TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Optical spectrometry for isotope analysis N2 - Isotope analysis is a tool for material research. For example, it may provide information about the provenance of a sample or changes in dynamic systems. Here is presented optical spectroscopy as an analytical alternative to mass spectrometry for isotope quantification based on the isotopic shift of atoms and diatomic molecules. T2 - Isotopic Tools for the Investigation of Materials WS 21/22 CY - Leoben, Austria DA - 01.10.2021 KW - Isotopes KW - HR-CS-AAS KW - Lithium KW - Atomic absorption spectrometry KW - Diatomic molecules PY - 2022 AN - OPUS4-56495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Laser spectroscopy methods for calcium isotope analysis N2 - Calcium isotope analysis can be an important tool for paleoclimate studies of the carbon cycle, as well in carbon capture technology, but its utility is limited by challenges using conventional mass spectrometry. We propose a new fast, precise, and high-throughput technology based on multiple complementary high-resolution spectroscopies analyzed by machine-learning. T2 - Seminars Chemical Physics Caltech CY - Pasadena, CA, USA DA - 13.04.2022 KW - Calcium KW - Atomic spectroscopy KW - CaF KW - Calcium monofluoride KW - Carbon cycle KW - Doppler effect KW - Sub-doppler spectroscopy KW - Laser spectroscopy PY - 2022 AN - OPUS4-56499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Tanz der Moleküle: Herkunftsbestimmung mittels optischer Spektroskopie N2 - Wie lässt sich die Herkunft von Rohstoffen, Lebensmitteln oder Umweltschadstoffen einfacher, schneller und kostengünstiger als mit bisherigen Methoden bestimmen? Die Dissertation zeigt auf, dass man das grundlegende physikalische Prinzip einer Isotopverschiebung mit in Adlershof entwickelten Optik-Instrumenten für die Herkunftsbestimmung nutzen kann. Die entwickelte Methode ermöglicht es in Zukunft den Ursprung von Rohstoffen, Lebensmitteln oder Umweltschadstoffen kostengünstiger und wesentlich schneller bestimmen, als dies mit bisherigen Methoden möglich ist. Kann man das grundlegende physikalische Prinzip einer Isotopieverschiebung mit einem Optik-Instrument für die Herkunftsbestimmung nutzen? Carlos Abad hat eine wegweisende Methode entwickelt, die es in Zukunft ermöglicht den Ursprung von Rohstoffen, Lebensmitteln oder Umweltschadstoffen kostengünstiger und wesentlich schneller bestimmen, als dies mit bisherigen Techniken möglich ist. T2 - Dissertationspreis Adlershof 2019 CY - Berlin, Germany DA - 12.02.2020 KW - Herkunftsbestimmung KW - Isotopenanalyse KW - Isotope KW - Optischer Spektroskopie KW - Coltan PY - 2020 AN - OPUS4-51993 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Ultrafast spectroscopy - Femtosecond electron diffraction N2 - Currently, two main high speed processes can be investigated: electromagnetic absorption and electromagnetic scattering. At the summer university of the School of Analytical Sciences Adlershof (SALSA-HU), a series of 5 articles were presented to ilustrate the potential of ultrafast spectroscopy, from IR band assignment to monitoring time resolved structural changes. First, by studying light absorption is possible to do assignment and interpretation of IR bands in small molecules and to study the influence of ligands or labeled molecules in protein structures. Second, by studying light scattering is possible to monitoring photoinduced structural changes in solid materials. This presentation contains a study of photoinduced structural changes monitored by light scattering in condensed matter. T2 - SALSA Summer University 2017 CY - Berlin, Germany DA - 19.09.2017 KW - Ultrafast spectroscopy KW - Femtosecond electron diffraction KW - Spin crossover KW - Photoexcitation KW - Structural dynamics PY - 2017 AN - OPUS4-42120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotope analysis by molecular absorption spectrometry N2 - The use of molecular absorption spectrometry (MAS) for the determination of isotope amount ratios is here discussed. Preliminary results on the determination of isotope ratios of boron, copper and magnesium in reference materials are here presented and compared with their certificates. T2 - Adlershofer Kolloquium Analytik CY - Berlin, Germany DA - 13.06.2017 KW - Isotope KW - Molecular absorption KW - HR-CS-MAS KW - Isotopic shift KW - Spectrometry KW - Isotope ratio PY - 2017 AN - OPUS4-40574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Advances and Applications of Molecular Absorption Spectrometry: from Non-Metals to Isotope Analysis N2 - Wie kann Nicht-Messbares messbar gemacht werden? Die Antwort der Dissertation auf diese zentrale Frage der analytischen Chemie lautet: die Anwendung der hochauflösenden optischen Spektroskopie der diatomischen Moleküle. In der Arbeit wird in einem ersten Schritt in Grafitöfen, die wie Chemiereaktoren funktionieren, und durch die Anwendung verschiedener analytischer Methoden die diatomische Molekülbildung nachvollzogen. In einem zweiten Schritt werden die aufgedeckten Mechanismen auf die Bestimmung von Nichtmetallen und die Analyse von Isotopen angewendet. Die Isotopenanalytik ist das zukunftsweisendes Herzstück der Dissertation und von alltäglicher und politischer Relevanz: Mittels dieser Technik lässt sich die Herkunft von Lebensmitteln aber auch Chemiewaffen kostengünstiger und wesentlich schneller bestimmen als mit bisherigen Methoden der Massenspektrometrie. Möglich ist die Bestimmung, da alles um uns herum aus Atomen verschiedener Elemente besteht und die meisten Elemente mehrere Isotope haben. Isotope unterscheiden sich hinsichtlich ihres Gewichts, da sie über eine unterschiedliche Anzahl an Neutronen verfügen. Die Informationen über das Verhältnis von schweren und leichten Isotopen lässt sich nutzen, um zu bestimmen wo etwas entstanden ist. Jeder Ort auf unserem Planeten hat seinen persönlichen Element- und Isotopenanteil (Isotopenfingerabdruck). Das in der Arbeit angewandte Instrument misst das Verhältnis indirekt und nutzt hierzu die Interaktion zwischen Licht und Materie. Für das schwerere Isotop wird mehr Licht/Energie benötigt, um es in Bewegung zu bringen, als für das leichtere. Diese kleinen Unterschiede an Energie, die wir dafür aufwenden müssen, werden gemessen und ermöglichen die Herkunftsbestimmung. Damit leistet die Arbeit nicht nur einen wichtigen Beitrag zur Grundlagenforschung in der analytischen Chemie, sondern kann mit den aufgezeigten Ergebnissen auch Anwendung in den Bereichen Verbraucherschutz, Umweltforschung und Waffenkontrolle finden. N2 - The present work covers two main aspects of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS), an analytical technique for elemental trace analysis. First, a comprehensive mechanistic study of molecule formation in graphite furnaces is presented, which is a key step into the recovery of analytical signals. For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in HR-CS-GFMAS. A zirconium coating catalyzes the CaF formation, and its structure was investigated. 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 (SEM-EDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. Here a mechanism is proposed, where ZrO2 works 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. Second, analytical methods were developed by using HR-CS-MAS as detector for non-metals and isotope analysis. Therefore, the determination of organic absorbable chlorine in water, the quantification of fluorine in consume care products with declared perfluorinated ingredients, and the determination of sulfur content in crude oils were investigated. Finally, the high resolution of the instrumentation allows to measure isotopic shifts with high precision in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of boron and magnesium were investigated, establishing so the potential of HR-CS-MAS for the accurate and precise determination of isotopic amount ratios. T2 - Applied Photonics Award 2020 CY - Jena, Germany DA - 22.09.2020 KW - Herkunftsbestimmung KW - Isotopenanalyse KW - Isotope KW - Optischer Spektroskopie PY - 2020 AN - OPUS4-51996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Lippitz, Andreas A1 - Benemann, Sigrid A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Jakubowski, Norbert A1 - Huang, M.-D. A1 - Florek, S. A1 - Becker-Ross, H. T1 - A proposed mechanism of action of permanent modifiers for molecular absorption spectrometry: the case of calcium monofluoride N2 - High-Resolution Continuum Source Molecular Absorption Spectrometry (HR-CS-MAS) with graphite furnace atomizers has been successfully used for the analytical determination of non-metals. The use of permanent modifiers (or coatings) for molecule formation is necessary, but their mechanisms of action remain unclear. In order to understand and improve the current analytical methods, we present a comprehensive mechanistic study of molecule formation in graphite furnaces: a key step into the recovery of analytical signals. Therefore, a well-known system for fluorine determination was studied: the molecule formation of CaF, with Zr as permanent modifier. Through a kinetic approach, an Arrhenius plot showed a pseudo first order reaction respect to F-. By spectroscopic methods (XPS, XAS, EDX) it was possible to elucidate an intermediate state. Here a mechanism is proposed, where ZrO2 works as heterogeneous catalyst: after a pyrolytic step, it is activated to the intermediate state of ZrO(OCaF) and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. With this analytical information, improved surface modifications and coatings for graphite furnaces can be designed and some of them, for example with Zr nanoparticle and Zr xerogels are here presented. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Fluorine KW - High-resolution continuum source Molecular Absorption Spectrometry KW - HR-CS-MAS KW - Zirconium oxide KW - Modifier KW - Coating PY - 2017 AN - OPUS4-39902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - On developments of continuum source atomic and molecular absorption spectrometry N2 - Der Bunsen-Kirchhoff-Preis 2022 wurde am 23.06.2022 anlässlich der analytica conference in München an Dr. Carlos Abad verliehen - in Anerkennung seiner exzellenten Entwicklungen im Bereich der continuum source atomic absorption spectrometry (CS-AAS). Dr. Carlos Abad ist ein herausragender Experte auf dem Gebiet der Atom- und molekularen Absorptionsspektrometrie. insbesondere trug er maßgeblich zur substanziellen Weiterentwicklung von Echelle-Spektrometern für die CS-AAS bei. So gelang es, einen quantitativen Zugang zu Elementen wie Bor, Chlor, Fluor und Schwefel, mittels AAS zu erreichen. Erstmals demonstriert Dr. Carlos Abad am Beispiel eines Zr-Modifier, dass durch die Zeitauflösung der eingesetzten Echelle-Systeme mechanistische Untersuchungen zur Wirkung des Modifiers im Graphitrohrofen möglich sind. Besonders hervorzuheben sind seine Arbeiten zum Einsatz der CS-AAS für die Analyse von Isotopen, die eine Genauigkeit aufweist, welche an die der Multikollektor-induktiv gekoppelten Plasma-Massenspektrometrie (MC-ICP-MS) heranreicht. Damit ergeben sich völlig neue Einsatzmöglichkeiten für technologisch hochrelevante Applikationen, wie z.B. die Untersuchung der Alterung von Lithium-Batterien oder die Lithium-Analyse in Blutserum. T2 - Analytica Conference: Bunsen-Kirchhoff-Preis 2022 der Deutsche Arbeitskreis für Analytische Spektroskopie (DAAS) CY - Munich, Germany DA - 23.06.2022 KW - Isotopes KW - Fluorine KW - Halogens KW - Non-metals KW - HR-CS-MAS KW - HR-CS-AAS KW - Bunsen-Kirchhoff-Preis KW - Continuum source atomic absorption spectrometry KW - Zr-Modifier KW - Graphite furnace KW - Lithium PY - 2022 AN - OPUS4-56500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Origin, Provenance, and Isotope analysis N2 - Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice. All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis. T2 - Berlin Sciendce Week – Zukunftsorte – Innovation Made in Berlin CY - Berlin, Germany DA - 07.11.2019 KW - Isotope analysis KW - Optical spectroscopy KW - Provenance KW - Iisotopic signature KW - Isotopic fingerprints PY - 2019 AN - OPUS4-49889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotope analysis by high-resolution optical spectroscopy: a tool for planetary science N2 - Isotope analysis can be used to determine the age and provenance of geological samples. Modern techniques in optical spectrometry allow us a stand-off isotope analysis. This seminar will discuss how planetary science with the next Moon and Mars missions drive optical spectrometry into precise and accurate isotope analysis and how BAM will contribute. T2 - Adlershofer Kolloquium CY - Online meeting DA - 19.05.2020 KW - Provenance KW - Dating KW - Isotopes KW - Optical spectroscopy KW - Isotopic shift KW - Planetary science PY - 2020 AN - OPUS4-51995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Breaking the wall of uncertain origin N2 - Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice. All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis. T2 - Falling Walls Lab Adlershof CY - Berlin, Germany DA - 27.09.2019 KW - Isotope analysis KW - Optical spectroscopy KW - Provenance PY - 2019 AN - OPUS4-49882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - New approaches in isotope analysis - molecular absorption spectrometry N2 - Variations in the isotope amount composition of some elements like lithium, boron, magnesium, calcium and copper have been used as proof of provenance of a sample and to describe geological processes. Routinely, isotope compositions are determinate by mass spectrometry; the working horse of the isotope analysis. However, mass spectrometric methods are expensive, time consuming and they require a high qualified analysist. Here an alternative faster and low cost optical method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Stable isotope amount composition of X= Li, B, Mg, Ca, Cu and Sr have been determined by monitoring the absorption spectrum of their monohydride (XH) in graphite furnace HR-CS-MAS. T2 - Seminar at Princeton University CY - Princeton, NJ, USA DA - 16.10.2017 KW - Isotope KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - HR-CS-MAS KW - Isotopic shift KW - Graphite furnace KW - Isotope ratio PY - 2017 AN - OPUS4-43538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - You, Zengchao A1 - Richter, Silke A1 - Benner, Philipp A1 - Recknagel, Sebastian T1 - The use of reference materials to improve the calibration strategy in glow discharge optical emission spectroscopy with machine learning N2 - Glow discharge optical emission spectroscopy (GD-OES) is a technique for the analysis of solids such as metals, semiconductors, and ceramics. A low-pressure glow discharge plasma is applied in this system, which ‘sputters’ and promotes the sample atoms to a higher energy state. When the atoms return to their ground state, they emit light with characteristic wavelengths, which a spectrometer can detect. Thus, GD-OES combines the advantages of ICP-OES with solid sampling techniques, which enables it to determine the bulk elemental composition and depth profiles. However, direct solid sampling methods such as glow-discharge spectroscopy require reference materials for calibration due to the strong matrix effect. Reference materials are essential when the accuracy and reliability of measurement results need to be guaranteed to generate confidence in the analysis. These materials are frequently used to determine measurement uncertainty, validate methods, suitability testing, and quality assurance. In addition, they guarantee that measurement results can be compared to recognized reference values. Unfortunately, the availability of certified reference materials suited to calibrate all elements in different matrix materials is limited. Therefore various calibration strategies and the preparation of traceable matrix-matched calibration standards will be discussed. Machine learning is an essential component of the growing field of data science. Through statistical methods, algorithms are trained to make classifications or predictions, uncovering key insights within data mining projects. Therefore, it was tried in our work to combine GD-OES with machine learning strategies to establish a new and robust calibration model, which can be used to identify the elemental composition and concentration of metals from a single spectrum. For this purpose, copper reference materials from different manufacturers, which contain various impurity elements, were investigated using GD-OES. The obtained spectra information are evaluated with different algorithms (e.g., gradient boosting and artificial neural networks), and the results are compared and discussed in detail. T2 - Winter Conference on Plasma Chemistry 2022 CY - Tucson, AZ, USA DA - 17.01.2022 KW - GDOES KW - Machine learning KW - Reference materials KW - Calibration KW - Cooper PY - 2022 AN - OPUS4-56497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotopic analysis by high-resolution optical spectroscopy N2 - Isotope analysis can be used to determine the age and provenance of geological samples or to study dynamic systems like Li-ion batteries. Modern techniques in optical spectrometry allow us a fast and slow-cost isotope analysis. These techniques include high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) and laser ablation molecular isotopic spectrometry. This seminar will discuss our recent work on precise and accurate isotope analysis of boron, magnesium, and lithium with geology, climate, and energy research applications. T2 - Recent Trends in Chemical Science and Technology, Christian College Chengannur, India CY - Online meeting DA - 29.09.2020 KW - Isotopes KW - Optical spectrometry KW - Machine learning PY - 2020 AN - OPUS4-51997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Analytical applications of high resolution continuum source molecular absorption spectrometry N2 - High-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) has been apply for the determination of non-metals and isotope analysis, extending so the application range of atomic absorption spectrometry (AAS). This seminar is divides in two main parts. First, here is presented a comprehensive mechanistic study of molecule formation in graphite furnaces, a key step into the recovery of analytical signals in AAS and MAS. Therefore, a well-known system for fluorine determination was studied: the molecule formation of CaF, with Zr as permanent modifier. Through a kinetic approach, an Arrhenius behaved pseudo first order reaction respect to F- was observed and by spectroscopic methods (XPS, XAS, EDX) an intermediate state was possible to be elucidated. Here it is proposed a mechanism, where zirconium works as heterogeneous catalyst: after a pyrolytic step, it is activated the intermediate ZrO(OCaF) and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. Second, we have developed analytical methods using HR-CS-MAS as detector for quantification of fluorine in consume-care products with declared per-fluorinated ingredients. Ad, the high resolution of the instrumentation allows identify isotopic shifts in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of B were investigated and so the potential of HR-CS-MAS for the determination of isotopic ratios is established. T2 - Brown Bag Lecture SALSA Humboldt Universität zu Berlin CY - Berlin, Germany DA - 18.04.2017 KW - Fluorine KW - Molecular absorption KW - Graphite furnace KW - Isotopes KW - Boron PY - 2017 AN - OPUS4-40075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Simultaneous multielemental analysis of crude oils by high-resolutions absorption spectrometry N2 - When crude oil arrives at a refinery it needs a lot of processing before it is suitable for cracking into lighter fractions. Sulfur has to be extracted to meet ultra-low sulfur legislation for most of the fuel grades, and desalination is a crucial process as chlorine within salts is corrosive to refinery equipment. Measuring the amounts of sulfur and chlorine within crude oil is the first step in a complex clean-up process. Heavy metals, such as vanadium, nickel and iron need to be removed too. These metals can poison the catalyst used to crack the oil into lighter fractions. This is costly as it reduces the useful life of the catalyst. Like chlorine, heavy metals also have a corrosive effect on the plant. There is some evidence that the presence of some metals in the final product can reduce performance. A fast determination of elements and size of suspended particles is vital for diagnosis and safeguard of refinery equipment. However, sample preparation for current analytical methods consumes precious time and lost particle size information. High-resolution continuum source graphite furnace absorption spectrometry (HR-CS-GFAS) is proposed as a fast analytical method for elemental determination in crude oils and potentially for simultaneous multielement and particle size analysis. This HR-CS-GFAS instrumentation is coupled to a modular simultaneous echelle spectrometer (MOSES) and provides a full optical window with high resolution (from 180 to 900 nm with bandwidth λ/170,000). By using this set-up, it is possible to generate a multiparameter 3D spectral image (atomic and molecular lines, isotopic shift, atomization delay, and intensities). The generated spectral images can be analyzed by multivariate regressions for the elemental and particle size analysis. Additionally, if several atomic and molecular lines are simultaneously measured, they may be used in multi-energy calibration (MEC), a method based on the use of many wavelengths of the same absorbing/emitting entity to improve the accuracy in analytical atomic spectrometry. This MEC approach combined with multivariate image analysis allows the quantification of selected elements (Si, Al, Ni, Fe, V, S, and Cl) and overcomes matrix effects. T2 - Chevron Seminar- Group Chemical Characterization and Atomic Spectroscopy CY - Richmond, CA, USA DA - 22.10.2019 KW - Crude oil KW - Multielemental analysis KW - HR-CS-AAS KW - Optical spectroscopy KW - MOSES PY - 2019 AN - OPUS4-49885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Optical spectrometry for isotope analysis N2 - Isotope analysis plays a critical role in various disciplines, including environmental science, archaeology, and forensic investigations. Traditional methods such as mass spectrometry provide precise isotopic data but often require complex, costly setups and extensive sample preparation. As an alternative, optical spectrometry has emerged as a versatile and less invasive technique. This presentation explores the advancements and applications of optical spectrometry methods in isotope analysis, emphasizing their benefits and challenges. T2 - University of Calgary PHYS 561 - Stable And Radioactive Isotope - Winter 2024 CY - Online meeting DA - 07.03.2024 KW - Isotopes KW - HR-CS-MAS KW - Chemometrics KW - Laser Ablation Molecular Absorption spectrometry KW - LAMIS PY - 2024 AN - OPUS4-59948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Winckelmann, Alexander A1 - Morcillo, Dalia A1 - Jegieka, Dennis A1 - Vogl, Jochen A1 - Florek, S. A1 - Recknagel, Sebastian T1 - Isotope analysis through the integration of chemometrics into optical spectroscopy N2 - Lithium (Li), Boron (B), Nitrogen (N), Magnesium (Mg), and Calcium (Ca) are pivotal elements across various spheres such as the hydrosphere, biosphere, and lithosphere, significantly impacting (bio-) geochemical and physiological processes. These elements exhibit stable isotopes with substantial roles in geological, environmental, and biological studies. The traditional method for measuring isotope amount ratios has been through mass spectrometry, which, despite its accuracy, comes with high operational costs, the need for skilled operators, and time-consuming sample preparation processes. Combining optical spectroscopy with chemometrics introduces an innovative, cost-effective approach by the hand of high-resolution continuum source atomic and molecular absorption spectrometry (HR-CS-AAS and HR-CS-MAS) for the analysis of isotope ratios in Li, B, N, Mg, and Ca. By analyzing the atomic or molecular absorption spectrum of the in-situ generated cloud of atoms of diatomic molecules (e.g., Li, BH, NO, MgF, CaF) during the electronic transition from the fundamental state, this method allows for the rapid determination of isotope ratios directly from sample solutions without the need for complex sample preparation. For each element, the respective atomic or molecule's absorption spectrum was deconvoluted into its isotopic components using partial least squares regression or machine learning algorithms. Robust calibration models were developed, calibrated with enriched isotope, and validated against certified reference materials. Spectral data underwent preprocessing to optimize the modeling to determine the optimal number of latent variables. The findings showcase that this optical spectrometric method yields results that agree with those obtained via inductively coupled plasma mass spectrometry (ICP-MS), offering a promising, cost-effective, and rapid alternative for isotope analysis with precisions as low as ± 0.2‰. This approach is a significant advancement in analytical chemistry, providing a new way to study isotope variations in biological, environmental, and geological samples. T2 - Analytica Conference CY - Munich, Germany DA - 09.04.2024 KW - Isotopes KW - HR-CS-MAS KW - Chemometrics KW - Lithium KW - Boron KW - Magnesium KW - Nitrogen PY - 2024 AN - OPUS4-59946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Winckelmann, Alexander A1 - Hoffmann, Volker A1 - You, Zengchao A1 - Richter, Silke A1 - Recknagel, Sebastian T1 - What does GD-OES reveal about the aging and manufacturing processes of lithium-ion batteries? N2 - Glow-Discharge Optical Emission Spectroscopy (GD-OES), a powerful analytical technique, sheds light on the two critical aspects of lithium-ion batteries (LIBs): manufacturing and aging 1, 2. We optimized cell production in manufacturing by adjusting parameters, including cathode doping, electrolyte concentration, and pressing force. GD-OES provided in-depth elemental composition and homogeneity analysis, which is crucial for identifying optimal manufacturing conditions. These findings were validated by electrochemical impedance spectroscopy, confirming the quality of the manufactured batteries. Shifting the focus to aging, we use GD-OES for fluorine depth profiling, a key element in understanding polymer and electrolyte degradation. However, fluorine presents analytical challenges. We addressed this by substituting argon with a neon:argon mixture, which significantly enhanced fluorine detection sensitivity. This advancement not only improves accuracy but also holds the potential to guide sustainable and cost-efficient manufacturing strategies. Through its versatility, GD-OES has proven to be a powerful tool for not only optimizing LIB manufacturing processes but also gaining deeper insights into their aging mechanisms. This research extends beyond academic interest, offering tangible benefits for the industry by translating into improved battery quality, extended lifespan, and overall performance. T2 - The 6th International Glow Discharge Spectroscopy Symposium CY - Liverpool, United Kingdom DA - 21.04.2024 KW - GD-OES KW - Depth profiles KW - Lithium KW - Battery KW - Fluorine KW - Aging KW - Manufacturing KW - Glow-discharge PY - 2024 AN - OPUS4-59945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Stable isotope analysis via hydrides using molecular absorption spectrometry N2 - Small variations in the isotopic composition of some elements have been used as proof of provenance of mineral and biological samples, to describe geological processes, and to estimate a contamination source. Routinely, isotope compositions are measured by mass spectrometry; the working horse of the isotope analysis. However, mass spectrometric methods are expensive, time-consuming and they require a high qualified analyst. Here, an alternative faster and low-cost optical method for isotope ratio determination is investigated: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Stable isotope amount composition of X = Li, B, Mg, Ca and Sr have been determined by monitoring the absorption spectra of their in situ generated hydrides (XH) in graphite furnace HR-CS-MAS. For example, the system of two stable isotopes of boron (10B and 11B) was studied via its hydride for the electronic transition X1Σ+ → A1Π (Fig. 1a). The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, isotopic composition of samples and reference materials are calculated by a partial least square regression (PLS). For this, a spectral library is built by using samples with known isotope composition. Results are metrologically compatible with those reported by mass spectrometric methods. [1] Similar results are obtained for n isotope systems like Mg (24Mg, 25Mg, and 26Mg), where isotope shift of their isotopologues can be resolved as shown in Fig.1 b. The extension of this methodology to other elements like Li, Ca and Sr is discussed [2]. References: [1] C. Abad, S. Florek, H. Becker-Ross, M.-D. Huang, H.-J. Heinrich, S. Recknagel, J. Vogl, N. Jakubowski, U. Panne, Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers, Spectrochim. Acta, Part B, 136 (2017) 116-122. [2] C. Abad et al., unpublished results, 2018. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Isotope KW - HR-CS-MAS KW - Mono-hydride KW - Spectrometry PY - 2018 AN - OPUS4-45826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Morcillo, Dalia A1 - Winckelmann, Alexander A1 - Richter, Silke A1 - Vogl, Jochen A1 - Riedel, Jens A1 - Recknagel, Sebastian A1 - Panne, Ulrich T1 - Applications of atomic absorption spectrometry for lithium isotope analysis N2 - An alternative method for lithium isotope analysis by using high-resolution atomic absorption spectrometry (HR-CS-AAS) is proposed herein. This method is based on monitoring the isotope shift of approximately 15 pm for the electronic transition 22P←22S at around the wavelength of 670.8 nm, which can be measured by state-of-the-art HR-CS-AAS. Isotope analysis can be used for (i) the traceable determination of Li concentration and (ii) isotope amount ratio analysis based on a combination of HR-CS-AAS and spectral data analysis by machine learning (ML). In the first case, the Li spectra are described as the linear superposition of the contributions of the respective isotopes, each consisting of a spin-orbit doublet, which can be expressed as Gaussian components with constant spectral position and width and different relative intensity, reflecting the isotope ratio in the sample. Precision was further improved by using lanthanum as internal spectral standard. The procedure has been validated using human serum-certified reference materials. The results are metrologically comparable and compatible with the certified values. In the second case, for isotope amount ratio analysis, a scalable tree boosting ML algorithm (XGBoost) was employed and calibrated using a set of samples with 6Li isotope amount fractions ranging from 0.06 to 0.99 mol mol−1. The training ML model was validated with certified reference materials. The procedure was applied to the isotope amount ratio determination of a set of stock chemicals and a BAM candidate reference material NMC111 (LiNi1/3Mn1/3Co1/3O2), a Li-battery cathode material. These determinations were compared with those obtained by MC-ICP-MS and found to be metrologically comparable and compatible. The residual bias was −1.8‰, and the precision obtained ranged from 1.9‰ to 6.2‰. This precision was sufficient to resolve naturally occurring variations. The NMC111 cathode candidate reference material was analyzed using high-resolution continuum source atomic absorption spectrometry with and without matrix purification to assess its suitability for technical applications. The results obtained were metrologically compatible with each other. T2 - Colloquium Spectroscopicum Internationale XLII (CSI XLII) CY - Gijón, Spain DA - 30.05.2022 KW - Lithium KW - HR-CS-AAS KW - Chemometrics KW - Atomic spectrometry PY - 2022 AN - OPUS4-56498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Molecular absorption spectrometry: a fast and accurate optical method for boron isotope analysis comparable to mass spectrometry N2 - Boron presents two stable isotopes, 10B and 11B and due to their relatively large mass difference (~ 10%) isotope fractionation leads to considerable isotope amount ratio variations n(10B)/n(11B) in natural occurrence. These have been used as a proof of provenance of mineral and biological samples, to estimate a contamination source and to the determination of geological processes by erosion or subduction. Additionally, boron is employed in the nuclear industry due to the capability of its isotope 10B to thermal-neutron capture and therefore 10B enriched boric acid solutions are used in the cooling system of thermonuclear facilities and in the alloying of steel and carbides for protective shielding. Usually, isotope ratio variations are determined by mass spectroscopic methods. Here an alternative faster and low cost method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Boron isotope amount ratios have been determined by monitoring the absorption spectrum of boron monohydride (BH) in graphite furnace HR-CS-MAS. Bands (0→0) and (1→1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, a precision and accuracy of the method of ± 0.5 ‰ for the evaluated spectral region around 437.1 nm is reported here. This accuracy and precision is comparable with those obtained by thermal ionization mass spectrometry (TIMS) and multiple collector inductively coupled plasma mass spectrometry (MC-ICP-MS) for boron isotope ratio measurements. T2 - 30. Tag der Chemie CY - Berlin, Germany DA - 05.07.2017 KW - Boron isotopes KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - HR-CS-MAS KW - Isotopic shift KW - Boron monohydride KW - Isotope ratio KW - Molecular absorption KW - Memory effect KW - Graphite furnace PY - 2017 AN - OPUS4-41060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Muench, S. A1 - Okruss, M. A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Optical spectrometry versus mass spectrometry for stable isotope analysis of B and Mg N2 - Mass spectrometric methods (MC-ICP-MS and TIMS) are without doubt the working horse of stable isotope analysis. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time consuming. We propose a lower-cost and faster optical alternative for the analysis of isotope ratios of selected elements: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Stable isotope amount compositions of boron (B) and magnesium (Mg) were determined based on the absorption spectra of in-situ generated mono-hydrides and halide (MH and MX) using graphite furnace HR-CS-MAS. The use of a modular simultaneous echelle spectrograph (MOSES) helps to find the maximal isotope shift in the diatomic molecular spectra produced in a graphite furnace by using isotopic spike solutions. Isotopes of boron (10B and 11B) were studied via their hydrides for the electronic transition X 1Σ+ → A 1Π. The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, the isotopic composition of samples can be calculated by a partial least square regression (PLS). For this, a spectral library was built by using samples and spikes with known isotope composition. Boron isotope ratios measured by HR-CS-MAS are identical with those measured by mass spectrometric methods at the 0.15 ‰ level. Similar results were obtained for a multiple isotope system like Mg (24Mg, 25Mg, and 26Mg), where isotope shifts of their isotopologues can be resolved in the MgF molecule for the electronic transition X 2Σ → A 2 Πi. The extension of this methodology to other elements like Li, Ca, Cu, and Sr is discussed. T2 - 13. Symposium „Massenspektrometrische Verfahren der Elementspurenanalyse“ zusammen mit dem 26. ICPMS-Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Isotope KW - HR-CS-MAS KW - Isotopic shift KW - Spectrometry KW - Boron monohydride KW - Magnesium monofluoride KW - Molecular absorption spectrometry PY - 2018 AN - OPUS4-45868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Muench, S. A1 - Okruss, M. A1 - Mao, X. A1 - Gonzalez, J. A1 - Zorba, V. A1 - Recknagel, Sebastian A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Stable isotope analysis of magnesium by optical spectrometry N2 - Magnesium is a naturally occurring element that can be found in several mineral forms in the earth crust. This element presents three stable isotopes 24Mg, 25Mg and 26Mg with a natural abundance of 79%, 10%, and 11% respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight isotope amount ratio variations n(26Mg)/n(24Mg) in biological and geological samples. Traditionally, isotope amount ratios have been measured by mass spectrometric methods. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time-consuming. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi and X 2Σ → B 2Σ+ around wavelengths 358 nm and 268 nm respectively. In the case of LAMIS, it was studied the MgF molecule for the electronic transitions A 2Πi → X 2Σ as well as the MgO molecule for the electronic transition A 1Π+ → X 1Σ around 500 nm. The MgF and MgO spectra are composed by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by a partial least square regression (PLS) calibrated with enriched isotope spikes. The isotope amount ratios in rock samples with and without matrix separation were analyzed. Resulting delta values were obtained with precisions ranging between 0.2-0.5 ‰. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared with MC-ICP-MS. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Isotope analysis KW - HR-CS-MAS KW - LIBS KW - MC-ICP-MS KW - Magnesium PY - 2019 AN - OPUS4-49876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Muench, S. A1 - Okruss, M. A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Chemometric analysis of High resolution spectra for precise and accurate isotope amount ratio determination N2 - Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope amount ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, an optical spectrometric method has been proposed as faster and low-cost alternative for the analysis of isotope ratios: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). For the determination of Mg isotope ratios in selected rock reference materials, the high-resolution molecular absorption spectrum of in-situ generated MgF molecule was studied applying multivariate analysis and the results compared with MC-ICP-MS. Samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectra were recorded for MgF for the electronic transition X 2Σ → B 2Σ+. The MgF spectrum is described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS). A PLS model was built and calibrated with enriched isotope spikes and certified reference materials. Spectra data was preprocessed by a derivate of second order and venetian blinds cross-validation was employed for finding the optimum latent variables. Finally, the model was refined by a genetic algorithm which identified the best subset of variables for a precise and accurate regression. Results are compatible with those obtained by MC-ICP-MS with an accuracy of ± 0.3‰ with uncertainties ranging between 0.02 to 0.6‰. T2 - Colloquium Analytische Atomspektroskopie CANAS 2019 CY - Freiberg, Germany DA - 23.09.2019 KW - Isotope analysis KW - Chemometric KW - Multivariate analysis KW - HR-CS-MAS KW - Molecular spectrum KW - Magnesium PY - 2019 AN - OPUS4-49878 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Muench, S. A1 - Okruss, M. A1 - Mao, X. A1 - Zorba, V. A1 - Recknagel, Sebastian A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - A comparative analysis of optical spectrometry methods and MC-ICP-MS for stable isotope analysis of magnesium in geological samples N2 - Society for Applied Spectroscopy (SAS) Atomic Section Student Award. Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS), and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope ratios in selected rock reference materials, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied and their results compared with MC-ICP-MS. By HR-CS-MAS, samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi, and X 2Σ → B 2Σ+. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A 2Πi → X 2Σ, as well as direct analysis by the MgO molecule for the electronic transition A 1Π+ → X 1Σ. The MgF and MgO spectra are described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Results were accurate with precisions ranging between 0.2 ‰ and 0.8 ‰ (2 SD, n= 10) for HR-CS-GFMAS. No statistically significant differences were observed for samples w/o matrix extraction. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of direct analysis, however the precision is lower due the lack of solid isotopic calibration standards. T2 - SciX 2019. 46th Annual North American Meeting of the Federation of Analytical Chemistry and Spectroscopy Societies (FACSS) CY - Palm Springs, CA, USA DA - 13.10.2019 KW - Isotope analysis KW - Diatomic molecule KW - Magnesium KW - MC-ICP-MS KW - HR-CS-MAS KW - LIBS PY - 2019 AN - OPUS4-49883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Muench, S. A1 - Okruss, M. A1 - Mao, X. A1 - Gonzalez, J. A1 - Zorba, V. A1 - Recknagel, Sebastian A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Critical evaluation of optical spectrometry vs mass spectrometry for stable isotope analysis N2 - Mass spectrometric Methods MC-ICP-MS and TIMS) are without doubt the working horse of stable isotope analysis. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time consuming. Optical spectrometric methods are proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) and laser ablation molecular isotopic spectrometry (LAMIS). First, stable isotope amount compositions of boron (B) and magnesium (Mg) were determined based on the absorption spectra of in-situ generated heteronuclear diatomic molecules (MH or MX) in graphite furnace HR-CS-MAS. The use of a modular simultaneous echelle spectrograph (MOSES) helps to find the maximal isotope shift in the diatomic molecular spectra produced in a graphite furnace by using isotopic spike solutions. Isotopes of boron (10B and 11B) were studied via their hydrides for the electronic transition X 1Σ+ → A 1Π. The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, the isotopic composition of samples can be calculated by a partial least square regression (PLS). For this, a spectral library was built by using samples and spikes with known isotope composition. Boron isotope ratios measured by HR-CS-MAS are identical with those measured by mass spectrometric methods at the 0.15 ‰ level. Similar results were obtained for a multiple isotope system like Mg (24Mg, 25Mg, and 26Mg), where isotope shifts of their isotopologues can be resolved in the MgF molecule for the electronic transition X 2Σ → A 2 Πi. Finally, the application of molecular spectrometry via emission by LAMIS is compared and discussed. T2 - European Winter Conference on Plasma Spectrochemistry EWCPS 2019 CY - Pau, France DA - 03.02.2019 KW - Isotope analysis KW - HR-CS-MAS KW - LIBS KW - MS-ICP-MS KW - Optical spectroscopy KW - Mass spectrometry PY - 2019 AN - OPUS4-49874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Recknagel, Sebastian A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Following fluorinated drugs by molecular absorption spectrometry – from cancer cells to body fluids N2 - Fluorine has been widely introduced into pharmaceutical drugs. Due to the high C-F bond strength, a single atom substitution with fluorine produces drastic desirable and tunable changes in the molecular properties. However, the clinical monitoring of these drugs is not straightforward. Organofluorine compounds are elusive for a non-targeted analysis; a significant problem in fluorine determination is the lack of suitable detection techniques. Standard atomic absorption and emission spectrometers cannot access fluorine, because their resonance lines lie in the VUV spectral range below 100 nm. In the case of conventional inductively coupled argon plasmas (ICP), the plasma energy is too low to generate a significant population of excited fluorine atoms. Recently, our group introduces high-resolution continuum source absorption spectrometry (HR-CS MAS) as a new way for the indirect monitoring of fluorinated compounds. Main benefits of HR-CS-MAS includes low limits of detection, complete analyte recovery, simple to no sample preparation, and short time analysis. T2 - 16th Annual Congress of International Drug Discovery Science and Technology 2018 CY - Cambridge, MA, USA DA - 16.08.2018 KW - Fluorine KW - Anti-cancer KW - Capecitabine KW - Fluorouracil KW - HR-CS-MAS PY - 2018 AN - OPUS4-45822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Stable isotope amount ratio analysis by using high-resolution continuum source molecular absorption spectrometry N2 - Analysis of stable isotopes has been used as proof of provenance of mineral and biological samples, to estimate a contamination source and to determine geological processes. This kind of analysis needs high accuracy and precision for reliable conclusions. Currently, stable isotope analysis is dominated by mass spectrometric techniques that are time consuming and expensive. Here we present a fast and low cost alternative for isotope analysis of boron and magnesium: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Two stable isotope systems were evaluated separately: boron (10B:11B) and magnesium 24Mg:25Mg:26Mg). Their isotope amount ratios were estimated by monitoring their absorption spectra in-situ generated monohydrides. The molecular absorption spectrum of a XH molecule (X= B or Mg) with n isotopes would be a linear combination of n isotopologue spectra and the amount of each component (isotope) could be calculated by a multivariate regression (n= 2 and 3 for B and Mg respectively). For the Analysis of boron certified reference materials (CRM), the band 1→1 for the electronic transition X1Σ+ → A1Π was measured around wavelength 437.1 nm. Since boron has a Memory effect in graphite furnaces, a combination of 2 % (v/v) hydrogen gas in argon, 1 % trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers were used during the BH vaporization at 2600 °C. Partial least square regression (PLS) for analysis of samples was applied. For this, a spectral library with different isotope ratios for PLS regression was created. Magnesium does not have memory effect. Therefore, only 2 % of hydrogen in argon as gas modifier during vaporization at 2500 °C was employed for analysis of magnesium CRM. Absorption spectra of MgH for the X2Σ→A2Π electronic transition (band 0→0) were recorded around wavelength 513.45 nm. A similar PLS procedure to the BH was applied. Results for B and Mg CRM are metrologically compatible with those reported by mass spectrometric methods. An accuracy of 0.08 ‰ for B and 0.1 ‰ Mg was obtained as the average deviation from the isotope CRM. Expanded uncertainties with a coverage factor of k = 2 range between 0.10 - 0.40 ‰. T2 - SAS meeting FACSS / SciX Conference 2017 CY - Reno, NV, USA DA - 08.10.2017 KW - Boron isotopes KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - Graphite furnace KW - Molecular absorption PY - 2017 AN - OPUS4-43528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Mao-Dong, H. A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Determination of isotope ratios by molecular absorption spectrometry N2 - Boron and Magnesium present two and three stable isotopes respectevely. It is due to their relatively large mass difference (~ 10%) that isotope fractionation leads to considerable isotope amount ratio variations in the nature. These have been used as a proof of provenance of mineral and biological samples, to estimate a contamination source and to the determination of geological processes by erosion or subduction. Additionally, boron is employed in the nuclear industry due to the capability of its isotope 10B to thermal-neutron capture and therefore 10B enriched boric acid solutions are used in the cooling system of thermonuclear facilities and in the alloying of steel and carbides for protective shielding. Traditionally, isotope ratio variations have been determined by mass spectroscopic methods. Here an alternative faster and low cost method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Isotope amount ratios have been determined by monitoring the absorption spectrum of boron monohydride (BH) for boron and Magnesium monofluoride (MgF) for magnesium in a graphite furnace HR-CS-MAS. Bands (0→0) and (1→1) were evaluated. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained are metrologically compatible with those reported by mass spectrometric methods. Moreover, a precision and accuracy of the method of ± 0.5 ‰. This accuracy and precision is comparable with those obtained by thermal ionization mass spectrometry (TIMS) and multiple collector inductively coupled plasma mass spectrometry (MC-ICP-MS) for boron isotope ratio measurements T2 - Analytik Jena Days CY - Idstein, Germany DA - 26.06.2019 KW - Isotope anaylsis KW - HR-CS-MAS KW - Boron KW - Magnesium KW - Optical spectroscopy KW - Diatomic molecule PY - 2019 AN - OPUS4-49877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Tatzel, Michael A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Stable isotope analysis of magnesium by optical spectrometry N2 - Magnesium (Mg) is a major element in a range of silicate and carbonate minerals, the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg with natural abundances of 79 %, 10 %, and 11 %, respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight variations of isotope amount ratios n(26Mg)/n(24Mg) in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods and isotope ratios are expressed as deviation from an internationally agreed upon material, i.e. the zero-point of the δ-value scale. Drawbacks of this method include the high costs for instruments and their operation, experienced operators and elaborate, time-consuming chromatographic sample preparation. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high- resolution continuum source graphite furnace molecular absorption spectrometry (HR- CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X2Σ → A2Πi and X 2Σ → B2Σ+ around wavelengths 358 nm and 268 nm, respectively. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A2Πi → X2Σ as well as the MgO molecule for the electronic transition A1Π+ → X1Σ around 500 nm. The MgF and MgO spectra are described by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Isotope amount ratios in rock samples with and without matrix separation were analyzed. Calculated δ-values were accurate and obtained with precisions ranging between 0.2 ‰ and 0.5 ‰ (1 SD, n = 10). On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared to MC-ICP-MS. T2 - Seminars Earth Surface Geochemistry- Deutsches GeoForschungsZentrum GFZ CY - Potsdam, Germany DA - 06.08.2019 KW - Isotope analysis KW - Magnesium KW - HR-CS-MAS KW - LIBS KW - Diatomic KW - Optical spectroscopy PY - 2019 AN - OPUS4-49904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Chapartegui, Ander A1 - Péter, G. T1 - Alcoholism clinical biomarkers and mass spectrometry N2 - Heavy alcohol induces several chronic diseases, including cirrhosis. Consequently, cirrhotic patients need liver transplantation. However, alcoholic patients are not suitable for this. How can be physicians sure of non-alcohol consumption of a potential organ receptor? Monitoring of biomarkers by mass spectrometric techniques is today the most suitable option. This subject was discussed at the Graduate School of Analytical Science Adlershof (SALSA) in Berlin, as a part of a lecture series in analytical science. T2 - Analytical Challenges - School of Analytical Sciences Adlershof CY - Berlin, Germany DA - 12.12.2017 KW - Alcoholism KW - Biomarkers KW - Mass spectrometry KW - Transferrin PY - 2017 AN - OPUS4-43535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abdelshafi, Nahla A. A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Electrochemical Immunosensor for Drug Monitoring T2 - 11th Internatinal Biosensor Conference BBMEC T2 - 11th Internatinal Biosensor Conference BBMEC CY - Regensburg DA - 2015-09-26 PY - 2015 AN - OPUS4-34509 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abderrazak, H. A1 - Marestin, C. A1 - Ibtissem, J. A1 - Mercier, R. A1 - Casablanca, H. A1 - Souissi, R. A1 - Weidner, Steffen A1 - Jaffrezic, N. A1 - Chatti, Saber T1 - Synthesis of new bio based adsorbent phases N2 - Over the years, industrial and human activities and agricultural practices have caused a serious threat to human health and the environment. Indeed, it has been demonstrated that these activities are responsible for the presence of pollutants in the soil, air and water. Water is one of the most strategic issues today, as it is associated with the living world. Therefore, water pollution is becoming a universal scourge that leads to environmental degradation, decrease of water quality and threatens public health. Water pollution is mainly due to the discharge of certain harmful chemical compounds that are not very or not at all biodegradable (phenolic compounds, heavy metals, hydrocarbons, dyes, pesticides, etc.) by various industries: chemical, pharmaceutical, textile, food processing, etc. The impact of these industrial effluents on fauna and flora is very harmful. A sensitization of the socio-economic actors and the public, accompanied by a severe regulation in relation to the discharges, would contribute to fight against this drift, but also, by the development of effective methods allowing to remove these pollutants, not only in an analytical purpose but also of depollution. Thus and within the framework of the preservation of an environment with regard to any anthropogenic activity, our research topic relates to the use of original biosourced polymeric phases for the extraction of the organic compounds and the heavy metals in aqueous mediums. Therefore, we have proceeded to the synthesis and characterization of a large variety of monomers, polymers and cross-linked materials. These products, partially derived from biomass, contain various functional groups with the ability to interact with chemical components without discriminating effect. The developed polymer phases have been successfully used for the adsorption of some organic pollutants and heavy metals in synthetic aqueous solutions. T2 - 12. Journees maghreb-europe. Matériaux et Applications aux Dispositifs et Capteurs CY - Monastir, Tunisia DA - 08.11.2022 KW - Organic-inorganic adsorbents KW - Semi-Interpenetrating Network KW - Poly(ether-sulfone) KW - Reversible adsorption. PY - 2022 AN - OPUS4-56286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abel, Andreas A1 - Zapala, P. A1 - Michels, H. A1 - Skrotzki, Birgit T1 - Microstructure-Property-Correlation of a Mo-Ti-B alloyed iron aluminide N2 - Iron aluminides depict a sustainable and light-weight material class which could be employed in many applications requiring high strength at intermediate to high temperatures. According to first results, the alloy Fe-26Al-4Mo-0.5Ti-1B surpasses conventional materials in wet corrosion resistance and creep resistance up to 650 °C. For these reasons, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated to transfer these findings into a standardised materials dataset and to derive best practices for processing. In the first place, a set of different microstructures adjusted by varying casting methods, wall thicknesses and heat treatments was investigated and correlated with hardness on macro and micro scale. Correlations were drawn between solidification rates and resulting grain sizes and hardness. The effect of vacancy hardening was only verified for wall thickness as low as 2.5 mm. Moreover, a common decrease of macrohardness after a heat treatment at 1000 °C for 100 h was observed irrespective of casting process or wall thickness. This effect was linked with an unexpected decrease of the complex boride phase fraction which acts as a hardening phase. T2 - Intermetallics 2021 CY - Bad Staffelstein, Germany DA - 04.10.2021 KW - Fe-Al alloys KW - Intermetallics KW - Iron aluminides KW - Heat treatment KW - Wall thickness KW - Centrifugal casting KW - Die casting KW - Investment casting KW - Microstructure KW - Hardness KW - Complex borides PY - 2021 AN - OPUS4-53617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abel, Andreas A1 - Zapala, P. A1 - Michels, H. A1 - Skrotzki, Birgit T1 - Ambient and high-temperature mechanical properties of intermetallic Fe3Al alloys with complex borides N2 - Due to the increasing scarcity of critical raw materials current high-temperature materials are sought to be replaced by alloys based on more abundant metals. One possibility within the class of intermetallics are iron aluminides, which combine sustainability and cost-efficiency with the prospect of mass savings. Iron aluminides show competitive specific strength up to 700 °C and excellent creep and wet corrosion resistance by small additions of Mo, Ti and B. Nevertheless, a Mo content of above 2 at.% which is needed for optimum corrosion resistance results in enhanced brittleness, especially at room temperature. This is why alloys with these Mo fractions were only mechanically tested under compressive loading so far. Still, testing of static and creep properties under tensile loading is required for reliable component design. Besides high standards for crack-free processing, data acquisition for tensile loads is especially complicated by environmental embrittling effects for iron aluminides. To cope with these challenges, the AiF research project “WAFEAL – Materials applications for iron aluminides” was initiated. The main goal is to collect standardised data on ambient and high-temperature tensile properties and creep properties. Samples with a nominal composition of Fe-26Al-4Mo-0.5Ti-1B [at.%] were manufactured via centrifugal casting in ceramic shell moulds followed by machining. Heat treatment for homogenisation and final polishing were carried out where appropriate. A summary of the achieved tensile and creep properties such as yield and tensile strength, maximum elongation, secondary creep rate and stress exponents will be given. Results will be also discussed regarding the influence of temperature, stress level and microstructure on the damage mechanisms. Furthermore, the effect of different alloy concentrations on the mechanical response at different temperatures will be outlined within a small experimental series. T2 - MSE Congress 2022 CY - Darmstadt, Germany DA - 27.09.2022 KW - Fe-Al alloys KW - Intermetallics KW - Iron aluminides KW - Tensile data KW - High temperature mechanical properties KW - Creep data KW - Fractography PY - 2022 AN - OPUS4-55993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abel, Andreas A1 - Zapala, P. A1 - Michels, H. A1 - Skrotzki, Birgit T1 - Microstructural evolution of Fe-26Al-4Mo-0.5Ti-1B with varying wall thicknesses N2 - With an increasing demand in more efficient fuel consumption to reduce CO2 emissions, weight reductions in high-temperature materials at affordable costs gain increasing attention. One potential candidate is the intermetallic material class of iron aluminides, combining the advantages in mass savings, high temperature performance and recyclability of resources. The alloy Fe-26Al-4Mo-0.5Ti-1B was selected to study the microstructural features evolving from two casting processes, five wall thicknesses and three final conditions. Conclusions are drawn upon the correlations of processing variables, grain sizes and hardness. T2 - DGM Fachausschuss "Intermetallische Phasen" CY - Online meeting DA - 09.02.2021 KW - Intermetallics KW - Iron aluminides KW - Fe-Al alloys KW - Wall thickness KW - Microstructure PY - 2021 AN - OPUS4-52288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abel, Andreas A1 - Zapala, P. A1 - Skrotzki, Birgit T1 - Materials Applications FeAl (WAFEAL) N2 - The increasing importance of resource availability and closed-loop material cycles are driving materials research to reduce alloying content in conventional materials or even substitute them with more sustainable alternatives. Intermetallic iron aluminide alloys (FeAl) present a potential alternative. Many alloy concepts for improved high-temperature properties or ductility have already been successfully implemented in casting technologies on a laboratory scale. However, successful testing of FeAl alloys on an industrial scale was still pending at the beginning of the project. Therefore, the aim of the project was to develop simulation-based casting concepts for industrial casting processes using the base alloy Fe-26Al-4Mo-0.5Ti-1B and to narrow down process limits by means of hot cracking tests. Findings were transferred into practice-oriented guidelines for casting of iron aluminides, which is accessible to future applicants in SMEs. The focus was placed on centrifugal casting combined with investment casting or die casting. In addition to numerous design and casting process parameters, heat treatments and alloying additions (Al, Mo, B) were varied to determine the influence of alloying elements on castability, microstructure and mechanical properties. Data from microstructure analyses (microscopic imaging, determination of grain sizes as well as phase compositions and volume fractions, fractography), mechanical tests (hardness measurements, compression tests, ambient and high-temperature tensile tests, creep tests) as well as measurements of thermophysical properties could be generated on the base alloy. Correlations of materials data with process variables allowed conclusions to be drawn on strengthening mechanisms and ductility of the alloy and how they can be controlled in terms of processing and component design. Successful casting of highly complex components with thin wall thicknesses and optimised alloy compositions points out prospects for new fields of application. T2 - FVV Transfer + Netzwerktreffen | Informationstagung – Frühjahr 2023 CY - Würzburg, Germany DA - 29.03.2023 KW - Fe-Al alloys KW - Intermetallics KW - Iron aluminides KW - Microstructure-property-correlation KW - High temperature mechanical properties KW - Creep data KW - Tensile data KW - Fractography KW - Casting PY - 2023 AN - OPUS4-57248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abele, M. A1 - Kern, Simon A1 - Maiwald, Michael A1 - Falkenstein, S. A1 - Meyer, Klas A1 - Friedrich, Y. A1 - Korth, K. T1 - Industrielle Anwendungen der Niederfeld-NMR-Spektroskopie für die Prozess- und Qualitätskontrolle von Silanen N2 - Trialkoxysilane haben sich in den vergangenen Jahren als vielseitig einsetzbare Organosilane erwiesen. Die Einsatzgebiete erstrecken sich vom Witterungsschutz von Bauwerken über haftvermittelnde Eigenschaften in der Glasfaserindustrie, bei Dicht- und Klebstoffen, in Farben und Lacken bis hin zur Modifizierung von polymeren Werkstoffen. Kommerzielle Benchtop-NMR-Spektrometer haben das Potential auch im Bereich der Silanchemie als Online-Methode zur Reaktionsüberwachung und für die Qualitätskontrolle eingesetzt zu werden. Interessante NMR-Kerne für die oben genanntem Produkte sind 1H und 29Si. In einer gemeinsamen Forschungskooperation zwischen EVONIK und BAM wurde anhand verschiedener Fallstudien die Anwendbarkeit der Niederfeld-NMR-Spektroskopie zur chemischen Analyse von Silanen evaluiert. Im Zuge der Fallstudien wurde gezeigt, wie Niederfeld-NMR-Spektroskopie die Möglichkeiten der Konzentrationsmessung auf neue Anwendungsgebiete erweitert, in denen bestehende Technologien wie z. B. NIR, Raman, UV/VIS, etc. mangels Referenzdaten nicht quantitativ eingesetzt werden können. Fallstudie 1: Oligomerisierung Eine Fallstudie setzte dazu an, den Hydrolyse- und Kondensationsverlauf mit einer geeigneten Online-NMR-Analytik zu beobachten, den Reaktionsfortschritt der Hydrolyse und Kondensation auf dieser Basis besser zu verstehen und zu optimieren. Zu diesem Zweck werden durch Zugabe von Wasser zunächst die Alkoxysubstituenten eines Trialkoxysilans hydrolysiert und entsprechende Silanole gebildet. Diese können dann über eine SiOH-Funktion an den zu modifizierenden Werkstoff anbinden und über weitere Silanolgruppen unter Ausbildung von Siloxaneinheiten vernetzen. Fallstudie 2: Spaltung von cyclischen Silanverbindungen In einer weiteren Fallstudie wurde die Kinetik der Aufspaltungen einer cyclischen Silanverbindung untersucht. Die Online-NMR-Analytik kam hierbei sowohl im Labor als auch in der industriellen Produktionsanlage zum Einsatz. Hierfür wurde eine vollständig automatisierte Einhausung verwendet, welche den Einsatz eines kommerziellen NMR-Spektrometers in explosionsgeschützten Bereichen ermöglicht. Fallstudie 3: Qualitätskontrolle für Produktmischungen von Trialkoxysilanen Für Produktmischungen eines Trialkoxysilans und weiteren Bestandteilen wie u. a. org. Stabilisatoren, Organozinnverbindungen, eines aromatischen Amins und org. Peroxide wurden quantitative 1H-Spektren akquiriert und eine automatische Auswertungsmethode basierend auf Indirect Hard Modeling (IHM) entwickelt. Für die Nebenkomponenten, deren Stoffmengenanteile bis zu 3 Mol-% betragen, wurden durch die zugrunde gelegte Methode typischerweise korrekte experimentelle Stoffmengenanteile gefunden, die weniger als 0,2 Mol-% vom Referenzwert abweichen. T2 - 15. Kolloquium Arbeitskreis Prozessanalytik CY - Marl, Germany DA - 25.11.2019 KW - Prozessanalytik KW - Qualitätskontrolle KW - Silane KW - Online-NMR-Spektroskopie KW - Trialkoxysilane PY - 2019 AN - OPUS4-49825 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abraham, O. A1 - Niederleithinger, Ernst A1 - Schmidt, F. A1 - Dalsgaard-Soerensen, J. A1 - Thoens, S. A1 - Chapeleau, X. A1 - Ferria, H. T1 - Infrastar Training School on Fatigue and Reliability Analysis of Structures - Training for Assessment of Risk N2 - The Infrastar training school provides lectures and hands-on training to Master and PhD students, early-stage researchers and (young) professionals on all aspects of asset management of civil infrastructures with respect to fatigue of materials. It is organized yearly since 2019 and up to 20 profiles are selected to attend the 3.5-day training. A team of 7 teachers provides insight in multi-disciplinary and intersectoral basic concepts in three core fields, ranging from the design to the dismantling of the structures (bridges and wind turbines): 1. Monitoring and auscultation, 2. Structural and action models, 3. Reliability, risk and decision analyses. Each year, a recognized expert is invited to deliver a keynote lecture to raise interest in a specific aspect of one of the fields covered. The presentation is recorded and published on the training school website. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Doctoral School KW - Fatigue KW - Reliability KW - Concrete PY - 2022 AN - OPUS4-56349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abraham, O. A1 - Niederleithinger, Ernst A1 - Chapeleau, B. A1 - Klikowicz, P. A1 - Brühwiler, E. A1 - Bassil, A. A1 - Wang, Xin A1 - Chakraborty, J. A1 - Bayane, I. A1 - Leduc, D. A1 - Salamak, M. A1 - Katunin, A. A1 - Sörensen, J. D. T1 - Addressing the need to monitor concrete fatigue with non destructive testing: preliminary results of infrastar European project N2 - Fatigue is one of the most prevalent issues, which directly influences the service life expectancy of concrete structures. Fatigue has been investigated for years for steel structures. However, recent findings suggest that concrete structures may also be significantly subjected to the fatigue phenomena that could lead to premature failure of certainfatigue prone structural elements. To date, fatigue of reinforced concrete has been given little focus. and Kknowledge on the influence factors and durability/capacity effects on this material should be improved. Current technological means to measure fatigue in civil structures like bridges and wind turbines (both onshore and offshore) are outdated, imprecise and inappropriate. Meanwhile, this topic has got much more attention as dynamic loading on concrete structures plays an increasing role, e.g. in bridges with increasing traffic and heavier trucks, in wind energy production due to inherent vibrations e.g. in offshore wind turbine support structures affected by wind and waves. The European Innovative Training Networks (ITN) Marie Skłodowska-Curie Actions project INFRASTAR (Innovation and Networking for Fatigue and Reliability Analysis of Structures - Training for Assessment of Risk) provides research training for 12 PhD students. The project aims to improve knowledge for optimizing the design of new structures as well as for more realistic verification of structural safety and more accurate prediction of the remaining fatigue lifetime of existing structures. First, the INFRASTAR research framework is detailed. Then it will be exemplified through the presentation of the major results of the four PhD students involved in the work package dealing with auscultation and monitoring. This includes the development and improvement of Fiber Optics (FO) and Coda Wave Interferometry (CWI) for crack sizing and imagery, new sensor technologies and integration, information management, monitoring strategy for fatigue damage investigation and lifetime prediction. T2 - ASNT SMT/NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 27.8.2018 KW - Concrete KW - Fatigue KW - Non-destructive testing KW - Reliabiilty PY - 2018 AN - OPUS4-45862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abram, Sarah-Luise A1 - Mrkwitschka, Paul A1 - Prinz, Carsten A1 - Rühle, Bastian A1 - Kuchenbecker, Petra A1 - Hodoroaba, Vasile-Dan A1 - Resch-Genger, Ute T1 - Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements N2 - In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles. The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum. 1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties. 2. Iron oxide nanoparticles are under development as new candidate reference material at BAM. 3. Narrow particle size distribution confirmed by light scattering and electron microscopy. T2 - Nanosafety 2020 CY - Online meeting DA - 05.10.2020 KW - Iron oxide nanoparticles KW - Reference material KW - Particle size KW - Electron microscopy KW - Nanoplattform PY - 2020 AN - OPUS4-52774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Acikalin, Hatice Aydan T1 - Schutzkonzepte I - Grundlagen zur sicheren Durchführung chemischer Reaktionen T2 - DECHEMA-Weiterbidlungskurs "Sicherheit chemischer Reaktionen" T2 - DECHEMA-Weiterbidlungskurs "Sicherheit chemischer Reaktionen" CY - Berlin, Germany DA - 2012-03-26 PY - 2012 AN - OPUS4-25642 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Acikalin, Hatice Aydan T1 - Schutzkonzepte II - Druckentlastung und Rückhaltung von gefährlichen Stoffen aus Druckentlastungseinrichtungen T2 - DECHEMA-Weiterbildungskurs "Sicherheit chemischer Reaktionen" T2 - DECHEMA-Weiterbildungskurs "Sicherheit chemischer Reaktionen" CY - Berlin, Germany DA - 2012-03-26 PY - 2012 AN - OPUS4-25643 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Acikalin, Hatice Aydan A1 - Schalau, Bernd T1 - Quantitative Risikoanalyse - Grundlagen und Vorgehensweise der BAM T2 - Fortbildungslehrgagn des LANUV "Gefahren- und Risikoanalyse" T2 - Fortbildungslehrgagn des LANUV "Gefahren- und Risikoanalyse" CY - Essen, Germany DA - 2011-05-04 PY - 2011 AN - OPUS4-24474 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Acikalin, Hatice Aydan A1 - Schalau, Bernd A1 - Drewitz, Yvonne T1 - Quantitiative Risk analysis in the Process Industries: Methodology of BAM and Case Studies T2 - 8th European Congress of Chemical Engineering T2 - 8th European Congress of Chemical Engineering CY - Berlin, Germany DA - 2011-09-25 PY - 2011 AN - OPUS4-24475 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Acikalin, Hatice Aydan T1 - Schutzkonzepte I - Grundlagen zur sicheren Durchführung chemischer Reaktionen T2 - DECHEMA-Weiterbildung "Sicherheit chemischer Reaktionen" T2 - DECHEMA-Weiterbildung "Sicherheit chemischer Reaktionen" CY - Berlin, Germany DA - 2011-03-28 PY - 2011 AN - OPUS4-24739 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Acikalin, Hatice Aydan T1 - Schutzkonzepte II Druckentlastung und Rückhaltung von gefährlichen Stoffen aus Druckentlastungseinrichtungen T2 - DECHEMA-Weiterbildungskurs "Sicherheit chemischer Reaktionen" T2 - DECHEMA-Weiterbildungskurs "Sicherheit chemischer Reaktionen" CY - Berlin, Germany DA - 2011-03-28 PY - 2011 AN - OPUS4-24740 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Acikalin, Hatice Aydan T1 - Praktische Erfahrungen zur Bewertung der Leistungsfähigkeit von Sicherheitsmanagementsystemen T2 - 18. Fachgespräch Anlagensicherheit 2009 T2 - 18. Fachgespräch Anlagensicherheit 2009 CY - Bad Dürkheim, Germany DA - 2009-04-21 PY - 2009 AN - OPUS4-19233 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Acikalin, Hatice Aydan T1 - Managementsystem-Standards und -Normen für Anlagensicherheit - Aussagen des Leitfadens SFK-GS-31 und Anhangs III der Störfallverordnung T2 - ProcessNet Arbeitsausschuss "Risikomanagement" T2 - ProcessNet Arbeitsausschuss "Risikomanagement" CY - Frankfurt am Main, Germany DA - 2009-11-03 PY - 2009 AN - OPUS4-20245 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -