soukka, T. T1 - Quenching of the upconversion luminescence of NaYF4:Yb3+,Er3+ and NaYF4:Yb3+,Tm3+ nanophosphors by water: the role of the sensitizer Yb3+ in non-radiative relaxation N2 - We have studied the mechanisms of water-based quenching of the upconversion photoluminescence of upconverting nanophosphors (UCNPs) via luminescence decay measurements for a better understanding of the non-radiative deactivation pathways responsible for the relatively low upconversion luminescence efficiency in aqueous solutions. This included both upconversion luminescence measurements and the direct excitation of emissive energy states of Er3+ and Yb3+ dopants in NaYF4:Yb3+,Er3+ UCNPs by measuring the decays at 550 and 655 nm upon 380 nm excitation and at 980 nm upon 930 nm excitation, respectively. The luminescence intensities and decays were measured from both bare and silanized NaYF4:Yb3+,Er3+ and NaYF4:Yb3+,Tm3+ UCNPs in H2O and D2O. The measurements revealed up to 99.9% quenching of the upconversion photoluminescence intensity of both Er3+ and Tm3+ doped bare nanophosphors by water. Instead of the multiphonon relaxation of excited energy levels of the activators, the main mechanism of quenching was found to be the multiphonon deactivation of the Yb3+ sensitizer ion caused by OH-vibrations on the surface of the nanophosphor. Due to the nonlinear nature of upconversion, the quenching of Yb3+ has a higher order effect on the upconversion emission intensity with the efficient Yb–Yb energy migration in the ~35 nm nanocrystals making the whole nanophosphor volume susceptible to surface quenching effects. The study underlines the need of efficient surface passivation for the use of UCNPs as labels in bioanalytical applications performed in aqueous solutions. PY - 2015 DO - https://doi.org/10.1039/c5nr02100f SN - 2040-3364 SN - 2040-3372 VL - 7 IS - 27 SP - 11746 EP - 11757 PB - RSC Publ. CY - Cambridge AN - OPUS4-33815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Pilch, A. A1 - Würth, Christian A1 - Kaiser, Martin A1 - Wawrzynczyk, D. A1 - Kurnatowska, M. A1 - Arabasz, S. A1 - Prorok, K. A1 - Samoc, M. A1 - Strek, W. A1 - Bednarkiewicz, A. T1 - Shaping luminescent properties of Yb3+ and Ho3+ co-doped upconverting core-shell ß-NaYF4 nanoparticles by dopant distribution and spacing N2 - At the core of luminescence color and lifetime Tuning of rare earth doped upconverting nanoparticles (UCNPs), is the understanding of the Impact of the particle architecture for commonly used sensitizer (S) and activator (A) Ions. In this respect, a series of core@Shell NaYF4 UCNPs doped with Yb3+ and Ho3+ ions are presented here, where the same dopant concentrations are distributed in different particle architectures following the scheme: YbHo core and YbHo@..., ...@YbHo, Yb@Ho, Ho@Yb, YbHo@Yb, and Yb@YbHo core-Shell NPs. As refealed by quantitative steady-state and time-resolved luminescence studies, the relative spatial Distribution of the A and S ions in the UCNPs and their protection from surface quenching has a critical Impact on ther luminescence characteristics. Although the increased amount of Yb3+ Ions boosts UCNP Performance by amplifying the Absorption, the Yb3+ ions can also efficiently dissipate the energy stored in the material through energy Migration to the surface, thereby reducing the Overall energy Transfer Efficiency to the activator ions. The results provide yet another proof that UC Phosphor chemistry combined with materials Engineering through intentional core@shell structures may help to fine-tune the luminescence Features of UCNPs for their specific future applications in biosensing, bioimaging, photovoltaics, and Display technologies. KW - Fluorescence KW - Upconversion KW - NIR KW - Nonlinear KW - Nanoparticle KW - Surface chemistry KW - Quantum yield KW - Liftetime KW - Nanocrystal KW - Lanthanide KW - Ho(III) KW - Yb(III) KW - Mechanism KW - Absolute flourescence KW - Excitation power density dependence PY - 2017 DO - https://doi.org/10.1002/smll.201701635 SN - 1613-6810 VL - 13 IS - 47 SP - 1701635, 1 EP - 13 PB - WILEY-VCH Verlag GmbH & co. KGaA CY - Weinheim AN - OPUS4-43629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Frost, K. A1 - Lüth, Peter A1 - Schmidt, Martin A1 - Simon, K. A1 - Uhlig, S. T1 - Interlaboratory test 2023 on the method DIN EN 15188:2021-07 "Determination of the spontaneous ignition behaviour of dust accumulations" - Final report of results N2 - The test method DIN EN 15188:2021-07 “Determination of the spontaneous ignition behaviour of dust accumulations” is applied to characterize the self-ignition behaviour of combustible dusts. The experimental basis for describing the self-ignition behaviour of a given dust is the determination of the self-ignition temperatures (TSI) of differently-sized volumes of the dust sample by isoperibolic hot storage experiments (storage at constant oven temperatures) in commercially available ovens. The results measured this way reflect the dependence of the self-ignition temperatures on the volume of a dust accumulation. Several internal investigations in the past (e.g. interlaboratory tests in 2010-2011 and 2015-2016) have shown significant differences between the lab-specific results of hot storage tests of the former version of the revised DIN EN 15188:2021-07 (DIN EN 15188:2007). Therefore, an improvement of the test method DIN EN 15188:2007 was necessary. After a rather long and extensive series of various improvements (methodological modifications), the interlaboratory test in 2015-2016 demonstrated an acceptable reliability of the test method and a satisfactory measurement uncertainty if the modifications described in the interlaboratory test are taken into account. On the basis of this interlaboratory test in 2015, this subsequently led to a revision of the standard, whereby, in addition to the methodological improvements, the measurement uncertainty to be taken into account could now also be specified for the first time in this standard. The revised DIN EN 15188:2021-07 was published in 2021 and can now be applied by laboratories. This report provides the laboratory results of the first interlaboratory test 2023 on the revised method DIN EN 15188:2021-07 and summarizes the results of the assessment of laboratory performance. KW - DIN EN 15188:2021-07 KW - Spontaneous ignition KW - Interlaboratory test KW - Round robin test KW - Proficiency test KW - Dangerous goods KW - Hazardous substances KW - Measurement uncertainty KW - Gefahrgut KW - Gefahrstoff KW - Qualitätssicherung KW - Ringversuch KW - Selbstentzündung KW - Staub KW - Dust PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614560 SN - 978-3-9818564-6-0 DO - https://doi.org/10.26272/opus4-61456 SP - 1 EP - 51 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin ET - 1. AN - OPUS4-61456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Williams, S. H. A1 - Hilger, A. A1 - Kardjilov, N. A1 - Manke, I. A1 - Strobl, M. A1 - Douissard, P.A. A1 - Martin, T. A1 - Riesemeier, Heinrich A1 - Banhart, J. T1 - Detection system for microimaging with neutrons N2 - A new high-resolution detector setup for neutron imaging has been developed based on infinity-corrected optics with high light collection, combined with customized mounting hardware. The system can easily be installed, handled and fitted to any existing facility, avoiding the necessity of complex optical systems or further improved electronics (CCD). This is the first time optical magnification higher than 1:1 has been used with scintillator-based neutron detectors, as well as the first implementation of infinity corrected optics for neutron imaging, achieving the smallest yet reported effective pixel size of 3.375 µm. A novel transparent crystal scintillator (GGG crystal) has been implemented with neutrons for the first time to overcome limitations of traditional powder scintillators (Li6/ZnS, Gadox). The standardized procedure for resolution measurements with the Modulation Transfer Function (MTF) is summarized to facilitate comparison between instruments and facilities. Using this new detector setup, a resolution of 14.8 µm with a field of view of 6 mm × 6 mm has been achieved while maintaining reasonable count times. These advances open a wide range of new possible research applications and allow the potential for additional future developments. KW - Instrumentation for neutron sources KW - Neutron radiography KW - Neutron detectors (cold, thermal, fast neutrons) PY - 2012 DO - https://doi.org/10.1088/1748-0221/7/02/P02014 SN - 1748-0221 VL - 7 IS - P02014 SP - 1 EP - 26 PB - Inst. of Physics Publ. CY - London AN - OPUS4-26433 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 - Fittschen, U.E.A. A1 - Möckel, R. A1 - Schreiner, M. A1 - klinger, M. A1 - Radtke, Martin A1 - Meyer, B. A1 - Guhl, S. A1 - Renno, A. A1 - Godinho, J. A1 - Gloaguen, R. A1 - Gutzmer, J. T1 - Bundling analytical capacities to understand phase formation in recycling of functional materials N2 - Transitioning from combustion engine-driven transportation to e-mobility demands a paradigm shift – from a system geared to maximize energy efficiency (i.e. fuel consumption) to a system that may be constrained by the availability of high technology (critical) metals required for electrical energy storage systems and drives. In the wake of these developments efforts in securing new resources of these metals from recycling of end-of-life products are increasing steadily. Recycling of Li-Ion batteries has recently been evaluated. The results pinpoint to a critical need for understanding slag Formation and its dependence on metal components like Mn under extreme conditions. This will allow researchers to predict optimal Operation setting and to react quickly to changing market demands (which may be Li or Co at one point but may also shift to Ni or rare earth elements (REE)). The long-term goal is to control the formation of specific phases in slags allowing for a Maximum yield of elements of interest and optimal recovery in the separation processes that follows. The combination of data on the physical micro structure and local chemistry of the multi-Phase products during and after processing will help to understand and derive thermodynamic and kinetic data on its formation. In this paper we are giving an overview on the analytical challenges and approaches to provide robust data on local element concentration and species (especially Mn which is a common component of next generation Li-ion batteries cathodes), spanning the dimensions from the nanometer scale to the bulk material. The complementary interactions of X-rays and electrons make them ideal probes to collect Interface and “in-depth” information. Before- and -after studies as well as in situ structural changes and Phase (trans)formation, changes in elemental and elemental species (e.g. oxidation state) distribution may be tracked by X-ray diffraction (XRD), X-ray fluorescence microscopy and X-ray Absorption spectroscopy. The application of such advanced analytical tools will not only provide essential clues during early lab-based experiments towards the development of new recycling technologies, but may also be deployed for on-line and in-line monitoring of industrial processes. KW - Synchrotron KW - XANES KW - Slags KW - Battery PY - 2019 DO - https://doi.org/10.4028/www.scientific.net/MSF.959.183 SN - 1662-9752 VL - 959 SP - 183 EP - 190 PB - Trans Tech Publ. AN - OPUS4-48900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Lippitz, Andreas A1 - Hodoroaba, Vasile-Dan A1 - Schmid, Thomas A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Zirconium permanent modifiers for graphite furnaces used in absorption spectrometry: understanding their structure and mechanism of action N2 - The mechanism of action of zirconium permanent modifiers on graphite surfaces was investigated in order to understand its influence on the analytical signal in atomic and molecular absorption spectrometry (AAS/MAS). For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEMEDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. We propose here a mechanism, where ZrO2 acts as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. No evidence of the formation of zirconium carbide was found. Consequently, as the CaF formation is catalysed by a heterogeneous catalyst, surface modifications with ZrO2 nanoparticles and ZrO xerogels were investigated in order to increase the surface area. Their influence was evaluated in the molecule formation of CaF, CaCl, CaBr, and CaI. Graphite furnace modification with zirconium oxide nanoparticles proves to be the best choice for fluorine analysis with a signal enhancement of more than eleven times with respect a non-coated graphite furnace. However, the influence of zirconium modifications in the analytical signals of Cl, and I is lower than the F signals or even negative in case of the Br. Understanding zirconium modifiers as heterogeneous catalysts offers a new perspective to AAS and MAS, and reveals the potential of surface analytical methods for development of improved permanent modifiers and graphite furnace coatings. KW - Zirconium KW - HR-CS-MAS KW - Graphite furnace KW - Nanoparticles KW - Xerogel KW - Calcium monofluoride KW - Absorption spectrometry PY - 2018 UR - https://pubs.rsc.org/en/content/articlelanding/2018/ja/c8ja00190a DO - https://doi.org/10.1039/C8JA00190A SN - 0267-9477 VL - 33 IS - 12 SP - 2034 EP - 2042 PB - Royal Society of Chemistry AN - OPUS4-46775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Martin A1 - Erdt, René A1 - Gödde, M. A1 - Salg, S. A1 - Ittemann, L. T1 - Selbstentzündungsverhalten von Feststoffen: Validierung der Extrapolation von Labortests mit Hilfe halbtechnischer Versuche bis 1 m³ N2 - Vorgestellt wird ein 2018 gestartetes Projekt zur Überprüfung der Extrapolation von im Labormaßstab ermittelten Selbstentzündungstemperaturen auf technisch relevante Volumina. Für die Ermittlung reaktionskinetischer Daten von Feststoffschüttungen stehen eine Reihe von Untersuchungsmethoden zur Verfügung. Dies sind thermische Analysen wie z.B. die differential scanning calorimetry DSC sowie Mikrokalorimetrie zur hochgenauen Messung von Wärmeströmen, bei denen sehr geringe Probenmengen zum Einsatz kommen. In der Regel wird das Selbstentzündungsverhalten jedoch mit Hilfe von isoperibolen oder adiabaten Warmlagerungsversuchen beurteilt, hier liegen die Probenvolumina üblicherweise im Bereich von ca. 100 cm³ bis zu einigen Litern. Die Extrapolation über mehrere Größenordnungen auf technische Volumina birgt Unsicherheiten, da mit Zunahme des Lagervolumens veränderte Start- und Randbedingungen vorliegen können. Zudem besteht die Möglichkeit, dass bei in technischen Lagern vorherrschenden niedrigen Temperaturen Reaktionen ablaufen, die in Standard- Laborversuchen nicht erfasst werden aber einen wesentlichen Einfluss auf das Selbstentzündungsverhalten aufweisen können. Hauptziel des Projektes ist es daher, die im Labormaßstab vorhandenen Prüfeinrichtungen durch einen Versuchsstand zur Untersuchung von Probengrößen von bis zu 1000 dm³ zu erweitern, die Eignung (oder Nichteignung) der etablierten Methoden nachzuweisen und im Labormaßstab nicht erfassbare Einflussgrößen zu ermitteln. Zudem sollen anhand der kleinskaligen Tests Entscheidungskriterien abgeleitet werden, ob eine Extrapolation nach den derzeit üblichen Methoden zulässig ist. T2 - 15. BAM-PTB-Kolloquium zur chemischen und physikalischen Sicherheitstechnik CY - Brunswick, Germany DA - 21.05.2019 KW - Spontanious ignition KW - Self-ignition KW - Minimum ignition temperature KW - Dust layers KW - Große Volumina KW - Explosionsschutz KW - Selbstentzündung KW - DSC PY - 2019 DO - https://doi.org/10.7795/210.20190521B SP - 1 EP - 15 PB - Physikalisch-Technische Bundesanstalt (PTB) AN - OPUS4-48939 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zakel, S. A1 - Schröder, Volkmar A1 - Askar, Enis A1 - Gabel, D. A1 - Hirsch, W. A1 - Kleinert, J. A1 - Krause, U. A1 - Krietsch, Arne A1 - Meistes, J. A1 - Sachtleben, A. A1 - Schmidt, Martin T1 - Sicherheitstechnische Kenngrößen des Explosionsschutzes von hybriden Stoffgemischen - Normungsfähige Bestimmungsverfahren N2 - In diesem Verbundvorhaben werden standardisierte Messverfahren für hybride Gemische erarbeitet, die der Bestimmung sicherheitstechnischer Kenngrößen des Explosionsschutzes dienen. Unter einem hybriden Gemisch wird dabei ein mehrphasiges System aus Brenngas oder brennbarem Dampf, sowie Luft und brennbarem Staub verstanden. Die Veröffentlichung der Ergebnisse erfolgt in einem Abschlussbericht und als DIN-Spezifikation (DIN SPEC). Diese DIN SPEC versetzt Prüfinstitute und Industrie in die Lage, Explosionsgefahren beim Betrieb technischer Anlagen mit hybriden Gemischen einzuschätzen und damit Prozesse sowohl sicherer als auch effizienter zu steuern. Dieses Projekt wird im Rahmen des WIPANOProgramms (Wissens- und Technologietransfer durch Patente und Normen) vom BMWi gefördert. T2 - 14. Fachtagung Anlagen-, Arbeits- und Umweltsicherheit CY - Köthen, Germany DA - 07.11.2019 KW - Explosionsschutz KW - Sicherheitstechnische Kenngrößen KW - Hybride Gemische KW - Normung PY - 2019 SN - 978-3-89746-220-5 SP - 73 CY - Frankfurt am Main AN - OPUS4-49954 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manso, M. A1 - Pessanha, S. A1 - Guerra, M. A1 - Reinholz, Uwe A1 - Afonso, C. A1 - Radtke, Martin A1 - Lourenco, H. A1 - Carvalho, M. L. A1 - de Oliveira Guilherme Buzanich, Ana T1 - Assessment of Toxic Metals and Hazardous Substances in Tattoo Inks Using Sy-XRF, AAS, and Raman Spectroscopy N2 - Synchrotron radiation X-ray fluorescence spectroscopy, in conjunction with atomic absorption and Raman spectroscopy, was used to analyze a set of top brand tattoo inks to investigate the presence of toxic elements and hazardous substances. The Cr, Cu, and Pb contents were found to be above the maximum allowed levels established by the Council of Europe through the resolution ResAP(2008)1 on requirements and criteria for the safety of tattoos and permanent makeup. Raman analysis has revealed the presence of a set of prohibited substances mentioned in ResAP(2008)1, among which are the pigments Blue 15, Green 7, and Violet 23. Other pigments that were identified in white, black, red, and yellow inks are the Pigment White 6, Carbon Black, Pigment Red 8, and a diazo yellow, respectively. The present results show the importance of regulating tattoo ink composition. KW - Synchrotron KW - Tattoo inks KW - XRF KW - Toxic metals KW - Hazardous substances PY - 2019 DO - https://doi.org/10.1007/s12011-018-1406-y VL - 187 IS - 2 SP - 596 EP - 601 PB - Springer AN - OPUS4-47369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Constantinescu, B. A1 - Bugoi, R. A1 - Cojocaru, V. A1 - Radtke, Martin A1 - Calligaro, T. A1 - Salomon, J. A1 - Pichon, L. A1 - Röhrs, S. A1 - Ceccato, D. A1 - Oberländer-Târnoveanu, E. A1 - Ionescu, C. A1 - Pop, D. T1 - Dacian bracelets and Transylvanian gold: ancient history and modern analyses KW - SRXRF KW - Gold KW - Archaeometrie KW - Authentication KW - Provenance KW - XRF KW - Micro-PIXE KW - Micro SR-XRF KW - Or KW - Authentification KW - FX PY - 2009 SN - 0399-1237 VL - 33 SP - 221 EP - 225 PB - Groupe CY - Rennes AN - OPUS4-23172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mans, C. A1 - Simons, C. A1 - Hanning, S. A1 - Janßen, A. A1 - Alber, D. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Bühler, A. A1 - Kreyenschmidt, M. T1 - New polymeric candidate reference materials for XRF and LA-ICP-MS - development and preliminary characterization N2 - A set of ten calibration materials based on acrylonitrile-butadiene-styrene terpolymer (ABS) containing the elements Br, Pb, Cd, Cr, and Hg was produced in order to control polymer samples in regard to the restriction on the use of certain hazardous substances (RoHS) directive. The materials were produced with respect to the special demands of X-ray fluorescence analysis (XRF) and inductively coupled plasma mass spectrometry in combination with laser ablation (LA-ICP-MS). The mass fractions of all elements were 0-1500 mg/kg and the materials were produced as granulates and solid discs with a diameter of 40 mm and thicknesses of 1, 2, and 6 mm. It could be shown that the signals measured by XRF strongly depend on the thickness of polymeric samples. Macroscopic homogeneity was assessed with XRF measuring a total of 180 samples. The microscopic homogeneities were determined for a material with average elemental mass fractions with the aid of synchrotron radiation (SR) µ-XRF and LA-ICP-MS. Sufficient macroscopic and microscopic homogeneities for all elements could be achieved. It was observed that organic additives show a better homogeneity than oxides. XRF and LA-ICP-MS were successfully calibrated with the new materials. Limits of detection were in the range of 0.4-22 mg/kg for XRF and 2.3-26.8 mg/kg for LA-ICP-MS. The materials are considered as candidate reference materials (RM) by the Federal Institute of Materials Research and Testing (BAM, Germany). KW - XRF KW - LA.ICP-MS Plastics KW - RoHS KW - CRM PY - 2009 DO - https://doi.org/10.1002/xrs.1120 SN - 0049-8246 VL - 38 IS - 1 SP - 52 EP - 57 PB - Wiley CY - Chichester AN - OPUS4-18681 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 - Simons, C. A1 - Mans, C. A1 - Hanning, S. A1 - Janßen, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Ostermann, Markus A1 - Michaelis, Matthias A1 - Wienold, Julia A1 - Alber, D. A1 - Kreyenschmidt, M. T1 - Study on microscopic homogeneity of polymeric candidate reference materials BAM H001-BAM H010 by means of synchrotron µ-XRF and LA-ICP-MS N2 - In this study the microscopic homogeneity of the newly developed plastic reference materials BAM H001-BAM H010 was investigated. The materials consist of an acrylonitryle-butadien-styrene terpolymer, doped with different amounts of the elements Br, Cd, Cr, Hg and Pb. For the quantitative determination of the degree of homogeneity, a procedure proposed by Kempenaers et al. (Fresenius J. Anal. Chem., 2001, 369, 733-737) was used. On every sample an extensive number of different points were analyzed and standard deviation for every element mentioned above was used to calculate a minimal sampling mass that is necessary to reach a certain level of uncertainty caused by inhomogeneity (mmin,5%). The experiments were taken out with synchrotron µ-XRF (SR µ-XRF) at BESSYII in Berlin and by laser ablation inductively coupled plasma mass spectroscopy (LA-ICP-MS). The calculated values for mmin,5% of both techniques showed comparable results for all elements. It could be shown that the materials are suitable for calibration of micro analytic techniques if at least 64 µg are used. KW - XRF KW - LA-ICP-MS KW - RoHS KW - CRM PY - 2010 DO - https://doi.org/10.1039/b917008a SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 40 EP - 43 PB - Royal Society of Chemistry CY - London AN - OPUS4-20938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strüder, L. A1 - Hartmann, R. A1 - Holl, P. A1 - Ihle, S. A1 - Huth, M. A1 - Schmidt, J. A1 - Tham, Ch. A1 - Kanngießer, B. A1 - Baumann, J. A1 - Renno, A. A1 - Grenzer, J. A1 - Radtke, Martin A1 - Abboud, A. A1 - Pietsch, U. A1 - Soltau, H. T1 - High Speed, High Resolution imaging spectrometers based on pnCCDs for XRF and XRD applications N2 - For many years pnCCDs have been well known as X-ray detectors for spectroscopic imaging in many fields of science: X-Ray Fluorescence analysis (XRF), X-ray Diffraction (XRD) with light sources in large accelerator facilities as well as with laboratory light sources or with X-rays from celestial sources in X-ray astronomy. A brief introduction in GEXRF (Grazing Emission XRF) measurements with a laboratory laser produced plasma source will be given, PIXE (Particle Induced X-ray Emission) measurements and D2XRF (Double Dispersive X-Ray Fluorescence) and Slicing experiments with pnCCDs coupled to polycapillary optics performed at the BESSY synchrotron will be shown. Energy-dispersive Laue diffraction with ultra-hard X-rays for the analysis of defects in metals will conclude the overview of spectroscopic X-ray imaging measurements in the field of structure and dynamics of matter. KW - PnCCD KW - Synchrotron KW - XRF PY - 2016 DO - https://doi.org/10.1017/S1431927616001355 VL - 22 IS - S3 SP - 100 EP - 101 AN - OPUS4-38884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Constantinescu, B. A1 - Bugoi, R. A1 - Cojocaru, V. A1 - Radtke, Martin A1 - Calligaro, T. A1 - Salomon, J. A1 - Pichon, L. A1 - Röhrs, S. A1 - Ceccato, D. A1 - Oberländer-Târnoveanu, E. T1 - Micro-SR-XRF and micro-PIXE studies for archaeological gold identification - The case of Carpathian (Transylvanian) gold and of Dacian bracelets N2 - Trace-elements are more significant for provenancing archaeological metallic artifacts than the main components. For gold, the most promising elements are platinum group elements (PGE), Sn, Te, Sb, Hg and Pb. Several small fragments of natural Transylvanian gold – placer and primary – were studied by using micro-PIXE technique at the Legnaro National Laboratory AN2000 microbeam facility, Italy and at the AGLAE accelerator, C2RMF, Paris, France and by using micro synchrotron radiation X-ray fluorescence (micro-SR-XRF) at BESSY synchrotron, Berlin, Germany. The goal of the study was to identify the trace-elements, especially Sn, Sb and Te. A spectacular application to five Dacian gold bracelets authentication is presented (Sn and Sb traces). KW - Micro-PIXE KW - Micro-SR-XRF KW - Gold KW - Dacian bracelets KW - Transylvania PY - 2008 DO - https://doi.org/10.1016/j.nimb.2008.03.054 SN - 0168-583X SN - 1872-9584 VL - 266 IS - 10 SP - 2325 EP - 2328 PB - Elsevier CY - Amsterdam AN - OPUS4-17736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Denker, A. A1 - Hahn, Oliver A1 - Kanngießer, B. A1 - Malzer, W. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Röhrs, S. A1 - Reiche, I. A1 - Stege, H. T1 - Chemie der Kunst - Zerstörungsfreie Analyse von Kunst- und Kulturgütern N2 - Naturwissenschaftliche Informationen, insbesondere die chemische Zusammensetzung der Objekte, können Hinweise auf die Hintergründe der Objektherstellung liefern, die der alleinigen kunsthistorischen Begutachtung verborgen blieben. Es können nicht nur Fragen nach dem Prozess, Zeitpunkt und Ort der Herstellung beantwortet werden. Die chemische Analyse gibt auch Hinweise auf Ereignisse und Veränderungen, die erst nach der Fertigstellung des Objektes erfolgten. So werden Alterungsphänomene oder historische Überarbeitungen und Restaurierungen aufgedeckt, aber auch Konservierungsstrategien zur Erhaltung der Kunstwerke unterstützt. Durch den technologischen Fortschritt im Bereich der röntgenanalytischen Methoden, die berührungsfrei, ohne Probennahme und ohne Schädigung für das Untersuchungsobjekt arbeiten, erschließen sich dem Analytiker erstmalig Möglichkeiten, auch sehr wertvolle und fragile Objekte zerstörungsfrei zu untersuchen. PY - 2003 DO - https://doi.org/10.1515/mt-2003-0003 SN - 0025-5300 VL - 45 IS - 11-12 SP - 485 EP - 503 PB - Carl Hanser Verlag CY - München AN - OPUS4-2745 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Qureshi, Navid A1 - Morrow, Ryan A1 - Eltoukhy, Samar A1 - Grinenko, Vadim A1 - de Oliveira Guilherme Buzanich, Ana A1 - Onykiienko, Yevhen A. A1 - Kulbakov, Anton A1 - Inosov, Dmytro S. A1 - Adler, Peter A1 - Valldor, Martin T1 - Noncollinear Magnetic Structures in the Chiral Antiperovskite β-Fe2SeO N2 - We present the magnetic properties of the chiral, polar, andpossibly magnetoelectric antiperovskite β-Fe2SeO as derived from magnet-ization and specific-heat measurements as well as from powder neutrondiffraction and Mössbauer experiments. Our macroscopic data unambig-uously reveal two magnetic phase transitions at TN1 ≈ 103 K and TN2 ≈ 78K, while Rietveld analysis of neutron powder diffraction data reveals anoncollinear antiferromagnetic structure featuring magnetic moments inthe a−b plane of the trigonal structure and a ferromagnetic moment alongc. The latter is allowed by symmetry between TN1 and TN2, weakly visible inthe magnetization data yet unresolvable microscopically. While theintermediate phase can be expressed in the trigonal magnetic spacegroup P31, the magnetic ground state is modulated by a propagation vectorq = (1/2 1/2 0) resulting in triclinic symmetry and an even more complexlow-temperature spin arrangement which is also reflected in the Mö ssbauer hyperfine patterns indicating additional splitting of Fesites below TN2. The complex noncollinear spin arrangements suggest interesting magnetoelectric properties of this polar magnet. KW - EXAFS KW - Antiperovskite KW - Magnetic structure PY - 2024 DO - https://doi.org/10.1021/acs.inorgchem.4c02916 SN - 0020-1669 VL - 63 IS - 48 SP - 22712 EP - 22720 PB - American Chemical Society (ACS) AN - OPUS4-63116 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 - GEN A1 - Schlosser, S. A1 - Radtke, Martin A1 - Pernicka, E. T1 - Vultures hit by beam PY - 2005 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2004.pdf#page=497 SN - 0179-4159 SP - 497 EP - 499 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-7385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias A1 - Radtke, Martin A1 - Krumrey, M. A1 - Hasche, K. A1 - Schädlich, S. A1 - Frank, W. T1 - Electron probe microanalysis (EPMA) measurement of thin-film thickness in the nanometre range N2 - The thickness of thin films of platinum and nickel on fused silica and silicon substrates has been determined by EPMA using the commercial software STRATAGEM for calculation of film thickness. Film thickness ranged in the order 10 nm. An attempt was made to estimate the confidence range of the method by comparison with results from other methods of analysis. The data show that in addition to the uncertainty of the spectral intensity measurement and the complicated fitting routine, systematic deviation caused by the underlying model should be added. The scattering in the results from other methods does not enable specification of a range of uncertainty, but deviations from the real thickness are estimated to be less than 20%. KW - Electron probe microanalysis KW - EPMA KW - Thin films KW - Thickness measurement KW - X-rays PY - 2002 DO - https://doi.org/10.1007/s00216-002-1514-5 SN - 1618-2642 SN - 1618-2650 VL - 374 SP - 631 EP - 634 PB - Springer CY - Berlin AN - OPUS4-7090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Denker, A. A1 - Hahn, Oliver A1 - Merchel, Silke A1 - Radtke, Martin A1 - Kanngießer, B. A1 - Malzer, W. A1 - Röhrs, S. A1 - Reiche, I. A1 - Stege, H. T1 - Röntgenanalytik für Kunstwerke und Kulturgüter N2 - Naturwissenschaftler arbeiten mit Archäologen, Kunsthistorikern und Restauratoren zusammen, um Materialinformationen über Kunstwerke mit den Erkenntnissen aus Altertumsforschung, Kunstgeschichte und Denkmalpflege zu verbinden. Röntgenfluoreszenz und Röntgenemission sind die Methoden der Wahl, wenn wertvolle und fragile Objekte zerstörungsfrei zu untersuchen sind. KW - Synchrotron KW - XRF analysis KW - Drawings KW - Paintings KW - Ink KW - Art objects KW - Archaeometry KW - Röntgenfluoreszenzanalyse (RFA) KW - Zeichnungen KW - Gemälde KW - Tinten KW - Kunstobjekte KW - Archäometrie PY - 2005 SN - 1439-9598 SN - 1521-3854 VL - 53 IS - 2 SP - 118 EP - 123 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-6898 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilhelm, Stefan A1 - Kaiser, Martin A1 - Würth, Christian A1 - Heiland, J. A1 - Carrillo-Carrion, C. A1 - Muhr, V. A1 - Wolfbeis, Otto S. A1 - Parak, W.J. A1 - Resch-Genger, Ute A1 - Hirsch, T. T1 - Water dispersible upconverting nanoparticles: effects of surface modification on their luminescence and colloidal stability N2 - We present a systematic study on the effect of surface ligands on the luminescence properties and colloidal stability of β-NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), comparing nine different surface coatings to render these UCNPs water-dispersible and bioconjugatable. A prerequisite for this study was a large-scale synthetic method that yields ~2 g per batch of monodisperse oleate-capped UCNPs providing identical core particles. These ~23 nm sized UCNPs display an upconversion quantum yield of ~0.35% when dispersed in cyclohexane and excited with a power density of 150 W cm-2, underlining their high quality. A comparison of the colloidal stability and luminescence properties of these UCNPs, subsequently surface modified with ligand exchange or encapsulation protocols, revealed that the ratio of the green (545 nm) and red (658 nm) emission bands determined at a constant excitation power density clearly depends on the surface chemistry. Modifications relying on the deposition of additional (amphiphilic) layer coatings, where the initial oleate coating is retained, show reduced non-radiative quenching by water as compared to UCNPs that are rendered water-dispersible via ligand exchange. Moreover, we could demonstrate that the brightness of the upconversion luminescence of the UCNPs is strongly affected by the type of surface modification, i.e., ligand exchange or encapsulation, yet hardly by the chemical nature of the ligand. KW - upconverting nanoparticles (UCNPs) KW - Luminescence KW - surface modification PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-324071 DO - https://doi.org/10.1039/c4nr05954a SN - 2040-3364 SN - 2040-3372 VL - 7 IS - 4 SP - 1403 EP - 1410 PB - RSC Publ. CY - Cambridge AN - OPUS4-32407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Böttger, S. A1 - Rosenberg, D. A1 - Menzel, M. A1 - Jensen, W. A1 - Busker, M. A1 - Gotlib, Z. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Wobrauschek, P. A1 - Streli, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline N2 - An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml⁻¹ to μg ml⁻¹). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NISTwater 1640. Low limits of detection of less than 100 fg absolute (10 pg ml⁻¹) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. KW - TXRF KW - TXRF-XANES KW - Sample changer KW - BAMline KW - Re-XANES PY - 2016 DO - https://doi.org/10.1107/S1600577516001995 SN - 1600-5775 VL - 23 IS - 3 SP - 820 EP - 824 PB - International Union of Crystallography AN - OPUS4-38656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Menzel, M. A1 - Scharf, O. A1 - Novak, S. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Hischenhuber, P. A1 - Buzanich, Günter A1 - Meyer, A. A1 - Lopez, V. A1 - McIntosh, K. A1 - Streli, C. A1 - Havrilla, G. A1 - Fittschen, U. T1 - Shading in TXRF: calculations and experimental validation using a color X-ray camera N2 - Absorption effects in total reflection X-ray fluorescence (TXRF) analysis are important to consider, especially if external calibration is to be applied. With a color X-ray camera (CXC), that enables spatially and energy resolved XRF analysis, the absorption of the primary beam was directly visualized for mL-droplets and an array of pL-droplets printed on a Si-wafer with drop-on-demand technology. As expected, deposits that are hit by the primary beam first shade subsequent droplets, leading to a diminished XRF signal. This shading effect was quantified with enhanced precision making use of sub-pixel analysis that improves the spatial resolution of the camera. The measured absorption was compared to simulated results using three different model calculations. It was found they match very well (average deviation < 10%). Thus errors in quantification due to absorption effects can be accounted for in a more accurate manner. KW - absorption KW - X-ray Fluorescence analysis PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-359000 DO - https://doi.org/10.1039/C5JA00127G IS - 10 SP - 2184 EP - 2193 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-35900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hahn, Oliver A1 - Denker, A. A1 - Merchel, S. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Wolff, T. ED - Armbruster, B. ED - Eilbracht, H. ED - Hahn, Oliver ED - Heinrich-Tamaska, O. T1 - Zerstörungsfreie Analyse von Metallartefakten - Eine Fallstudie N2 - Die naturwissenschaftliche Analyse historischer Materialen ermöglicht die Beantwortung kulturhistorischer Fragestellungen, die mit kunsthistorischen oder archäologischen Ansätzen allein nicht zu leisten sind. In dieser Studie wurden sechs römische Münzen mit unterschiedlich stark ausgeprägten Korrosionsschichten an unbehandelten und polierten Stellen mit vier zerstörungsfreien analytischen Methoden untersucht: Hoch- und Niederenergie Protonen Induzierter Röntgenemission (HE-/PIXE), Synchrotronstrahlungsinduzierte-Röntgenfluoreszenzanalyse (SY-RFA) und Mikro-Röntgenfluoreszenzanalyse (Mikro-RFA) mit einem mobilen Gerät. Aufgrund von Unterschieden in den Messbedingungen und dem Einfluss der Patina-Schichten auf diese ergaben sich nur für wenige Elemente Übereinstimmungen in den quantitativen Daten. Zur Validierung zukünftiger Messkampagnen mit verschiedenen Methoden sind daher Vergleichstudien unerlässlich. N2 - Investigations of physical properties and chemical composition of ancient materials generate important data for answering culture-historical questions that cannot be solved by art historical and archaeological methods alone. This contribution reports on the analysis of six Roman coins, with different degrees of corrosion layers in parts that were not handled or polished, using four non-destructive methods: low-energy particle-induced X-ray emission (PIXE, 2 MeV), high-energy PIXE (68 MeV), μ-X-ray fluorescence (XRF) spectrometry with a portable device and synchrotron-radiation induced XRF. Because of differences in the conditions needed for measurement and the influence of the layers of patina on these measurements, there were few elements where the quantitative data were in agreement. Thus comparative analyses are essential to validate future measurement projects using different methods. KW - Zerstörungsfreie Prüfung KW - Protoneninduzierte Röntgenemission KW - Röntgenfluoreszenzanalyse KW - Non-destructive testing KW - Particle-induced X-ray emission KW - X-ray fluorescence analysis PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-385702 SN - 978-3-9816751-5-3 VL - Berlin studies of the ancient world, Band 35 SP - 117 EP - 137 PB - Edition Topoi CY - Berlin AN - OPUS4-38570 LA - deu 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 - 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 -