TY - CONF A1 - Traub, Heike A1 - Saatz, Jessica A1 - Ascher, Lena A1 - Boyraz, B. A1 - Hahndorf, J. A1 - Schnorr, J. A1 - Schellenberger, E. A1 - Tauber, R. T1 - Unraveling the interaction of MRI contrast agents with tissue using LA ICP MS N2 - Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is increasingly used to study the distribution of metal-containing drugs, imaging probes and nanomaterials in connection with disease related changes and therapy progress. Additionally, biomolecules can be detected indirectly by using metal-tagged antibodies. The extracellular matrix (ECM) is, besides the cells, an important component of all body tissues. The macromolecular network of the ECM consists of structural proteins (e.g., collagen, elastin) and proteoglycans composed of highly negatively charged carbohydrates, the glycosaminoglycans (GAGs), which are covalently linked to a protein core. Many diseases, including inflammatory processes and tumors, are associated with characteristic ECM changes at an early stage. Recent studies have shown that contrast agents for magnetic resonance imaging (MRI), which are based on gadolinium containing chelate complexes or iron oxide nanoparticles, can bind themselves to ECM components. To elucidate the role of GAGs like keratan sulfate (KS) and its modification state in disease, highly specific tools are necessary. As a complement to conventional immunohistochemistry LA-ICP-MS was applied to investigate the distribution of KS in tissue thin sections using a well characterized anti-KS antibody labelled with metal ions. Furthermore, LA-ICP-MS was used for the detection of MRI contrast agents and the identification of their target cells and molecules in tissue samples from animal models, e.g. for cardiovascular diseases. The results show the possibilities of LA-ICP-MS for the elucidation of pathological tissue changes. T2 - European Workshop on Laser Ablation (EWLA 2022) CY - Berne, Switzerland DA - 12.07.2022 KW - Laser ablation KW - Imaging KW - ICP-MS KW - Antibody PY - 2022 AN - OPUS4-55315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane A1 - Juritsch, Elevtheria A1 - Richter, Matthias T1 - Development of a procedure for the analysis of the emissions of VVOCs N2 - Several aspects were explored towards the standardization of a suitable procedure. The use of gaseous standards is necessary and a standard gas mixture containing 60 substances was successfully generated and employed for further investigations. The suitability of different chromatography columns was addressed: The use of PLOT (Porous Layer Open Tubular) columns is well suitable for VVOC analysis. The recoveries of the 60 analytes on several adsorbents and their combinations were determined: A combination of a graphitized carbon black and a carbon molecular sieve showed great results for all analytes. Carbon molecular sieves adsorb water which can impair the analysis. Different options such as purging, the use of a drying system or splitting were investigated for water removal. This contribution will present experimental results supporting the standardization of a method for VVOC analysis. T2 - Indoor Air conference CY - Kuopio, Finland DA - 12.06.2022 KW - Analytical method KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lilensten, L. A1 - Provost, K. A1 - Perrière, L. A1 - Fonda, E. A1 - Couzinié, J. A1 - Amman, F. A1 - Radtke, Martin A1 - Dirras, G. A1 - Guillot, I. T1 - Experimental investigation of the local environment and lattice distortion in refractory medium entropy alloys N2 - EXAFS analysis of pure elements, binary and ternary equiatomic refractory alloys within the Nb-Zr-Ti-Hf- Ta system is performed at the Nb and Zr K-edges to analyze the evolution of the chemical local environ- ment and the lattice distortion. A good mixing of the elements is found at the atomic scale. For some compounds, a distribution of distances between the central atom and its neighbors suggests a distortion of the structure. Finally, analysis of the Debye-Waller parameters shows some correlation with the lat- tice distortion parameter δ², and allows to quantify experimentally the static disorder in medium entropy alloys. KW - BAMline KW - Refractory alloys KW - EXAFS KW - Debye-Waller parameter PY - 2022 DO - https://doi.org/10.1016/j.scriptamat.2022.114532 SN - 1359-6462 VL - 211 SP - 1 EP - 6 PB - Elsevier Ltd. AN - OPUS4-55287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raab, A. A1 - Vogl, Jochen A1 - Solovyev, N. A1 - El-Khatib, Platt A1 - Costas-Rodriguez, M. A1 - Schwab, K. A1 - Griffin, E. A1 - Platt, B. A1 - Theuring, F. A1 - Vanhaecke, F. T1 - Isotope signature of iron, copper and zinc in mouse models (L66 and 5XFAD) and their controls used for dementia research N2 - Introduction: The influence of copper, iron and zinc concentrations on the formation of ß-amyloid plaques and neurofibrillary tangles in Alzheimer’s disease (AD) is widely discussed in the community. The results from human and animal studies so far are mixed with some studies showing a correlation and others not. From a number of studies, it is known that disease state and isotopic composition of essential elements can be coupled. Aim: The aim of the study was to identify changes in element content and isotopic composition in two transgenic mouse models used in AD research compared to their genetic WT relatives and to establish whether element content and isotopic signature between different laboratories is comparable. Methods: ß-amyloid (5xFAD) and tau overexpressing (L66) mice together with their matching wild-types were bred at dedicated facilities in accordance with the European Communities Council Directive (63/2010/EU). Serum and brain were sampled after sacrifice and the samples distributed among the participants of the study. The tissues were acid digested for total element determination and high-precision isotope ratio determination. Element content was determined by either sector-field or quadrupole-based inductively coupled plasma mass spectrometry (ICPMS). For the determination of isotope ratios multi-collector ICPMS was used. Results: Total copper content was significantly higher for L66 and their matched WT compared to 5xFAD and WT. Brains of L66 mice contained more Fe in brain than their WT, Zn and Cu were not significantly different between L66 and WT. Whereas 5xFAD mice had a slightly lower Cu and slightly higher Zn concentration in brain compared to WT. The isotopic signature in brain of L66 mice for Fe was different from their controls, whereas Zn isotope ratios were influenced in 5xFAD mice compared to their WT. The Cu isotopic ratio did not seem to be influenced in either strain. In serum, the shifts were less pronounced. Conclusion: Even though neither Tau-protein nor amyloid precursor protein are known to be metal-dependent / -containing proteins, the overexpression of both influences the Fe, Cu and Zn metabolism in brain and to some extent also in serum as can be seen not only using total element determination but probably more clearly studying the isotopic signature of Fe, Cu and Zn. T2 - The International Conference of Trace Elements and Minerals (ICTEM) 2022 CY - Aachen, Germany DA - 05.06.2022 KW - Isotope ratio KW - Isotope delta value KW - Metrology KW - Alzheimer disease KW - Measurement uncertainty PY - 2022 AN - OPUS4-55204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schühle, Florian A1 - Richter, Matthias T1 - Bereitstellung qualitätsgesicherter VOC-Aufnahmeraten für axiale Passivsammler N2 - Quality assured uptake rates for passive sampling of indoor air VOCs Passive sampling of VOCs with Tenax® TA and thermal desorption GC-MS analysis is a simple, cost efficient and representative method to determine VOCs concentrations in indoor air. In theory, the uptake into the passive sampler is only dependent on the diffusion coefficient of the analyte in air and the geometry of the sampler (ideal adsorption). For characterization, the uptake rate (UR) is used, defined as the ratio of the uptaken mass and the product of ambient concentration and exposure time. Various reported effective uptake rates (UR,eff) differ considerably from ideal values (UR,id). Literature values in national and international standards, are essentially sorted by the applicable exposure time, while detailed information about the corresponding concentration range is lacking. Moreover the number of itemized substances is limited. The aim of this study was to review and expand this set of uptake rates by determination of own quality assured laboratory values.The determined uptake rates are considered accurate in terms of RSD and comparability to literature values and can be recommended for exposure times of seven days at 50 100 µg/m³ (approximately 100 300 ppm min). Seven day uptake rates in ISO16017 2 and ASTM D6196 are not generally suited for this purpose, as has been exemplarily shown for benzene. N2 - Die passive Probenahme von VOC (Volatile Organic Compounds) mit Tenax® TA und Thermodesorption GC/MS Analytik ist eine einfache, kosteneffiziente und repräsentative Methode zur Bestimmung der VOC-Konzentrationen in der Innenraumluft. In der Theorie ist die Stoffaufnahme in den Passivsammler nur abhängig vom Diffusionskoeffizienten der Substanz in Luft und der Geometrie des Sammlers (ideale Adsorption). Um sie zu charakterisieren, wird die Aufnahmerate (UR), definiert als Quotient der Massenaufnahme und dem Produkt aus Konzentration und Expositionszeit, verwendet. Viele effektive Aufnahmeraten (UR,eff) unterscheiden sich beträchtlich von idealen (theoretischen) Werten (UR,id). Literaturwerte sind in nationalen und internationalen Normen lediglich für bestimmte Expositionszeiten vorgegeben, während detaillierte Informationen über den zugehörigen Konzentrationsbereich fehlen. Außerdem ist die Anzahl der insgesamt in der Literatur beschriebenen Substanzen begrenzt. Das Ziel der vorgestellten Studie ist es diesen Fundus an Aufnahmeraten zu begutachten und zu prüfen und ihn durch die Bestimmung eigener qualitätsgesicherter Laborwerte zu ergänzen. Die bestimmten Aufnahmeraten werden als akkurat bezüglich ihrer relativen Standardabweichung und Vergleichbarkeit zu Literaturwerten betrachtet und können für Expositionszeiten von 7 Tagen bei Konzentrationen von 50 100 µg/m³ (ca. 100 300 ppm min) empfohlen werden. Die Sieben Tage Aufnahmeraten aus ISO16017 2 und ASTM D6196 sind nicht generell für diesen Zweck geeignet, wie exemplarisch für Benzol gezeigt wurde. T2 - Kongress 29. WaBoLu-Innenraumtage CY - Berlin, Germany DA - 24.05.2022 KW - IAQ KW - VOC KW - Passive sampling KW - Uptake rate PY - 2022 SN - 978-3-949241-04-8 AN - OPUS4-55209 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane A1 - Juritsch, Elevtheria A1 - Richter, Matthias T1 - Weiterentwicklung und Validierung eines leistungsfähigen Verfahrens zur Bestimmung von VVOCs aus Bauprodukten und in der Innenraumluft N2 - Mehrere Aspekte wurden im Hinblick auf die Standardisierung eines geeigneten Verfahrens für die Analyse sehr flüchtiger organischer Verbindungen (VVOCs) untersucht. Die Verwendung gasförmiger Standards ist notwendig und es wurde ein stabiles Standardgasgemisch aus 60 Substanzen erfolgreich erzeugt und auf Stabilität und Reaktivität überprüft. Die Eignungsuntersuchung verschiedener Chromatographiesäulen ergab, dass PLOT-Säulen (Porous Layer Open Tubular) für die VVOC-Analytik gut geeignet sind. Für die 60 Analyten wurden Wiederfindungsraten auf mehreren Adsorbenzien und deren Kombinationen bestimmt. Dabei zeigte eine Kombination aus einem graphitierten Ruß und einem Kohlenstoff-Molekularsieb hervorragende Ergebnisse für alle Zielkomponenten. Nachteilig an Kohlenstoff-Molekularsieben ist, dass sie Wasser adsorbieren, was die Analyse beeinträchtigen kann. Zur Wasserentfernung wurden verschiedene Optionen wie das Trockenspülen oder der Einsatz eines Trocknungssystems untersucht. T2 - WaBoLu Innenraumtage CY - Berlin, Germany DA - 24.05.2022 KW - Analytische Methode KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55281 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Harald A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Alexandra A1 - Rasmussen, K. A1 - Rauscher, H. T1 - Counting Small Particles in Electron Microscopy Images — Proposal for Rules and Their Application in Practice N2 - Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials. KW - Nano KW - Particle size distribution KW - Nanoparticle KW - Nanomaterial KW - OECD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551891 DO - https://doi.org/10.3390/nano12132238 SN - 2079-4991 VL - 12 IS - 13 SP - 2238 PB - MDPI CY - Basel AN - OPUS4-55189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittner, Maria A1 - Kerndorff, A. A1 - Ricking, M. A1 - Bednarz, M. A1 - Obermaier, N. A1 - Lukas, M. A1 - Asenova, M. A1 - Bordós, G. A1 - Eisentraut, Paul A1 - Hohenblum, P. A1 - Hudcova, H. A1 - Humer, F. A1 - István, T. G. A1 - Kirchner, M. A1 - Marushevska, O. A1 - Nemejcová, D. A1 - Oswald, P. A1 - Paunovic, M. A1 - Sengl, M. A1 - Slobodnik, J. A1 - Spanowsky, K. A1 - Tudorache, M. A1 - Wagensonner, H. A1 - Liska, I. A1 - Braun, U. A1 - Bannick, C. G. T1 - Microplastics in the Danube River Basin: A First Comprehensive Screening with a Harmonized Analytical Approach N2 - In this study, carried out within the Joint Danube Survey 4, a comprehensive microplastic screening in the water column within a large European river basin from its source to estuary, including major tributaries, was realized. The objective was to develop principles of a systematic and practicable microplastic monitoring strategy using sedimentation boxes for collection of suspended particulate matter followed by its subsequent analysis using thermal extraction desorption-gas chromatography/mass spectrometry. In total, 18 sampling sites in the Danube River Basin were investigated. The obtained suspended particulate matter samples were subdivided into the fractions of >100 μm and <100 μm and subsequently analyzed for microplastic mass contents. The results showed that microplastics were detected in all samples, with polyethylene being the predominant polymer with maximum contents of 22.24 μg/mg, 3.23 μg/mg for polystyrene, 1.03 μg/mg for styrene-butadiene-rubber, and 0.45 μg/mg for polypropylene. Further, polymers such as different sorts of polyester, polyacrylates, polylactide, and natural rubber were not detected or below the detection limit. Additional investigations on possible interference of polyethylene signals by algae-derived fatty acids were assessed. In the context of targeted monitoring, repeated measurements provide more certainty in the interpretation of the results for the individual sites. Nevertheless, it can be stated that the chosen approach using an integrative sampling and determination of total plastic content proved to be successful. KW - Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS), monitoring KW - Microplastics KW - River KW - Suspended particulate matter (SPM) KW - Sedimentation box (SB) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551444 DO - https://doi.org/10.1021/acsestwater.1c00439 VL - 2 IS - 7 SP - 1174 EP - 1181 PB - ACS Publications AN - OPUS4-55144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Theiner, S. A1 - Corte Rodriguez, M. A1 - Traub, Heike ED - Golloch, A. T1 - Novel applications of lanthanoids as analytical or diagnostic tools in the life sciences by ICP-MS based techniques N2 - Inductively coupled plasma-mass spectrometry (ICP-MS) is a well-established analytical method offering high sensitivity and multi-element analysis. ICP-MS has found acceptance in various application areas ranging from material analysis to applications in the life sciences. Within the last 15 years new strategies for the sensitive detection and accurate quantification of biomolecules in complex biomedical samples have been developed. Recent instrumental improvements have contributed to this progress. As most of the biomolecules do not contain endogenous metals etectable with ICP-MS, bioconjugation with artificial metal-containing tags based on metal-loaded chelate complexes or nanoparticles is increasingly applied to determine biomolecules indirectly. Especially, the combination of immunohistochemical workflows using lanthanoid-tagged antibodies and ICP-MS detection provides new insights in the complexity and interdependency of cellular processes. Single-cell ICP-MS, also termed as mass cytometry, allows high-dimensional analysis of biomarkers in cell populations at single-cell resolution. For that purpose, lanthanoid isotope labelled antibodies are used to detect their corresponding target molecules. The visualisation of the elemental distribution is possible with laser ablation ICP-MS (LA-ICPMS) at high spatial resolution. Especially, the combination of LA with ICP time-of-flight mass spectrometry, also referred to as imaging mass cytometry (IMC), opens new possibilities for multiparametric tissue imaging at the single-cell level and even below. The lanthanoid localisation and concentration can be linked to their conjugated antibody target providing valuable information about surface markers, intracellular signalling molecules to measure biological function, and the network state of an individual cell in a tissue. This book chapter focuses on new applications, where the multi-element capabilities of ICP-MS are used for the detection of lanthanoids applied as artificial elemental stains or tags for biomolecules and in particular antibodies. KW - ICP-MS KW - Laser ablation KW - Cell KW - Antibody KW - Immunohistochemistry KW - Lanthanoid KW - Mass cytometry KW - Imaging PY - 2022 SN - 978-3-11069-645-5 SN - 978-3-11069-636-3 DO - https://doi.org/10.1515/9783110696455-013 SP - 399 EP - 444 PB - De Gruyter CY - Berlin, Boston ET - 2. rev. and exten. edition AN - OPUS4-55118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - A fast and simple PFAS extraction method for soil sample analysis using HR-CS-GFMAS N2 - Per- and polyfluorinated alkyl substances (PFASs) are a substance class of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their different chemical and physical properties as well as the high number of target substances. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate a realistic PFAS pollution level. PFAS sum parameters compromise 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. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for indirect 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 of c(F) 2.7 µg/L. Here, we describe a fast and simple extraction method for the determination of the EOF using HR-CS-GFMAS in soil samples. Common approaches for the EOF determination use solid phase extraction (SPE). To omit the bias of this time consuming and expensive step we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol. Comparison of the method with and without an SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. In the next step, the applicability of our method was tested for other solid matrices. In view of steadily increasing numbers of PFASs, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFASs in the future. T2 - Analytica conference CY - München, Germany DA - 21.06.2022 KW - PFAS KW - HR-CS-GFMAS KW - Soil KW - Fluorine KW - SPE PY - 2022 AN - OPUS4-55124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao A1 - Akkus, A. A1 - Weisheit, W. A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique T1 - Multi element analysis in soil using nitrogen microwave inductively coupled plasma mass spectrometry (MICAP MS) N2 - Due to the fast growth of industry and the use of metal-containing compounds such as sewage sludge in agricultural fields, soil pollution associated with heavy metals presents a terrifying threat to the environment. Throughout the world, there are already 5 million sites of soil contaminated by heavy metals1. Some heavy metals pollutants can influence food chain safety and food quality, which in turn affects human health. According to the German Federal Soil Protection and Contaminated Site Ordinance (BBodSchV) 13 heavy metals such as arsenic (As), lead (Pb) and cadmium (Cd) are classified as heavily toxic to human health2. Therefore, elemental analysis and precise quantification of the heavy metals in soil are of great importance. Inductively coupled plasma mass spectrometry (ICP-MS) emerged as a powerful technique for trace analysis of soil due to its multi-element capability, high sensitivity and low sample consumption. However, despite its success and widespread use, ICP-MS has several persistent drawbacks, such as high argon gas consumption, argon-based polyatomic interferences and the need for complicated RF-power generators. Unlike argon-based ICP, the nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) uses nitrogen as plasma gas, which eliminates high operating costs associated with argon-gas consumption as well as the argon-based interferences3. For the first time, the applicability of MICAP-MS for elemental analysis of environmental soils is investigated in this work. For this purpose, 7 reference- and 3 random soil samples containing vanadium (V), cobalt (Co), zink (Zn), copper (Cu), chrome (Cr), mercury (Hg), As, Pb and Cd are digested with aqua regia and used for analysis. Concentrations of selected elements are determined using MICAP-MS and validated using ICP-MS. Sensitivities, limits of detection and gas consumption for both methods are compared and discussed in detail. Moreover, the performance of MICAP-MS under different nitrogen plasma gas concentrations is investigated and compared T2 - Spectroscopium Colloquium CY - Gijon, Spain DA - 30.05.2022 KW - Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) KW - Multi-element analysis KW - Soil KW - Nitrogen plasma PY - 2022 AN - OPUS4-55181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kader, A. A1 - Kaufmann, Jan Ole A1 - Mangarova, D. B. A1 - Moeckel, J. A1 - Brangsch, J. A1 - Adams, L. C. A1 - Zhao, J. A1 - Reimann, C. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Buchholz, R. A1 - Karst, U. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Iron Oxide Nanoparticles for Visualization of Prostate Cancer in MRI N2 - Prostate cancer (PCa) is one of the most common cancers in men. For detection and diagnosis of PCa, non-invasive methods, including magnetic resonance imaging (MRI), can reduce the risk potential of surgical intervention. To explore the molecular characteristics of the tumor, we investigated the applicability of ferumoxytol in PCa in a xenograft mouse model in two different tumor volumes, 500 mm3 and 1000 mm3. Macrophages play a key role in tumor progression, and they are able to internalize iron-oxide particles, such as ferumoxytol. When evaluating T2*-weighted sequences on MRI, a significant decrease of signal intensity between pre- and post-contrast images for each tumor volume (n = 14; p < 0.001) was measured. We, furthermore, observed a higher signal loss for a tumor volume of 500 mm3 than for 1000 mm3. These findings were confirmed by histological examinations and laser ablation inductively coupled plasma-mass spectrometry. The 500 mm3 tumors had 1.5% iron content (n = 14; sigma = 1.1), while the 1000 mm3 tumors contained only 0.4% iron (n = 14; sigma = 0.2). In vivo MRI data demonstrated a correlation with the ex vivo data (R2 = 0.75). The results of elemental analysis by inductively coupled plasma-mass spectrometry correlated strongly with the MRI data (R2 = 0.83) (n = 4). Due to its long retention time in the blood, biodegradability, and low toxicity to patients, ferumoxytol has great potential as a contrast agent for visualization PCa. KW - Imaging KW - Nanoparticle KW - Cancer KW - Iron oxide KW - ICP-MS KW - Magnetic resonance imaging PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550075 DO - https://doi.org/10.3390/cancers14122909 VL - 14 IS - 12 SP - 1 EP - 13 PB - MDPI CY - Basel, Switzerland AN - OPUS4-55007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Cakir, Cafer Tufan T1 - Big to Small - Getting Smarter@BAMline N2 - In this talk an overview about artificial intelligence/machine learning applications @BAMline is given. In the first part, the use of neural networks for the quantification of XRF measurements and the decoding of coded-aperture measurements are shown. Then it is shown how Gaussian processes and Bayesian statistics can be used to achieve an optimal alignment of the set-up and in general for optimization of measurements. T2 - Forschungsseminar Institut für Optik und Atomare Physik TU Berlin CY - Berlin, Germany DA - 25.10.2022 KW - Artificial Inelligence KW - Machine Learning KW - Bayesian Statistics KW - Gaussian process KW - Neural network KW - BAMline KW - Synchrotron PY - 2022 AN - OPUS4-56249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - From Egypt to Hiddensee – Analysis of Gold with Synchrotron Radiation IV N2 - Gold is one of the seven metals already known in antiquity and was used from time immemorial as a medium of exchange and for the production of jewelry because of its luster and rarity. In addition, it is easy to work and largely resistant to chemical influences. Investigations of gold using synchrotron radiation excited X-ray fluorescence analysis are non-destructive and provide information about the chemical elements present in the sample under investigation. The investigations presented here at BAMline focus on questions such as the origin, manufacturing process, and association of gold findings. The different questions are explained by a number of examples ranging from the Viking treasure from Hiddensee to the Nebra Sky Disk and finds from Egypt. The find from Bernstorf is discussed in detail. A Bayesian treatment of the authenticity is shown. T2 - Ringvorlesung Einführung in die Archäometrie CY - Berlin, Germany DA - 04.11.2022 KW - Synchrotron KW - BAMline KW - Bayesian Statistics KW - Gold KW - Röntgenfluoreszenz PY - 2022 AN - OPUS4-56252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - News from the BAMline N2 - A presentation of recent measurements at the BAMline with focus on AI and ML applications T2 - Seminar: Strahlenphysikalische Anwendungen in Technik und Medizin CY - Vienna, Austria DA - 18.05.2022 KW - Synchrotron KW - BAMline KW - Bayesian Statistics KW - Gold KW - X-ray fluorescence PY - 2022 AN - OPUS4-56253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Cakir, Cafer Tufan A1 - de Oliveira Guilherme Buzanich, Ana T1 - Getting more efficient – The use of Bayesian optimization and Gaussian processes at the BAMline N2 - For more than 20 years, BAM is operating the BAMline at the synchrotron BESSY II in Berlin Adlershof. During this time, the complexity of the setup and the amount of data generated have multiplied. To increase the effectiveness and in preparation for BESSY III, algorithms from the field of machine learning are increasingly used. After a short introduction to BO and GP, the first example is the automatic alignment of our double multilayer monochromator (DMM). The second example is the optimization of measurement time in XRF scanning. T2 - SNI2022 conference CY - Berlin, Germany DA - 05.09.2022 KW - Artificial Inelligence KW - Machine Learning KW - Bayesian Statistics KW - Gaussian process KW - X-ray fluorescence KW - BAMline PY - 2022 AN - OPUS4-56255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sieber, M. J. A1 - Wilke, M. A1 - Appelt, O. A1 - Oelze, Marcus A1 - Koch-Müller, M. T1 - Melting relations of Ca–Mg carbonates and trace element signature of carbonate melts up to 9 GPa – A proxy for melting of carbonated mantle lithologies N2 - The most profound consequences of the presence of Ca–Mg carbonates (CaCO3–MgCO3) in the Earth’s upper mantle may be to lower the melting temperatures of the mantle and control the melt composition. Low-degree partial melting of a carbonate-bearing mantle produces CO2-rich, silica-poor melts compositionally imposed by the melting relations of carbonates. Thus, understanding the melting relations in the CaCO3–MgCO3 system facilitates the interpretation of natural carbonate-bearing silicate systems. We report the melting relations of the CaCO3–MgCO3 system and the partition coefficient of trace elements between carbonates and carbonate melt from experiments at high pressure (6 and 9 GPa) and temperature (1300–1800 ◦C) using a rocking multi-anvil press. In the absence of water, Ca–Mg carbonates are stable along geothermal gradients typical of subducting slabs. Ca–Mg carbonates (∼ Mg0.1–0.9Ca0.9–0.1CO3) partially melt beneath mid-ocean ridges and in plume settings. Ca–Mg carbonates melt incongruently, forming periclase crystals and carbonate melt between 4 and 9 GPa. Furthermore, we show that the rare earth element (REE) signature of Group-I kimberlites, namely strong REE fractionation and depletion of heavy REE relative to the primitive mantle, is resembled by carbonate melt in equilibrium with Ca-bearing magnesite and periclase at 6 and 9 GPa. This suggests that the dolomite–magnesite join of the CaCO3–MgCO3 system might be useful to approximate the REE signature of carbonate-rich melts parental to kimberlites. KW - High pressure experiments KW - Laser Ablation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561197 DO - https://doi.org/10.5194/ejm-34-411-2022 SN - 0935-1221 VL - 34 IS - 5 SP - 411 EP - 424 PB - Copernicus Publications CY - Göttingen AN - OPUS4-56119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Lisec, Jan T1 - CorMID - Correct Mass Isotopologue Distribution Vectors N2 - The investigation of metabolic fluxes and metabolite distributions within cells by means of tracer molecules is a valuable tool to unravel the complexity of biological systems. Technological advances in mass spectrometry (MS) technology such as atmospheric pressure chemical ionization (APCI) coupled with high resolution (HR), not only allows for highly sensitive analyses but also broadens the usefulness of tracer-based experiments, as interesting signals can be annotated de novo when not yet present in a compound library. However, several effects in the APCI ion source, i.e., fragmentation and rearrangement, lead to superimposed mass isotopologue distributions (MID) within the mass spectra, which need to be corrected during data evaluation as they will impair enrichment calculation otherwise. Here, we present and evaluate a novel software tool to automatically perform such corrections. We discuss the different effects, explain the implemented algorithm, and show its application on several experimental datasets. This adjustable tool is available as an R package from CRAN. KW - Mass Spectrometry KW - Software KW - R package KW - Mass Isotopomer Distribution KW - Flux Analysis PY - 2022 UR - https://github.com/cran/CorMID/ PB - GitHub CY - San Francisco, CA, USA AN - OPUS4-56442 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 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 - JOUR A1 - Langenhan, Jennifer A1 - Jaeger, Carsten A1 - Baum, K. A1 - Simon, M. A1 - Lisec, Jan T1 - A Flexible Tool to Correct Superimposed Mass Isotopologue Distributions in GC‐APCI‐MS Flux Experiments N2 - The investigation of metabolic fluxes and metabolite distributions within cells by means of tracer molecules is a valuable tool to unravel the complexity of biological systems. Technological advances in mass spectrometry (MS) technology such as atmospheric pressure chemical ionization (APCI) coupled with high resolution (HR), not only allows for highly sensitive analyses but also broadens the usefulness of tracer‐based experiments, as interesting signals can be annotated de novo when not yet present in a compound library. However, several effects in the APCI ion source, i.e., fragmentation and rearrangement, lead to superimposed mass isotopologue distributions (MID) within the mass spectra, which need to be corrected during data evaluation as they will impair enrichment calculation otherwise. Here, we present and evaluate a novel software tool to automatically perform such corrections. We discuss the different effects, explain the implemented algorithm, and show its application on several experimental datasets. This adjustable tool is available as an R package from CRAN. KW - Mass Spectrometry KW - Isotopologue Distribution KW - Metabolic Flux KW - R package PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547318 DO - https://doi.org/10.3390/metabo12050408 VL - 12 IS - 5 SP - 1 EP - 10 PB - MDPI AN - OPUS4-54731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaeger, Carsten A1 - Lisec, Jan T1 - Towards Unbiased Evaluation of Ionization Performance in LC-HRMS Metabolomics Method Development N2 - As metabolomics increasingly finds its way from basic science into applied and regulatory environments, analytical demands on nontargeted mass spectrometric detection methods continue to rise. In addition to improved chemical comprehensiveness, current developments aim at enhanced robustness and repeatability to allow long-term, inter-study, and meta-analyses. Comprehensive metabolomics relies on electrospray ionization (ESI) as the most versatile ionization technique, and recent liquid chromatography-high resolution mass spectrometry (LC-HRMS) instrumentation continues to overcome technical limitations that have hindered the adoption of ESI for applications in the past. Still, developing and standardizing nontargeted ESI methods and instrumental setups remains costly in terms of time and required chemicals, as large panels of metabolite standards are needed to reflect biochemical diversity. In this paper, we investigated in how far a nontargeted pilot experiment, consisting only of a few measurements of a test sample dilution series and comprehensive statistical analysis, can replace conventional targeted evaluation procedures. To examine this potential, two instrumental ESI ion source setups were compared, reflecting a common scenario in practical method development. Two types of feature evaluations were performed, (a) summary statistics solely involving feature intensity values, and (b) analyses additionally including chemical interpretation. Results were compared in detail to a targeted evaluation of a large metabolite standard panel. We reflect on the advantages and shortcomings of both strategies in the context of current harmonization initiatives in the metabolomics field. KW - Mass Spectrometry KW - Non-targeted analysis KW - Method development PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548065 DO - https://doi.org/10.3390/metabo12050426 VL - 12 IS - 5 SP - 1 EP - 13 PB - MDPI AN - OPUS4-54806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Lisec, Jan T1 - IsoCor N2 - Despite numerous advantages offered by hyphenation of chromatography and electrokinetic separation methods with multicollector (MC) ICP-MS for isotope analysis, the main limitation of such systems is the decrease in precision and increase in uncertainty due to generation of short transient signals. To minimize this limitation, most authors compare several isotope ratio calculation methods and establish a multi-step data processing routine based on the precision and accuracy of the methods. However, to the best of our knowledge, there is no universal data processing tool available that incorporates all important steps of the treatment of the transient signals. Thus, we introduce a data processing application (App) IsoCor that facilitates automatic calculation of isotope ratios from transient signals and eases selection of the most suitable method. The IsoCor App performs baseline subtraction, peak detection, mass bias correction, isotope ratio calculation and delta calculation. The feasibility and reliability of the App was proven by reproducing the results from isotope analysis of three elements (neodymium, mercury and sulfur) measured on-line via hyphenated systems. The IsoCor App provides trackability of the results to ensure quality control of the analysis. KW - Shiny-App KW - ICP-MS KW - Software PY - 2022 UR - https://github.com/cran/IsoCor/ PB - GitHub CY - San Francisco, CA, USA AN - OPUS4-56307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Kulow, A. A1 - Reinholz, Uwe A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Streli, C. A1 - Fittschen, U. E. A. A1 - Hampel, S. T1 - Energy Resolved Imaging with Coded Apertures N2 - Our aim is to develop a simple and inexpensive method for full field X-ray fluorescence imaging.We combine an energydispersive array detector with a coded aperture to obtain high resolut ion images. To obtain the information from the recorded image a reconstruction step is necessary. The reconstruction methods we have developed, were tested on simulated data and then applied to experimental data. The first tests were carried out at the BAMline @BESSY II. This method enables the simultaneous detection of multiple elements,which is important e.g. in the field of catalysis. T2 - SRI 2021 CY - Online meeting DA - 28.3.2022 KW - Synchrotron KW - BAMline KW - Machine Learning KW - Coded Aperture PY - 2022 AN - OPUS4-56298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steinhäuser, Lorin A1 - Piechotta, Christian A1 - Westphalen, Tanja A1 - Kaminski, Katja T1 - Evaluation, comparison and combination of molecularly imprinted polymer solid phase extraction and classical solid phase extraction for the preconcentration of endocrine disrupting chemicals from representative whole water samples N2 - Estrogens are endocrine disrupting chemicals and of high concerns due to demonstrated harmful effects on the environment and low effect levels. For monitoring and risk assessment, several estrogens were included in the "watch list" of the EU Water Framework Directive which sets very low environmental quality standard (EQS) levels for Estrone (E1) and 17β-Estradiol (E2) of 0.4 ng L−1 and for 17α-Ethinylestradiol (EE2) of 0.035 ng L−1 requiring sensitive detection methods, as well as extensive sample preparation. A sensitive, derivatization-free, isotope dilution calibration HPLC-MS/MS method for a panel of 5 selected estrogens (including the 3 estrogens of the EU WFD watchlist), and a procedure for the reproducible preparation of a representative whole water matrix including mineral water, humic acids and solid particulate matter are presented. These are used in a diligent comparison of classical solid phase extraction (SPE) on hydrophilic-lipophilic balanced (HLB) phase to SPE on an estrogen-specific molecularly imprinted polymer phase (MISPE) for ultra-trace levels of the analytes (1–10 ng L−1). Additionally, a two-step procedure combining HLB SPE disks followed by MISPE is evaluated. The tow-step procedure provides superior enrichment, matrix removal and sample throughput while maintaining comparable recovery rates to simple cartridge SPE. Estimated method quantification limits (MQLs) range from 0.109–0.184 ng L−1 and thus meet EQS-levels for E1 and E2, but not EE2. The representative whole water matrix provides a reproducible comparison of sample preparation methods and lays the foundation for a certified reference material for estrogen analysis. The presented method will serve as the basis for an extended validation study to assess its use for estrogen monitoring in the environment. KW - Estrogens KW - Whole water samples KW - Molecular imprinted polymers KW - EU-WFD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563547 DO - https://doi.org/10.1016/j.talo.2022.100163 SN - 2666-8319 VL - 6 SP - 1 EP - 5 PB - Elsevier B.V. CY - Amsterdam, Niederlande AN - OPUS4-56354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - HR-CS-GFMAS as a new screening method for emerging pollutants – per- and polyfluoroalkyl substances (PFASs) in the environment N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of several thousand individual compounds. Many PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods 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. 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 of c(F) 2.7 µg/L. In the present work a HR-CS-GFMAS method for EOF analysis was utilized for suspended particulate matter (SPM) analysis in German rivers in time lines from 2005–2020. Therefore, time and spatial resolved trends were investigated. In addition, SPM samples were analyzed for the Σ41PFAS using target analysis based on UHPLC-HRMS. Overall, target analysis drastically underestimated the total PFAS burden in SPM of German rivers compared to the EOF HR-CS-GFMAS analysis. Using a fluorine mass balance approach, only 0.2% to 38.6% of the EOF was explainable using the Σ41PFAS determined with target analysis. Our study highlights the need to integrate PFAS sum parameters (e.g., EOF with HR-CS-GFMAS) in PFAS risk assessment strategies. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - SPM PY - 2022 AN - OPUS4-56392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbrich, Adelina-Elisa A1 - An Stepec, Biwen Annie A1 - Koerdt, Andrea A1 - Meermann, Björn T1 - Deciphering microbiological influenced corrosion processes on steel with single cell-ICP-ToF-MS N2 - Microbiologically influenced corrosion (MIC) is a highly unpredictable process dictated by the environment, microorganisms, and the respective electron source. Interaction pathways between cells and the metal surface remain unclear. The development of this novel single cell-inductively coupled plasma-time of flight-mass spectrometry analytical method and a MIC-specific staining procedure facilitate the investigation of steel-MIC interactions. With this it is possible to analyze the multi-elemental fingerprint of individual cells. The detection method revealed elemental selectivity for the corrosive methanogenic archaeal strain Methanobacterium-affiliated IM1. The interface between material and environmental analysis thus receives special attention, e.g., when considering MIC on solid steel. Hence, the possible uptake of individual elements from different steel samples is investigated. Results showed the cells responded at a single-cell level to the different types of supplemented elements and displayed the abilities to interact with chromium, vanadium, titanium, cobalt, and molybdenum from solid metal surfaces. The information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts, thus combining modern methods of analytical sciences with materials research. References. T2 - Future WiNS CY - Berlin, Germany DA - 07.12.2022 KW - Single cell KW - Microbiological influenced corrosion MIC KW - Sc-ICP-ToF-MS KW - Method development KW - Ir DNA staining approach KW - Carbon steel corrosion PY - 2022 AN - OPUS4-56567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alcalde-Vasquez, R. A1 - Moreno-Pedraza, A. A1 - Rosas-Román, I. A1 - Guillén-Alonso, H. A1 - Riedel, Jens A1 - Partida-Martínez, L. P. A1 - Winkler, R. T1 - MoBiMS: A Modular Miniature Mass Analyzer for the Real-Time 2 Monitoring of Gases and Volatile Compounds in Biological Systems N2 - Living organisms constantly interact with their environment, including through the exchange of gases. Respiration and the release and uptake of volatile organic compounds (VOCs) create dynamic microenvironments in biological systems. Studying the kinetics of volatiles in biological systems requires expensive instruments, and data analysis is challenging. Therefore, we aimed to design a minimal analytical device for measuring the composition of gaseous mixtures in realtime. We built the ‘Modular Biological Mass Spectrometer’ (MoBiMS) from 3D-printed parts and custom sensors to fit a wide array of experimental set-ups. We tested the chemical detection range and temporal resolution of the MoBiMS employing pure compounds and complex biological samples. Compounds with a higher than 0.4 mmHg vapor pressure and a molecular weight up to 154 g/mol were reliably sensed within seconds. The generated electron impact (EI) spectra were directly comparable with standard databases like the NIST EI library. Under a direct analysis approach, the MoBiMS identified the characteristic odor of banana (Musa sp.), that is, isoamyl acetate; tracked the dynamics of CO2 release while the Alka-Seltzer® reaction occurred showed the kinetics of the transient production and consumption of carbon dioxide during photosynthesis. MoBiMS also discriminated between volatile compounds ions coming from tobacco (Nicotiana benthamiana) leaves and the surrounding air through untargeted analysis. The small footprint of the MoBiMS and its relatively low energy consumption facilitate in situ analyses, as an additional gas supply is not necessary with EI ionization. The MoBiMS is easy to assemble, and its construction and operation are very cost-efficient compared to commercial devices. The analytical performance of the MoBiMS is suitable for real-time studies of biological systems, environmental monitoring, and medical diagnostics. KW - Mass spectrometry KW - Instrumentation KW - Miniaturization KW - Volatiles PY - 2022 DO - https://doi.org/10.1016/j.microc.2021.107090 SN - 0026-265X VL - 175 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-56528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van Wasen, S. A1 - You, Yi A1 - Beck, S. A1 - Riedel, Jens A1 - Volmer, D. A. T1 - Laser Ablation Secondary Electrospray Ionization for In Situ Mass Spectrometric Interrogation of Acoustically-Levitated Droplets N2 - The composition of acoustically levitated droplets was probed by a novel combination of mid-IR laser evaporation and subsequent postionization via secondary electrospray ionization. The combination of microliter samples and subnanoliter sampling provided time-resolved interrogation of droplets and allowed for a kinetic investigation of the laser-induced release of the analyte, which was found to strongly depend on the analytes. The observed substancespecific delayed release of the analytes permitted baseline-separated discrimination of the analytes, ideal for the study of complex samples. The additionally applied postionization scheme was found to enable efficient detection of small volatile compounds as well as peptides. The detection of small molecules and peptides occurred under very different sampling geometries, pointing to two distinct underlying ionization mechanisms. Overall, our results suggest that the experimental setup presented in this study can serve as a widely applicable platform to study chemical reactions in acoustically levitated droplets as model reactors. KW - Acoustic levitation KW - Mass spectrometry KW - Electrospray KW - Laser ablation PY - 2022 DO - https://doi.org/10.1021/acs.analchem.2c03800 SN - 0003-2700 VL - 2022 SP - 1 EP - 5 PB - ACS Publications CY - Washington AN - OPUS4-56531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn A1 - Faßbender, Sebastian A1 - Tukhmetova, Dariya A1 - Rodiouchkina, K. A1 - Vanhaecke, F. T1 - On-line hyphenation of capillary electrophoresis with multicollector-ICP-MS (CE/MC-ICP-MS) for species-specific isotope ratio analysis of sulfur species N2 - In many scientific fields, isotopic analysis can offer valuable information, e.g., for tracing the origin of food products, environmental contaminants, forensic and archaeological samples (provenance determination), for age determination of minerals (geochronological dating) or for elucidating chemical processes. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different elemental species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared with data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was high enough to distinguish the rivers from one another by the isotopic signature of the river water sulfate. Next to environmental applications, a current field is species-specific isotopic analysis of biomolecules, as sulfur is the only covalently bound constituent of proteins which can be analyzed by MC-ICP-MS. Data analysis of transient signals in terms of isotope ratio determination is further issue - we developed a small free accessible App allowing for fast data analysis taking relevant aspects (e.g., mass bias correction, peak picking, …) into account. T2 - SCIX 2022 CY - Cincinnati, OH, USA DA - 02.10.2022 KW - CE KW - MC-ICP-MS KW - Speciation Analysis KW - Species-specific Isotope ratios PY - 2022 AN - OPUS4-56543 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuner, Maximilian A1 - Kühn, Susanne A1 - Koch, Matthias A1 - Haase, Hajo T1 - Cleaving ergot alkaloids - development of a novel food screening method N2 - Mycotoxins (toxic compounds formed by fungi) in food and feed have caused problems for mankind since the beginning of time. The group of ergot alkaloids plays a special role in human history. Several tens of thousands of deaths during the middle ages caused by to ergotism (the disease caused by continuous intake of ergot alkaloid contaminated food) underscore the importance of reliable analytical methods to ensure food safety. More than 50 compounds belong to the group of ergot alkaloids. The 12 most found structures – the major ergot alkaloids – are typically measured, when it comes to ergot alkaloid quantification. High performance liquid chromatography (HPLC) with a fluorescence detector (FLD) is typically used to quantify the ergot alkaloid content. The main disadvantage of this method are the high costs for calibration standards (12 different calibration substances are required). But also, the time and effort required for the analysis of 12 peaks and overlapping signals that occur in complex food samples such as bread. As all ergot alkaloids share the ergoline structure and just differ in the substituents attached to this backbone, measurement of all ergot alkaloids in one sum parameter presents a time and cost saving alternative. The most important step for the development of such a sum parameter method is the reaction used to transfer all ergot alkaloids to one uniform structure. Two promising reactions, the acidic esterification to lysergic acid methyl ester and hydrazinolysis to lysergic acid hydrazide, were examined for possible use in a routine analysis method. In addition to yield and reaction rate, factors such as handling of the reaction and the possibility of parallel sample workup play a role. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - Ergot alkaloids KW - Screening PY - 2022 AN - OPUS4-56585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuner, Maximilian T1 - Quantification of ergot alkaloids - a glimpse into the future N2 - Mycotoxins (toxins formed by fungi) in food and have caused problems for mankind since the beginning of time. The group of ergot alkaloids plays a special role in human history. Several tens of thousands of deaths during the middle ages caused by to ergotism (the disease caused by continuous intake of ergot alkaloid contaminated food) underscore the importance of reliable analytical methods to ensure food safety. More than 50 compounds belong to the group of ergot alkaloids. The 12 most found structures – the major ergot alkaloids – are typically measured, when it comes to ergot alkaloid quantification. High performance liquid chromatography (HPLC) with a fluorescence detector (FLD) is typically used to quantify the ergot alkaloid content. The main disadvantage of this method are the high costs for calibration standards (12 different calibration substances are required). But also the time and effort required for the analysis of 12 peaks and overlapping signals that occur in complex food samples such as bread. As all ergot alkaloids share the ergoline structure and just differ in the substituents attached to this backbone, measurement of all ergot alkaloids in one sum parameter presents a time and cost saving alternative. The most important step for the development of such a sum parameter method is the reaction used to transfer all ergot alkaloids to one uniform structure. In the talk two promising reactions, the acidic esterification to lysergic acid methyl ester and hydrazinolysis to lysergic acid hydrazide, are examined for possible use in a routine analysis method. In addition to yield and reaction rate, factor such as the handling of the reaction and the possibility of parallelization play a role. Next to the current status of the ongoing research project, in this talk, current approaches to ergot alkaloid quantitation will be discussed. T2 - FOODMETNET MycoTWIN JOINT TRAINING COURSE 2022 CY - Gebze, Turkey DA - 22.11.2022 KW - Ergot alkaloids KW - Sum Parameter PY - 2022 AN - OPUS4-56586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von der Au, Marcus A1 - Meermann, Björn T1 - MDG-ICP-MS - A Versatile Tool for Quantification in the field of Single Particle ICP-MS Using Isotopic Dilution N2 - In the interest of exploring their potential in the field of single particle analysis, a Microdroplet Generator (MDG) was coupled to an ICP-ToF-MS. Isotopic Dilution Analysis was also incorporated for the size determination of three different Platinum Nanoparticles samples (50, 63 and 70 nm). The performance of the technique was validated by comparison to traditional size characterization techniques (sp-ICP-ToF-MS, TEM), while the robustness of the technique was proven by incorporating NaCl in the samples’ matrix, up to 100 mg/L. T2 - SciX 2022 CY - Cincinnati, OH, USA DA - 02.10.2022 KW - MDG KW - ICP-TOF-MS KW - Nanoparticle PY - 2022 AN - OPUS4-56554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pollard, M. A1 - Heck, M. A1 - Wilhelm, M. A1 - Weidner, Steffen T1 - Functionalized Poly(ethylene glycol)s (PEGs) as a Reference Material for Detection of Polymeric end Groups via SEC Hyphenated with FTIR and 1H-NMR (80 MHz) N2 - With the online coupling (or hyphenation) of chemically-resolved spectroscopy detection with classical size-exclusion chromatography (SEC) it is possible to correlate polymer molecular size with chemical structure in a single in-situ or on-flow measurement. Medium-resolution 1H-NMR (60 MHz) spectroscopy (i.e., “desktop NMR”) and Fouriertransform Infrared Spectroscopy (FTIR) have both been developed as coupled methods (SEC-MR-NMR, SEC-FTIR) for the detection of polymer analytes by monitoring e.g. alkene or carbonyl functionality.1,2 Here, we have investigated the potential for the detection of polymer end groups, using a slightly higher field-strength spectrometer (80 MHz 1H Larmor frequency) and taking advantage of a columnless injection method that provides bulk spectra for reference. End-functionalized polymers were synthesized by reaction of PEG with toluene isocyanate, yielding ,-functionalized polymers with exactly 2 IR- and NMR-detectable functional groups per chain, as proven by MALD-TOF mass spectrometry. We have investigated the sensitivity (limit of detection) and spectral resolution for these functional groups in chloroform, THF, and water. Results have demonstrated a good feasibility for the simultaneous online detection of PEG backbone (M~4000 g/mol) and these end groups at the level of ca. 2 mol%. T2 - 33rd International Symposium on Chromatography CY - Budapest DA - 18.09.2022 KW - Size exclusion chromatography KW - Polyethyleneglycol KW - MALDI-TOF MS KW - NMR PY - 2022 AN - OPUS4-56716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Anderhalten, L. A1 - Silva, R. V. A1 - Morr, A. A1 - Wang, S. A1 - Smorodchenko, A. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Mueller, S. A1 - Boehm-Sturm, P. A1 - Rodriguez-Sillke, Y. A1 - Kunkel, D. A1 - Hahndorf, J. A1 - Paul, F. A1 - Taupitz, M. A1 - Sack, I. A1 - Infante-Duarte, C. T1 - Different Impact of Gadopentetate and Gadobutrol on Inflammation-Promoted Retention and Toxicity of Gadolinium Within the Mouse Brain N2 - Objectives: Using a murine model of multiple sclerosis, we previously showed that repeated administration of gadopentetate dimeglumine led to retention of gadolinium (Gd) within cerebellar structures and that this process was enhanced with inflammation. This study aimed to compare the kinetics and retention profiles of Gd in inflamed and healthy brains after application of the macrocyclic Gd-based contrast agent (GBCA) gadobutrol or the linear GBCA gadopentetate. Moreover, potential Gd-induced neurotoxicity was investigated in living hippocampal slices ex vivo. Materials and Methods: Mice at peak of experimental autoimmune encephalomyelitis (EAE; n = 29) and healthy control mice (HC; n = 24) were exposed to a cumulative dose of 20 mmol/kg bodyweight of either gadopentetate dimeglumine or gadobutrol (8 injections of 2.5 mmol/kg over 10 days). Magnetic resonance imaging (7 T) was performed at baseline as well as at day 1, 10, and 40 post final injection (pfi) of GBCAs. Mice were sacrificed after magnetic resonance imaging and brain and blood Gd content was assessed by laser ablation-inductively coupled plasma (ICP)-mass spectrometry (MS) and ICP-MS, respectively. In addition, using chronic organotypic hippocampal slice cultures, Gd-induced neurotoxicity was addressed in living brain tissue ex vivo, both under control or inflammatory (tumor necrosis factor α [TNF-α] at 50 ng/μL) conditions. Results: Neuroinflammation promoted a significant decrease in T1 relaxation times after multiple injections of both GBCAs as shown by quantitative T1 mapping of EAE brains compared with HC. This corresponded to higher Gd retention within the EAE brains at 1, 10, and 40 days pfi as determined by laser ablation-ICP-MS. In inflamed cerebellum, in particular in the deep cerebellar nuclei (CN), elevated Gd retention was observed until day 40 after last gadopentetate application (CN: EAE vs HC, 55.06 ± 0.16 μM vs 30.44 ± 4.43 μM). In contrast, gadobutrol application led to a rather diffuse Gd content in the inflamed brains, which strongly diminished until day 40 (CN: EAE vs HC, 0.38 ± 0.08 μM vs 0.17 ± 0.03 μM). The analysis of cytotoxic effects of both GBCAs using living brain tissue revealed an elevated cell death rate after incubation with gadopentetate but not gadobutrol at 50 mM. The cytotoxic effect due to gadopentetate increased in the presence of the inflammatory mediator TNF-α (with vs without TNF-α, 3.15% ± 1.18% vs 2.17% ± 1.14%; P = 0.0345). Conclusions: In the EAE model, neuroinflammation promoted increased Gd retention in the brain for both GBCAs. Whereas in the inflamed brains, efficient clearance of macrocyclic gadobutrol during the investigated time period was observed, the Gd retention after application of linear gadopentetate persisted over the entire observational period. Gadopentetate but not gadubutrol appeared to be neurotoxic in an ex vivo paradigm of neuronal inflammation. KW - Imaging KW - ICP-MS KW - Gadolinium KW - Contrast agent KW - Laser ablation KW - Brain KW - Multiple sclerosis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546910 DO - https://doi.org/10.1097/RLI.0000000000000884 SN - 0020-9996/22/0000–0000 VL - 57 IS - 10 SP - 677 EP - 688 PB - Wolters Kluwer N.V. CY - Alphen aan den Rijn, The Netherlands AN - OPUS4-54691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martins, Ines A1 - Al-Sabbagh, Dominik A1 - Bentrup, U. A1 - Marquardt, Julien A1 - Schmid, Thomas A1 - Scoppola, E. A1 - Kraus, Werner A1 - Stawski, Tomasz A1 - de Oliveira Guilherme Buzanich, Ana A1 - Yusenko, Kirill A1 - Weidner, Steffen A1 - Emmerling, Franziska T1 - Formation Mechanism of a Nano-Ring of Bismuth Cations and Mono-Lacunary Keggin-Type Phosphomolybdate N2 - A new hetero-bimetallic polyoxometalate (POM) nano-ring was synthesized in a one-pot procedure. The structure consists of tetrameric units containing four bismuth-substituted monolacunary Keggin anions including distorted [BiO8] cubes. The nano-ring is formed via self-assembly from metal precursors in aqueous acidic medium. The compound (NH4)16[(BiPMo11O39)4] ⋅ 22 H2O; (P4Bi4Mo44) was characterized by single-crystal X-ray diffraction, extended X-ray absorption fine structure spectroscopy (EXAFS), Raman spectroscopy, matrix-assisted laser desorption/ionisation-time of flight mass spectrometry (MALDI-TOF), and thermogravimetry/differential scanning calorimetry mass spectrometry (TG-DSC-MS). The formation of the nano-ring in solution was studied by time-resolved in situ small- and wide-angle X-ray scattering (SAXS/WAXS) and in situ EXAFS measurements at the Mo−K and the Bi−L3 edge indicating a two-step process consisting of condensation of Mo-anions and formation of Bi−Mo-units followed by a rapid self-assembly to yield the final tetrameric ring structure. KW - Bismuth KW - In situ EXAFS KW - In situ SAXS/WAXS KW - Lacunary Keggin ion KW - Polyoxometalates KW - Self-assembly PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546823 DO - https://doi.org/10.1002/chem.202200079 SN - 0947-6539 VL - 28 IS - 27 SP - 1 EP - 7 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Meermann, Björn T1 - Schnelle und einfache Extraktion von PFAS aus Bodenproben: Optimierte EOF-Bestimmung mittels HR-CS-GFMAS N2 - Per- und polyfluorierte Alkylsubstanzen (PFAS) bilden eine sehr komplexe Schadstoffgruppe mit über 6300 Einzelsubstanzen, die in vielfältiger Form in die Umwelt eingetragen werden. Für ein effektives Monitoring dieser Schadstoffklasse benötigt es ein Zusammenspiel aus Summenparameter-Analytik zur hot-spot-Identifizierung und Klassifizierung von Belastungssituationen sowie einer nachgeschalteten target-Analytik zur Identifizierung von Eintragswegen, die zugleich ein tieferes Verständnis von Transformationsprozessen ermöglicht. In diesem Beitrag präsentieren wir eine optimierte Extraktions-Methode für die PFAS-Summenparameteranalytik. Mit Hilfe dieser können bisher verwendete zeit- und kostenintensive Festphasenextraktionen (SPE) umgangen und PFAS-Extraktionseffizienzen gesteigert werden. Die methodische Bestimmungsgrenze (LOQ) war mit 10,30 μg/kg (Fluor pro Bodenprobe) ausreichend für alle 9 untersuchten Realbodenproben. KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - PFAS KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction KW - Böden PY - 2022 UR - https://www.gdch.de/fileadmin/downloads/Netzwerk_und_Strukturen/Fachgruppen/Umweltchemie_Oekotoxikologie/mblatt/2022/Heft122.pdf SN - 1618-3258 VL - 28 IS - 1 SP - 12 EP - 15 PB - Gesellschaft Deutscher Chemiker AN - OPUS4-54417 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knoche, Lisa A1 - Lisec, Jan A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - LC-HRMS-Based Identification of Transformation Products of the Drug Salinomycin Generated by Electrochemistry and Liver Microsome N2 - The drug salinomycin (SAL) is a polyether antibiotic and used in veterinary Medicine as coccidiostat and growth promoter. Recently, SAL was suggested as a potential anticancer drug. However, transformation products (TPs) resulting from metabolic and environmental degradation of SAL are incompletely known and structural information is missing. In this study, we therefore systematically investigated the formation and identification of SAL derived TPs using electrochemistry (EC) in an electrochemical reactor and rat and human liver microsome incubation (RLM and HLM) as TP generating methods. Liquid chromatography (LC) coupled to high-resolution mass spectrometry (HRMS) was applied to determine accurate masses in a suspected target analysis to identify TPs and to deduce occurring modification reactions of derived TPs. A total of 14 new, structurally different TPs were found (two EC-TPs, five RLM-TPs, and 11 HLM-TPs). The main modification reactions are decarbonylation for EC-TPs and oxidation (hydroxylation) for RLM/HLM-TPs. Of particular interest are potassium-based TPs identified after liver microsome incubation because these might have been overlooked or declared as oxidated sodium adducts in previous, non-HRMS-based studies due to the small mass difference between K and O + Na of 21 mDa. The MS fragmentation pattern of TPs was used to predict the position of identified modifications in the SAL molecule. The obtained knowledge regarding transformation reactions and novel TPs of SAL will contribute to elucidate SAL-metabolites with regards to structural prediction. KW - Salinomycin KW - Ionophore antibiotics KW - Transformation product KW - Electrochemistry KW - Rat/human liver microsomes KW - HRMS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542543 DO - https://doi.org/10.3390/antibiotics11020155 SN - 2079-6382 VL - 11 IS - 2 SP - 155 PB - MDPI CY - Basel AN - OPUS4-54254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Boyraz, B. A1 - Saatz, Jessica A1 - Pompös, I.-M. A1 - Gad, Michel A1 - Dernedde, J. A1 - Maier, A.-M. B. A1 - Moscovitz, O. A1 - Seeberger, P. H. A1 - Traub, Heike A1 - Tauber, R. T1 - Imaging Keratan Sulfate in Ocular Tissue Sections by Immunofluorescence Microscopy and LA-ICP-MS N2 - Carbohydrate-specific antibodies can serve as valuable tools to monitor alterations in the extracellular matrix resulting from pathologies. Here, the keratan sulfate-specific monoclonal antibody MZ15 was characterized in more detail by immunofluorescence microscopy as well as laser ablation ICP-MS using tissue cryosections and paraffin-embedded samples. Pretreatment with keratanase II prevented staining of samples and therefore demonstrated efficient enzymatic keratan sulfate degradation. Random fluorescent labeling and site-directed introduction of a metal cage into MZ15 were successful and allowed for a highly sensitive detection of the keratan sulfate landscape in the corneal stroma from rats and human tissue. KW - Laser ablation KW - Imaging KW - Glycosaminoglycan KW - ICP-MS KW - Immunohistochemistry KW - Immunofluorescence KW - Tissue PY - 2022 DO - https://doi.org/10.1021/acsabm.1c01240 VL - 5 IS - 2 SP - 853 EP - 861 PB - American Chemical Society CY - Washington AN - OPUS4-54341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Casali, C. A1 - Feiler, Torvid A1 - Heilmann, Maria A1 - Braga, D. A1 - Emmerling, Franziska A1 - Grepioni, F. T1 - Too much water? Not enough? In situ monitoring of the mechanochemical reaction of copper salts with dicyandiamide N2 - n situ monitoring of mechanochemical reactions between dicyandiamide (DCD) and CuX2 salts (X = Cl−, NO3−), for the preparation of compounds of agrochemical interest, showed the appearance of a number of phases. It is demonstrated that milling conditions, such as the amount of water added in wet grinding and/or the milling frequency, may affect the course of the mechanochemical reactions, and drive the reaction towards the formation of different products. It has been possible to discover by in situ monitored experiments two novel crystalline forms, namely the neutral complexes [Cu(DCD)2(OH2)2(NO3)2] (2) and [Cu(DCD)2(OH2)Cl2]·H2O (4), in addition to the previously known molecular salt [Cu(DCD)2(OH2)2][NO3]2·2H2O (1, DIVWAG) and neutral complex [Cu(DCD)2(OH2)Cl2] (3, AQCYCU), for which no synthesis conditions were available. Compounds 2 and 4 were fully characterized via a combination of solid-state techniques, including X-ray diffraction, Raman spectroscopy and TGA. KW - Mechanochemistry KW - In situ PY - 2022 DO - https://doi.org/10.1039/d1ce01670a VL - 24 IS - 6 SP - 1292 EP - 1298 PB - RSC AN - OPUS4-54344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - von der Au, Marcus A1 - Wittwer, Phillip A1 - Roesch, Philipp A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Meermann, Björn T1 - A fast and simple PFAS extraction method utilizing HR–CS–GFMAS for soil samples N2 - Here, we describe an optimized fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) in soils utilizing high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR–CS–GFMAS). To omit the bias of the solid phase extraction (SPE) step commonly used during the analysis of extractable organically bound fluorine (EOF) we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol without any additional SPE. Four extraction steps were representative to determine a high proportion of the EOF (>80% of eight extractions). Comparison of the optimized method with and without an additional SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. Differences of up to 94% were observed which were not explainable by coextracted inorganic fluoride. Therefore, not only a more accurate but also a more economic as well as ecologic method (bypassing of unnecessary SPE) was developed. The procedural limit of quantification (LOQ) of the developed method was 10.30 μg/kg which was sufficient for quantifying EOF concentrations in all tested samples. For future PFAS monitoring and potential regulative decisions the herein presented optimized extraction method can offer a valuable contribution. KW - Per- and polyfluorinated alkly substances (PFASs) KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Soils KW - Solid phase extraction (SPE) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction PY - 2022 DO - https://doi.org/10.1016/j.chemosphere.2022.133922 VL - 295 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-54359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frisch, M. A1 - Raza, M. H. A1 - Ye, M.-Y. A1 - Sachse, René A1 - Paul, B. A1 - Gunder, R. A1 - Pinna, N. A1 - Kraehnert, R. T1 - ALD-coated mesoporous iridium-titanium mixed oxides: Maximizing iridium utilization for an outstanding OER performance N2 - With the increasing production of renewable energy and concomitant depletion of fossil resources, the demand for efficient water splitting electrocatalysts continues to grow. Iridium (Ir) and iridium oxides (IrOₓ) are currently the most promising candidates for an efficient oxygen evolution reaction (OER) in acidic medium, which remains the bottleneck in water electrolysis. Yet, the extremely high costs for Ir hamper a widespread production of hydrogen (H₂) on an industrial scale. Herein, the authors report a concept for the synthesis of electrode coatings with template-controlled mesoporosity surface-modified with highly active Ir species. The improved utilization of noble metal species relies on the synthesis of soft-templated metal oxide supports and a subsequent shape-conformal deposition of Ir species via atomic layer deposition (ALD) at two different reaction temperatures. The study reveals that a minimum Ir content in the mesoporous titania-based support is mandatory to provide a sufficient electrical bulk conductivity. After ALD, a significantly enhanced OER activity results in dependency of the ALD cycle number and temperature. The most active developed electrocatalyst film achieves an outstanding mass-specific activity of 2622 mA mg(Ir)⁻¹ at 1.60 V(RHE) in a rotating-disc electrode (RDE) setup at 25 °C using 0.5 m H₂SO₄ as a supporting electrolyte. KW - Acidic oxygen evolution reaction KW - Atomic layer deposition KW - Electrocatalysis KW - Iridium oxide KW - Soft-templated mesoporous films PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542651 DO - https://doi.org/10.1002/admi.202102035 SN - 2196-7350 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munir, R. A1 - Lisec, Jan A1 - Swinnen, J. V. A1 - Zaidi, N. T1 - Too complex to fail? Targeting fatty acid metabolism for cancer therapy N2 - Given the central role of fatty acids in cancer pathophysiology, the exploitation of fatty acid metabolism as a potential antineoplastic therapy has gained much attention. Several natural and synthetic compounds targeting fatty acid metabolism were hitherto identified, and their effectiveness against cancer cell proliferation and survival was determined. This review will discuss the most clinically viable inhibitors or drugs targeting various proteins or enzymes mapped on nine interconnected fatty acid metabolism-related processes. We will discuss the general significance of each of these processes and the effects of their inhibition on cancer cell progression. Moreover, their mechanisms of action, limitations, and future perspectives will be assessed. KW - Fatty acids KW - Fatty acid synthesis KW - Fatty acid desaturation KW - Fatty acid uptake KW - Cancer therapy PY - 2022 DO - https://doi.org/10.1016/j.plipres.2021.101143 SN - 0163-7827 VL - 85 SP - 1 EP - 12 PB - Elsevier AN - OPUS4-53864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munir, R. A1 - Noureen, N. A1 - Bashir, M. A1 - Shoaib, N. A1 - Ashraf, A. A1 - Lisec, Jan A1 - Zaidi, N. T1 - Cancer Awareness Measure (CAM) and Cancer Awareness Measure MYthical Causes Scale (CAM‑MY) scores in Pakistani population N2 - Lifestyle modifications could prevent almost one‑third to one‑half of all cancer cases. The awareness of cancer risk factors could motivate people to make such changes in their behaviors and lifestyles. This work aims to investigate the cancer awareness level in the Pakistani population. Telephone interviews of 657 individuals in Pakistan were carried out using the Cancer Awareness Measure (CAM) and Cancer Awareness Measure–MYthical Causes Scale (CAM‑MY). We observed that participants scored significantly better on the CAM scale than the CAM‑MY scale, and CAM scores were negatively associated with CAM‑MY scores. Years of formal education or a biology major at undergraduate or graduate level did not affect our population’s cancer awareness levels. Age displayed a weak but statistically significant negative association with CAM scores. Most participants failed to identify modifiable cancer risk factors, e.g., low physical activity. Efforts should be made to improve awareness of modifiable risk factors. We observed that brief training sessions could markedly improve people’s understanding of cancer risk factors and myths. KW - Cancer KW - Cancer awareness measure KW - Cancer risk PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548960 DO - https://doi.org/10.1038/s41598-022-13012-8 SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 10 PB - Nature Publishing Group CY - London AN - OPUS4-54896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - An improved method for the determination of PFAS using HR-CS-GFMAS via GaF detection N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods 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. 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 of c(F) 2.7 µg/L. Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a Ga pretreatment as described by Gawor et al. resulting in overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analyzed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for EOF determination in soils. T2 - ESAS - CSSC CY - Brno, Czech Republic DA - 04.09.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2022 AN - OPUS4-55782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - An improved method for the determination of PFAS using HR-CS-GFMAS via GaF detection N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods 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. 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 of c(F) 2.7 µg/L. Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a Ga pretreatment as described by Gawor et al. resulting in overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analyzed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for EOF determination in soils. T2 - SALSA - Communicating Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2022 AN - OPUS4-55783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbrich, Adelina-Elisa A1 - An-Stepec, Biwen A1 - Koerdt, Andrea A1 - Meermann, Björn T1 - Multielemental analysis of MIC organisms grown on solid steel samples by means of single cell-ICP-ToF-MS N2 - Inductively coupled plasma-time of flight-mass spectrometry (ICP-ToF-MS) enables the analysis of the multi-element fingerprint of individual cells due to a (quasi-)simultaneous detection of about 70 elements of the periodic table. The interface between material and environmental analysis thus receives special attention, e.g., when considering corrosion processes. Microbiologically influenced corrosion (MIC) is a highly unpredictable phenomenon due to the influence of the environment, microbial communities involved and the respective electron source. However, the interaction pathway between cells and the metal surface remains unclear. The development of the MIC-specific ICP-ToF-MS analytical method presented here, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis and will enable clarification of the processes taking place. For this, a MIC-specific staining procedure was developed which ensures the analysis of intact cells. It allows the studies of archaea at a single cell level which is extremely scarce compared to other well characterized organisms. Additionally, the single cell ICP-ToF-MS is used for the analysis of archaea involved in MIC of steel. Hence, the possible uptake of individual elements from different steel samples is investigated - the information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts, thus combining modern methods of analytical sciences with materials research. T2 - DGMS Young Scientists Fall Meeting 2022 CY - Hünfeld, Germany DA - 28.09.2022 KW - Single cell KW - Microbiological influenced corrosion MIC KW - Sc-ICP-ToF-MS KW - Method development PY - 2022 AN - OPUS4-55910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Bliesener, Lilly A1 - Weiss, Tilman A1 - Koch, Matthias T1 - Marker Substances in the Aroma of Truffles N2 - The aim of this study was to identify specific truffle marker substances within the truffle aroma. The aroma profile of different truffle species was analyzed using static headspace sampling with gas chromatography mass spectrometry analysis (SHS/GC-MS). Possible marker substances were identified, taking the additional literature into account. The selected marker substances were tested in an experiment with 19 truffle dogs. The hypothesis “If trained truffle dogs recognize the substances as supposed truffles in the context of an experiment, they can be regarded as specific” was made. As it would be nearly impossible to investigate every other possible emitter of the same compounds to determine their specificity, this hypothesis was a reasonable approximation. We were interested in the question of what it is the dogs actually search for on a chemical level and whether we can link their ability to find truffles to one or more specific marker substances. The results of the dog experiment are not as unambiguous as could have been expected based on the SHS/GC-MS measurements. Presumably, the truffle aroma is mainly characterized and perceived by dogs by dimethyl sulfide and dimethyl disulfide. However, as dogs are living beings and not analytical instruments, it seems unavoidable that one must live with some degree of uncertainty regarding these results. KW - Truffle KW - Volatile organic compounds; KW - Gas chromatography KW - Mass spectrometry KW - Canine olfactometry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556116 DO - https://doi.org/10.3390/molecules27165169 SN - 1420-3049 VL - 27 IS - 16 SP - 1 EP - 19 PB - MDPI CY - Basel AN - OPUS4-55611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane A1 - Juritsch, Elevtheria A1 - Richter, Matthias T1 - Development of a procedure for the analysis of the emissions of VVOCs – Results of a research project N2 - Since 1997, the Committee for Health-related Evaluation of Building Products (AgBB) has been developing the basis for building regulations for protection against indoor health risks that may arise when building products are used. In 2009, the AgBB decided to include relevant VVOCs in the assessment procedure. The ISO 16000-6 (2021) states that the use of the thermal desorption gas chromatography technique is appropriate for VVOCs, if adaptations are considered. However, a suitable method for the trustworthy quantification of VVOC emissions from building products and in the indoor air is still missing. This webinar will present the results of a research project on the development of a procedure for VVOC analysis: • identification of the gaps towards standardization • investigations on gas standards and the suitability of chromatography columns • investigations on sorbent combinations and water management • validation of the method and screening of VVOC emissions from building products. T2 - Webinar organized by Umweltbundesamt and BAM CY - Online meeting DA - 13.09.2022 KW - Analytical method KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Spallanzani, Roberta A1 - Koga, K. A1 - Cichy, S. A1 - Wiedenbeck, M. A1 - Schmidt, B. A1 - Oelze, Marcus A1 - Wilke, M. T1 - Lithium and boron difusivity and isotopic fractionation in hydrated rhyolitic melts N2 - Lithium and boron are trace components of magmas, released during exsolution of a gas phase during volcanic activity. In this study, we determine the difusivity and isotopic fractionation of Li and B in hydrous silicate melts. Two glasses were synthesized with the same rhyolitic composition (4.2 wt% water), having diferent Li and B contents; these were studied in difusion-couple experiments that were performed using an internally heated pressure vessel, operated at 300 MPa in the temperature range 700–1250 °C for durations from 0 s to 24 h. From this we determined activation energies for Li and B difusion of 57±4 kJ/mol and 152±15 kJ/mol with pre-exponential factors of 1.53 × 10–7 m2/s and 3.80× 10–8 m2 /s, respectively. Lithium isotopic fractionation during difusion gave β values between 0.15 and 0.20, whereas B showed no clear isotopic fractionation. Our Li difusivities and isotopic fractionation results difer somewhat from earlier published values, but overall confrm that Li difusivity increases with water content. Our results on B difusion show that similarly to Li, B mobility increases in the presence of water. By applying the Eyring relation, we confrm that B difusivity is limited by viscous fow in silicate melts. Our results on Li and B difusion present a new tool for understanding degassing-related processes, ofering a potential geospeedometer to measure volcanic ascent rates. KW - Hydrated silicate melts KW - Stable isotopes KW - Diffusion KW - Isotopic fractionation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554496 DO - https://doi.org/10.1007/s00410-022-01937-2 VL - 177 IS - 8 SP - 1 EP - 17 PB - Springer AN - OPUS4-55449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - New possibilities in single cell analysis via ICP-ToF-MS – zooming into the region where materials meet environment N2 - Materials are key for our modern communities; current life seems nearly impossible without concrete, plastic and metal. In particular metals play important roles in all areas of our daily life - from building materials to high tech products. However, due to the increasing consumption of metals and corresponding waste production, an elevated release of metals from buildings and consumer goods into the environment takes place. Furthermore, metals in direct contact with the environment undergo corrosion processes which leads also to a release of metals into the (aquatic) environment. Besides this immediate metal release, the lifespan of products/buildings are substantially reduced – hence unnecessary economic costs arise. Thus, research in this regard is needed within the force field of metal/material  environment. However, to evaluate the environmental impact of materials as well as developing “safe” materials, new analytical methods are highly needed. One promising powerful tool in this regard is single cell-ICP-ToF-MS for multi-elemental analysis on a single cell/organism level. Within this presentation the concept, strength as well as challenge of single cell-ICP-MS are briefly introduced. Afterwards, two application examples are presented: (i) assessing the environmental impact of metals and (ii) the impact of the environment on metal-based materials and the derivation of potential environmental-friendly material protection strategies. These applications highlight the strength of new analytical approaches to explore the durability and safety of newly developed materials. Thus, analytical chemistry is one corner stone to transformation of modern society into circular economy (CEco). (i) Diatoms are located at the bottom of the food chain. Thus, toxicological relevant metals taken up by diatoms can possibly accumulate within the food web and cause harmful effects. Diatoms are a common test system in ecotoxicology. To investigate potential metal uptake and harmful effects on a single cell level, we developed an on-line single cell-ICP-ToF-MS approach for multi-elemental diatom analysis. Our approach is a new potential tool in ecotoxicological testing for metal-based materials. (ii) Next to classical corrosion processes, microorganisms are responsible for so called microbially influenced corrosion (MIC). MIC is a highly unpredictable process relying on the interaction pathways between cells and the metal surface. To shed light on MIC processes and derivate potential metal protection strategies, we applied single cell-ICP-ToF-MS for MIC research on a single bacteria/archaea level. It turned out that microorganism are taking up particular metals from alloys - thus, single bacteria-ICP-ToF-MS will enable the development of environmental friendly corrosion protection strategies. T2 - 10th Nordic Conference on Plasma Spectrochemistry CY - Loen, Norway DA - 12.06.2022 KW - sc-ICP-ToF-MS KW - Material - Environment interaction KW - Diatom, Bacteria PY - 2022 AN - OPUS4-55533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Golusda, L. A1 - Kühl, A. A. A1 - Lehmann, M. A1 - Dahlke, K. A1 - Mueller, S. A1 - Boehm-Sturm, P. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Schnorr, J. A1 - Freise, C. A1 - Taupitz, M. A1 - Biskup, K. A1 - Blanchard, V. A1 - Klein, O. A1 - Sack, I. A1 - Siegmund, B. A1 - Paclik, D. T1 - Visualization of inflammation in experimental colitis by magnetic resonance imaging using very small superparamagnetic iron oxide particles N2 - Inflammatory bowel diseases (IBD) comprise mainly ulcerative colitis (UC) and Crohn´s disease (CD). Both forms present with a chronic inflammation of the (gastro) intestinal tract, which induces excessive changes in the composition of the associated extracellular matrix (ECM). In UC, the inflammation is limited to the colon, whereas it can occur throughout the entire gastrointestinal tract in CD. Tools for early diagnosis of IBD are still very limited and highly invasive and measures for standardized evaluation of structural changes are scarce. To investigate an efficient non-invasive way of diagnosing intestinal inflammation and early changes of the ECM, very small superparamagnetic iron oxide nanoparticles (VSOPs) in magnetic resonance imaging (MRI) were applied in two mouse models of experimental colitis: the dextran sulfate sodium (DSS)-induced colitis and the transfer model of colitis. For further validation of ECM changes and inflammation, tissue sections were analyzed by immunohistochemistry. For in depth ex-vivo investigation of VSOPs localization within the tissue, Europium-doped VSOPs served to visualize the contrast agent by imaging mass cytometry (IMC). VSOPs accumulation in the inflamed colon wall of DSS-induced colitis mice was visualized in T2* weighted MRI scans. Components of the ECM, especially the hyaluronic acid content, were found to influence VSOPs binding. Using IMC, colocalization of VSOPs with macrophages and endothelial cells in colon tissue was shown. In contrast to the DSS model, colonic inflammation could not be visualized with VSOP-enhanced MRI in transfer colitis. VSOPs present a potential contrast agent for contrast-enhanced MRI to detect intestinal inflammation in mice at an early stage and in a less invasive manner depending on hyaluronic acid content. KW - Inflammation KW - Imaging KW - Immunohistochemistry KW - MRI KW - Nanoparticle KW - Extracellular matrix KW - Laser ablation KW - ICP-MS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555395 DO - https://doi.org/10.3389/fphys.2022.862212 SN - 1664-042X VL - 13 IS - July 2022 SP - 1 EP - 15 PB - Frontiers Research Foundation CY - Lausanne AN - OPUS4-55539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falqueto, J. B. A1 - Clark, A. H. A1 - Štefančič, A. A1 - Smales, Glen Jacob A1 - Vaz, C. A. F. A1 - Schuler, A. J. A1 - Bocchi, N. A1 - Kazzi, M. E. T1 - High performance doped Li-rich Li1+xMn2–xO4 cathodes nanoparticles synthesized by facile, fast, and efficient microwave-assisted hydrothermal route N2 - Li-rich nanoparticles of Li1+xMn2–xO4 doped with Al, Co, or Ni are successfully synthesized using a facile, fast, and efficient microwave-assisted hydrothermal route. Synchrotron X-ray diffraction confirms the formation of the crystalline cubic spinel phase type. X-ray absorption spectroscopy analysis at the Co and Ni K- and L-edges verifies that the dopants are within the Li1+xMn2–xO4 spinel structure and are inactive during cycling in the bulk and at the surface. Moreover, we demonstrate that nanocrystallinity and cationic doping play an important role in improving the electrochemical performance with respect to LiMn2O4 microparticles. They significantly reduce the charge-transfer resistance, lower the first cycle irreversible capacity loss to 6%, and achieve a capacity retention between 85 and 90% after 380 cycles, with excellent Coulombic efficiency close to 99% without compromising the specific charge at a 5C cycling rate. Furthermore, the Mn K- and L-edges attest that after long cycling, the Mn oxidation state in the bulk differs from that at the surface caused by the Mn disproportion reaction; however, the cationic doping helps mitigate the Mn dissolution with respect to the undoped Li1+xMn2–xO4 nanoparticles, as indicated by inductively coupled plasma atomic emission spectrometry. KW - XAS KW - SAXS KW - Li-ion battery KW - Cathode material KW - Spinel KW - The MOUSE PY - 2022 DO - https://doi.org/10.1021/acsaem.2c00902 SN - 2574-0962 VL - 5 IS - 7 SP - 8357 EP - 8370 PB - ACS Publ. CY - Washington, DC AN - OPUS4-55359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Mauch, Tatjana A1 - Riedel, Juliane T1 - Development of a Hydrazine-Based Solid-Phase Extraction and Clean-Up Method for Highly Selective Quantification of Zearalenone in Edible Vegetable Oils by HPLC-FLD N2 - Rapid, cost-efficient, and eco-friendly methods are desired today for routine analysis of the Fusarium mycotoxin zearalenone (ZEN) in edible vegetable oils. Liquid chromatography with fluorescence detection (HPLC-FLD) is commonly used to reliably control the specified ZEN maximum levels, which requires efficient sample clean-up to avoid matrix interferences. Therefore, a highly selective extraction and clean-up method based on reversible covalent hydrazine chemistry (RCHC) using hydrazine-functionalized silica was developed. This efficient solid-phase extraction (SPE) involves reversible hydrazone formation of ZEN with the hydrazine moiety covalently bound to a solid phase. Optimal conditions were achieved with 1 mL SPE cartridges filled with 400 mg of hydrazine-functionalized silica. The developed RCHC-SPE method was validated in an interlaboratory comparison study (ILC) with twelve participants analyzing six edible vegetable oils with a focus on maize oils. The derived method parameters (ZEN recovery 83%, repeatability 7.0%, and reproducibility 18%) meet the performance criteria of Commission Regulation (EC) No 401/2006. The developed RCHC-SPE-based HPLC-FLD method allows the reliable quantification of ZEN in the range of 47–494 μg/kg for different types of edible vegetable oils, also for matrix-reach native oils. Due to the high efficiency, the significantly reduced matrix load helps to extend the lifetime of analytical equipment. Furthermore, the re-useability of the RCHC-SPE cartridges contributes to an eco-friendly approach and reduced analysis costs. To our knowledge, this is the first report on ZEN quantification in edible vegetable oils based on manual RCHC-SPE cartridges. Due to its high performance, the developed RCHC-SPE method is a promising alternative to the current European standard method EN 16924:2017 (HPLC-FLD part). KW - Mycotoxin KW - Food KW - Reversible covalent hydrazine chemistry (RCHC) KW - Quantitative determination PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554812 DO - https://doi.org/10.3390/toxins14080549 VL - 14 IS - 8 PB - MDPI CY - Basel AN - OPUS4-55481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knoche, Lisa A1 - Lisec, Jan A1 - Koch, Matthias T1 - Analysis of electrochemical and liver microsomal transformation products of lasalocid by LC/HRMS N2 - Rationale: Lasalocid (LAS), an ionophore, is used in cattle and poultry farming as feed additive for its antibiotic and growth-promoting properties. Literature on transformation products (TP) resulting from LAS degradation is limited. So far, only hydroxylation is found to occur as the metabolic reaction during the LAS degradation. To investigate potential TPs of LAS, we used electrochemistry (EC) and liver microsome (LM) assays to synthesize TPs, which were identified using liquid chromatography high-resolution mass spectrometry (LC/HRMS). Methods: Electrochemically produced TPs were analyzed online by direct coupling of the electrochemical cell to the electrospray ionization (ESI) source of a Sciex Triple-TOF high resolution mass spectrometer. Then, EC-treated LAS solution was collected and analyzed offline using LC/HRMS to confirm stable TPs and improve their annotation with a chemical structure due to informative MS/MS spectra. In a complementary approach, TPs formed by rat and human microsomal incubation were investigated using LC/HRMS. The resulting data were used to investigate LAS modification reactions and elucidate the chemical structure of obtained TPs. Results: The online measurements identified a broad variety of TPs, resulting from modification reactions like (de-)hydrogenation, hydration, methylation, oxidation as well as adduct formation with methanol. We consistently observed different ion complexations of LAS and LAS-TPs (Na+; 2Na+ K+; NaNH4 +; KNH4 +). Two stable methylated EC-TPs were found, structurally annotated, and assigned to a likely modification reaction. Using LM incubation, seven TPs were formed, mostly by oxidation/hydroxylation. After the identification of LM-TPs as Na+-complexes, we identified LM-TPs as K+-complexes. Conclusion: We identified and characterized TPs of LAS using EC- and LM-based methods. Moreover, we found different ion complexes of LAS-based TPs. This knowledge, especially the different ion complexes, may help elucidate the metabolic and environmental degradation pathways of LAS. KW - Mass Spectrometry KW - Electrochemistry KW - ECR KW - Lasalocid KW - Ionophore KW - Transformation products PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553919 DO - https://doi.org/10.1002/rcm.9349 VL - 36 IS - 18 SP - 1 EP - 10 PB - Wiley online library AN - OPUS4-55391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - X-ray scattering for nanostructure quantification, and the quest for the perfect experiment N2 - Measuring an X-ray scattering pattern is relatively easy, but measuring a steady stream of high-quality, useful patterns requires significant effort and good laboratory organization. Such laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration). With the MOUSE, we have combined a comprehensive and highly automated laboratory workflow with a heavily modified X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, within a well-documented, FAIR-compliant data flow (akin to what is found at the more automated synchrotron beamlines). With two full-time researchers, our lab collects and interprets thousands of datasets, on hundreds of samples, for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data. This talk will briefly introduce the foundations of X-ray scattering, present the MOUSE project, and will highlight the proven utility of the methodology for materials science. Upgrades to the methodology will also be discussed, as well as possible avenues for transferring this holistic methodology to other instruments T2 - SNI 2022 CY - Berlin, Germany DA - 05.09.2022 KW - Methodology KW - X-ray scattering KW - Laboratory management KW - Instrumentation utilization KW - MOUSE KW - SAXS KW - WAXS KW - Automation PY - 2022 AN - OPUS4-55760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Steinhäuser, Lorin A1 - Lardy-Fontan, S. A1 - Lalere, B. A1 - Le Diouron, V. A1 - Heath, E. A1 - Ana Kovačič, A. A1 - Potalivo, M. A1 - de Zorzi, P. A1 - Centioli, D. A1 - Naykki, T. A1 - Viidanoja, J. A1 - Gökcen, T. A1 - Budzinski, H. A1 - Le Menach, K. A1 - Selih, V. T1 - EDC-WFD: A project to deliver reliable measurements for better monitoring survey and risks assessments. N2 - Monitoring programs should generate high-quality data on the concentrations of substances and other pollutants in the aquatic environment to enable reliable risk assessment. Furthermore, the need for comparability over space and time is critical for analysis of trends and evaluation of restoration of natural environment. Additionally, research work and exercises at the European level have highlighted that reliable measurements of estrogenic substances at the PNEC level are still challenging to achieve. The project EDC-WFD Metrology for monitoring endocrine disrupting compounds under the EU Water Framework Directive aims to develop traceable analytical methods for determining endocrine disrupting compounds and their effects, with a specific focus on three estrogens of the first watch list (17-beta-estradiol (17βE2), 17-alpha-ethinylestradiol (EE2), and estrone (E1)). Estrogens 17-alpha-estradiol (17E2) and estriol (E3) will be included to demonstrate the reliability of the developed methods and to support the requirements of Directive 2013/39/EC, Directive 2009/90/EC and Commission Implementation Decision (EU) 2018/840, hence improving the comparability and compatibility of measurement results within Europe. During the EDC-WFD project four selected effect-based methods (EBM) will be deeply investigated in order to improve their rationale use and their support in water quality assessment. In particular, the EBM sensitivity, specificity and accuracy on reference materials with single or mixture solutions of the five substances at a concentration of EQS values will be explored. This contribution will present the objectives and methods applied within the EDC-WFD project. T2 - EuChemS CY - Lisbon, Portugal DA - 29.08.2022 KW - WFD KW - Estrogens KW - Whole water samples KW - EQS PY - 2022 AN - OPUS4-57096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Kovačič, A. A1 - Steinhäuser, Lorin A1 - Heath, E. A1 - Lardy-Fontan, S. T1 - A method for monitoring estrogens in whole surface waters by GC-MS/MS N2 - Natural and synthetic estrogens are key endocrine-disrupting chemicals. Despite occurring at ultra-trace levels (below ng L-1), it is believed that they are contributing to an increase in feminized fish and other endocrine disruptive effects, and hence, their inclusion in the Watch list was not unexpected. One of the main sources ofestrogens to surface waters is wastewater effluent. Once in surface waters, they can partition into different compartments, i.e., water and suspended particulate matter. For this reason, there is an urgent need for a methodology to monitor estrogen levels below the environmental quality standards (EQS) set by the Water Framework Directive requirements. In this study, a precise and accurate gas chromatography-mass spectrometry method (GC-MS/MS) for the analysis of estrone (E1), 17β-estradiol (17β-E2), 17α-estradiol (17α- E2), 17-alpha-ethinylestradiol (EE2), and estriol (E3) in whole water samples with ng L-1 limit of quantification (LOQ) was developed and validated in accordance with CEN/TS 16800:2020 guidelines. T2 - IMSC 2022 CY - Maastricht, Netherlands DA - 27.08.2022 KW - EDC KW - WFD KW - GC-MS PY - 2022 AN - OPUS4-57097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Wortmann, U. G. A1 - Vogl, Jochen A1 - Schmid, Thomas T1 - Beautiful Pietàs in South Tyrol (Northern Italy): local or imported works of art? N2 - The study, dedicated to Beautiful Pietàs conserved in South Tyrol (Northern Italy), aims to establish, for the first time, a connection between Austroalpine raw materials and the high-fired gypsum mortars constituting the Gothic figure groups in question. The origin and chronology of this stylistically and qualitatively differing ensemble have been subject of art historical debate for nearly a century. The discourse is dominated by three main hypotheses: itinerary of an Austrian artist versus itinerary of the work of art created in an artist’s workshop in Austria versus itinerary of the stylistic vocabulary via graphical or three-dimensional models. The comparison of the δ34S values and the 87Sr/86Sr ratios of the gypsum mortars and Austroalpine sulphate deposits (in a compilation of own reference samples and literature data) points to the exploitation of sediments in the Salzkammergut and possibly also in the evaporite district of the Eastern Calcareous Alps, thus evidencing the import of the sculptures and not the activities of local South Tyrolean or itinerant artists. Two geochronological units are distinguishable: The Pietà in the Church St. Martin in Göflan can be assigned to Upper Permian raw material, whereas the metrologically consistent sculptures in the Church of Our Lady of the Benedictine Abbey Marienberg and in the Chapel St. Ann in Mölten correlate with deposits of the Early Triassic (or the Lower-Middle Triassic transition). The medieval gypsum mortars also differ in their mineralogical characteristics, i.e. in their geologically related minor components, as in the first case, characterised by a significant proportion of primary anhydrite, natural carbonate impurities mainly consist of calcite (partly converted to lime-lump-like aggregates), whereas in the second group dolomite (or rather its hydration products after pyrometamorphic decomposition) predominates, accompanied by celestine, quartz and potassium feldspar. The Pietà in the Cathedral Maria Himmelfahrt in Bozen turned out to be made of Breitenbrunn calcareous sandstone (Leitha Mountains, Burgenland, Austria), which is why the sample is not considered in the geochemical analysis. KW - High-fired gypsum mortar KW - Sulphur isotope KW - Strontium isotope KW - Polarised light microscopy KW - Raman microspectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545610 DO - https://doi.org/10.1186/s40494-022-00678-6 SN - 2050-7445 VL - 10 IS - 1 SP - 1 EP - 17 PB - Springer Nature AN - OPUS4-54561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Bresch, Harald A1 - Kipphardt, Heinrich A1 - Resch-Genger, Ute A1 - Koch, Matthias A1 - Rosner, M. T1 - Trends in selected fields of reference material production N2 - For more than 110 years, BAM has been producing reference materials for a wide range of application fields. With the development of new analytical methods and new applications as well as continuously emerging more stringent requirements of laboratory accreditation with regard to quality control and metrological traceability, the demand and requirements for reference materials are increasing. This trend article gives an overview of general developments in the field of reference materials as well as developments in selected fields of application in which BAM is active. This includes inorganic and metal analysis, gas analysis, food and consumer products, and geological samples. In addition to these more traditional fields of application, developments in the areas of optical spectroscopy, particulary fluorescence methods, and nanomaterials are considered. T2 - 150 years BAM: Science with impact CY - Berlin, Germany DA - 01.01.2021 KW - Reference material KW - ISO REMCO KW - Gas analysis KW - Food KW - Nanomaterials KW - Fluorescence PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548407 DO - https://doi.org/10.1007/s00216-022-03996-7 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - Topical collection: Analytical methods and applications in the materials and life sciences SP - 4281 EP - 4289 PB - Springer CY - Berlin AN - OPUS4-54840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernandez-Menendez, L. J. A1 - Mendez-Lopez, C. A1 - Abad Andrade, Carlos Enrique A1 - Fandino, J. A1 - Gonzalez-Gago, C. A1 - Pisonero, J. A1 - Bordel, N. T1 - A critical evaluation of the chlorine quantification method based on molecular emission detection in LIBS N2 - The entire process involving the determination of Cl by molecular emission detection in Laser-Induced Breakdown Spectroscopy (LIBS) is thoroughly studied in this paper. This critical evaluation considers how spectra are normalized, how interferences from other molecular species signals are removed, and how signal integration is applied. Moreover, a data treatment protocol is proposed to achieve reliable and accurate Cl determination from the CaCl molecular spectral signal, not requiring the use of more complex numerical approaches. Calcium chloride dihydrate (CaCl2⋅2H2O) and high purity anhydrite samples (CaSO4) are used to optimize the acquisition conditions and data treatment of CaCl emission signal. Using the developed protocol, calibration curves for Cl, covering the concentration range from 0 μg/g to 60,000 μg/g of Cl, are successfully achieved. Finally, the suitability of the proposed methodology for Cl determination is successfully applied in industrial gypsum waste samples, where the results obtained by LIBS are validated using high-resolution molecular absorption spectroscopy (HR-CS-MAS) and potentiometric titration. KW - Laser induced breakdown Spectrocopy (LIBS) KW - Molecular spectra KW - Chlorine determination KW - CaCl emission bands KW - Industrial gypsum PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544292 DO - https://doi.org/10.1016/j.sab.2022.106390 SN - 0584-8547 VL - 190 SP - 1 EP - 9 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-54429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tukhmetova, Dariya A1 - Lisec, Jan A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Data processing made easy: standalone tool for automated calculation of isotope ratio from transient signals – IsoCor N2 - Despite numerous advantages offered by hyphenation of chromatography and electrokinetic separation methods with multicollector (MC) ICP-MS for isotope analysis, the main limitation of such systems is the decrease in precision and increase in uncertainty due to generation of short transient signals. To minimize this limitation, most authors compare several isotope ratio calculation methods and establish a multi-step data processing routine based on the precision and accuracy of the methods. However, to the best of our knowledge, there is no universal data processing tool available that incorporates all important steps of the treatment of the transient signals. Thus, we introduce a data processing application (App) IsoCor that facilitates automatic calculation of isotope ratios from transient signals and eases selection of the most suitable method. The IsoCor App performs baseline subtraction, peak detection, mass bias correction, isotope ratio calculation and delta calculation. The feasibility and reliability of the App was proven by reproducing the results from isotope analysis of three elements (neodymium, mercury and sulfur) measured on-line via hyphenated systems. The IsoCor App provides trackability of the results to ensure quality control of the analysis. KW - Isotope ratio KW - Transient signal KW - MC-ICP-MS KW - Data processing KW - App PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559068 DO - https://doi.org/10.1039/D2JA00208F VL - 37 IS - 11 SP - 2401 EP - 2409 PB - Royal Society of Chemistry AN - OPUS4-55906 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 - JOUR A1 - You, Zengchao A1 - Akkus, Asli A1 - Weisheit, W. A1 - Giray, Thorsten A1 - Penk, Sibylle A1 - Buttler, Sabine A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique T1 - Multielement analysis in soils using nitrogen microwave inductively coupled atmospheric pressure plasma mass spectrometry N2 - In this study, we employed nitrogen microwave inductively coupled atmospheric-pressure plasma (MICAP) combined with quadrupole mass spectrometry (MS) and a liquid sample introduction system to analyze heavy metals in soils. The vanadium, cobalt, nickel, zinc, copper, chromium, arsenic, lead, and cadmium contents in seven reference and three environmental soil samples determined using MICAP-MS were within the uncertainty of the reference values, indicating that MICAP-MS is promising for soil analysis similar to the conventional inductively coupled plasma mass spectrometry (ICP-MS) technique. In addition, the limits of detection (LODs) and sensitivity of both techniques using N2 and Ar plasma were of the same order of magnitude. Furthermore, the performance of MICAP-MS under different N2 purity was investigated, and we found that the plasma formation and ionization efficiency were not influenced by the impurities in the gas. A prominent advantage of MICAP-MS is the low operating cost associated with gas consumption. In this work, MICAP-MS used nitrogen, which is cheaper than argon, and consumed 25% less gas than ICP-MS. Using low-purity N2 can further reduce the gas cost, making MICAP-MS more cost effective than ICP-MS. These results suggest that MICAP-MS is a promising alternative to ICP-MS for the analysis of heavy metals in the soil. KW - Soil KW - Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) KW - Nitrogen plasma KW - Multi-element analysis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561048 DO - https://doi.org/10.1039/d2ja00244b SN - 0267-9477 VL - 37 IS - 12 SP - 2556 EP - 2562 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-56104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Faßbender, Sebastian A1 - Chronakis, Michail A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Size determination of nanoparticles by ICP-ToF-MS using isotope dilution in microdroplets N2 - Within this work, the combination of a microdroplet generator and an ICP-ToF-MS for nanoparticle analysis is presented. For the size determination of platinum nanoparticles an on-line isotope dilution analysis approach was developed. The 194Pt/195Pt isotopic ratio was used for the characterization of the particles, while the 182W/183W isotopic ratio was monitored simultaneously for mass bias correction. The on-line ID-MDG-sp-ICP-ToF-MS approach was deployed for the size determination of three platinum nanoparticle samples (50 nm, 63 nm, 70 nm); for validation, complementary size characterization techniques (sp-ICP-ToF-MS and TEM) were used. The robustness of this technique was evidenced, by using sodium chloride concentrations up to 100 mg L−1 as a matrix component. Our new on-line ID MDG-sp-ICP-ToF-MS approach is a promising tool for the fast and reliable determination of nanoparticles' size in severe matrix concentrations, e.g., environmental samples. KW - ICP-ToF-MS KW - Nanoparticles KW - Isotope Dilution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552727 DO - https://doi.org/10.1039/D2JA00072E SN - 0267-9477 VL - 37 IS - 6 SP - 1203 EP - 1207 PB - Royal Society of Chemistry AN - OPUS4-55272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Advantages of N2-MICAP-MS for Trace Metal Analysis in Steel N2 - The climate and energy crisis are extreme challenges. One possible solution could be hydrogen technology. Safety is a big concern. Steel used for pipelines and storage is under permanent stress from low temperatures and high pressures. The content of different alloyed metals determines the performance of the steel. Nitrogen microwave inductively coupled atmosphere pressure plasma mass spectrometry (N2-MICAP-MS) is a promising method for trace metal analysis in steel. Nitrogen is cheap and can be generated on site. It has fewer interferences than argon. Additionally, MICAP-MS is very matrix tolerant, proving the matrix-matched calibration expendable. Safety in technology and chemistry is the mission of BAM. Providing reference methods and materials can create trust in future technologies like hydrogen. T2 - SALSA Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - Trace analysis KW - Steel KW - Microwave plasma KW - Mass spectrometry KW - Safety PY - 2022 AN - OPUS4-55792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Bornemann-Pfeiffer, Martin A1 - Guhl, Svetlana A1 - Wander, L. A1 - Kern, S. T1 - Integrierte und vernetzte Systeme und Prozesse – Eine Perspektive für die smarte Laborinfrastruktur N2 - Chemie- und Pharmaunternehmen müssen neue Wege gehen, um in einem sich wandelnden Umfeld erfolgreich zu überleben, und gleichzeitig flexiblere Wege der Produkt- und Prozessentwicklung finden, um ihre Produkte schneller auf den Markt zu bringen - vor allem hochwertige High-End-Produkte wie Feinchemikalien oder Arzneimittel. Dazu gehört auch das Potenzial der digitalen Technologien, um ein umfassenderes Wissensmanagement zu ermöglichen. Eine wichtige Wissensquelle sind analytische Labors, die Unternehmensweit aktiv sind – von F&E bis zur Produktion. Die ganzheitliche Einbindung von analytischen Labors und ein unternehmensweites Daten- und Wissensmanagement sind wichtige Bausteine zur Integration und Vernetzung aller Systeme und Prozesse. Das Potenzial von Daten aus der Produktion mit ihren Kontextinformationen wird heute oft noch nicht konsequent für ein umfassendes Verständnis der Produktion genutzt. Dieser Beitrag skizziert anhand von Beispielen einen möglichen ganzheitlicheren Ansatz zur Digitalisierung und zum Einsatz maschineller Verfahren in der Produktion von Spezialchemikalien und Pharmazeutika durch die Einführung integrierter und vernetzter Systeme und Prozesse. T2 - 6. Analytik-Tag des Institut für Energie- und Umwelttechnik e.V. (IUTA) CY - Duisburg, Germany DA - 10.11.2022 KW - Prozessindustrie KW - Online-NMR-Spektroskopie KW - Prozessanalytik KW - Digitalisierung KW - Datenauswertung KW - IUTA PY - 2022 AN - OPUS4-56226 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Bornemann-Pfeiffer, Martin A1 - Wander, Lukas A1 - Kowarik, Stefan A1 - Liehr, Sascha T1 - Modular process control with compact NMR spectroscopy: From field integration to fully automated data analysis N2 - Chemical and pharmaceutical companies need to find new ways to survive successfully in a changing environment, while finding more flexible ways of product and process development to bring their products to market faster - especially high-value, high-end products such as fine chemicals or pharmaceuticals. This is complicated by changes in value chains along a potential circular economy. One current approach is flexible and modular chemical production units that use multi-purpose equipment to produce various high-value products with short downtimes between campaigns and can shorten time-to-market for new products. Online NMR spectroscopy will play an important role for plant automation and quality control, as the method brings very high linearity, matrix independence and thus works almost calibration-free. Moreover, these properties ideally enable automated and machine-aided data analysis for the above-mentioned applications. Using examples, this presentation will outline a possible more holistic approach to digitalization and the use of machine-based processes in the production of specialty chemicals and pharmaceuticals through the introduction of integrated and networked systems and processes. T2 - Benchtop NMR: From Academia to Industry CY - Online meeting DA - 28.09.2022 KW - Digital Transformatioin KW - Process Industry KW - Benchtop NMR Spectroscopy KW - Procee Analytical Technology KW - Modular Production KW - Specialty Chemicals KW - Industry 4.0 PY - 2022 UR - https://eventos.fct.unl.pt/benchtop_nmr_workshop2022/pages/welcome AN - OPUS4-55850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Metrologie für fortschrittliche Wasserstoffspeicherlösungen – Das EU-Projekt MefHySto T1 - Metrology for advanced hydrogen storage solutions – The EU project MefHySto N2 - Das europäische Projekt MefHySto befasst sich mit dem Bedarf an großmaßstäblichen Energiespeichern, die für eine Umstellung der Energieversorgung auf erneuerbare Energien erforderlich sind. Eine solche Speicherung ist entscheidend, um Energie zu Spitzenzeiten zu liefern, wenn die erneuerbaren Energiequellen schwanken. Eine mögliche Lösung für die Energiespeicherung ist der großtechnische Einsatz von Wasserstoff. Die messtechnische Rückführbarkeit in der Energieinfrastruktur für die Wasserstoffspeicherung ist dann von entscheidender Bedeutung und eine bessere Kenntnis der chemischen und physikalischen Eigenschaften von Wasserstoff sowie rückführbare Messungen und validierte Techniken unverzichtbar. N2 - The European project MefHySto addresses the need of large-scale energy storage, which is required for a shift to renewable energy supply. Such storage is mandatory to supply energy at peak times when renewable sources fluctuate. A possible solution for energy storage is large-scale use of hydrogen. Metrological traceability in the energy infrastructure for hydrogen storage is then crucial and a better knowledge of the chemical and physical properties of hydrogen as well as traceable measurements and validated techniques are indispensable. KW - Wasserstoff KW - Wasserstoffspeicher KW - Infrastruktur KW - Metrologie KW - PEM-Wasserelektrolyse KW - Rückverstromung KW - Lastwechsel KW - Wasserstoff-Qualität PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556451 UR - https://gwf-gas.de/forschung-entwicklung/metrologie-fuer-fortschrittliche-wasserstoffspeicherloesungen-das-eu-projekt-mefhysto/ SN - 2366-9594 VL - 163 IS - 9 SP - 38 EP - 45 PB - Vulkan Verlag CY - Essen AN - OPUS4-55645 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, U. A1 - Bachem, G. A1 - Müller, A. A1 - Kittner, Maria A1 - Altmann, Korinna A1 - Meierdierks, J. A1 - Grathwohl, P. A1 - Lackmann, C. A1 - Simic, A. A1 - Velki, M. A1 - Hollert, H. T1 - Detection of plastics in soil N2 - Soil acts as a final sink for pollutants. Microplastics from different sources such as plastic mulching, littering, compost, sewage sludge, sedimentary deposition, and tyre abrasion are expected to be found in soil. However, representative and comprehensive information is missing on the sources, transport, and fate. Therefore, a reliable analysis method for microplastics in soils needs to be developed. The presented work describes the development of a procedure for microplastics analysis in soils. A representative sampling based on the on-site conditions and a sample preparation method was established and comprised of a drying step, the separation of microplastic particles > 1 mm, and a density separation for particles < 1 mm. The detection of the large microplastic particles (> 1 mm) was conducted with Attenuated Total Reflection - Fourier Transform infrared Spectroscopy (ATR-FTIR) , while Thermal Extraction Desorption - Gas Chromatography / Mass Spectrometry (TED-GC/MS) was applied for particles < 1 mm, gaining information on the type of polymer and mass fraction. Based on the established method, 14 environmental soil samples ? with different exposure of microplastics from agriculture, industrial sites, roads, and floods were investigated. Due to the arbitrary microplastic particle distribution among the samples for large microplastics, it was reasoned that the found particles were unrepresentative. In contrast, microplastic particles < 1 mm were discovered in a high mass in soil samples exposed to plastic mulching or fertilization with sewage sludge or compost (0 – 115 mg/kg). On average, microplastic contents detected in soil samples taken from a construction site and an inner-city lake were higher (13 – 238 mg/kg). As expected, microplastic content in soil sampled in proximity to roads was more pronounced in the upper soil layers. In contrast, very remote sampling sites, expectably uncontaminated, did not lead to the detection of microplastic regarding to thermoanalytical detection method. In a proof of concept experiment several in vivo and in vitro ecotoxicological tests were applied to evaluate the effect of microplastics (tyre abrasion, polystyrene containing hexabromocyclododecane) in natural soils. In summary, while no effects of the examined probes could be detected on higher levels of biological organization after exposures to earthworm E. andrei, significant changes in several oxidative stress related biomarkers were observed. T2 - SETAC Europe 2022 CY - Kopenhagen, Denmark DA - 15.05.2022 KW - Microplastic KW - TED-GC/MS KW - Soil PY - 2022 AN - OPUS4-55872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM-P213: BAM procedure for obtaining Cu delta values N2 - BAM participated in the CCQM pilot study P213 for obtaining copper isotope delta values. This presentations provides details on the MC-ICP-MS based measruement procedure, which has been applied to obtain such copper delta values. T2 - IRWG Meeting 2022 CY - Online meeting DA - 20.09.2022 KW - Isotope ratio KW - Copper KW - Metrology KW - Traceability KW - Uncertainty PY - 2022 AN - OPUS4-55864 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 - Raab, A. A1 - Solovyev, N. A1 - El-Kathib, Ahmed A1 - Vogl, Jochen A1 - Costas-Rodriguez, M. A1 - Vanhaecke, F. A1 - Schwab, K. A1 - Griffin, E. A1 - Platt, B. A1 - Theuring, F. T1 - Isotope signature of iron, copper and zinc in mouse models (L66 and 5XFAD) and their controls used for dementia research N2 - Introduction: The influence of copper, iron and zinc concentrations on the formation of ß-amyloid plaques and neurofibrillary tangles in Alzheimer’s disease (AD) is widely discussed in the community. The results from human and animal studies so far are mixed with some studies showing a correlation and others not. From a number of studies, it is known that disease state and isotopic composition of essential elements can be coupled. Aim: The aim of the study was to identify changes in element content and isotopic composition in two transgenic mouse models used in AD research compared to their genetic WT relatives and to establish whether element content and isotopic signature between different laboratories is comparable. Methods: ß-amyloid (5xFAD) and tau overexpressing (L66) mice together with their matching wild-types were bred at dedicated facilities in accordance with the European Communities Council Directive (63/2010/EU). Serum and brain were sampled after sacrifice and the samples distributed among the participants of the study. The tissues were acid digested for total element determination and high-precision isotope ratio determination. Element content was determined by either sector-field or quadrupole-based inductively coupled plasma mass spectrometry (ICPMS). For the determination of isotope ratios multi-collector ICPMS was used. Results: Total copper content was significantly higher for L66 and their matched WT compared to 5xFAD and WT. Brains of L66 mice contained more Fe in brain than their WT, Zn and Cu were not significantly different between L66 and WT. Whereas 5xFAD mice had a slightly lower Cu and slightly higher Zn concentration in brain compared to WT. The isotopic signature in brain of L66 mice for Fe was different from their controls, whereas Zn isotope ratios were influenced in 5xFAD mice compared to their WT . The Cu isotopic ratio did not seem to be influenced in either strain. In serum, the shifts were less pronounced. Conclusion: Even though neither Tau-protein nor amyloid precursor protein are known to be metal-dependent / -containing proteins, the overexpression of both influences the Fe, Cu and Zn metabolism in brain and to some extent also in serum as can be seen not only using total element determination but probably more clearly studying the isotopic signature of Fe, Cu and Zn. T2 - International Conference of Trace Elements and Minerals CY - Aachen, Germany DA - 05.06.2022 KW - Isotope delta value KW - Copper KW - Zinc KW - Iron KW - Dementia PY - 2022 AN - OPUS4-58230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander A1 - Hoffmann, V. A1 - Morcillo, Dalia A1 - Agudo Jácome, Leonardo A1 - Leonhardt, Robert A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique A1 - You, Zengchao T1 - Investigation of degradation of the aluminum current collector in lithium-ion batteries by glow-discharge optical emission spectroscopy N2 - Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - Lithium Ion Batteries KW - GD-OES KW - FIB KW - SEM KW - EDX PY - 2022 AN - OPUS4-56246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander A1 - Hoffmann, Volker A1 - Morcillo, Dalia A1 - Agudo Jácome, Leonardo A1 - Leonhardt, Robert A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique A1 - You, Zengchao T1 - Investigation of degradation of the aluminum current collector in lithium-ion batteries by GD-OES N2 - Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs. T2 - Empa Group Meeting CY - Dübendorf, Switzerland DA - 22.11.2022 KW - Lithium Ion Batteries KW - GD-OES KW - FIB KW - SEM KW - EDX PY - 2022 AN - OPUS4-56584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Why do I have to charge my phone twice a day? N2 - Aging Mechanisms of Lithium Batteries: How can we make batteries more durable and more sustainable in the future? Lithium batteries are particularly susceptible to ageing processes. During each charging and discharging process in an electric battery, lithium ions are deposited in the electrodes of the cell like in the pores of a sponge. Over time, however, fractures and cracks occur in the filigree structures. The result: more and more lithium ions no longer fit into the hollow spaces of the „sponge“, instead they accumulate in heaps around the electrodes and hinder the movement of other ions. The performance of the battery decreases. We present our new project, in which we are developing a fast and cost-effective method with which companies that produce lithium batteries can already assess the ageing behaviour of their batteries in the laboratory. T2 - Berlin Science Week 2022 CY - Online meeting DA - 10.11.2022 KW - Lithium Ion Batteries KW - Aging Mechanisms PY - 2022 UR - https://berlinscienceweek.com/de/event/why-do-i-have-to-charge-my-phone-twice-a-day/ UR - https://www.youtube.com/watch?v=bF7bQTY49rQ AN - OPUS4-56245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Certified reference material for the determination of hydrolytic resistance of borosilicate glass N2 - The preparation of certified reference material for the determination of hydrolytic resistance of borosilicate glass is described. Certified properties are the acid consumption according to the relevant standard procedures described in ISO 720, USP<660> and Ph.Eur. 3.2.1. T2 - 26. International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Borosilicate glass KW - CRM KW - Hydrolytic resistance PY - 2022 AN - OPUS4-55521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao A1 - Akkus, A. A1 - Weisheit, W. A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique T1 - Multi element analysis in soil using nitrogen microwave inductively coupled plasma mass spectrometry (MICAP MS) N2 - Due to the fast growth of industry and the use of metal-containing compounds such as sewage sludge in agricultural fields, soil pollution associated with heavy metals presents a terrifying threat to the environment. Throughout the world, there are already 5 million sites of soil contaminated by heavy metals1. Some heavy metals pollutants can influence food chain safety and food quality, which in turn affects human health. According to the German Federal Soil Protection and Contaminated Site Ordinance (BBodSchV) 13 heavy metals such as arsenic (As), lead (Pb) and cadmium (Cd) are classified as heavily toxic to human health2. Therefore, elemental analysis and precise quantification of the heavy metals in soil are of great importance. Inductively coupled plasma mass spectrometry (ICP-MS) emerged as a powerful technique for trace analysis of soil due to its multi-element capability, high sensitivity and low sample consumption. However, despite its success and widespread use, ICP-MS has several persistent drawbacks, such as high argon gas consumption, argon-based polyatomic interferences and the need for complicated RF-power generators. Unlike argon-based ICP, the nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) uses nitrogen as plasma gas, which eliminates high operating costs associated with argon-gas consumption as well as the argon-based interferences3. For the first time, the applicability of MICAP-MS for elemental analysis of environmental soils is investigated in this work. For this purpose, 7 reference- and 3 random soil samples containing vanadium (V), cobalt (Co), zink (Zn), copper (Cu), chrome (Cr), mercury (Hg), As, Pb and Cd are digested with aqua regia and used for analysis. Concentrations of selected elements are determined using MICAP-MS and validated using ICP-MS. Sensitivities, limits of detection and gas consumption for both methods are compared and discussed in detail. Moreover, the performance of MICAP-MS under different nitrogen plasma gas concentrations is investigated and compared. T2 - BAM Adlershofer Kolloquium CY - Online meeting DA - 21.06.2022 KW - Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) KW - Multi-element analysis KW - Soil KW - Nitrogen plasma PY - 2022 AN - OPUS4-55182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xiao, J. A1 - Vogl, Jochen A1 - Rosner, M. A1 - Jin, Z. T1 - Boron isotope fractionation in soil-plant systems and its influence on biogeochemical cycling N2 - Boron (B) is an essential mineral nutrient for higher plants. Although B plant nutrition is well studied, the B isotope fractionation at the soil-plant interface, within plant metabolism, and its influence on biogeochemical cycling is not fully understood. Boron concentrations and isotope variations (δ11B) of the dicotyledonous plants of Chenopodium album and Brassica napus and their growing soils along a climatic gradient were analyzed to decipher these unresolved issues of the B behavior. The boron concentrations and δ11B values show an increasing trend from roots to leaves for both plants, while a decreasing trend from flower to shell and to seed for Brassica napus. A large boron isotope fractionation occurs within the plants with median Δ11Bleaf-root ≈ +20‰, which is related to different boron transporters and transportation ways. Formation of borate dimerized rhamnogalacturonan II in cell and B(OH)3 transportation in xylem lead to heavier δ11B values from root to stem and leaf while B(OH)4􀀀 transportation in phloem lead to lighter δ11B values from flower to shell and seed. Although samples cover a distinct transect with systematically different climatic conditions, Δδ11B within the individual plant compartments and between the bulk plants and the soil available B do not show any systematic variation. This suggests that B uptake from the soil into Chenopodium album and Brassica napus occurs without a distinct isotope fractionation at the soil-plant interface (median Δ11Bbulkplant-soil = 􀀀 0.2‰) and plants are able to regulate boron uptake. Both the observed large B fractionation within plant and low or absent B isotope fractionation at the soil-plant interface may have profound implications for the biological and geological B cycle. If this observed boron behavior also exists in other plants, their litters would be an important source for exporting 11B-rich biological material from continental ecosystems via rivers to the global oceans. This may be helpful for the explanation of ocean B cycle and the increasing δ11B values over the Cenozoic. KW - Boron isotopic composition KW - Boron isotope fractionation KW - Soil available boron KW - Biological boron recycling KW - Chenopodium album KW - Brassica napus PY - 2022 DO - https://doi.org/10.1016/j.chemgeo.2022.120972 SN - 0009-2541 VL - 606 SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-55031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Kern, S. A1 - Guhl, Svetlana A1 - Bornemann-Pfeiffer, Martin A1 - Wander, Lukas A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy in the field: A Versatile Tool for Automated Continuous-Flow Production N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as, e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR appeared as preeminent online analytical method and allow using a modular data analysis tool, which even served as reliable reference method for further PAT applications (e.g. NIR spectroscopy). In the future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - DECHEMA Workshop "Sensorik für die Digitalisierung chemischer Produktionsanlagen" CY - Frankfurt am Main, Germany DA - 13.06.2022 KW - Compact NMR KW - Process Control KW - Modular Production KW - Process Analytical Technology PY - 2022 AN - OPUS4-55037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas T1 - Flexible Prozessanalytik für die pharmazeutische Produktion - Benchtop-NMR-Spektroskopie im industriellen Einsatz N2 - Im Rahmen des EU-Projekts „CONSENS – Integrated Control and Sensing“ wurde ein vollautomatisiertes, gemäß Atmosphère-Explosibles(ATEX)-Regeln zertifiziertes Analysatormodul auf Basis eines kommerziellen Benchtop-Kernspinresonanzspektrometers (Engl. nuclear magnetic resonance, NMR) entwickelt und im Umfeld einer modularen containerbasierten Produktionsanlage validiert. Auf Basis der gewonnenen Daten konnten sowohl eine iterative Optimierung der Prozessparameter erfolgen als auch Referenzdaten für die Kalibrierung eines Nahinfrarot-Spektrometers gewonnen werden. KW - Prozessanalytik KW - NMR-Spektroskopie KW - Modulare Produktion KW - Kalibriertransfer PY - 2022 VL - 12 IS - 3 SP - 122 EP - 129 PB - Editio Cantor Verlag CY - Aulendorf AN - OPUS4-55402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Kern, S. A1 - Guhl, Svetlana A1 - Bornemann-Pfeiffer, Martin A1 - Wander, L. T1 - Modular process control with compact NMR spectroscopy – From Field Integration to Automated Data Analysis N2 - Chemical and pharmaceutical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. A current approach uses flexible and modular chemical production units, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products. NMR spectroscopy appeared as excellent online analytical tool and allowed a modular data analysis approach, which even served as reliable reference method for further Process Analytical Technology (PAT) applications. Using the available datasets, a second data analysis approach based on artificial neural networks (ANN) was evaluated. Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously. In future, such fully integrated and interconnecting “smart” systems and processes can increase the efficiency of the production of specialty chemicals and pharmaceuticals. At the end of the article, ideas for solutions are discussed in order to speed up the implementation of new special products from the point of view of process analytics and to network the existing process chains more closely. T2 - PATriCK 2022 – Merck conference on PAT technology CY - Darmstadt, Germany DA - 19.10.2022 KW - Process Analytical Technology KW - Digitalisation KW - Process Industry KW - Online NMR Spectroscopy KW - Modular Production PY - 2022 AN - OPUS4-56089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Bornemann-Pfeiffer, Martin A1 - Wander, Lukas A1 - Kowarik, Stefan A1 - Liehr, Sascha A1 - Abele, M. A1 - Falkenstein, S. T1 - Modular process control with compact NMR spectroscopy – From field integration to automated data analysis N2 - Chemical and pharmaceutical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. A current approach uses flexible and modular chemical production units, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products. NMR spectroscopy appeared as excellent online analytical tool and allowed a modular data analysis approach, which even served as reliable reference method for further Process Analytical Technology (PAT) applications. Using the available datasets, a second data analysis approach based on artificial neural networks (ANN) was evaluated. Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously. In future, such fully integrated and interconnecting “smart” systems and processes can increase the efficiency of the production of specialty chemicals and pharmaceuticals. T2 - GIDRM Day (Gruppo Italiano Discussione Risonanze Magnetiche) - Data analysis and NMR: from fundamental aspects to health and material applications CY - Online meeting DA - 14.10.2022 KW - Process Control KW - Online NMR Spectroscopy KW - Industry 4.0 KW - Process Analytical Technology KW - Data Analysis KW - Machine-Assisted Workflows PY - 2022 DO - https://doi.org/http://www.gidrm.org/index.php/activities/workshops/2022-workshops/gidrm-day-data-analysis-and-nmr-from-fundamental-aspects-to-health-and-material-applications AN - OPUS4-56002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Bornemann-Pfeiffer, Martin A1 - Guhl, Svetlana A1 - Kern, Simon A1 - Meyer, Klas A1 - Wander, Lukas T1 - Integrated and Networked Systems and Processes - How NMR Spectroscopy Can Transform our Chemical and Pharmaceutical Production N2 - Chemical and pharmaceutical companies need to find new ways to survive successfully in a changing environment, while finding more flexible ways of product and process development to bring their products to market faster - especially high-value, high-end products such as fine chemicals or pharmaceuticals. This is complicated by changes in value chains along a potential circular economy. One current approach is flexible and modular chemical production units that use multi-purpose equipment to produce various high-value products with short downtimes between campaigns and can shorten time-to-market for new products. Online NMR spectroscopy will play an important role for plant automation and quality control, as the method brings very high linearity, matrix independence and thus works almost calibration-free. Moreover, these properties ideally enable automated and machine-aided data analysis for the above-mentioned applications. Using examples, this presentation will outline a possible more holistic approach to digitalization and the use of machine-based processes in the production of specialty chemicals and pharmaceuticals through the introduction of integrated and networked systems and processes. T2 - 43rd FGMR Annual Discussion Meeting CY - Karlsruhe, Germany DA - 12.09.2022 KW - Digital Transformatioin KW - Process Industry KW - Pharmaceuticals KW - Specialty Chemicals KW - Automation KW - Online NMR Spectroscopy KW - Industry 4.0 PY - 2022 AN - OPUS4-55715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin A1 - Kern, S. A1 - Wander, L. A1 - Meyer, Klas A1 - Maiwald, Michael T1 - Modular production involving benchtop NMR Current Application Examples Driven by Digitalization N2 - The demand for increasing product diversity in the chemical and pharmaceutical industry calls for new production processes that enable greater flexibility. Therefore, plants are needed which can be adapted to new processes in a fast manner and be scaled up and down easily to volatile market demands. Modular production techniques in combination with advanced process analytical technology (PAT) are considered as a promising solution able to fulfil these requirements. The success and acceptance of modular concepts in both new and existing plants is dependent of its reliability, easy applicability, and standardization. In recent past, enormous efforts were made to overcome existing barriers in a superordinate level, e.g. DEXPI, ENPRO, or MTP naming just a few. Here, we’d like to present a few, more hands-on, application examples which are shown in Figure 1 aiming to increase process flexibility and applicability. T2 - Achema 2022 CY - Frankfurt a.M., Germany DA - 22.08.2022 KW - Process analytical technology KW - NMR spectroscopy KW - Digitization PY - 2022 AN - OPUS4-55974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Bornemann-Pfeiffer, Martin A1 - Kern, S. A1 - Guhl, Svetlana A1 - Wander, Lukas A1 - Döring, T. A1 - Falkenstein, S. A1 - Abele, M. A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy in the field: A Versatile PAT Tool for Production of Specialty Chemicals N2 - Companies of chemical industry find themselves more often in a rapidly changing environment, e.g., due to variability of raw material quality or energy costs and efficiency. Process optimization and new process concepts become more and more important. For example, flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds like exothermic reactions with high heat dissipation. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR appeared as preeminent online analytical method and allow using a modular data analysis approach, which can even serve as reliable reference method for further calibration-dependent PAT applications (e.g., NIR spectroscopy). Based on experiences from these field studies an improved analyzer enclosure setup was developed and built, including the option of a secondary method besides NMR spectroscopy. Integrated control systems allow for a flexible implementation based on the available automation infrastructure at the chemical plant or pilot plant setup. In the future, fully integrated and intelligently interconnecting “smart” PAT systems and processes have the potential speed up the setup of production equipment for chemicals and pharmaceuticals and therefore help to reduce the time-to-market. T2 - Practical Applications of NMR in Industry Conference (PANIC) 2022 CY - La Jolla, CA, USA DA - 16.10.2022 KW - Process Analytical Technology KW - Benchtop NMR KW - Modular production PY - 2022 AN - OPUS4-56090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Bornemann-Pfeiffer, Martin A1 - Kern, S. A1 - Guhl, Svetlana A1 - Wander, Lukas A1 - Döring, T. A1 - Falkenstein, S. A1 - Abele, M. A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy in the field: A Versatile PAT Tool for Production of Specialty Chemicals N2 - Chemical companies must find new paths to successfully survive in a changing environment, especially by utilizing the potential of digital technologies. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Therefore, fully automated process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. It was used for direct loop advanced process control and real-time optimization of the process. Field studies in modular and conventional production plants show promising results gaining process knowledge. NMR appeared as preeminent online analytical method and allow using a modular data analysis tool, which even served as reliable reference method for further PAT applications (e.g. NIR spectroscopy). In the future, fully integrated and interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - ProcessNet and DECHEMA-BioTechNet Jahrestagungen 2022 with 13th ESBES Symposium CY - Aachen, Germany DA - 12.09.2022 KW - Process Analytical Technology KW - Benchtop NMR KW - Modular production PY - 2022 AN - OPUS4-55918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Bornemann-Pfeiffer, Martin A1 - Kern, S. A1 - Guhl, Svetlana A1 - Wander, Lukas A1 - Döring, T. A1 - Falkenstein, S. A1 - Abele, M. A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy in the field: A Versatile PAT Tool for Production of Specialty Chemicals N2 - Chemical companies must find new paths to successfully survive in a changing environment, especially by utilizing the potential of digital technologies. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Therefore, fully automated process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. It was used for direct loop advanced process control and real-time optimization of the process. Field studies in modular and conventional production plants show promising results gaining process knowledge. NMR appeared as preeminent online analytical method and allow using a modular data analysis tool, which even served as reliable reference method for further PAT applications (e.g. NIR spectroscopy). In the future, fully integrated and interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - 17. AKPAT Kolloquium 2022 CY - Amersfoort, Netherlands DA - 19.09.2022 KW - Process Analytical Technology KW - Benchtop NMR KW - Modular production PY - 2022 AN - OPUS4-55919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf A1 - Seeger, Stefan A1 - Brödner, Doris A1 - Erdmann, Kerstin A1 - Rasch, Fabian T1 - Chemical characterization of ultra-fine particles released from laser printers N2 - 11 laser printers from 5 manufacturers were purchased in 2017 and tested for their UFP emissions. Size resolved sampling of the emitted particles was done with a 13 stage (30 nm to 10 µm) low pressure cascade impactor. The sampled particles were analysed for their chemical composition by thermal extraction (vaporization at 290°C) followed by GC-MS analysis. High boiling cyclic siloxanes (D10 to D16) were detected as constituents of UFP from laser printers. In comparison to measurements in 2008, aliphatic long-chain alkanes (C22 to C34) were detected additionally as chemical constituents of UFP from most of the tested printers and their amounts were higher than for cyclic siloxanes. Printers of one manufacturer showed very low UPF emissions compared to the other manufacturers. T2 - Indoor Air Conference 2022 CY - Kuopio, Finland DA - 12.06.2022 KW - UFP KW - Thermal extraction KW - Cascade impactor PY - 2022 AN - OPUS4-55107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Billimoria, K. A1 - Diaz Fernandez, Y. A. A1 - Andresen, Elina A1 - Sorzabal-Bellido, I. A1 - Huelga-Suarez, G. A1 - Bartczak, D. A1 - Ortiz de Solórzano, C. A1 - Resch-Genger, Ute A1 - Goenaga Infante, H. T1 - The potential of bioprinting for preparation of nanoparticle-based calibration standards for LA-ICP-ToF-MS quantitative imaging N2 - This paper discusses the feasibility of a novel strategy based on the combination of bioprinting nano-doping technology and laser ablation-inductively coupled plasma time-of-flight mass spectrometry analysis for the preparation and characterization of gelatin- based multi-element calibration standards suitable for quantitative imaging. To achieve this, lanthanide up-conversion nanoparticles were added to a gelatin matrix to produce the bioprinted calibration standards. The features of this bioprinting approach were com- pared with manual cryosectioning standard preparation, in terms of throughput, between batch repeatability and elemental signal homogeneity at 5 μm spatial resolution. By using bioprinting, the between batch variability for three independent standards of the same concentration of 89 Y (range 0–600 mg/kg) was reduced to 5% compared to up to 27% for cryosectioning. On this basis, the relative standard deviation ( RSD ) obtained between three independent calibration slopes measured within 1 day also reduced from 16% (using cryosectioning ) to 5% (using bioprinting), supporting the use of a single standard preparation replicate for each of the concentrations to achieve good calibration performance using bioprinting. This helped reduce the analysis time by approximately 3-fold. With cryosectioning each standard was prepared and sectioned individually, whereas using bio-printing it was possible to have up to six different standards printed simultaneously, reducing the preparation time from approximately 2 h to under 20 min (by approxi- mately 6-fold). The bio-printed calibration standards were found stable for a period of 2 months when stored at ambient temperature and in the dark. KW - Environmental analysis KW - LA-ICP-MS KW - Lanthanide KW - Tag KW - Fluorescence KW - Nanoparticles KW - Reference material KW - Quality assurance KW - 3D-printing KW - Synthesis KW - Production KW - Multimodal PY - 2022 DO - https://doi.org/10.1093/mtomcs/mfac088 SN - 1756-591X VL - 14 IS - 12 SP - 1 EP - 9 PB - Oxford University Press CY - Oxford AN - OPUS4-57018 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tatzel, M. A1 - Frings, P. J. A1 - Oelze, Marcus A1 - Herwartz, D. A1 - Lünsdorf, K. A1 - Wiedenbeck, M. T1 - Chert oxygen isotope ratios are driven by Earth's thermal evolution N2 - The 18O/16O ratio of cherts (δ18Ochert) increases nearly monotonically by ~15‰ from the Archean to present. Two end-member explanations have emerged: cooling seawater temperature (TSW) and increasing seawater δ18O (δ18Osw). Yet despite decades of work, there is no consensus, leading some to view the δ18Ochert record as pervasively altered. Here, we demonstrate that cherts are a robust archive of diagenetic temperatures, despite metamorphism and exposure to meteoric fluids, and show that the timing and temperature of quartz precipitation and thus δ18Ochert are determined by the kinetics of silica diagenesis. A diagenetic model shows that δ18Ochert is influenced by heat flow through the sediment column. Heat flow has decreased over time as planetary heat is dissipated, and reasonable Archean-modern heat flow changes account for ~5‰ of the increase in δ18Ochert, obviating the need for extreme TSW or δ18Osw reconstructions. The seawater oxygen isotope budget is also influenced by solid Earth cooling, with a recent reconstruction placing Archean δ18OSW 5 to 10‰ lower than today. Together, this provides an internally consistent view of the δ18Ochert record as driven by solid Earth cooling over billion-year timescales that is compatible with Precambrian glaciations and biological. KW - Climate KW - Oxygen isotope ratios KW - Silica diagenesis KW - Early Earth KW - Heat flow PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569359 DO - https://doi.org/10.1073/pnas.2213076119 SN - 0027-8424 VL - 119 IS - 51 SP - 1 EP - 7 PB - National Academy of Sciences CY - Washington, DC AN - OPUS4-56935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bilsel, M. A1 - Gökçen, T. A1 - Binici, B. A1 - Isleyen, A. A1 - Piechotta, Christian A1 - Kar-wai, A. A1 - Krylov, A. A1 - Miheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - chenko, Irina Tka A1 - Perkola, N. A1 - Lewin, M. A1 - Hua, T. T1 - High polarity analyte(s) in aqueous media: determination of L-PFOA and L-PFOS in ground water N2 - The CCQM-K156 comparison was coordinated by TUBITAK UME on behalf of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) for National Measurement Institutes (NMIs) and Designated Institutes (DIs) which provide measurement services in organic analysis under the 'Comité International des Poids et Mesures' Mutual Recognition Arrangement (CIPM MRA). Perfluoro alkyl substances (PFAS) such as PFOS and PFOA have been used in numerous industrial applications and products. Because of their high stability and resistance to biodegradation, atmospheric photooxidation, direct photolysis and hydrolysis, they are extremely persistent in the environment. The European Union (EU) Water Framework Directive lists PFOS as a priority hazardous substance that poses a significant risk to the aquatic environment. The use of PFOS-containing Aqueous Film-Forming Foams (AFFFs) has been banned since June 2011 in the EU. As relatively water-soluble, effectively non-degradable compounds, PFOS and PFOA migrate to ground water. They are not removed in the conventional drinking water treatment, and therefore cause health risks in polluted areas. The EU Drinking Water Directive and the European Commission has proposed a limit value of 100 ng/L for the sum of 20 PFAS, including PFOS and PFOA. This study provides the means for assessing measurement capabilities for determination of high polarity measurands in a procedure that requires extraction, clean-up, analytical separation and detection. Successful participation in CCQM-K156 demonstrates measurement capabilities in determining mass fraction of organic compounds, with a molecular mass of 200 g/mol to 700 g/mol, having high polarity pKow -2, in a mass fraction range from 0.5 ng/kg to 500 ng/kg in aqueous media. Nine NMIs and DIs participated in the CCQM-K156 key comparison. Seven institutes reported their results. SPE was applied in the sample pre-treatment and LC-MS was applied for detection. All participating laboratories applied isotope dilution mass spectrometry (IDMS) techniques for quantification. Participants established the metrological traceability of their results using certified reference materials (CRMs) from NMIs with stated traceability; where commercially available high purity materials were used the purity was determined in-house. The CCQM-K156 results for L-PFOA and L-PFOS range from 2.75 ng/kg to 5.50 ng/kg with a % RSD of 19.5 % for L-PFOA and from 2.04 ng/kg to 4.45 ng/kg with a % RSD of 21.3 % for L-PFOS. The KCRV was assigned using a Hierarchical Bayesian Random Effects Model (HB REM) estimator from the values reported by six of the participants. One participant result of L-PFOS and one result of L-PFOA were excluded from the KCRV for technical reasons. The KCRV was 4.9 ng/kg ± 0.4 ng/kg for L-PFOA and 3.8 ng/kg ± 0.4 ng/kg for L-PFOS. The six institutes that were included in the assignment of consensus KCRV all agreed within their standard uncertainties. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - PFAS KW - Surface water KW - ILC KW - CCQM PY - 2022 DO - https://doi.org/10.1088/0026-1394/59/1A/08016 VL - 59 IS - 1A SP - 1 EP - 3 PB - IOP Publishing AN - OPUS4-58941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Michail Ioannis, Chronakis A1 - Marcus, von der Au A1 - Meermann, Björn T1 - Single cell-asymmetrical flow field-flow fractionation/ICP-time of flight-mass spectrometry (sc-AF4/ICP-ToF-MS): an efficient alternative for the cleaning and multielemental analysis of individual cells N2 - Asymmetrical Flow Field-Flow Fractionation (AF4), as a cleaning technique, was combined on-line with the multielemental analytical capabilities of an Inductively Coupled Plasma-Time of Flight-Mass Spectrometer (ICP-ToF-MS). In that manner, the heavy ionic matrix effect of untreated cells' samples can be significantly reduced. As a proof of concept, commercial baker's yeast cells were analysed. KW - AF4 KW - Single Cell KW - Cleaning PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576419 DO - https://doi.org/10.1039/d2ja00264g SN - 0267-9477 VL - 37 IS - 12 SP - 2691 EP - 2700 PB - Royal Society of Chemistry AN - OPUS4-57641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Frenzel, Olivia A1 - Piechotta, C. T1 - Identification of Metabolites and Transformation Products of Bisphenols N2 - Bisphenol A (BPA) is used in Polycarbonate, Polyacrylic resins, Polysulfones, Epoxy resins, and Polyetherimides. It is also used in recycled Polyvinyl chloride [1–3]. BPA has been classified as a substance of very high concern (SVHC) under REACH [4] due to its endocrine disrupting properties. The German competent authorities want to reduce the content of BPA in the environment. Possible substitutes for BPA are Bisphenol B (BPB), Bisphenol E (BPE), Bisphenol F (BPF), or Bisphenol S (BPS), as they are similar in structure. BPA-based materials have a wide area of application especially outside. These outdoor applications are exposed to different external influences, including physical, biological, mechanical and chemical influences. This results in damage and aging of the material with leaching or migration into the environment. There, the substance is transformed by various transformation processes. The emerging metabolites and transformation products (TPs) can have different properties than the parent substance. Understanding the fate and behavior of the emerging pollutants is very important. Therefore, different transformation products of selected bisphenols will be generated and analyzed: To investigate the fate of different bisphenols in water treatment plants technical transformation products [5] will be generated by chlorination, ozonization, the Fenton reaction, and UV-radiation. For the investigation of the fate of Bisphenols in surface water global radiation will be simulated with UVA-lamps Simulation of phase-I-metabolism with an electrochemical cell coupled to mass spectrometry (EC-MS). T2 - Anakon 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Transformation products KW - Bisphenols KW - Metabolites KW - Wastewater KW - Environment PY - 2022 AN - OPUS4-57374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Bornemann-Pfeiffer, Martin A1 - Wander, Lukas T1 - Integrierte und vernetzte Systeme und Prozesse – Prozessnahe Sensorik für die digital transformierte Prozessindustrie N2 - Unternehmen der Prozessindustrie müssen neue Wege finden, um in einem sich wandelnden Umfeld erfolgreich zu überleben, und gleichzeitig flexiblere Wege der Produkt- und Prozessentwicklung finden, um ihre Produkte schneller auf den Markt zu bringen – insbesondere hochwertige, hochwertige Produkte wie Feinchemikalien oder Arzneimittel. Dies wird zukünftig durch Veränderungen in den Wertschöpfungsketten entlang einer potenziellen Kreislaufwirtschaft erschwert. Anhand von Beispielen wird in diesem Vortrag ein möglicher ganzheitlicher Ansatz zur Digitalisierung und zum Einsatz maschineller Verfahren in der Produktion von Spezialchemikalien durch die Einführung integrierter und vernetzter Systeme und Prozesse skizziert. Es wird auch auf die aktuelle Technologie-Roadmap „Prozess-Sensoren 2027+“ eingegangen, die Ende 2021 erschienen ist. Im Zentrum dieser Roadmaps stehen Sensoren zur Erfassung von physikalischen und chemischen Messgrößen mittels spezifischer und unspezifischer Messverfahren, die zur Steuerung und dem besseren Verständnis von Prozessen dienen. Die Roadmap fasst die gemeinsame Technologie- und Marktsicht von Anwendern, Herstellern und Forschungs¬einrichtungen im Bereich Prozess-Sensorik in der verfahrenstechnischen Industrie zusammen. Digitalisierung und Nachhaltigkeit sind übergreifende Kernthemen der künftigen Entwicklung. T2 - 11. Fachtagung Prozessnahe Röntgenanalytik PRORA CY - Berlin, Germany DA - 24.11.2022 KW - Digital Transformatioin KW - Prozessindustrie KW - Sensorik KW - Prozessanalytik KW - Industrie 4.0 KW - PRORA PY - 2022 AN - OPUS4-56391 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Axel A1 - Altmann, Korinna A1 - Kocher, B. A1 - Braun, U. T1 - Determination of tire wear markers in soil samples and their distribution in a roadside soil N2 - Tire wear (TW) constitutes a significant source of microplastic in terrestrial ecosystems. It is known that particles emitted by roads can have an effect up to 100 m into adjacent areas. Here, we apply for the first-time thermal extraction desorption gas chromatography-mass spectrometry (TED-GC/MS) to determine TW in soil samples by detection of thermal decomposition products of styrene-butadiene rubber (SBR), without additional enrichment. Additionally, zinc contents were determined as an elemental marker for TW. Mixed soil samples were taken along three transects along a German motorway in 0.3, 2.0, and 5.0 m distance from the road. Sampling depths were 0–2, 2–5, 5–10, and 10–20 cm. Four fine fractions, 1 000–500, 500–100, 100–50, and <50 μm, were analyzed. TW contents based on SBR ranged from 155 to 15 898 mg kg−1. TW contents based on zinc were between 413 and 44 812 mg kg−1. Comparison of individual values of SBR and zinc reveals SBR as a more specific marker. Results confirm that most TW ends up in the topsoil within a 2 m distance. The sampling strategy resulted in representative data for a larger area. Standard deviations of quadruple TED-GC/MS determination of SBR were <10% for all grain size fractions. TED-GC/MS is a suitable analytical tool for determining TW in soil samples without the use of toxic chemicals, enrichment, or special sample preparation. KW - Microplastic KW - TED-GC/MS KW - Tire wear PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543344 DO - https://doi.org/10.1016/j.chemosphere.2022.133653 VL - 294 SP - 1 EP - 8 PB - Elsevier Ltd. AN - OPUS4-54334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Altmann, Korinna A1 - Abusafia, A A1 - Bannick, C-G A1 - Braun, U A1 - Crasselt, Claudia A1 - Dittmar, S A1 - Fuchs, M A1 - Gehde, M A1 - Hagendorf, C A1 - Heller, C A1 - Herper, D A1 - Heymann, S A1 - Kerndorff, A A1 - Knefel, M A1 - Jekel, M A1 - Lelonek, M A1 - Lunkenbein, T A1 - Obermaier, N A1 - Manhart, M A1 - Meurer, Maren A1 - Miclea, P-T A1 - Paul, A A1 - Richter, S A1 - Ricking, M A1 - Rohner, C A1 - Ruhl, A A1 - Sakai, Y A1 - Saravia Arzabe, C A1 - Scheid, C A1 - Schmitt, M A1 - Schnarr, M A1 - Schwertfirm, F A1 - Steinmetz, H A1 - Wander, Lukas A1 - Wiesner, Yosri A1 - Zechmeister, L T1 - RUSEKU - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt : Abschlussbericht N2 - Im Verbundprojekt RUSEKU wurde die Probenahme von Wasserproben entscheidend weiterentwickelt. Wichtig ist hierbei zu gewährleisten, dass genügend Merkmalsträger in jeder Probe untersucht werden. Es muss daher eine für den Probenahmeort repräsentative Beprobung hinsichtlich des Wasservolumens in Abhängigkeit der Partikelanzahl gewährleistet sein. Das Hauptaugenmerk lag im vorliegenden Projekt auf einer praxisnahen Beprobungsstrategie. Es wurden verschiedene Konzepte ausprobiert. • Grundsätzlich hat sich gezeigt, dass eine Stichprobe eine Momentaufnahme des MP-Massengehaltes zeigt. Es wird eine hohe Statistik, also eine Vielzahl an Messungen am gleichen Probenahmeort, benötigt, um eine valide Aussage über den MP-Gehalt zu machen. • Es zeigt sich, dass eine integrale Probenahme über mehrere Wochen mit dem SK routinemäßig möglich ist. Die erfassten MP-Massen sind reproduzierbar und robust. • Die DFZ ist für Stichproben geeignet. Partikel < 50 µm werden eventuell unterschätzt • Die fraktionierte Filtration kann für Stich- und Mischproben direkt im Feld genutzt werden. Fraktionen von 10 und 5 µm werden später im Labor Vakuum filtriert. Es erfolgt eine Fraktionierung der Probe mit Siebmaschenweiten von 1000, 500, 100, 50, 10 und 5 µm. • Die fraktionierte Filtration kann auch anschließend an die Beprobung mit dem SK zur Anwendung kommen. Wird die mit dem SK gewonnene Wasserprobe fraktioniert filtriert, kann neben einem MP-Gesamtgehalt auch eine Einschätzung über die Partikelgrößen gewonnen werden. • Für Wässer mit geringen Partikelzahlen wurde ein Messfiltertiegel entwickelt. Dieser hat eine Maschenweite von 6 µm. Seine Anwendung kann mögliche Verluste beim Transferieren vom Probenahmetool zum Messgefäß und mögliche Kontaminationen reduzieren. Die Optimierung der Probenahmestrategie wurde durch Modellversuche und Simulationen unterstützt. Modellversuche zum Sinkverhalten und Simulationen von MP in realen Gewässern verdeutlichten das komplexe Verhalten der Partikel. Es konnte gezeigt werden, dass Partikel ab einer bestimmten Größe (und kleiner) bei genügend starker Turbulenz sich in der Wassersäule unabhängig von ihrer Dichte verhalten und so auch MP mit kleiner Dichte (z.B. PE) in der gesamten Wassersäule zu finden sind. Es konnte mit dem TEM die Existenz von NP gezeigt werden. Ein wesentlicher Aspekt des RUSEKU Projektes war die Beprobung realer Kompartimente. Beprobt wurde neben Oberflächengewässern, das urbane Abwassersystem der Stadt Kaiserslautern, Waschmaschinenabwasser und Flaschenwasser. • In Oberflächengewässern wurde hauptsächlich PE gefunden. Je nach Probe und Gewässer konnten auch PP, PS, PET, PA, SBR und Acrylate nachgewiesen werden. • Im urbanen Abwassersystem der Stadt Kaiserslautern konnte an allen Probenahmestandorten MP nachgewiesen werden. Es wurde hauptsächlich PE, neben geringeren Mengen an PP, PS und SBR gefunden. Nach einem Regenereignis war der SBR Anteil deutlich erhöht. • Die Beprobung eines realen Wäschepostens, bestehend aus T-Shirts und Hemden mit PA/CO oder PES/CO Mischgewebe, zeigte einen PA- und PES-Austrag im Waschwasser. Der überwiegende Teil der detektierten Fasern ist aber auf Baumwolle zurückzuführen. Reine gravimetrische Messungen zur Detektion von MP führen zu einer starken Überschätzung. • In Flaschenwasser (PET-Flaschen) konnte MP detektiert werden. PET wurde nur im stillen Mineralwasser, nicht in Mineralwasser mit Kohlensäure gefunden werden. Teilweise wurde auch das MP-Material des Verschlusses im Wasser detektiert. • Für Luftproben konnte ein Aufbau zur größenselektiven Beprobung getestet werden. Neben der Probenahme hat das Projekt auch gezeigt, dass die TED-GC/MS geeignet für die MP-Detektion im Routinebetrieb ist. Die TED-GC/MS konnte weiter optimiert werden. Es wurden MP-Massen bestimmt. Im Projekt wurden erste realitätsnahe Referenzmaterialien für die MP Detektion hergestellt. Die Herstellung von realitätsnahen Polymeren in ausreichender Homogenität und Menge hat sich als große Herausforderung herausgestellt. KW - Mikroplastik KW - Probennahme KW - TED-GC/MS KW - Fraktionierte Filtration KW - Mikroplastikreferenzmaterial PY - 2022 SP - 1 EP - 201 AN - OPUS4-57800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul A1 - Jekel, M. A1 - Altmann, Korinna T1 - Qualitätssicherung bei der Analyse von Mikroplastik per TED GC/MS N2 - Die Thermo Extraktion Desorption Gas Chromatograpie Massen Spektrometrie (TED-GC/MS) ist ein schnelles thermoanalytisches Verfahren zur Bestimmung von Gehalten an Mikroplastik (MP). Die Kombination aus teils schwerflüchtigen Analyten und Kältebrücken führt zu Memory-Effekten, denen u.a. durch häufige Blindwertmessungen begegnet werden muss. Reduzierte Probedurchsätze sind die Folge. Um Messergebnisse abzusichern und den Gerätestatus bei gleichzeitig hoher Messleistung überwachen zu können, wurde die sequentielle Standardmethode überarbeitet. T2 - Tagung der Wasserchemischen Gesellschaft 2022 CY - Online meeting DA - 23.05.2022 KW - Mikroplastik KW - Thermoanalytik KW - TED-GC/MS KW - Qualitätssicherung PY - 2022 AN - OPUS4-55087 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bauer, J. A1 - Miclea, P.-T. A1 - Braun, U. A1 - Altmann, Korinna A1 - Turek, M. A1 - Hagendorf, C. T1 - Microplastic detection and analysis in water samples N2 - Microplastic detection in water samples becomes important for tracing microplastic sources. Microplastic may harm desalination facilities by blocking filters and disturbing the marine food chain. Thermo analytical methods such as pyrolysis gas chromatography mass spectroscopy, and spectroscopic methods like (micro) Raman spectroscopy or (micro) Fouriertransform infrared spectroscopy in combination with appropriate filters and sample preparation are suitable for analyzing microplastics on a scale from 1 µm to 1000 µm fast and unambiguous. While the thermo analytical methods are suitable for larger sample volumes, Raman spectroscopy and Fouriertransform infrared spectroscopy are able to detect and analyze single microplastic particles for instance in bottled water. Machine learning algorithms ensure a reliable classification of different plastic materials. T2 - International Conference on Sustainable Energy-Water-Environment Nexus in Desert Climate 2019 CY - Ar-Rayyan, Qatar DA - 02.12.2019 KW - Microplastics KW - Water samples PY - 2022 SP - 111 EP - 113 PB - Springer AN - OPUS4-56240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna A1 - Müller, A. A1 - Kittner, Maria A1 - Braun, U. T1 - Plastik in Böden: Mikroplastik-Ergebnisse N2 - In diesem Vortrag geht um die Vorstellung der Ergebnisse des UBA Projektes Plastik in Böden. Es werden Mikroplastik-Gehalte in verschiedenen Böden präsentiert. T2 - Fachgespräch "Plastik in Böden" CY - Online meeting DA - 28.03.2022 KW - Mikroplastik KW - Mikroplastik Böden KW - Mikroplastik-Analytik PY - 2022 AN - OPUS4-54648 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -