TY - CONF A1 - Gornushkin, Igor B. T1 - Plasma Fundamentals and Diagnostics N2 - This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures, thermodynamic properties, and electron number density). Particular emphasis will be placed on inductively coupled plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, micro reactions, pump and probe diagnostics, tomography, temporal and spatial resolution. Basis of plasma computer modeling will be presented. T2 - 2024 Winter Conference on Plasma Spectrochemistry CY - Tucson, Arizona, USA DA - 15.01.2024 KW - Plasma KW - Plasma fundamentals KW - Plasma diagnostics PY - 2024 AN - OPUS4-59430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döring, Sarah T1 - Optimization of surface-functionalized particles for improved antibody digestion N2 - Therapeutic monoclonal antibodies are the fastest-growing group of biological agents which generated a yearly turnover of USD 210 billion in 2022 and whose sales are expected to grow by 10% annually over the next 10 years. With steadily increasing market importance, analytical methods for reliable quantification of therapeutic antibodies also become more and more relevant. Liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) has become the main technology for antibody quantification. This approach, however, requires enzymatic digestion of the intact protein into peptides, for which a wide range of different protocols exists that often lead to different results depending on the digestion procedure or trypsin variants used. In particular, the amount and type of detergents added for protein unfolding prior to digestion is known to create significant bias in measurement results. The overall goal of the presented project is the application of novel thermostable and surface-functionalized trypsin particles for improved antibody digestion. Specifically, a trypsin-variant described in the literature exhibiting increased activity and thermal stability above 80°C, will be examined. The application of this enzyme should allow to perform digestion at elevated temperatures where the protein is naturally unfolding thereby increasing enzyme accessibility without the need for detergents. Furthermore, we will immobilize the thermostable trypsin onto the surface to further enhance enzyme stability, prevent self-digestion, and enable separation of trypsin from target peptides before LC–MS/MS analysis. As an immobilization platform, cheap and non-porous corundum particles will be used as these show high chemical stability and low levels of interaction of matrix proteins with the functionalized surface. adsorption. In a multidisciplinary collaboration with the SALSA Photonics Lab, we will investigate the characteristics of covalent enzyme binding and unspecific peptide binding using an interface-sensitive analytical tool, vibrational sum-frequency generation (VSFG) spectroscopy. The insights gained will not only lead to new competencies in peptide and enzyme surface analysis using VSFG spectroscopy in SALSA but will also significantly contribute to optimizing antibody quantification. T2 - SALSA STF24 Kick-Off Meeting CY - Berlin, Germany DA - 11.04.2024 KW - Antibody Quantification KW - Vibrational Sum-Frequency Generation Spectroscopy KW - LC-MS/MS KW - Enzyme Immobilisation KW - Corundum PY - 2024 AN - OPUS4-59864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blotevogel, J. T1 - Thermal Destruction of PFAS N2 - Thermal treatment processes are currently the only full-scale option for thedestruction of per- and polyfluoroalkyl substances (PFAS) in large waste streams. While all organic molecules including PFAS are susceptible to thermal destruction, their decomposition rates are controlled by process variables such as temperature, reaction atmosphere, and residence time. Concerns exist about the formation of products of incomplete destruction and their emission from hazardous waste incinerators. This talk will summarize the current stateof-the-art of thermal PFAS destruction, identify research needs, and showcase future research designed to address critical knowledge gaps. T2 - Department of Defense's (DoD) Energy and Environment Innovation Symposium CY - Washington DC, USA DA - 28.11.2023 KW - Thermal treatment KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2023 AN - OPUS4-58974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - HR-CS-GFMAS a new screening tool for per- and polyfluoroalkyl substances (PFAS) in the environment N2 - Per- and polyfluorinated alkyl substances (PFASs) are a large group of anthropogenic contaminates. Concerning are especially their persistent, bioaccumulative and toxic properties. Mostly, target-based approaches (e.g., LC-MS/MS) are utilized for the analysis of PFASs in the environment. But these approaches are limited to the availability of analytical grade standards and therefore drastically underestimate the total PFAS burden. Analytical approaches based on total fluorine for PFAS sum parameter analysis become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. Besides combustion ion chromatography (CIC), high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification in the low µg F L-1 range. Here, we present a comparison of total fluorine analysis methods – AOF vs. EOF and HR-CS-GFMAS vs. CIC. Therefore, surface water samples from the Spree River in Berlin, Germany were analyzed at 10 locations for total fluorine (TF), AOF and EOF. The AOF made up 0.14–0.81% of TF and the EOF 0.04–0.28% of TF while AOF concentrations were systematically higher. For the instrumental comparison, HR-CS-GFMAS was the more sensitive and precise method for fluorine analysis compared to CIC. T2 - ICOBTE / ICHMET 2023 CY - Wuppertal, Germany DA - 06.09.2023 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - WWTP KW - SPE PY - 2023 AN - OPUS4-58245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pramann, A. A1 - Vogl, Jochen A1 - Flierl, L. A1 - Rienitz, O. T1 - Determination of absolute (SI‐traceable) isotope ratios: The use of Gravimetric Isotope Mixtures N2 - The presentation is brief overview on how to use gravimetric isotope mixtures to determine SI traceable isotope ratios. There is no mass spectrometer on earth that directly measures isotope ratios. Mass spectrometers will always measure signal intensity ratios instead. The actual problem is that the measured intensity ratios differ more or less from the isotope ratios. The difference can be up to more than 10 % in case of lithium while it‘s below 1 % in case of the heavier elements like lead or uranium. Consequently, the signal intensity ratios are expressed for example in V/V depending on the type of mass spectrometer you are using, while the isotope ratios are expressed in mol/mol. This phenomenon is called Instrumental Isotopic Fractionation (or short IIF) but the more common name is still mass bias (even though this name is not entirely correct). To convert the measured into the isotope ratio usually a simple multiplication with a so-called correction (or short K) factor is done. Therefore, the problem is to determine the K factor. In absence of isotope reference materials the golden route is via gravimetric isotope mixtures, which will be explained within the presentation. T2 - CCRI-CCQM Workshop on the use of mass spectrometry in radionuclide metrology: Opportunities and challenges - Video Tutorial CY - Online meeting DA - 14.02.2023 KW - Absolute isotope ratio KW - Traceability KW - Uncertainty KW - Isotope mixtures PY - 2023 AN - OPUS4-57172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - Analyse von PFAS mittels (Non-)Target HRMS, dTOPA und EOF in Schwebstoff-Proben aus Zeitreihen der Umweltprobenbank N2 - Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse bestehend aus mehreren tausenden Einzelverbindungen. Unter PFAS zählen alle Verbindungen, die mindestens eine perfluorierte Methyl- (-CF3) oder Methylen-Gruppe (-CF2-) besitzen.[1] Somit zählt auch ein großer Teil der fluorierten Medikamente, Pflanzenschutzmittel oder Biozide in die PFAS-Substanzklasse. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“.[2] Die PFAS-Analytik ist wegen ihrer vielfältigen physikalisch-chemischen Eigenschaften und der sehr hohen Anzahl an PFAS eine große Herausforderung. Da es für viele Anwendungen noch ungewiss ist, welche PFAS verwendet werden, wie sie in die Umwelt gelangen und welche Transformations- bzw. Abbauprodukte entstehen, stoßen analytische Ansätze, die nur auf Einzelsubstanzen abzielen, hier an ihre Grenzen. PFAS-Summenparameter-Methoden, die darauf abzielen ein möglichst vollständiges Abbild der PFAS-Belastungssituation widerzuspiegeln, werden daher immer wichtiger. T2 - Wasser 2023 CY - Augsburg, Germany DA - 14.05.2023 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - SPM KW - Schwebstoffe KW - LC-HRMS PY - 2023 AN - OPUS4-57516 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wittwer, Philipp T1 - Results of ILC Data Treatment N2 - Results of the interlaboratory comparison study for data treatment were presented. They show, that nearly all participants found all the problems in the data. However, only a few corrected the problems, therefore making it one possible point to focus on in the knowledge sharing program. T2 - AGM POLMO Meeting 2024 CY - Paris, France DA - 21.05.2024 KW - JNP POLMO KW - ILC KW - Ringversuch PY - 2024 AN - OPUS4-60166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalgic, Mete-Sungur T1 - Lösemittelfreie Probenpräparation zur Untersuchung von Polymerblends mittels MALDI-TOF MS N2 - Die Probenpräparation ist ein wichtiger Schritt für die Qualität der Massenspektren in MALDI-TOF MS. Es werden Polymerproben, die lösungsmittelbasiert und lösungsmittelfrei präpariert worden sind, verglichen. Dabei werden die Intensitätsverhältnisse von ternären Mischungen von PEG-, PS- und PMMA-Polymeren beachtet. T2 - 28. Kolloquium - Massenspektrometrische Techniken zur Untersuchung synthetischer Polymere CY - Berlin, Germany DA - 14.05.2024 KW - Polymere KW - Massenspektrometrie KW - Probenpräparation PY - 2024 AN - OPUS4-60032 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ronen, A. A1 - Panglisch, S. T1 - Detection, Quantification and Treatment of Per and Polyfluoroalkyl substances (PFAS) in Groundwater N2 - The research project focuses on tackling the detection, measurement, and elimination of per- and polyfluoroalkyl substances (PFAS) from polluted groundwater, with a particular emphasis on addressing short (C4-C7) and ultrashort (C1-C3) chain PFAS. Given the widespread use of PFAS in various products, they are commonly found in groundwater near industrial and military sites in Germany and Israel. Moreover, recent regulations limiting the use of long chain PFAS have led industries to shift towards shorter chain alternatives. Hence, our efforts are geared towards refining detection, quantification, and removal methods for short and ultrashort chain PFAS. In terms of detection, ww are developing passive sampling devices capable of collecting and tracking the temporal distribution of PFAS species in groundwater. This will enable us to analyze contaminations in German and Israeli groundwater using cutting-edge analytical techniques. Additionally, contaminated groundwater will undergo a two-stage treatment process aimed at concentrating the relatively low PFAS concentrations using innovative membrane technologies such as closed-circuit reverse osmosis and mixed matrix composite nanofiltration membrane adsorbers. Subsequently, the streams containing higher PFAS concentrations will be treated through coagulation, with the remaining PFAS being adsorbed onto carbonaceous nanomaterials. The outcome of this research will include the creation of advanced tools for detecting, measuring, and eliminating PFAS from polluted groundwater, while also enhancing our understanding of the scope of these contaminations. T2 - German Israeli Water Technology Status Seminar CY - Koblenz, Germany DA - 18.06.2024 KW - Ground water KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2024 AN - OPUS4-60328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Franz-Georg T1 - Detektion, Quantifizierung und Entfernung von insbesondere ultrakurzkettigen PFAS in Grundwasser N2 - Da PFAS in großem Umfang in einer Vielzahl von Produkten verwendet wurde, sind sie im Grundwasser in der Nähe vieler industrieller und militärischer Anlagen weltweit zu finden. Darüber hinaus führten neue Vorschriften und Beschränkungen für die Verwendung von langkettigen PFAS zu einer vermehrten Produktion kurzkettiger Alternativen. Ultrakurzkettige PFAS (≥C3) können natürliche und anthropogene Barrieren durchdringen und schließlich in Trinkwasserquellen gelangen. Zudem entfernen die meisten gängigen Trinkwasser-aufbereitungsverfahren die ultrakurzkettigen PFAS nicht ausreichend. Im Kooperationsprojekt DEFEAT-PFAS wird daher das Ziel verfolgt, Wissenslücken über Nachweis, Quantifizierung und Entfernung von kurz- (C4-C7) und ultrakurzkettige (C1-C3) PFAS, in kontaminiertem Grundwasser zu schließen. Die israelischen und deutschen Projektpartner entwickeln dafür analytische Methoden and selektive Passivsammler, um das zeitliche Profil von PFAS-Spezies im Grundwasser zu erfassen und überwachen. Darüber hinaus ein zweistufiges Verfahren entwickelt, welches darauf ausgelegt ist, die relativ niedrigen PFAS-Konzentrationen im Grundwasser durch neuartige Membranverfahren, Umkehrosmose im Batchbetrieb mit geschlossenem Kreislauf sowie Verbund-Nanofiltrationsmembranen, zu konzentrieren. Anschließend werden die PFAS angereicherten Konzentrate mittels Koagulation behandelt und das verbleibende PFAS an kohlenstoffhaltigen Nanomaterialien adsorbiert. T2 - Workshop des Netzwerks Perflusan CY - Karlsruhe, Germany DA - 18.06.2024 KW - Grundwasser KW - Per- und Polyfluoroierte Alkylsubstanzen (PFAS) PY - 2024 AN - OPUS4-60334 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalgic, Mete-Sungur T1 - Discrimination effects in MALDI-MS of Ternary Polymer Mixtures N2 - MALDI-TOF MS is a viable method to determine molecular weights of polymers. However, quantification using MALDI-TOF MS presents specific challenges due to intensity biases caused by instrumental and sample-specific parameters. In this presentation, the influence of molar masses on MALDI-TOF mass spectra is explored. The intensities of a ternary PMMA blend with different mixture ratios are depicted in contour plots. T2 - SALSA Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - MALDI-TOF MS KW - Ternary polymer blends KW - PMMA PY - 2022 AN - OPUS4-62212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalgic, Mete-Sungur T1 - Einfluss der Konformation auf das Ionisationsverhalten in MALDI-TOF MS N2 - MALDI-TOF Massenspektrometrie ist eine wichtige Methode zur Bestimmung von Molekulargewichten von Polymeren. Jedoch wird die quantitative Analyse von Polymeren durch verschiedene Faktoren erschwert. In dieser Präsentation wird unter anderem der Einfluss der molaren Massen auf die Massenspektren näher betrachtet. Dabei werden Konturplots von ternären PMMA- und PS-Mischungen gezeigt. T2 - 27. Kolloquium - Massenspetrometrische von Polymeren CY - Berlin, Germany DA - 09.05.2023 KW - MALDI-TOF MS KW - Ternäre Polymermischungen KW - PMMA und PS PY - 2023 AN - OPUS4-62214 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Portesi, Chiara T1 - Metrology for food safety in the circular economy: targeted and screening methods for contaminants in food and recycled packaging N2 - Safeguarding consumers from potential harm caused by food contamination is of paramount importance to ensure food safety. The focus on safety is a central priority for European Commision lawmakers. Furthermore, as outlined in the EU circular economy action plan, the development of a sustainable food system is a critical objective. However, progress towards these goals can sometimes face obstacles, including the risk of eroding consumer confidence in food quality. Factors such as the increased use of recycled and sustainable packaging materials and the growing awareness of emerging contaminants necessitate immediate attention. To ensure a high level of food safety throughout production and distribution, it is crucial to improve and harmonise analytical techniques for contaminant quantification. This constitutes the basis for reliable data and compliance with regulations and for resolving disputes and minimising financial losses within the food industry. The ScreenFood project (June 2024 -May 2027) is funded by the European Metrology Partnership and aims to develop reference methods and reference materials for quantifying contaminants in both food and food packaging, with a specific emphasis on recycled materials. These metrological tools will aid industries and official food control in guaranteeing the delivery of safe food and sustainable packaging while adhering to regulatory requirements. Specific objectives of the project are i. To improve protocols for the quantification of the mineral oil aromatic hydrocarbons (MOAH) fraction and for the quantification of the fraction consisting of substances with three or more aromatic ring systems (3+MOAH); ii. To develop sensitive analytical procedures for detecting and quantifying per- and polyfluoroalkyl substances (PFAS) in selected matrices, in line with EU requirements; iii. To develop traceable and highly accurate reference materials for quality control and quality assurance purposes; iv. to develop screening methods addressing new/existing organic and inorganic contaminants, in virgin and recycled packaging, such as PET, and bio-based and reusable materials; v. To investigate the migration of contaminants from packaging into food simulants, as well as to foster the research in the discovery of Emerging and Novel PFAS through non-targeted screening. The consortium brings together 28 partners from EU metrological institutes, research centres, control laboratories, EU reference laboratories and industries. A large panel of collaborators and stakeholders is supporting the consortium in keeping the project aligned with EU and industrial priorities.  T2 - 11th International Symposium on RECENT ADVANCES IN FOOD ANALYSIS (RAFA) CY - Prague, Czech Republic DA - 05.11.2024 KW - Per- and Polyfluoroalkyl Substances (PFAS) KW - MOSH/MOAH KW - EU Project KW - Food KW - Food Contact Material (FCM) KW - ScreenFood PY - 2024 AN - OPUS4-62185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan T1 - Enhancing the Efficiency and Accessibility of Grazing Exit X-ray Absorption Spectroscopy for Corrosion and Layered Materials Analysis N2 - In the field of materials science, there is a critical need for efficient and effective characterization techniques, especially in the investigation of corrosion processes of compositionally complex alloys (CCAs) or the analysis of layered structures. This talk presents an advanced approach that combines grazing-exit X-ray absorption near-edge structure spectroscopy (GE-XANES) with Bayesian optimization (BO) to significantly improve the efficiency of data acquisition while retaining the depth-resolved, element-specific analysis capabilities that are critical for studying these materials under ambient conditions. Using a non-destructive, scan-free GE-XANES setup coupled with a pnCCD detector and grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry, our method enables precise analysis at sub-micrometer depths without the need for high vacuum environments or extensive sample preparation. The integration of BO reduces experimental time by a factor of 50, overcoming the practical limitations of conventional GE-XANES and increasing its applicability in the study of surface catalysis and corrosion processes. We validate this optimized approach through comparative studies on a CrCoNi alloy and a reference layered sample, demonstrating its potential to revolutionize materials analysis by increasing both efficiency and accessibility. T2 - Gesellschaft Deutscher Chemiker (GDCh) CY - Clausthal-Zellerfeld, Germany DA - 20.06.2024 KW - GEXRF KW - GEXANE KW - ML PY - 2024 AN - OPUS4-61788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zöllner, Moritz T1 - Thermal decomposition of dolomite: Raman spectroscopy as a thermometric tool for the analysis of carbonates in mortar binders. N2 - The reconstruction of the thermal history of minerals is an on-going challenge in the study of anthropogenic materials, e.g., ceramics and mortar binders. For millennia carbonate rocks have been used as the starting material, though the exact manufacturing procedures are often unknown. Preparatory parameters such as firing temperature, heating and cooling rates, soaking time, and kiln atmosphere greatly influence the chemical and structural properties of the resulting products. Analysis of replicas produced under well-defined laboratory conditions help identify indicators for such process parameters and therefore provide valuable insights into historical production workflows. Raman micro-spectroscopy is a valuable method here because of its high sensitivity for crystal-chemical alterations coupled with a high spatial resolution. Previous studies on pyrogenic anhydrite were able to distinguish between gypsum materials that were heated at different temperatures between 400 – 900 °C [1, 2]. The results of thermal experiments with natural dolomite powder between 500 – 900 °C are presented, evaluating the thermal decomposition of dolomite and the consequent formation of calcium carbonate. Raman measurements were performed at room temperature on calcinated samples, as well as subsequently hydrated and re-carbonated samples. A peak-fitting routine using python scripts was employed to extract the peak positions and the full width at half maximum (FWHM) values of the ν1-, ν4- and L-bands of the carbonates. The results reveal the formation of Mg-calcite from dolomite at 700 – 750 °C and the formation of Mg-free calcite after calcination above 750 °C and subsequent hydration and re-carbonation. The findings from the thermal experiments are compared with Raman-microscopy mappings on medieval and reenacted mortars containing dolomite. Mg-calcite with comparable peak position and FWHM values have been successfully identified, proving Raman spectroscopy to be a suitable tool for elucidating the manufacturing procedures of anthropogenic materials. T2 - European Mineralogical Conference 2024 CY - Dublin, Ireland DA - 18.08.2024 KW - Raman spectroscopy KW - Dolomite KW - Mineral thermometry PY - 2024 AN - OPUS4-61975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zöllner, Moritz T1 - Thermal decomposition of dolomite: Raman spectroscopy as a thermometric tool for the analysis of carbonates in mortar binders. N2 - High-spectral resolution Raman spectroscopy is a powerful tool for the chemical and structural analysis in material sciences. Beyond its usage for the qualitative identification of minerals, Raman spectroscopy has been applied for the quantitative characterisation of chemical phases. The precise measurement of Raman peak position and band width values allows for an empirical differentiation of chemically similar phases and thus provides valuable insights to the structural properties of a material. In the field of archaeometry, the crystal structure of minerals can be used to elucidate the preparatory parameters of historical samples, such as the firing temperature. Comparison of historical materials with replicas produced under well-defined laboratory conditions help identify indicators for such process parameters. Previous Raman studies on pyrogenic anhydrite were able to distinguish between gypsum materials that were heated at different temperatures between 400–900 °C [1–3]. The results of thermal experiments with natural dolomite powder between 500–900 °C are presented, evaluating the thermal decomposition of dolomite and the consequent formation of calcium carbonate. Raman measurements were performed with excitation at 532 nm and 1800 mm-1 grating at room temperature on calcinated samples, as well as subsequently hydrated and re-carbonated samples. These high-resolution conditions are necessary to resolve the individual spectral contributions of different calcium/magnesium carbonate species. However, this sensitivity does not come without potential pitfalls. While the usage of micro-Raman spectroscopy with high spectral resolution shows great promise for evaluating minor shifts in peak positions and band widths, several technical aspects must be considered. For example, great care must be taken to exclude the thermal impact of the highly focused Raman laser on the sample. Similarly, exact standard operating procedures have to be followed to circumvent mechanical hysteresis in the alignment of the spectrographs’ grating. The influence of these two effects is presented and effective countermeasures are introduced to avoid resulting systematic errors. Statistical reliability and chemical imaging both rely on the individual analysis of thousands of Raman spectra. Thus, besides the spectral acquisition, also highly automated data analysis must be applied. Therefore, a peak-fitting routine using python scripts was employed to extract the peak positions and the full width at half maximum (FWHM) values of the ν1-, ν4- and L-bands of the carbonates. The results reveal the formation of Mg-calcite from dolomite at 700–750 °C and the formation of Mg-free calcite after calcination above 750 °C and subsequent hydration and re-carbonation (Fig. 1a). The findings from the thermal experiments are compared with Raman-microscopy mappings on medieval and reenacted mortars containing dolomite. Mg-calcite with comparable peak position and FWHM values have been successfully identified (Fig. 1b), proving Raman spectroscopy to be a suitable tool for elucidating the manufacturing procedures of anthropogenic materials. T2 - 16th GeoRAMAN Conference CY - Rhodes, Greece DA - 24.09.2024 KW - Raman spectroscopy KW - Dolomite KW - Mineral thermometry PY - 2024 AN - OPUS4-61977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zöllner, Moritz T1 - Thermal decomposition of dolomite: Raman spectroscopy as a thermometric tool for the analysis of carbonates in mortar binders N2 - The reconstruction of the thermal history of minerals is an on-going challenge in the study of anthropogenic materials, e.g., ceramics and mortar binders. For millennia carbonate rocks have been used as the starting material, though the exact manufacturing procedures are often unknown. Preparatory parameters such as firing temperature, heating and cooling rates, soaking time, and kiln atmosphere greatly influence the chemical and structural properties of the resulting products. Analysis of replicas produced under well-defined laboratory conditions help identify indicators for such process parameters and therefore provide valuable insights into historical production workflows. Raman micro-spectroscopy is a valuable method here because of its high sensitivity for crystal-chemical alterations coupled with a high spatial resolution. Previous studies on pyrogenic anhydrite were able to distinguish between gypsum materials that were heated at different temperatures between 400–900 °C [1-3]. The results of thermal experiments with natural dolomite powder between 500–900 °C are presented, evaluating the thermal decomposition of dolomite and the consequent formation of calcium carbonate. Raman measurements were performed at room temperature on calcinated samples, as well as subsequently hydrated and re-carbonated samples. Raman band positions and the full width at half maximum (FWHM) values of the ν1-, ν4- and L-bands of the carbonates are extracted and reveal the formation of Mg-calcite from dolomite at 700–750 °C and the formation of Mg-free calcite after calcination above 750 °C and subsequent hydration and re-carbonation. The findings from the thermal experiments are compared with Raman-microscopy mappings on medieval and reenacted mortars containing dolomite. Mg-calcite with comparable peak position and FWHM values have been successfully identified, proving Raman spectroscopy to be a suitable tool for elucidating the manufacturing procedures of anthropogenic materials. T2 - SciX 2024 CY - Raleigh, NC, USA DA - 20.10.2024 KW - Raman spectroscopy KW - Dolomite KW - Mineral thermometry PY - 2024 AN - OPUS4-61978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zöllner, Moritz T1 - Raman spectroscopy as a thermometric tool for the analysis of mortar binders N2 - The reconstruction of the thermal history of anthropogenic materials is crucial for understanding historical manufacturing techniques. Preparatory parameters such as firing temperature, heating and cooling rates, soaking time, and kiln atmosphere significantly affect the chemical and structural properties of the final product. Comparing historical materials with replicas produced under well-defined laboratory conditions helps identify indicators for these parameters. This comparative approach is greatly enhanced by spectroscopic analyses. Raman spectroscopy has proven to be a powerful tool in this field due to its high sensitivity to crystal-chemical alterations and high spatial resolution. The results of thermal experiments with gypsum and carbonate raw materials at burning temperatures up to 1000 °C are presented. Precise measurements of Raman peak positions and Raman band widths enable the differentiation of chemically similar phases. Changes in the Raman band parameters are evident even after the subsequent hydration-hardening process of the fired samples, allowing the spectral discrimination of samples treated at different temperatures steps. These findings from the thermal experiments are further applied to Raman micro-spectroscopic mappings of medieval and reenacted mortars. The extracted Raman band parameters show comparable values between the experimental and real-life samples, proving Raman spectroscopy as a suitable tool for estimating the burning temperature and thus elucidating the manufacturing procedures of anthropogenic materials. T2 - Jahrestagung Archäometrie und Denkmalpflege 2025 CY - Dresden, Germany DA - 18.03.2025 KW - Raman spectroscopy KW - Mineral thermometry PY - 2025 AN - OPUS4-62778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Tobias T1 - Laser-Induced Breakdown Spectroscopy for Concrete Analysis: Applications and Practical Benefits N2 - Reinforced concrete structures are exposed not only to mechanical loads but also to chemical degradation, which can significantly impact their longevity and performance. Effective assessment and maintenance require a detailed understanding of the ingress of harmful species, such as chlorides or sulfates. Traditional analysis methods, like wet chemical analysis of drill dust or ground core samples, often require homogenization leading to the loss of crucial spatial information in sub-millimeter regions such as localized high concentrations of elements, e.g. in cracks. Laser-induced breakdown spectroscopy (LIBS) offers a cutting-edge solution, providing rapid, multi-element analysis with high spatial resolution from micrometer to millimeter scales. LIBS is capable of detecting both light and heavy elements, making it a powerful tool for detailed concrete analysis. Despite its clear advantages, LIBS is not commonly used in civil engineering. This presentation will showcase practical examples demonstrating the effectiveness and advantages of LIBS in concrete analysis, highlighting real-world applications provided by members of the “LIBS” subcommittee of the technical committee “Civil-Engineering” of the German Society for Non-Destructive Testing (DGZfP). Key examples will be discussed, including measurements from car parks or bridges, alongside an introduction to the newly released DGZfP leaflet B14 providing guidelines for the quantitative determination of chlorine content in concrete by LIBS. Furthermore, prospective applications of LIBS including material identification and classification for concrete recycling, and other emerging uses in civil engineering, will also be presented, showcasing the versatility and future potential of this technology. T2 - Conference on durability of building materials and systems in the transportation infrastructure CY - Mendrisio, Switzerland DA - 22.03.2025 KW - LIBS KW - Spectroscopy KW - Concrete KW - Structural Diagnostics PY - 2025 AN - OPUS4-62822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalichow, Dirk T1 - Laser Induced Breakdown Spectroscopy (LIBS) for the chemical investigation of concrete- Status of practical application and regulations in Germany N2 - The assessment and maintenance of reinforced concrete structures depends largely on knowledge of the chloride content and chloride ingress. Common methods are the wet chemical analysis of drill dust or powder from ground drill core segments. However, due to the homogenization process, this approach often fails to detect locally elevated chloride levels. A state-of-the-art alternative method is laser-induced breakdown spectroscopy (LIBS), which offers rapid analysis and the possibility of detecting several chemical elements simultaneously. This method is particularly characterized by its ability to measure light elements such as hydrogen, carbon or sodium. The spatial resolution of LIBS is usually 0.25 mm but can be increased to 0.1 mm or less if required. BARG, is the first commercial building materials laboratory in Germany to use LIBS in practice. The current LIBS setup enables rapid, spatial quantification of the chlorine content and at the same time the creation of element maps that visually represent the distribution of essential elements in the concrete. This method can be used to localize areas of elevated chlorine content, particularly in cracks or near reinforcing bars. With the ability to analyze several elements simultaneously, LIBS can determine measurement points associated with the cement phase and, taking into account the water content, relate the measured contents directly to the cement mass. The detailed ingress profiles determined by LIBS provide essential data for the estimation of accurate chlorine diffusion coefficients, which are crucial for probabilistic lifetime predictions. The estimation of the carbon distribution enables the localization of carbonated regions and their effect on the chloride distribution. The possibility of quantitatively determining the sulfur distribution also indicates areas that are affected by a possible sulfate attack. The presentation uses practical examples to demonstrate the possibilities and advantages of the LIBS method. In addition, the newly published leaflet B14 of the German Society for Non-Destructive Testing (DGZfP) will be presented, which describes the use of LIBS for the quantitative determination of chloride content in concrete. T2 - ICCRRR 2024 CY - Cape Town, South Africa DA - 04.11.2024 KW - Concrete KW - Chloride KW - Corrosion KW - Repair KW - Maintenance PY - 2024 AN - OPUS4-62481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -